gemini v - Micromeritics...The Gemini Windows® program is designed to enhance the operation of the Gemini V ana-lyzer, allowing you to prepare sample files, perform analyses, and

Gemini V

Operator’s Manual

V2.00

238-42801-01February 2006

Windows is a registered trademark of Microsoft Corporation.Adobe Acrobat is a registered trademark of Adobe Systems Incorporated.

© Micromeritics Instrument Corporation 2005, 2006. All rights reserved.

The software described in this manual is furnished under a license agreement and may be used or copied only in accordance with the terms of the agreement.

WARRANTY

MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment eachinstrument it manufactures to be free from defects in material and workmanship impairing its usefulness undernormal use and service conditions except as noted herein.

Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of anyinstrument or defective parts when returned prepaid to us and which our examination discloses to have beendefective. The purchaser is responsible for all transportation charges involving the shipment of materials for war-ranty repairs. Failure of any instrument or product due to operator error, improper installation, unauthorizedrepair or alteration, failure of utilities, or environmental contamination will not constitute a warranty claim. Thematerials of construction used in MICROMERITICS instruments and other products were chosen after extensivetesting and experience for their reliability and durability. However, these materials cannot be totally guaranteedagainst wear and/or decomposition by chemical action (corrosion) as a result of normal use.

Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date ofshipment.

No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect andauthorization to return the instrument or product. All repairs or replacements are made subject to factory inspec-tion of returned parts.

MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modificationsare made by persons other than its own authorized service personnel unless such work is authorized in writing byMICROMERITICS.

The obligations of this warranty will be limited under the following conditions:

1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under theirrespective brand names or trade names. We, therefore, make no express or implied warranty as to such prod-ucts. We shall use our best efforts to obtain from the manufacturer, in accordance with his customary prac-tice, the repair or replacement of such of his products that may prove defective in workmanship or materials.Service charges made by such manufacturer are the responsibility of the ultimate purchaser. This states ourentire liability in respect to such products, except as an authorized person of MICROMERITICS may other-wise agree to in writing.

2. If an instrument or product is found defective during the warranty period, replacement parts may, at the dis-cretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, checkvalves, seals, etc.

3. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) andstems, seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects.Such items which perform satisfactorily during the first 45 days after the date of shipment are assumed to befree of manufacturing defects.

Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought againstMICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manu-factures a special product to the purchaser’s specifications.

MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any ofits products other than the liability stated above. This warranty is in lieu of all other warranties, express orimplied, including, but not limited to, the implied warranties of merchantability or fitness for use.

One Micromeritics Drive Norcross, GA 30093-1877 Fax (770) 662-3696

Domestic Sales - (770) 662-3633 Domestic Repair Service - (770) 662-3666International Sales - (770) 662-3660 Customer Service - (770) 662-3636

Gemini V Windows Table of Contents

TABLE OF CONTENTS

1. GENERAL INFORMATIONOrganization of the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1

Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-3Internet Access . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4Online Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-5

Using Bookmarks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-5Using the Table of Contents, Index, and other Links. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-7

Table of Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-7Index. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-8Cross References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-8

Using the Find Command . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-9Printing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-10

Equipment Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-11 System Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-15

Location . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-15Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-15Cryogen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-15Degasser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-16Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-16

Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-17

2. INSTALLATIONUnpacking and Inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

Equipment Damage or Loss During Shipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1Equipment Return . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

Setting up the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-2Installing the Degasser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-6Installing the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7

Configuring the Gemini . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7Initial Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7

Verifying Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-10Using the Setup Program for Other Functions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-13

Installing Subsequent Software Versions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-15Adding an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-16Moving an Analyzer from one PC to another PC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-17Removing an Analyzer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-20Changing an Analyzer Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-21Uninstalling the Analysis Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-22

3. USER INTERFACETurning On the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1Using the Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-1

Feb 06 i

Table of Contents Gemini V Windows

Report System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1Online Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2Shortcut Keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2Dialog Boxes and Subdialog Boxes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4Selecting Files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6File Name Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9

Menu Structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11Help Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11

4. OPERATIONAL PROCEDURESSpecifying Sample File Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1

Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3

Creating Sample Information Files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5Basic and Restricted Formats . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7

Creating Parameter Files. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-11Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-12

Performing an Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14Verifying Regulator Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14Verifying Vacuum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14Checking the Cryogen Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14

Dewar Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-14Preparing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-15Cleaning and Labeling Sample and Balance Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16Weighing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-18Installing the Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-20Starting the Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-21

Printing File Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-23Listing File Statistics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-24Exporting Isotherm Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-25Generating Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-26

Multiple Samples Overlay . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-27Multiple Graphs Overlay . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-30

5. FILE MENUDescription . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3

Sample Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7Restricted Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9

ii Feb 06


Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-10Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-12Adsorptive Properties. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-18Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-19

Summary Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-22Isotherm Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-23BET/Langmuir Surface Area Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-25t-Plot Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-28BJH Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-34

Tabular Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-38Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-40

Dubinin Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-42Tabular Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-44Transformed Isotherm Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-45Pore Volume Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-46

MP-Method Report Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-47Tabular Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-49Plot Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-50

Options Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-52Sample Log Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-52Collected/Entered Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-53

Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-56Save As. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-56Save All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-57Close. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-57Close All. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-57Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-58List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-59Export. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-61Convert. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-63Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-64

6. UNIT MENUDescription . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-1Start Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-2Start Po Measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-5Show Instrument Schematic. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-6Show Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-8Show Instrument Log. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-9Unit Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6-11

7. REPORTS MENUDescription . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-1Start Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-3Close Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-5Open Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-5SPC Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7-6

Feb 06 iii

Table of Contents Gemini V Windows

Regression Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7Control Chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-11Printed Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14

Header . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14Onscreen Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14

Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-15Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-18

Tabular Reports. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-18Graphs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19

Zoom Feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-21Axis Cross Hair. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-21

Report Examples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22Isotherm Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22BET Surface Area Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23t-Plot Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-24BJH Adsorption Pore Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25BJH Adsorption Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-26Options Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-27Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-28Sample Log Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-29

8. OPTIONS MENUDescription . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1Option Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2

Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3Restricted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3

Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4Graph Grid Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-5Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6

Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8

Parameter Files Directory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-12Service Test Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-12

9. TROUBLESHOOTING AND MAINTENANCETroubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3

Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3Recovering from a Power Failure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3Replacing Analysis Port Frit and O-Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4Performing a Blank Analysis for Diagnostic Purposes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5

10. ORDERING INFORMATION

iv Feb 06


A. ERROR MESSAGES2400 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-12500 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-84000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-106000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-13

B. CALCULATIONSFree-Space Correction Algorithms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1

Determining the Free-Space Correction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1Measured . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1Calculated. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1

Applying the Free-Space Correction to Quantities Adsorbed . . . . . . . . . . . . . . . . . . . . . . . . .B-2Surface Area Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-3

BET . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-3Langmuir Surface Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-4

t-Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-6BJH Pore Volume and Area Distribution. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-8

Explanation of Terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-8Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-9Compendium of Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-17

Dubinin-Radushkevich. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-18Dubinin-Astakhov . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-20MP-Method Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-24

C. ANALYZING SAMPLES WITH TOTAL SURFACE AREA OF 1.0 m2 OR LESSStraight-Wall Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-1Bulb Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-3Hanging Filler Rods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-4

INDEX

Feb 06 v

Gemini V Windows Organization of the Manual

1. GENERAL INFORMATION

The Gemini Windows® program is designed to enhance the operation of the Gemini V ana-lyzer, allowing you to prepare sample files, perform analyses, and generate reports in a Windows environment.

If you are upgrading a keypad version of the Gemini analyzer to the Windows environment, you may disconnect your keypad and store it in a safe location. The keypad is not required for Windows operation. If you ordered the Windows program with your Gemini analyzer, a key-pad is not included.

The Gemini Windows option consists of the following items:

• Operator’s manual• One communications cable*• CD-based software

*A communication cable is required for each Gemini you attach to the computer; you can attach up to four Geminis to one computer.

Organization of the Manual

This manual describes how to install, operate, and maintain the Gemini analyzer. The manual is organized as follows:

Before disconnecting your keypad, refer to Configuring the Gemini, page 2-7 and ensure that data transmission parameters are configured properly.

Chapter 1 General InformationProvides general information about the Gemini Windows program.

Chapter 2 INSTALLATIONProvides instructions for installing the hardware and software.

Chapter 3 USER INTERFACEProvides basic software interface.

Chapter 4 OPERATIONAL PROCEDURESProvides steps-by-step instructions on the operations for the Gemini Windows software.

Feb 06 1-1

Organization of the Manual Gemini V Windows

Chapter 5 FILE MENUProvides a description of the commands on the File menu.

Chapter 6 UNIT MENUProvides a description of the commands on the Unit menu.

Chapter 7 REPORTS MENUProvides a description of the commands on the Reports menu.

Chapter 8 OPTIONS MENUProvides a description of the commands on the Options menu.

Chapter 9 TROUBLESHOOTING AND MAINTENANCEProvides troubleshooting and maintenance information.

Chapter 10 ORDERING INFORMATIONProvides ordering information.

Appendix A ERROR MESSAGESLists the error messages that may be displayed by the software; includes a cause and action for each.

Appendix B CALCULATIONSContains the calculations used by the software to produce reports.

Appendix C ANALYZING SAMPLES WITH TOTAL SURFACE AREA OF 1.0 m2 OR LESSProvides information on analyzing samples with a total surface area of 1.0 m2 or less.

Index INDEXProvides quick access to a subject matter

1-2 Feb 06

Gemini V Windows Organization of the Manual

Conventions

This manual uses the symbols shown below to identify notes of importance, warnings, and cautions:

Notes contain important information pertinent to the subject matter.

Warnings contain information that help you prevent actions that may cause personal injury.

Cautions contain information that help you prevent actions that may damage the analyzer.

Feb 06 1-3

Internet Access Gemini V Windows

Internet Access

Visit www.micromeritics.com to learn more about Micromeritics, its products, and applica-tions. Our site is user-friendly, easy to navigate, and informative. Its content is summarized below.

Be sure to browse our site to see the many ways in which we can assist you.

About Micromeritics A brief history of Micromeritics, office locations, awards/certifications, and career opportunities with Micromeritics

Products Product information and printable brochures

Applications Application Notes, Product Bulletins, Tech Tips, Technical Articles/papers, and important application links

Online Catalog Catalog of instruments and accessories, allowing you to place your order online

News and Press Press releases, Events calendar, microReports, and latest Micromeritics news updates

Lab Service Provides laboratory tips and access to the Micromeritics Analytical Services web site

Customer Support Customer support contacts, product registration, instrument training information, Material Safety Data Sheets, and account registration

Contact Us Contact information, office locations, maps and driving directions to the Micromeritics facility, and registration for the microReport newsletter

1-4 Feb 06

Gemini V Windows Online Manual

Online Manual

For your convenience, the Operator’s Manual is available online. You can access the manual by selecting Help, then Operator’s Manual from the analysis program main menu. The manual appears in an Adobe® Acrobat® reader.

Following are some tips to help you quickly locate the information you need in the manual. Refer to the Adobe Acrobat Help system (click the Help button on the Acrobat menu) for more information on the Acrobat features you can use while viewing the manual.

Using Bookmarks

Click the Bookmarks tab to list and access the topics included in the manual.

You can use the + and − buttons next to topics as they are used in Windows Explorer to expand or collapse the topic list.

Navigation Pane Topic Pane

Bookmarks

Topics

Feb 06 1-5

Online Manual Gemini V Windows

To display a topic, click the topic name in the Bookmarks section. The related information appears in the topic pane of the window as shown in the following example.

Click bookmarkto display topic.

1-6 Feb 06


Using the Table of Contents, Index, and other Links

Links provide direct access to selected information. All links appear in blue type. Links are contained in:

• the table of contents• index entries• cross-references within the manual

Table of Contents

To display the table of contents, click Table of Contents in the Bookmarks section. When the table of contents is displayed, you can click an entry to display its associated page. For example, clicking Using the Software in the table of contents, displays the page containing information about the software.

Click topic name in table of contents to display topic.

Feb 06 1-7


Index

To use the index in the online manual, click the Bookmarks tab, scroll down to INDEX (the last topic in Bookmarks), then click the + button to expand the index. The letters A through Z are displayed. Click a letter to display its corresponding index entries as shown in the following example.

Cross References

Cross-references work in the same manner. In the example below, clicking on the cross-reference, FILE MENU (shown on the screen in blue type) will display the first page of the chapter describing the commands found on the File menu.

FILE MENU

Provides a description of the commands available on the File menu.

Click a letter to display its index entries.

1-8 Feb 06


Using the Find Command

The Adobe Acrobat Find command provides another method of easily accessing specific information. For example, suppose you want to know how the Save as command works. You could select Edit > Find from the Adobe Acrobat menu, then enter Save as in the Find dialog. The following example shows the results.

Feb 06 1-9


Printing

You can print the entire manual, a selected page, or range of pages. There are several options for printing. You can:

• Select the printer icon ( ) on the Adobe Acrobat toolbar.

A standard Print dialog is displayed. Select the page(s) to print, then click OK. When using this option (or the next one), be sure to enter the page number(s) displayed in Adobe Acrobat; do not use the page number(s) listed in the footer(s) of the manual.

• Select File > Print.

A standard Print dialog is displayed. Select the page(s) to print, then click OK.

• Click the Thumbnails tab.

Thumbnails of manual pages are displayed.

a. Click the pages you want to print.

b. Right-click to display a shortcut menu, then select Print Pages.

c. A standard Print dialog is displayed; click OK.

Enter this number.

Do not use number in footer of the manual.

Thumbnails tab

1-10 Feb 06

Gemini V Windows Equipment Description

Equipment Description

The Gemini Analyzer is an easy-to-use, fully automatic, single- or multipoint surface area and pore size analyzer. After an analysis is started, data are collected, calculations performed, and results displayed without further operator intervention. The frequent calibrations associated with currently available flowing-gas systems are not required.

Gemini provides rapid and accurate sample analysis, including selectable calculation of the following sample characteristics:

• Single-point BET surface area• Multipoint BET surface area• Multipoint Langmuir surface area• t-Method micropore volume and area• BJH Method (Gemini 2380 only)• Dubinin (Gemini 2380 only)• MP-Method (Gemini 2380 only)• Total pore volume• Statistical Process Control (SPC) reports

As many as 50 data points can be collected and reported in the BET, Langmuir, or t-Method range. Additionally, Gemini can report discrete point adsorption isotherms consisting of up to 1,000 adsorption points. If you have the Gemini V 2380, you can also report on the desorption isotherm.

Analysis results can also be edited by specifying which points are to be included in surface area or t-Method calculations. The Gemini software automatically recalculates the results and generates a new report.

The Gemini analyzer is controlled by commands entered through the software. The opera-tional status of the analyzer can be continually monitored on the instrument schematic (accessed from the Unit menu).

The primary function of the Gemini is to determine the surface area of solid materials. It uses a static volumetric technique in which the analysis gas flows into a tube containing the sample and into a balance tube, at the same time. The internal volume and the temperature surround-ing both tubes are maintained at identical conditions. The only difference is the presence of the sample in the sample tube.

Feb 06 1-11

Equipment Description Gemini V Windows

Figure 1-1. Gemini V Analyzer

The sample and balance tubes are immersed in a single liquid nitrogen bath which maintains isothermal conditions for both tubes. The analysis gas is then delivered to the sample tube by a servo valve mechanism. The delivery rate of analysis gas flow into the balance tube is con-trolled by another servo valve connected to a differential pressure transducer. This differential pressure transducer measures the pressure imbalance between the sample and balance tubes, which is caused by the adsorption of the analysis gas onto the sample. As the sample adsorbs analysis gas, the pressure drops in the sample tube. The servo valve continuously restores the pressure balance between two tubes by admitting more gas into the sample tube. The end result is that the Gemini maintains a constant pressure of analysis gas over the sample while varying the rate of analysis gas delivery to match exactly the rate at which the sample can adsorb the gas.

1-12 Feb 06

Gemini V Windows Equipment Description

The following schematic shows the components of Gemini’s plumbing system. As shown in the diagram, gas enters the system and is admitted into two reservoirs: the sample reservoir and the balance reservoir. From there it flows into the sample and balance tubes. The flow of gas through the system is controlled by three transducers and a series of valves.

Figure 1-2. Plumbing Diagram

Vacuum Valve

Adsorptive Valve

Helium Valve

Volume Adsorbed Transducer

Sample Reservoir Valve

Sample Reservoir

Sample Servo Valve

Balance Transducer

Sample Port Valve

Sample Transducer

Sample Tube

Dewar

Balance Reservoir Valve

Balance Reservoir

Balance Servo Valve

Balance Port Valve

Balance Adjustment Screw

Balance Tube

Select Unit > Instrument Schematic to view a graphical representation of the schematic on your computer screen.

Feb 06 1-13

Equipment Description Gemini V Windows

Gemini requires only pure nitrogen as the analysis gas, even for most low surface area sam-ples. The analyzer requires no flow regulator, gas mixer, or mixed gases to operate. Surface areas as low as 0.01 m2/g are easily determined with excellent precision using nitrogen gas as the adsorbate. Optionally, helium may be used to determine any slight differences in volume between the balance tube and the sample tube (differential free space). The Gemini uses this information to automatically compensate even for these small differences in calculating analy-sis results.

The design of Gemini avoids many errors which may occur with other surface area analysis equipment:

• Any free space associated with the sample tube is offset by an identical amount in the balance tube.

• Any thermal gradient in the coolant bath is the same for both the sample and balance tubes and produces a net effect of zero.

• Non-ideal gas behavior occurs in both the sample and balance tubes, cancelling negative effects on sample analysis.

• Gas-mixture separation, which may occur in flowing-gas systems due to thermal diffusion, cannot occur because mixed gases are not used.

1-14 Feb 06

Gemini V Windows System Requirements

System Requirements

Location

When selecting a location for the Gemini analyzer, keep the following in mind:

• The analyzer performs best in a relatively constant temperature environment.

• It should be installed on a workbench about 0.92 m (36 in.) high in a location free of drafts from sources such as a forced-air heating or cooling system.

• The slots in the rear panel, which provide ventilation, should not be blocked.

• The analyzer should not be placed near an outside window; exposure to direct sunlight may cause the temperature to vary.

Gases

Compressed gases are required for sample analysis with the Gemini analyzer. Gas bottles and a rack for storage of these bottles should be located near the analyzer. As an alternative, outlets from a central source may be provided nearby. Gas sources must be able to supply flow rates of 4 liters per minute at 15 psig (103.5 kPa).

Appropriate two-stage regulators which have been leak-checked and specially cleaned are required. Pressure relief valves should be set to no more than 30 psig. Gas regulators are avail-able from Micromeritics (refer to Chapter 10, page 10-1 for ordering information).

When helium is used for differential free-space measurement and nitrogen is used as the adsor-bate gas, they should be of the following purity or better:

Cryogen

Liquid nitrogen is used as the cryogen to cool the sample during analysis. An easy-to-use liq-uid nitrogen transfer system, the Model 021, which eliminates the need to pressurize storage Dewars is available from Micromeritics (refer to Chapter 10, page 10-1 for ordering information).

Helium purity of 99.9% (For analysis of materials with very low surface areas, Micromeritics recommends use of helium with purity of 99.995%.)

Nitrogen purity of 99.9%

Feb 06 1-15

System Requirements Gemini V Windows

Degasser

Samples must be free of moisture and other contaminants before analysis. Easy-to-operate, low-cost degassers — the SmartPrep 065, the FlowPrep 060, and the VacPrep 061 — are available from Micromeritics (refer to Chapter 10, page 10-1 for ordering information). If using the SmartPrep, a menu is added to the Gemini menu bar, allowing control of the Smart-Prep through the Gemini software.

Vacuum Pump

An external vacuum pump equipped with an anti-suckback valve is required for sample analy-sis with the Gemini analyzer. Any vacuum source achieving vacuums better than 20 x 10-3 mmHg at the instrument inlet may be used. An appropriate vacuum pump is available from Micromeritics (refer to Chapter 10, page 10-1 for ordering information).

A device to reduce oil vapor backstreaming is recommended.

The vacuum pump used with the Gemini must have an anti-suckback valve to prevent oil from being admitted to the instrument should the power fail while the system is under vacuum. Pumps available from Micromeritics are equipped with an anti-suckback valve.

1-16 Feb 06

Gemini V Windows Specifications

Specifications

The Gemini analyzer has been designed and tested to meet the specifications provided below.

Characteristic Specification

Applicability

Surface Area: 0.1 m2 to above 300 m2, total; 0.01 m2/g and higher, specific

Pore Volume: 4 x 10-6 cm3/g

Pressure Measurement

Pressure Measurement Range: 0 to 950 mmHg

P/Po Resolution: <10-4

Relative Pressure Range: 0 to 0.98 P/Po (adsorption only)

Pressure Resolution: <0.1 mmHg

Accuracy and Linearity: Better than ± 0.5%(Transducer manufacturer’s specification)

Vacuum System

External: Vacuum source achieving 20 x 10-3 mmHg (or better) at the instrument inlet, and having a device to reduce oil vapor backstreaming is recommended.

The system must have an anti-suckback valve to prevent oil from being admitted into the Gemini should there be a power failure.

Environment

Temperature: 10 to 35 ºC (50 to 96 ºF) operating0 to 50 ºC (32 to 122 ºF) non-operating

Humidity: 20% to 80% relative, non-condensing

Feb 06 1-17

Specifications Gemini V Windows


Sample Tubes / Dewar

Standard Tube: The standard tube has a 0.95-cm (3/8-in.) outside diameter and is 15.5 cm (6.1 in.) long with 6.5 cm3 of volume. Sample capacity is approximately 2.0 cm3.

Large Tube: The bulb of the large tube has a 1.9-cm (3/4-in.) outside diameter and is 3.8 cm (1-1/2 in.) long. The tube is 15.5 cm (6.1 in.) long. It yields a 12.0-cm3 volume. Sample capacity is approximately 6.0 cm3.

Dewar: 8 hours (approximately)

Electrical

Voltage: 90 to 265 VAC

Frequency: 50/60 Hz

Power: 150 VA maximum

Gases

Adsorbate: Optimized for nitrogen in a liquid nitrogen sample bath. Gemini may be used with non-corrosive adsor-bate gases having vapor pressures at both room and bath temperatures that are acceptably high relative to the resolution of the 1,000 mmHg pressure trans-ducer.Typically, oxygen, argon, carbon dioxide, butane, methane, and other light hydrocarbons will produce useful data above absolute pressures of a few mmHg.

Physical

Height: 52.4 cm (20.6 in.)

Width: 43.8 cm (17.3 in.)

Depth: 30.5 cm (12.0 in.)

Weight: 22 kg (48.4 lbs)

1-18 Feb 06

Gemini V Windows Specifications


Minimum requirements: Pentium 333 MHz computer (or equivalent)CD-ROM drive128 megabytes of main memory1-gigabyte hard driveRS-232 portSVGA monitor; 800 x 600 minimum resolution required (1024 x 768 recommended)Windows 2000 or Windows XP Professional*

*This requirement also applies to any third-party software that is used in conjunction with the Gemini program.

Feb 06 1-19

Gemini V Windows Unpacking and Inspection

2. INSTALLATION

This chapter describes how to:

• unpack and inspect the equipment• setup and install the analyzer, page 2-2• install the software, page 2-7 • verify operation, page 2-10• use the Setup program for other functions, page 2-13

Unpacking and Inspection

When you receive the shipping cartons, carefully compare the Packing List with the equip-ment actually received and check the equipment for any damage during shipment. Be sure to sift through all packing material before declaring equipment missing.

Equipment Damage or Loss During Shipment

If equipment is damaged or lost in transit, you are required to make note of the damage or loss on the freight bill. The freight carrier, not Micromeritics, is responsible for all damage or loss occurring during shipment. If you discover damage or loss of equipment during shipment, report the condition to the carrier immediately.

Equipment Return

Micromeritics strives to ensure that all items arrive safely and in working order. Occasionally, due to circumstances beyond our control, a customer may receive equipment which is not in working order. When equipment has been damaged (either during shipment or in use) and you wish to return the equipment to Micromeritics for repair or replacement, please follow the steps below:

1. Pack the instrument in its original shipping carton if possible. If the original carton is unavailable, for a nominal fee, Micromeritics can provide another carton for your use.

2. Tag or otherwise identify the defective equipment, noting the defect and, if possible, the circumstances under which the defect occurs.

If you need to declare equipment as damaged or lost, save the shipping cartons. The claims investigator must examine the cartons in order to complete the inspection report.

Failure to package your instrument properly may result in shipping damage.

Feb 06 2-1

Setting up the Analyzer Gemini V Windows

3. Make reference to the sales order or purchase order for the equipment, and provide the date the equipment was received.

4. Notify a Micromeritics Service representative of the defect and request shipping instructions. The Service Department will assign a Return Material Authorization (RMA) number to your return and provide shipping information.

Setting up the Analyzer

The analyzer should be checked to make sure it is operating properly before actual analyses are attempted. The remainder of this chapter describes how to install the analyzer and verify operation.

1. Insert one end of the power cord into the input power connector at the rear of the analyzer (refer to Figure 2-2. Rear Panel Connections, page 2-4 for rear panel connectors) and the other end into the appropriate power source.

2. Attach an appropriate regulator to the nitrogen gas bottle. Leave the gas bottle shut-off valve closed until instructed otherwise. (Suitable regulators are available from Micromeritics. See Chapter 10, page 10-1 for ordering information.)

3. If the regulator has a 1/8-in. outlet, proceed to Step 4. If the regulator has a 1/4-in. outlet, attach the reducer fitting to the outlet of the regulator shut-off valve and tighten the regulator shut-off valve nut.

Do not overtighten the fittings. Doing so can collapse the brass fitting and cause a leak.

When using nitrogen, or other safe gases, it is recommended that a pressure relief valve be included in the regulator assembly. Do not set this valve above 30 psig. The pressure relief valve should not be installed if hazardous gases are used. A pressure relief valve is available from Micromeritics; refer to Ordering Information, page 10-1.

2-2 Feb 06

Gemini V Windows Setting up the Analyzer

Figure 2-1. Connecting Gas Bottle to the Regulator

4. Attach the copper tubing to the regulator shut-off valve or to the brass reducer fitting.

5. Attach the other end of the copper tubing to the fitting on the back of the analyzer.

6. If you are using helium for differential free-space measurement, repeat steps 2 through 5 for the helium gas bottle.

Bottle Shut-Off Valve

Shut-Off Valve Nut

Two-Stage Pressure Reducing Regulator

Gas Bottle

Brass Reducer Fitting

Copper Tubing

Regulator Shut-Off Valve Pressure Control

Knob

Minimum recommended tank pressure is 200 psig. Check the tank pressure periodically to ensure that it exceeds 200 psig.

Feb 06 2-3

Setting up the Analyzer Gemini V Windows

Figure 2-2. Rear Panel Connections

Adsorptive Connector

Helium Connector Vacuum Connector

Software Card Connector

On/Off Switch

Power Supply Indicators

RS-232 Serial Connector

Keypad Connector(not used with Windows software)

Power Supply Connector

He N2

Printer Connector

2-4 Feb 06

Gemini V Windows Setting up the Analyzer

7. Attach an adequate length of vacuum pump tubing (that will fit over the 1/2-in. analyzer connector) to a vacuum pump and to the port labeled on the back of the analyzer. Use hose clamps to keep the hose in place. (An appropriate vacuum pump is available from Micromeritics; refer to Chapter 10, page 10-1 for ordering information.)

8. Connect one end of your RS-232 communications cable to the connector labeled RS-232 on the back of the analyzer. Connect the other end of the cable to the computer.

9. Record the analyzer serial number/computer port number combination for each analyzer you attach to the computer. This information is required when installing the software.

10. Connect one end of the printer cable to the input connector on the printer. Connect the other end of the cable to the printer port on the computer.

11. Hold the Gemini Software Card with the label facing toward the keypad connector. Insert the card (notched end first) into the connector on the rear panel of the analyzer and press firmly to lock into place.

If you plan to install multiple instruments on your computer, you may need a USB to add the required ports (refer to Chapter 10 for ordering information). If you are supplying the USB, be sure that its installation software includes the most current drivers for your operating system; the USB kit from Micromeritics includes the proper drivers.

Power must be off when removing or installing the software card. Removing or installing the card while power is applied to the unit corrupts the software program. Wait at least 30 seconds after turning power off before removing or installing the card. This allows any stored power charge to drain.

The software card must be properly inserted in the Gemini connector during operation. It is best to keep it installed at all times, even when power to the unit is turned off.

Notched End of Software Card

Label

Software Connector

Keypad Connector(not used with Windows)

Eject Button

Feb 06 2-5

Installing the Degasser Gemini V Windows

12. Prepare your vacuum pump using the instructions in its accompanying manual. It is also recommended that you use a device to prevent oil vapor backstreaming. Appropriate vacuum pumps and oil vapor kits are available from Micromeritics (refer to Chapter 10, page 10-1 for ordering information).

13. Plug in the vacuum pump power cord.

14. Plug the computer power cord into an appropriate power source.

15. Set the gas supply regulators to 15 psig (103.4 kPa). Purge the gas supply lines of air before using the analyzer by loosening the gas line connectors on the rear panel of the instrument. Let them remain open about 30 seconds, then tighten.

16. Loosen the port fittings and remove the plugs from the sample and balance ports.

Installing the Degasser

Micromeritics has three degassers that can be used for preparing your samples for analysis with the Gemini V analyzer.

• SmartPrep 065: degasses up to six samples simultaneously at up to 400 ºC with flow-ing gas. Adds a menu to the Gemini menu bar allowing you complete control of the SmartPrep through the Gemini Windows program.

• VacPrep 061: Prepares up to six samples for surface area and pore structure analysis. Uses flowing gas or evacuation by vacuum up to 400 ºC.

• FlowPrep 060: Prepares samples for adsorption analysis. Uses flowing gas passed over a heated sample up to 400 ºC.

If you ordered a degasser with your Gemini analyzer, install it using the instructions provided in its accompanying manual. If you did not order a degasser with your Gemini and wish to do so, refer to Chapter 10, page 10-1 for ordering information.

2-6 Feb 06

Gemini V Windows Installing the Software

Installing the Software

The Gemini Windows program can also be installed on a computer other than the one control-ling the analyzer. This allows you to:

• create or edit sample and parameter files• generate reports on completed sample files

Review the Micromeritics PROGRAM License Agreement for restrictions on the use of another copy of the Gemini Windows program.

Configuring the Gemini

If you ordered your Gemini analyzer with Gemini Windows, your Gemini is configured cor-rectly; continue with Initial Installation.

If you are upgrading from a keypad version of the Gemini, ensure that the following parame-ters are specified as shown before disconnecting the keypad and installing the Gemini Windows software:

• Data Transmission setup: Baud rate: 9600Data bits: 8Stop bits: 1Parity: NoneXon/Xoff protocol: Disabled

• System Options setup:Language: English

Initial Installation

The Gemini Windows program is supplied on a CD-ROM. After initial installation, the Setup program is used to perform other analyzer functions such as moving an analyzer and uninstall-ing the software. Refer to Using the Setup Program for Other Functions, page 2-13.

Perform the following steps to install the program:

1. Turn on the analyzer, then turn on the computer.

2. Insert the CD into the CD-ROM drive.

3. Select Start from the Status bar, then Run from the Start menu.

Proceed to Step 5 if AutoPlay is enabled on your computer; Setup will start automatically and display the New Installation dialog.

Feb 06 2-7

Installing the Software Gemini V Windows

4. Enter the drive designator for the CD-ROM drive, followed by setup. For example:

e:setup

Alternatively, you can click Browse, navigate to the CD-ROM drive, and select setup.exe.

5. Click OK; the New Installation dialog is displayed.

The Destination Folder group box displays the amount of current disk space, the amount of disk space required for the analysis program, and the directory into which the application will be installed. If you wish to install the application into a different directory, click Browse to choose the directory.

6. For quick access to the application, select the checkbox just below the Destination Folder group box to add an icon to your desktop.

7. The Gemini Windows icon is added to the Micromeritics folder by default. If you prefer a different folder, enter or select one from the drop-down list.

8. The Install this application for All Users option defaults as selected; this enables anyone to operate the Gemini Windows program. If you deselect this option, only the person logged into the operating system at the time of installation is allowed to open and operate the program.

9. Click Next; the Analyzer Configuration dialog is displayed.

Deselect this option only if you wish to restrict operation of the Gemini program to the person logged into the operating system at the time of installation.

Displays the amount of current disk space and the amount required for installation of the application. Also displays the directory into which the application will be installed.

Select this option to add the Gemini Windows icon to your desktop for quick access to the application.

2-8 Feb 06

Gemini V Windows Installing the Software

10. In the Step 1 group box, click the radio button for the number of analyzers to be attached to this computer. If you are attaching multiple analyzers, make sure your computer contains enough communication ports to accommodate them. A USB kit is available from Micromeritics if you need to add ports (refer to Chapter 10, page 10-1 for ordering information).

11. In the Step 2 group box, enter the analyzer serial number(s) and the port(s) to which each is attached.

12. Click Next; the Installation Complete dialog containing the Readme file is displayed.

13. Use the scroll bar to read the contents of the file, then click Finish to close the dialog.

14. Remove the Setup CD and store in a secure location.

15. After installation, you may be prompted to reboot the computer; click OK to reboot. If you click Cancel and choose not to reboot your system, the Gemini program may not function properly.

Choose 0 (zero) if you are installing this program for data reduction on a computer other than the one controlling the analyzer.

With monitor resolution set at 600 x 800 (minimum resolution), you may have to use the scroll bars to view the contents of some dialogs. You may wish to set your monitor resolution to 1024 x 768 to avoid the need for scrolling.

Feb 06 2-9

Verifying Operation Gemini V Windows

Verifying Operation

Perform an analysis using the carbon reference material supplied in your accessories kit to ver-ify that the analyzer is operating properly.

1. Fill the Dewar with liquid nitrogen to about 2.5 cm (1 in.) from the top; allow it to equilibrate to ambient conditions (approximately 20 minutes).

2. Prepare the sample tube, balance tube, and reference material for analysis (refer to Performing an Analysis, page 4-14).

3. Install your sample tube (containing the sample) onto a port of the degassing unit; degas your sample using the conditions in the Reference Material booklet.

If you have a SmartPrep installed, a SmartPrep menu is added to the Gemini menu bar.

a. Select SmartPrep > Start; the Automatic Degas dialog is displayed.

b. Click Browse to the right of the port on which the sample tube is installed.

c. Select the sample file you created (step 3) from the Files list window, then click OK to return to the Automatic Degas dialog.

d. Click Start to begin degassing.

4. After the sample has been degassed, remove the sample from the degas port and install onto the sample port. Install the balance tube onto the balance port:

Minimize sample exposure to air by completing the steps rapidly. Samples with 2% or more of total surface area composed of microporous material may benefit by being loaded while still hot from the degas unit.

When handling sample tubes that are still hot, it is recommended that you weigh the sample after analysis. The sample mass may be entered in the sample file after analysis and the results recalculated.

Wear proper insulated gloves when handling hot sample tubes. Handling hot sample tubes with bare hands could cause burns.

2-10 Feb 06

Gemini V Windows Verifying Operation

a. Place the connector nut, ferrule, and O-ring onto the sample tube stem.

b. If you are using a bulb-type tube, place the Dewar cover over the sample tube. Attach the sample tube to the analysis port. Make sure it is fully seated in the port. Secure it in place by screwing the connector nut onto the analysis port. Hand-tighten the connector nut.

If you are using a straight-wall tube, place the Dewar cover under the sample tube and slide it to the top of the tube.

c. If the balance tube is not already installed, attach it to the balance port following procedures similar to those described in steps a and b.

5. Place the liquid nitrogen Dewar onto the elevator, then close the doors to the sample compartment.

The sample tube ferrule is tapered slightly on one end. The ferrule may be installed onto the sample tube with the tapered end in the up or down position.

O-ring

Ferrule

Connector Nut

Sample Tube

It is not necessary to remove and replace the balance tube between analyses unless it has been contaminated or you are using a different size sample tube.

Be sure the doors are closed before beginning an analysis. If an abnormal condition causes the analyzer to operate at an excessive pressure, the sample or balance tubes could dislodge from its port, possibly breaking the Dewar and causing personal injury or damage to the equipment.

Feb 06 2-11

Verifying Operation Gemini V Windows

6. Select Unit > Start analysis; the Analysis dialog is displayed with the Start Analysis dialog positioned on top.

7. Select carbonr.smp from the Files list window, then click OK; the Analysis dialog is fully displayed. This file has been included with the analysis program for your convenience in verifying operation.

8. Click Report After Analysis; select the desired destination, then click OK to return to the Analysis dialog.

9. In the Mass field, enter the sample mass (weight).

10. Click Start to begin the analysis.

After the analysis has completed, a report is generated automatically to the destination you chose on the Analysis screen. Compare the results with those in the Reference Material book-let. If the results do not match:

• contaminants may have been in the flow path since this is the first analysis after gas line connection

• an incorrect weight was entered in the Mass field

Verify that the value you entered in the Mass field is correct and repeat the analysis. If the results of the second analysis fail to match, contact your Micromeritics service representative.

2-12 Feb 06

Gemini V Windows Using the Setup Program for Other Functions

Using the Setup Program for Other Functions

After initial installation of the Gemini Windows program, the application setup program can be used to:

• Upgrade software, page 2-15• Add an analyzer, page 2-16• Move an analyzer from one computer to another computer, page 2-17• Remove an analyzer from the computer, page 2-20• Change the analyzer setup, page 2-21• Uninstall the analysis program, page 2-22

To start the application setup program:

1. Ensure that the analysis program is not operating.

2. Insert the CD-ROM into your CD-ROM drive.

3. Select Start from the Status bar, then Run from the Start menu.

4. Enter the drive designator of the CD-ROM drive, followed by setup. For example: e:setup.

Alternatively, you can click Browse, navigate to your CD-ROM drive, and select setup.exe.

5. Click OK; the setup Welcome screen showing the options available is displayed.

Proceed to Step 5 if AutoPlay is enabled on your computer; Setup will start automatically and display the New Installation dialog.

Feb 06 2-13

Using the Setup Program for Other Functions Gemini V Windows

6. Select the operation you wish to perform. Procedures for performing each operation are in subsequent sections.

After the requested operation is completed, the setup Welcome screen is again displayed. A confirmation message indicating completion of the operation is shown in the lower section of the dialog.

7. After you have completed all desired operations, click Exit to close the dialog.

Indicates status of last operation.

2-14 Feb 06


Installing Subsequent Software Versions

When you install a software upgrade, existing data files are not overwritten. There are three types of subsequent installations; the software version controlled by the setup program is:

• a later version than the version installed on the computer• the same version as the version installed on the computer• an earlier version than the version installed on the computer

The setup program automatically detects which type of installation applies and customizes the selection in the Setup dialog accordingly.

1. Start the Setup program. Refer to Using the Setup Program for Other Functions, page 2-13

2. Choose the software option (only the applicable option will display); it will be one of the following:

• Upgrade software to version (number) from version (number)• Reinstall software version (number)• Downgrade software to version (number) from version (number)

3. Click Start File Installation; the application installs the software and redisplays the setup Welcome dialog. If no other operations are desired using this dialog, click Exit to close the dialog.

Feb 06 2-15


Adding an Analyzer

Add an analyzer to the existing application as follows:

1. Start the Setup program. Refer to Using the Setup Program for Other Functions, page 2-13.

2. From the Setup dialog, select Add an analyzer, then click Next; the Set up analyzer being added dialog is displayed:

3. Enter the serial number of the analyzer being added and the communications port to which it is to be connected.

4. Click Next to complete the operation.

5. Click Exit to close the dialog.

Be sure the analyzer you are adding and the computer are connected with an RS-232 communications cable.

2-16 Feb 06


Moving an Analyzer from one PC to another PC

You can move an analyzer, along with its status files, from one computer (Source PC) to another computer (Destination PC).

1. Install the analysis program on the destination computer. Refer to Initial Installation, page 2-7. Be sure to select 0 as the number of instruments; all related instrument information will be transferred in the Move operation.

If the analysis program is already installed on the destination computer, proceed to Step 2.

2. Start the application setup program on the source computer. Refer to Using the Setup Program for Other Functions, page 2-13.

3. In the Setup dialog, select Move an analyzer from one PC to another PC, then click Next; the Move analyzer operation dialog is displayed.

4. Select Source PC, then click Next; the following dialog is displayed.

This operation does not move sample or parameter files. To move these files, use a file management program such as Explorer or a backup/restore utility.

Feb 06 2-17


5. In the Step 1 group box, select the analyzer that is to be moved.

6. In the Step 2 group box, choose a location in which the moved files will be stored. If possible, choose a floppy drive or a shared network drive. If this is not possible, select a local folder. After the files are placed there, use a folder transfer utility to copy this folder from the Source PC to the Destination PC.

7. Click Next; the files are moved and the setup Welcome screen is displayed.

8. Start the application setup program on the destination computer.

9. In the Setup dialog, select Move an analyzer from one PC to another PC; the Move analyzer operation dialog is displayed (shown on previous page).

10. Select Destination PC, then click Next; the following dialog is displayed.

2-18 Feb 06


11. In the Step 1 group box, enter the serial number of the analyzer being moved and the communications port to which it will be attached.

12. In the Step 2 group box, click Browse and choose the location of the moved files.

13. Click Next; the files are moved and the setup Welcome dialog is displayed.


Feb 06 2-19


Removing an Analyzer

You can remove an analyzer from the computer as follows. When you remove an analyzer, the status files are removed as well.


2. From the Setup dialog, select Remove an analyzer, then click Next; the Remove an analyzer dialog is displayed.

3. From the drop-down list, choose the serial number of the analyzer you wish to remove.

4. Click Remove; the analyzer is removed and the Welcome screen is again displayed.


2-20 Feb 06


Changing an Analyzer Setup

Change the analyzer setup as follows:


2. From the Setup dialog, select Change analyzer setup, then click Next; the Change analyzer setup dialog is displayed.

3. From the drop-down list, choose the analyzer whose setup you wish to change.

4. Enter the new port number in the space provided.

5. Click Next; the change is completed and the Welcome dialog is again displayed.


Feb 06 2-21


Uninstalling the Analysis Program

When you uninstall the Gemini Windows program, the application removes the analysis pro-gram, status files, analyzer setup files, and resulting empty directories. It does not remove data files. Perform the following steps to uninstall the program:


2. From the Setup dialog, select Uninstall, then click Next; the Uninstall dialog is displayed.

3. Click Uninstall; the Select Uninstall Method dialog is displayed.

4. Choose one of the following:

2-22 Feb 06


• Automatic: click Next; the system uninstalls the analysis program automatically and the setup Welcome dialog redisplays.

• Custom: click Next; a series of dialogs is displayed, allowing you to choose the files you wish to uninstall. After all files are selected and uninstalled, the setup Welcome dialog redisplays.

5. Click Exit to close the Welcome dialog.

Feb 06 2-23

Gemini V Windows Turning On the Analyzer

3. USER INTERFACE

This chapter provides information for:

• turning on the analyzer• using the software• Gemini menu structure, page 3-10

Turning On the Analyzer

Simply place the On/Off switch on the rear panel of the analyzer in the On position. The green indicator light on the front panel illuminates when the analyzer is on. Allow the system to warm up for at least 30 minutes before performing analyses. For analyses that require very precise results, allow the analyzer to warm up while the sample is being prepared.

Using the Software

The Gemini Windows program requires familiarity with standard Windows operations such as using the mouse, menus, and dialog boxes. While this manual provides brief instructions for such standard operations, you may have to refer to your Windows documentation or to its online help system to clarify functions which are specific to Windows.

Report System

The Gemini software includes a report system which allows you to manipulate and customize reports. You can zoom in on portions of the graphs or shift the axes to examine fine details. Scalable graphs can be copied to the clipboard and pasted into other applications. Reports can be customized with your choice of fonts and a company logo added to the report header for an impressive presentation. Refer to Onscreen Reports, page 7-14 for a description of the options available for reports.

Online Manual

A complete online manual is provided on the Help menu. Refer to Online Manual, page 1-5 for tips on using the manual.

Feb 06 3-1

Using the Software Gemini V Windows

Shortcut Menus

Shortcut menus (sometimes referred to as context-sensitive menus or pop-up menus) are avail-able for onscreen graphs and tabular reports. These menus are accessed by selecting the item for which you want to display its menu and clicking the right mouse button. For example, right-click in a column of an onscreen report and the following menu is displayed.

Shortcut Keys

Shortcut keys can be used to activate some menu commands. Shortcut keys or key combina-tions (if assigned) are listed to the right of the menu item. Instead of opening the menu and choosing the command, simply press the key combination. For example, to open a sample information file, press F2; the Open Sample Information dialog is displayed.

You can also use shortcut keys to access a menu or any function that contains an underlined letter by pressing Alt plus the underlined letter in the command. For example, to access the File menu, press Alt, then F.

Table 3-1 provides a list of the keys available for the Gemini Windows program.

3-2 Feb 06

Gemini V Windows Using the Software

Table 3-1. Shortcut Keys

Key(s) Function

F1 Access online operator’s manualF2 Open a sample information file

Clear the field of existing date (Select Dates dialog)F3 Open an analysis conditions file

Insert the current date (Select Dates dialog)F4 Open an adsorptive properties file

Display a calendar from which to choose a date (Select Dates dialog)F5 Open a report options fileF6 Tile windowsF7 Cascade windowsF8 Start reportF9 Close all open reportsAlt + F4 Exit the analysis program

Shift + F2 List sample information filesShift + F3 List analysis conditions filesShift + F4 List adsorptive properties filesShift + F5 List report options filesShift + F9 Access shortcut menu on onscreen reports

Feb 06 3-3


Dialog Boxes and Subdialog Boxes

Dialog boxes are displayed when an item followed by an ellipsis (...) is selected. Subdialog boxes are displayed when a push button on a dialog box is selected. These dialogs may contain one or more of the following:

Data entry field These fields may be either numeric (numbers only) or alphanumeric (numbers, letters, or printable characters). If you make an invalid entry in either of these fields, an error message occurs.

Information bar Some dialog boxes contain information pertinent to the selected field in an information bar across the bottom of the dialog. For example, a range is shown for fields in which numeric entries are required.

List A list contains selections from which you may choose one or more items. To select an item on the list, position the mouse pointer on the desired selection, then double-click. An item is selected if it is preceded with a check mark. Alternatively, you can select the item and press the Spacebar.

Displays range for selected field.

Indicates item is selected.

3-4 Feb 06


Push Button A push button is used to display subdialog boxes in which to enter additional information about the subject matter. For example, this push button displays a dialog for specifying a range of dates (explained later in this chapter).

Push buttons also may be used to cause an action. For example, Cancel closes the open dialog box, discarding any information you may have entered.

Radio Button Radio buttons are contained within a group box. These buttons are used to select options; you may choose only one item.

Check Box Check boxes also are used to select options. You may make as many selections as you wish.

Drop-down List A drop-down list is indicated by a down arrow to the right of the field. Drop-down lists contain a list of options from which you may choose one.

Feb 06 3-5


The following push buttons are common to many of the dialogs in the Gemini program:

Selecting Files

Sample information is stored in files and saved under file names. Certain dialogs contain a Files list box, which displays a list of files available for that particular operation. For example, the Open Sample Information dialog:

From the list of files in the Files list box, move the mouse pointer to the file you wish to open and double-click.

You may limit the list of files displayed in the Files list box by choosing one or more of the following:

• Use a wildcard character in the path name you enter in the File name field.

Wildcard characters such as * and ? can be used to filter file names. For example in the dialog box shown above, you can limit the list of files displayed to those beginning with ga by entering ga*.smp.

Browse Displays a dialog box which allows you to select a file for the subject matter.

Replace Allows you to copy file values from an existing file into the one you are creating. You then can edit the values in the new file without changing the ones in the original file.

Displays the current directory.

Displays all files of the type in the Status field and within the date range specified.

The Status drop-down list does not appear on the Open dialogs for parameter files.

3-6 Feb 06


• Enter a range of dates. Select Date Range; the Select Dates dialog is displayed.

Select the Show Date Range radio button. This enables the From and To fields allow-ing you to enter a beginning and ending date. Alternatively, you can double-click in each field to display a calendar to choose a date. The range of dates remains the default until you change the dates or select Show All Dates.

For convenience, the following function keys are available when the Select Dates dia-log box is displayed:

You may change the date format by using the International Date Format function on the Windows Control Panel.

• Select a file status from the Status drop-down list. Table 3-2 describes each file status.

F2 Clears the fieldF3 Inserts the current dateF4 Displays a calendar from which you may select a date

Selects the yearSelects the month

Click the desired date

The status drop-down list does not appear on the File, Open dialogs for parameter files.

Feb 06 3-7


Table 3-2. File Status and Description

• Navigate to a different directory. The current directory is displayed just above the Directories list box. You can change directories by double-clicking a directory in the Directories list box, double-clicking [...] to move up one level, or by entering the desired directory in the File Name field. For example, enter C:\2380files\sample\*.smp to display sample files in the 2380files\sample directory on your local drive.

Status DescriptionAll All sample information files in the specified directory and within the

specified range of dates.Analyzing Sample information files that are currently being used for analysis or are

in the degassing process.Complete Sample information files that were used in an analysis that has been

completed.Entered Sample information files that contain manually entered data.No analysis Sample information files that have not been used to perform an analysis.Prepared Sample information files that have been used in an automatic degas

operation, but not for an analysis.Preparing Sample information files currently being used in an automatic degas

operation.

Double-click to move up one level.

Double-click to open the listed directory.

Displays the current directory.

3-8 Feb 06


File Name Conventions

For sample information files, a default file name (the next available sequence number) and a default extension display. For Degas conditions, Analysis conditions, Adsorptive properties, and Report options, only a default extension displays.

The following table shows the file name extensions for the Gemini Windows program.

Table 3-3. Default File Name Extensions

File Type Extension

Sample information SMP

Degas conditions DEG

Analysis conditions ANC

Adsorptive properties ADP

Report options RPO

Export to disk (ASCII) EXP

Report to disk RPT

List to disk LST

Thickness curve THK

The following types are available for reports saved from the Report window:

Report REP

Spreadsheet XLS

ASCII TXT

Feb 06 3-9

Menu Structure Gemini V Windows

Menu Structure

All functions for the Gemini Windows program are located on menus which are accessed from the Menu bar. Each menu contains commands, and in some cases a submenu. A submenu is indicated when the command is followed by an arrow.

Brief descriptions of each menu are provided below; refer to the chapter given in parentheses for a detailed description of the options contained on that menu.

File Allows you to manage sample and parameter files. (Chapter 5, FILE MENU)

Unit <n> Enables you to perform analyses. A unit menu is displayed for each attached unit. (Chapter 6, UNIT MENU)

SmartPrep Displayed when a SmartPrep is being used to prepare samples. Refer to the SmartPrep manual for an explanation of the commands on this menu item.

Reports Enables you to generate, open, and close reports. (Chapter 7, REPORTS MENU)

Options Allows you to choose sample editing mode, select data presentation formats, and specify a location for predefined parameter files. (Chapter 8, OPTIONS MENU)

Windows Enables you to arrange the windows and icons on your screen. It also displays the names of all open windows. (this chapter, page 3-11)

Help Provides access to the online manual. (this chapter, page 3-11)

Submenu

Command

Menu Bar

Menu Name

3-10 Feb 06

Gemini V Windows Menu Structure

Windows

The Windows menu also displays all open files; the active window is preceded with a check mark.

Help Menu

Tile Resizes all open windows and arranges them side by side so that the contents of all open windows are visible.

Cascade Resizes all open windows and arranges them in a stacked fashion. The active window is positioned on top of the stack. Each window’s title remains visible, making it easy to select other windows.

Arrange Icons Arranges the symbols for all minimized windows in an orderly manner.

Operator’s Manual Provides a copy of the operator’s manual in Adobe® PDF format.

If the Gemini program is installed offline, the software will not detect an analyzer and, therefore, both operator manuals will be enabled.

About Gemini Displays information about the Gemini Windows program.

Feb 06 3-11

Gemini V Windows Specifying Sample File Defaults

4. OPERATIONAL PROCEDURES

This chapter contains brief step-by-step instructions on how to:

• specify sample file defaults, beginning on this page• create sample information files, page 4-5• define parameter files, page 4-8 • perform an analysis, page 4-14• print file contents, page 4-23• generate a list of information on a sample or parameter file, page 4-24• export isotherm data in a sample information file, page 4-25 • overlay graphs, page 4-26

This chapter does not contain detailed descriptions of the dialogs used to perform these proce-dures. Refer to Chapters 5 through 8 for dialog descriptions. Use the index in the online manual to assist you in locating the appropriate dialog.

Specifying Sample File Defaults

You can specify sample defaults in the Basic or Advanced format. The defaults you specify are the ones you see when you create a new sample file in the respective format. Therefore, it is best to specify (or enter) parameters that you plan to use most frequently. For example; specify defaults for your most commonly analyzed sample material. You can always edit parameters in the sample file when it is created. The Gemini Windows system automatically generates sam-ple information file names and uses the values you specify as the defaults.

Basic Format

Perform the following steps to define defaults for a sample information file in the Basic for-mat. The defaults you specify in this format also display as the defaults for sample files in the Restricted format.

1. Select Options > Sample defaults; the Basic Sample Defaults dialog is displayed.

Select Options > Option Presentation and ensure that Basic is selected as the format.

Feb 06 4-1

Specifying Sample File Defaults Gemini V Windows

2. In the Sequence field, specify a default string. This is the number that is incrementally sequenced and displays in the File name field when you select File > Open > Sample information. You can use up to eight characters.

3. In the field on the right of the Sample line, enter a format for the sample identification. Be sure to include the $ symbol if you wish to have the sample file number included as part of the identification. You can use up to 42 alphanumeric characters.

4. Enter a default value in the Mass field. An approximate weight is sufficient; a more accurate weight can be entered later.

5. Enter a default value in the Density field. This value is only applicable when using a calculated free space; it is ignored for all other types of free space.

6. Select the down arrow to the right of the parameter fields to choose default parameter files:

• Degas conditions• Analysis conditions• Adsorptive properties• Report options

7. Click Save, then Close.

You also can edit the word Sample. For example, you may prefer to use Material or Test. You can enter up to 15 characters in this field.

4-2 Feb 06

Gemini V Windows Specifying Sample File Defaults

Advanced Format

The Advanced Sample Defaults dialog resembles a set of index cards. You can move from one set of parameters to another by clicking the parameter tab or by using Next and Prev. The val-ues you specify in the parameter portions of the sample file (Degas Conditions, Analysis Conditions, Adsorptive Properties, and Report Options) are saved as the defaults for newly created parameter files.

For example, after specifying defaults for a sample file in the Advanced format:

• Select File > Open > Sample Information, then Yes to create the file, and the defaults you specify display for all parameters.

• Select File > Open > Analysis Conditions, name and create the file, and the defaults you specify in the Analysis Conditions portion of the Advanced Sample Defaults dia-log display in the fields.

1. Select Options > Sample Defaults, the Advanced Sample Defaults dialog is displayed.

2. In the Sequence field, specify a default string for the sample file number; you can use up to eight characters. This is the number that appears in the File name field when you select File > Open > Sample information.

3. In the right-side field of the Sample line, enter a format for the sample’s identification. You can enter up to 42 characters. Be sure to include the $ symbol if you wish to have the sample file number (Sequence) included as part of the identification.

Select Options > Option Presentation and ensure that Advanced is selected as the format.

Feb 06 4-3

Specifying Sample File Defaults Gemini V Windows

4. Edit the Operator and Submitter lines as desired. Or have them omitted entirely by selecting Omit.

5. Enter a default value in the Mass field. An approximate value will suffice; a more accurate value for the sample mass can be entered at the time of analysis.

6. Enter a default value in the Density field. This value is only applicable when using a calculated free space; it is ignored for all other types of free space.

7. Choose whether you wish to have data collected automatically or if you plan to enter data. This option can be changed (if desired) when a sample file is created.

8. Click the Degas Conditions tab. Specify degassing criteria, then click Save.

9. Click the Analysis Conditions tab. Choose the analysis conditions appropriate for your most commonly analyzed material, then click Save.

10. Click the Adsorptive Properties tab. Specify gas characteristics, then click Save.

11. Click the Report Options tab. Choose desired reports, using to specify details; then click Save.

12. Click Close to close the dialog.

It is not necessary to click Save on each dialog. Clicking Save once on any dialog after all defaults have been specified is sufficient. All dialog defaults will be saved.

4-4 Feb 06

Gemini V Windows Creating Sample Information Files

Creating Sample Information Files

A sample information file must be assigned to every sample that is analyzed. When you create a sample file, you can accept the default values specified using Sample defaults, or you can edit them as desired. You can create a sample information file using the Advanced, Basic, or Restricted format.

Advanced Format

The Advanced format allows you to customize the parameters of a sample information file. Refer to Advanced on page 5-5 for a description of the fields associated with creating sample information files.

1. Select File > Open > Sample information; the Open Sample Information File dialog is displayed.

2. Accept the next sequenced file number or enter a new name in the File name field; you can use up to eight characters.

3. Click OK, then Yes to create the file; the Sample Information dialog is displayed

The defaults that appear in the fields are the ones specified in Sample defaults.

4. Accept the default identification in the Sample field or change it to an appropriate one. The dialog in Step 3 shows the sample file number because the dollar ($) symbol was used when specifying sample defaults.

5. Edit the Operator and/or Submitter fields as needed. If these fields are not displayed, they were selected to be omitted in Sample defaults.

These fields do not display if you selected Omit when specifying Sample defaults.

If a sample information file already exists containing the values you wish to use in this file, you can click Replace All to copy those values into this one. You can still edit the values after they are loaded.

Feb 06 4-5

Creating Sample Information Files Gemini V Windows

6. Enter the sample’s mass (if different from the default value) in the Mass field.

7. Enter a value in the Density field (or accept the default). This value is only applicable when using a calculated free space; it is ignored for all other types of free space.

8. Choose whether you wish to enter data or have it collected automatically by the system.

9. Click Save to save the information you entered.

10. The steps for completing the remaining parameters of the sample information file are explained in subsequent sections:

• Defining Degas Conditions, page 4-8• Defining Analysis Conditions, page 4-10• Defining Adsorptive Properties, page 4-11• Defining Report Options, page 4-12

Simply click on the tabs to open its associated dialog.

Use the Comments window to record specifics of the analysis or its conditions. Anything you enter in this window is displayed in the report header.

4-6 Feb 06

Gemini V Windows Creating Sample Information Files

Basic and Restricted Formats

Sample information files are created in the Basic and Restricted formats using predefined parameter files. Refer to Basic on page 5-7 for a description of the fields associated with creat-ing sample information files.

1. Select File > Open > Sample information; the Open Sample Information File dialog is displayed.

2. Accept the next sequenced file number or enter a new name in the File name field; you can use up to eight characters.

3. Click OK, then Yes to create the file; the Sample Information dialog is displayed.

The defaults that appear in the fields are the ones specified in Sample defaults.

4. Accept the default identification or change it to an appropriate one. The dialog above shows the sample file number because the dollar ($) symbol was used when specifying Sample defaults.

5. Enter the sample’s mass (if different from the default value) in the Mass field.

6. Enter a value in the Density field (or accept the default). This value is only applicable when using a calculated free space; it is ignored for all other types of free space.

7. Using the down arrows to the right of each parameter field, select an appropriate file (or accept the defaults). You can review or edit the contents of these files by switching to the Advanced format if desired.


Use this push button to enter pertinent sample or degassing informa-tion. The information you enter is printed in the Sample Log Report.

Use this push button to copy parameters from an existing file into the current one.

Not displayed when using the Restricted format.

If you are using the Restricted format, you cannot switch to the Advanced format.

Feb 06 4-7

Creating Parameter Files Gemini V Windows

Creating Parameter Files

The following file types can exist as part of the sample information file or as an individual parameter file:

• Degas conditions, this page• Analysis conditions, page 4-10• Adsorptive properties, page 4-11• Report options, page 4-12

Having these files exist independently allows you to use them over and over again.

Several predefined parameter files (located in the params directory) are included with the Gemini program. Although these files may come close to the needs of your laboratory, you may wish to define additional ones. Or you can use a predefined file as a starting point. This is easily accomplished by creating a new file and then selecting Replace. A dialog is displayed so that you can select the existing file containing the values you wish to use. After the values are copied into the current file, you can edit the values as desired; the original file remains intact and ready for the next use.

If you wish to have parameter files display in the drop-down list on the Basic Sample Informa-tion dialog, be sure to save them to the directory specified as the Parameter Files Directory (see Parameter Files Directory, page 8-12 for additional information).

Degas Conditions

Degas Conditions files contain degassing information for preparing samples. The conditions specified in this dialog are applied automatically if you have a SmartPrep degasser installed. If you are not using a SmartPrep, you can use this dialog to record the conditions used on an external degassing unit.

Perform the following steps to define a degas conditions file:

1. Select File > Open > Degas Conditions; the Open Degas Conditions dialog is displayed.

2. Enter a name (up to eight characters) in the File name field, then click OK.

Be sure the directory specified is the Parameter files directory if you wish to have it display in the drop-down list in the Basic Sample Information dialog. (Refer to Parameter Files Directory in Chapter 8 for additional information.)

4-8 Feb 06

Gemini V Windows Creating Parameter Files

3. Click Yes to create the file; the Degas Conditions dialog is displayed.

4. Enter a description in the Description field. Be sure to use an intuitive description so that you can recognize it easily.

5. Specify up to 5 sets of degas conditions (soak temperature, ramp rate, and soak time).


Feb 06 4-9


Analysis Conditions

Analysis conditions specify the data used to guide an analysis. An analysis conditions file may be assigned a unique name, and you can direct any sample to be analyzed according to the con-ditions in any existing analysis conditions file. Refer to Analysis Conditions, page 5-12 for a detailed description of the fields on this dialog.

1. Select File > Open > Analysis Conditions; the Open Analysis Conditions File dialog is displayed.


3. Click Yes to create the file; the Analysis Conditions dialog is displayed.

4. Enter a description (up to 42 characters) in the Description field. Use an intuitive description, one that will help you identify the type of sample you plan to analyze using these analysis conditions.

5. Specify points for your pressure table. Use the push buttons adjacent to the table to assist you in creating your table.

6. Click the following push buttons to define associated analysis conditions:

• Preparation• Free space• Po and T• Analysis Method


Be sure the directory specified is the Parameter files directory if you want this file to display in the drop-down list of the Basic Sample Information dialog. (Refer to Parameter Files Directory in Chapter 8 for additional information.)

4-10 Feb 06


Adsorptive Properties

Adsorptive properties specify the characteristics of the gases used in the Gemini analyzer. Refer to Adsorptive Properties, page 5-18 for a detailed description of the fields on this dialog.

1. Select File > Open > Adsorptive properties; the Open Adsorptive Properties File dialog is displayed.


3. Click Yes to create the file; the Adsorptive Properties dialog is displayed.

4. Enter the name of the adsorptive gas in the Adsorptive field, then enter its mnemonic.

5. Enter the appropriate information (or accept the defaults) in the following fields.

• Non-ideality factor• Density conversion factor• Molecular cross-sectional area


Be sure the directory specified is the Parameter files directory if you want this file to display in the drop-down list of the Basic Sample Information dialog. (Refer to Parameter Files Directory in Chapter 8 for additional information.)

Feb 06 4-11


Report Options

Report options specify the types of reports to be generated from an analysis or manually entered data. They also help you customize details of reports such as axis scale, axis range, column headings, and components of thickness curve equations.

You can customize report options files to accommodate the requirements of your analyses. For example, you can generate a simple report that lets you determine the basic characteristics of the sample. Then use that report to make choices about the variables you want to include in lengthier, more sophisticated reports. You can specify for reports to be generated automatically after each analysis, or you can generate reports at any time during or after an analysis. How-ever, a report generated during an analysis only includes data collected up to the time of the report. Refer to Report Options, page 5-19 for a detailed description of the fields on this dialog.

Define report options as follows:

1. Select File > Open > Report Options; the Open Report Options File dialog is displayed.


3. Click Yes to create the file; the Report Options dialog is displayed.

4. Enter a description (up to 42 characters) in the Description field. Enter an identifier that gives a more intuitive description of the file’s contents. For example, BJH Adsorption Report Options.

Be sure the directory specified is the Parameter files directory if you want this file to display in the drop-down list of the Basic Sample Information dialog. (Refer to Parameter Files Directory, page 8-12 for additional information.)

A report is selected when it is preceded with a check mark.

4-12 Feb 06


5. Select Show report title and enter the title you wish to appear at the top of the report. Or deselect this option if you prefer not to have a report title.

6. If you wish to compare the same type of graph from multiple files, click Overlays and choose the files. Then be sure you edit the graph from the Selected Reports window and choose Samples from the Overlay drop-down list.

7. The reports that may be generated are listed in the Selected Reports list. Select reports by double-clicking on the desired report. Reports are deselected in the same manner. A report is selected when it is preceded by a check mark.

You can edit some reports by highlighting the desired report and clicking Edit.

8. Click Save, then Close

If your company logo exists as a bitmap (bmp) or enhanced metafile (emf), you can have it display in the report header by selecting Show graphic. Click Browse to select the file; use the Height and Width fields to specify the size.

Feb 06 4-13

Performing an Analysis Gemini V Windows

Performing an Analysis

There are several activities you must perform before analyzing a sample. Depending upon the standard procedures at your laboratory, these activities may be performed at the beginning of the day or at the beginning of a shift. Before loading a sample for analysis, verify the follow-ing:

• Appropriate regulator pressure settings• Adequate vacuum • Adequate cryogen level in Dewar• Samples prepared and weighed

Verifying Regulator Pressure

Verify that the regulator pressure for the nitrogen and helium cylinders are set to a level between 15 and 18 psig (103.4 and 124.1 kPa).

Verifying Vacuum

The vacuum level must be better than 20 x 10-3 mmHg at the instrument inlet. Most two-stage vacuum pumps, such as the one available from Micromeritics, will provide a vacuum level of about 5 x 10-3 mmHg.

Checking the Cryogen Level

Ensure that the liquid nitrogen level in the Dewar is approximately 2.5 cm (1 in.) from the top.

Dewar Precautions

We recommend the following be observed when handling Dewars containing liquefied gases:

• Protect yourself by wearing 1) goggles (or a face shield), 2) an insulated or rubber apron, and 3) insulated gloves.

• When pouring liquefied gases from one container to another: 1) cool the receiving con-tainer gradually to minimize thermal shock, 2) pour the liquefied gas slowly to prevent splashing, and 3) vent the receiving container to the atmosphere.

Check the gas tank pressure to ensure that it is greater than 200 psig. Pressures less than 200 psig may cause the sample to be inadequately saturated, resulting in inaccurate data or termination of analysis.

Always handle Dewars with care. Any product incorporating a vacuum is a potential safety hazard and should be treated with caution. Always observe the precautions listed below.

4-14 Feb 06

Gemini V Windows Performing an Analysis

• Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases (or other materials of extremely low temperature). Do not use a glass or metal stirring rod unless it is coated with some type of protective coating.

• Do not remove the mesh covering from the Dewar flask. This covering is in place to minimize the risk of flying particles if the Dewar is accidentally knocked over or dropped and broken.

• Do not handle heavy objects above the Dewar. If unavoidable, place a protective cover over the Dewar’s opening. If an object of sufficient weight is accidentally dropped into the Dewar, shattering may occur.

Preparing Samples

Before analyzing a sample, make sure you adequately degas it according to your standard lab-oratory procedures. You should also degas the balance tube prior to its first use.

The sample and balance tubes must be cleaned (using an ultrasonic cleaning unit) and ade-quately degassed to obtain accurate analysis results. The following procedures are recommended.

If you are analyzing a sample with a total surface area of 1.0 m2 or less, filler rods should be used in the balance and sample tubes. Refer to Appendix C for instructions.

Feb 06 4-15


Cleaning and Labeling Sample and Balance Tubes

Table 4-1. Materials Required for Cleaning and Weighing Sample and Balance Tubes

Clean the sample and balance tubes as follows.

1. Turn on the drying oven and set the oven temperature to 75 ºC.

2. Check the bowl of the ultrasonic cleaning unit to make sure it is clean.

3. Using a ratio of 5 grams of Alconox (or equivalent detergent) per 500 mL of warm water, fill the bowl of the ultrasonic unit with enough water to cover the entire tube. Make sure the detergent is dissolved before placing the tube into the water. If too much detergent is used, it may be difficult to rinse from the tube.

4. Fill the tube with warm water and place it in the bowl of the ultrasonic cleaning unit. Turn on the ultrasonic cleaning unit for approximately 15 minutes.

After you have cleaned a balance tube and attached it to the analyzer, you may leave it in place for repeated analyses. You need to change the balance tube only if it becomes contaminated or if you change the size of the sample tube being used. The balance tube size must always match the sample tube size.

Ultrasonic cleaning unit Sample tube brushAlconox or other suitable detergent Sample and balance tubesRubber gloves or lint-free cloth Sample tube stopperIsopropyl alcohol FunnelNitrogen or helium Weighing supportFume hoodBalance for weighing sampleDrying oven

4-16 Feb 06


5. Using either rubber gloves or lint-free cloth (but not bare hands), remove the tube from the bowl.

6. Clean the interior of the tube with the brush included in the accessories kit.

7. Rinse the tube thoroughly with hot water. Then rinse it again with isopropyl alcohol, using a waste container to collect used isopropyl alcohol.

8. Dry the interior of the tube using nitrogen or helium, under a fume hood, with a tubing extension long enough and small enough in diameter to fit inside the tube.

9. Stand the tube on the rack in the oven and bake for two hours at 75 ºC.

10. Remove the tube from the oven and allow to cool.

11. Wipe a rubber stopper with a lint-free cloth. Label the tube and stopper for identification.

12. Fill the tube with helium or nitrogen as in Step 8, then install the stopper. This must be done quickly to prevent air, dust, or moisture from entering the tube.

If isopropyl alcohol is unavailable, deionized water may be used to rinse the tube.

To obtain an accurate weight of a degassed sample, the same gas type must be present in the sample tube during both weighings; that is, when weighed without and with sample present. Buoyancy differences can cause significant errors when helium is used inconsistently.

Feb 06 4-17


Weighing the Sample

To weigh a sample prior to analysis, follow the steps below.

1. Place the sample weighing support on the balance. Zero the balance and allow it to stabilize.

2. Place the sample tube with stopper onto the sample weighing support.

3. Record the stabilized weight as the empty sample tube weight. Remove the sample weighing support and sample tube set from the balance.

4. Place a sample weighing container onto the balance. Zero the balance and allow it to stabilize.

5. Slowly add the sample to the weighing container. Record the weight of the sample as the sample weight prior to degassing.

6. Remove the rubber stopper from a prepared sample tube.

Weighing Support

Do not touch the sample with bare hands while completing the next step. Doing so could affect the accuracy of the analysis results.

4-18 Feb 06


7. Slowly pour the sample from the weighing container into the sample tube using a funnel.

8. Insert the rubber stopper.

9. Degas the sample according to your standard laboratory procedures.

10. Weigh the sample tube, sample, and rubber stopper. Record the weight as the sample plus sample tube weight.

Funnel

If your sample has a total surface area of 1.0 m2 or less, filler rods should be used in the balance and sample tubes. Refer to Appendix C, page C-1 for instructions.

Feb 06 4-19


Installing the Sample Tube

Follow the steps below to attach the sample tube to the analysis port and the balance tube to the balance port. Minimize sample exposure to air by completing the steps rapidly.

1. Place the connector nut, ferrule, and O-ring onto the sample tube stem.

2. Attach the sample tube to the analysis port. Make sure it is fully in the port. Secure it in place by screwing the connector nut onto the analysis port. Hand-tighten the connector nut.

3. If the balance tube is not already installed, attach it to the balance port following procedures similar to those described in steps 1 and 2.


O-ring

Ferrule

Connector Nut

Sample Tube

It is not necessary to remove and replace the balance tube between analyses unless it has been contaminated or you are using a different size sample tube.

4-20 Feb 06


Starting the Analysis

After the sample has been weighed, degassed, and installed on the analysis port, perform the following steps to begin the analysis:

1. Place a Dewar filled with liquid nitrogen (to about 1 in. from the top) on the elevator. Be sure it has equilibrated to ambient conditions (takes approximately 20 minutes).

2. Close the sample compartment door.

3. Select Unit > Start analysis; the Analysis dialog is displayed with the Start Analysis dialog positioned on top.

4. Choose a file for your analysis and click OK; the Analysis dialog containing the parameters of the selected file is displayed.

5. Verify parameters and make any changes you feel necessary. Click Browse to choose a different file.

Be sure the doors are closed before beginning an analysis. If an abnormal condition causes the analyzer to operate at an excessive pressure, the sample or balance tube could dislodge from its port, possibly breaking the Dewar and causing personal injury or damage to the equipment

You can also accept the next sequenced number and create a new file if desired. If you choose this method, however, you can only use the predefined files from the drop-down lists.

Feb 06 4-21


6. To generate a report automatically after the analysis, click Report After analysis and choose report output options. You can generate reports to the screen, a printer, or to a file. If you choose Screen, many options for manipulating and customizing your reports are provided from the Report window. You can also print to a printer from the Report window. Or if you prefer, you can choose not to generate reports after analysis and generate them later using the Start Report command on the Reports menu.

7. Click Start to begin the analysis; as data are collected, the graph is drawn in the window.

8. Click Next to perform another analysis; the first view of the Analysis dialog is displayed.

Make sure the elevator is all the way down. If it is not all the way down, hazardous conditions can result.

4-22 Feb 06

Gemini V Windows Printing File Contents

Printing File Contents

Print enables you to print the contents of one or more files to the screen, a printer, or a file. For example, if you choose Analysis Conditions, you will receive the parameters used for all anal-ysis conditions associated with the file(s). The print dialog is common to all file types.

Perform the following steps to print the contents of a sample or parameter file:

1. Select File > Print.

2. From the Print drop-down menu, select the type of file for which you wish to have information. A dialog similar to the one shown below is displayed.

3. From the Files list box, choose the desired file(s). You can choose multiple files, by holding down Ctrl while making your selections.

4. At the Destination field, click on the down arrow and choose a destination for the list output. If you choose File as the destination, enter a name in the File name field. If you choose Printer, the Copies field is enabled allowing you to print up to four copies.

5. Click OK, contents of the requested file(s) are sent to the specified destination.

Displays the type of file on which you requested informa-tion; in this example a Sample Information file.

Does not display for Parameter files.

Feb 06 4-23

Listing File Statistics Gemini V Windows

Listing File Statistics

You can generate a list of the following information on one or more sample or parameter files:

• File name• Date the file was created (or last edited)• Time the file was created (or last edited)• File identification• File status

Perform the following steps to generate a list:

1. Select File > List.

2. From the List drop-down menu, select the type of file for which you wish to have information. A dialog similar to the one shown below is displayed.

3. From the Files list box, choose the desired file(s). If you wish to include all files in the list, leave all files deselected.

4. At the Destination field, click on the down arrow and choose a destination for the list output. If you choose File as the destination, enter a name in the File name field. If you choose Printer, the Copies field is enabled allowing you to print up to four copies.

5. Click OK, a list for the requested file(s) is sent to the specified destination.

Displays the type of file on which you requested informa-tion; in this example a Sample Information file.

Does not display for Parameter files.

4-24 Feb 06

Gemini V Windows Exporting Isotherm Data

Exporting Isotherm Data

The Export option on the File menu allows you to copy the isotherm data in the sample infor-mation file and reformat it in ASCII text. If saved to a File, the data can be imported into applications, such as spreadsheets. The output file consists of four columns containing the absolute pressure, relative pressure, specific volume adsorbed, and the elapsed time.

1. Select File > Export; the Export Sample File dialog is displayed.

2. From the Files list box, select the file(s) you wish to export. To choose multiple files, hold down Ctrl while making your selections.

3. Choose an output destination. When you choose File as the destination, the File name field is enabled so that you may enter a name (or you can accept the default). If you have selected multiple files, each file is exported as its file name with the extension .ISO.

4. Click OK; the file(s) is(are) exported to the specified destination.

Feb 06 4-25

Generating Graph Overlays Gemini V Windows

Generating Graph Overlays

Use graph overlays when you wish to compare graphically results for multiple samples or multiple graphs for one sample. Graphical lines are differentiated by the use of varying sym-bols and reported in a legend on the report.

Graph overlays can be implemented in two ways:

• Multiple Sample Overlays Overlay results for up to eight samples on top of a previously selected sample.

• Multiple Graph OverlaysOverlay two different types of graphs from one sample. The multiple graph overlay capability exists only for the Gemini 2380 for the following reports:

BJH Adsorption BJH Desorption MP-Method

Graph overlays can be generated only using the Advanced format.

4-26 Feb 06

Gemini V Windows Generating Graph Overlays

Multiple Samples Overlay

1. Select File > Open > Sample Information to display the Open Sample Information File dialog.

2. Select a sample on which to overlay graphs of other samples, then click OK; the Sample Information dialog is displayed.

3. Click the Report Options tab to display the Report Options dialog.

4. Make your report (or graph) selections.

5. Choose the type of graph and perform the steps indicated:

Ensure that the Advanced mode is selected; if not, you must switch to the Advanced mode before proceeding.

If overlaying this type of graph... Then...Isotherm Select Isotherm, then click Edit to display the Isotherm Report

Options dialog. Choose the type of plot(s) you wish to use in the overlay(s).Click Options for each type of plot you choose; the related Plot options dialog is displayed.Select Overlay samples.Click OK to return to the Isotherm Report Options dialog.Click OK to return to the main Report Options dialog.

Feb 06 4-27


6. Click Overlays; the Graph Overlay Samples dialog is displayed.

7. Click Browse to the right of the Sample 1 field; a Plot Overlay Sample Selection dialog is displayed.

If overlaying this type of graph... Then...BETLangmuir Surface Areat-Plot

Select the report for which you want an overlay, then click Edit. A Report Options dialog for that report (or graph) is displayed. Select Overlay samples and do any other editing you wish.Click OK to return to the main Report Options dialog.

Dubinin

(Gemini 2380 only)

Select Dubinin, then click Edit. A Report Options dialog for Dubinin is displayed.Select the desired graph, then click Edit. An options dialog for that graph is displayed (for example, dV/dD Pore Volume).Select Overlay samples and do any other editing you wish.Click OK to return to Dubinin Options dialog Click OK to return to the main Report Options dialog.

BJH AdsorptionBJH DesorptionMP-Method

(Gemini 2380 only)

Select BJH Adsorption (or Desorption) or MP-Method, then click Edit; an associated Report Options dialog is displayed.Select the desired graph, then click Edit. An options dialog for that graph is displayed.Click on the down-arrow at the Overlay field and select Samples; do any other editing you wish.Click OK; the BJH (or MP-Method) options dialog reappears. Do any other editing you wish. Click OK; the main Report Options dialog reappears.

4-28 Feb 06


8. Choose a sample file, then click OK. You may choose up to eight files in this manner.

9. After selecting the desired number of sample files, click OK to return to the main Report Options dialog.

10. Click Save if you wish to save your Selected Reports list. If you do not wish to save, all of the options regarding overlays and anything else are available as your reports are generated.

11. Select Reports > Start Report. The Start Report screen is displayed with the name of your primary file in the File name field. (This screen looks like the Open Sample Information File screen.)

12. Click OK; the Select Reports dialog is displayed. Ensure that the desired graph is selected (preceded with a check mark), then click OK.

Feb 06 4-29


Multiple Graphs Overlay

Remember that multiple graph overlays can be done on the Gemini 2380 only for the follow-ing types of plots:

• BJH Adsorption• BJH Desorption• MP-Method

1. Select File > Open > Sample Information to display the Open Sample Information File dialog box.

2. Select a sample for which you want to overlay two graphs; then click OK. The Sample Information dialog box is displayed.

3. Click the Report Options tab to display the Report Options dialog.

4. Make your report (or graph) selections.

5. From the Selected Reports list, select the graph for which you want multiple graph overlays, then select Edit. A Report Options dialog for that report (or graph) is displayed (this example shows BJH Adsorption).

4-30 Feb 06


6. Select a graph type, then click Edit; an options dialog for that specific item is displayed (this example shows dV/dw Pore Volume Options).

7. Click the down arrow at the Overlay field and select a graph type from the list. This selection will be overlaid on the graph selected in the Variable field.

8. Click OK to return to the BJH Adsorption Report Options dialog; do any editing you wish.

9. Click OK to return to the main Report Options dialog.

10. Click Save to save your Selected Reports list. If you do not wish to save the selections, all of the options regarding overlays and anything else are still available as your reports are gemerated.

11. Select Reports > Start Report. The Start Report screen is displayed with the name of your primary file in the File name field.

12. Click OK; the Select Reports dialog is displayed. Ensure that the desired graph is selected (preceded with a check mark), then click OK.

These two graphs will be overlaid.

Feb 06 4-31

Gemini V Windows Description

5. FILE MENU

The File menu contains options which allow you to manage sample and parameter files.

Description

Listed below are brief descriptions of the File menu options. Detailed descriptions follow this section.

Open Allows you to open an existing sample or parameter file, or to create a new one. Page 5-3.

Save Saves the file in the active window. Page 5-56.

Save As Enables you to save the file in the active window as a different name. You also can use this option to save a subset of the sample file as a parameter file. Page 5-56.

Save All Saves all open files. Page 5-57.

Close Closes the file in the active window. Page 5-57.

Close All Closes all open files. Page 5-57.

Print Enables you to print the contents of a sample or parameter file. Page 5-58.

Feb 06 5-1

Description Gemini V Windows

List Generates a list of certain information for sample or parameter files. Page 5-59.

Export Exports the isotherm data contained in a sample file. Page 5-61.

Convert Allows you to convert StarDriver Files to a format compatible with Gemini Windows. Page 5-63.

Exit Exits the Gemini Windows program. Page 5-64.

5-2 Feb 06

Gemini V Windows Open

Open

Open allows you to create a new sample or parameter file, or to open an existing one.

When you select to open a sample or parameter file, a dialog similar to the one shown below is displayed.

Refer to Selecting Files on page 3-6 for a description of the other fields on this dialog box.

File name For sample information files, this field contains the next sequenced file name generated by the software. You can accept this number or enter a different name.

For parameter files, the file name displayed includes the wild card (*) and a default extension as follows:

*.DEG for degas conditions*.ANC for analysis conditions*.ADP for adsorptive properties*.RPO for report options

If you are creating a new file, enter a name in the File name field. If you are opening an existing file, select a file from the list.

You can enter up to eight characters in the File name field for sample or parameter files.

Title bar indicates the type of file you are opening; in this example, a Sample Information file.

Does not display for parameter files.

Feb 06 5-3

Open Gemini V Windows

Sample Information

Sample information files contain information used to control the analysis. Therefore, every analysis must be linked with a sample information file before the analysis can proceed. A sam-ple information file is comprised of the following:

• sample identification• degas conditions (if using automatic degassing)• analysis conditions• adsorptive properties• report options• collected/entered data (when an analysis has been completed)

Parts of the sample information file can also exist as parameter files which are separate from the sample information file itself. Having these files exist independently allows you to use them as many times as you wish. For example, if you typically use the same analysis condi-tions for many of your analyses, you can create an analysis conditions file containing those conditions. Then when you create your sample file, select that file for your analysis conditions. After it becomes part of the new sample file, you can edit it in any way you wish without changing the file from which it was copied.

Sample information files are presented in three formats: Advanced, Basic and Restricted.

• Advanced Presents all parts of the sample information file in a single dialog containing tabs like that of an index card file. Each tab opens an associated dialog. Use this format to cus-tomize files.

• Basic Presents the entire sample information file in a single dialog. With this format, you can quickly create a sample information file using previously defined parameter files. This format also allows you to switch to the Advanced format to view or edit parameters.

• Restricted Presents the sample information file in a single dialog similar to the Basic format. With the Restricted format, however, you cannot switch to the Advanced format to edit parameters. Some menu items also are unavilable.

Specify or change your format by selecting Option presentation from the Options menu.

5-4 Feb 06


Advanced

When you open an existing sample information file or create a new one using the Advanced format, all parts of the sample file are displayed in a tabbed dialog. The Advanced format allows you to customize sample files. Refer to Advanced Format, page 4-5 for step-by-step instructions for creating an Advanced sample information file.

The prompts for the Sample, Operator, and Submitter fields may be customized by selecting Options > Sample defaults. Refer to Sample Defaults, page 8-6 for information on custom-izing these prompts.

Sample Displays the description of the file you are opening. If this is a new file, the description specified in sample defaults is displayed. You may enter a new description or add to the existing one.

Range: 50 alphanumeric characters

OperatorSubmitter

Enter the name of the operator who will be performing the analysis and the name of the person (or department) submit-ting the sample for analysis. The label(s) for these fields may be customized to read differenly or omitted from displaying at all using the options available in sample defaults.

Range: 40 characters

Mass Enter the sample’s mass.

Feb 06 5-5


Density Enter the density of the sample to be analyzed. This value is used only for the Calculated free-space method. An approxi-mate value (± 2%) will provide sufficient free-space correc-tion in most cases.

Type of Data Choose whether data are to be collected automatically by the analysis program or manually entered.

If you choose Manually entered, an “Entered” tab is added so that you may enter the desired data.

Add Log Entry Displays a dialog (shown on page 5-8) allowing you to enter information relating to the sample file. For example, if auto-matic degassing is not being used, you may wish to enter external degassing information. Any information you enter here is printed as part of the sample log report. You may make multiple entries by selecting this push button as many times as you wish.

Replace All Allows you to copy an existing sample file’s values into the current sample information file. A dialog is displayed so that you may select the desired file. You may edit the values in the new file; the file from which they were copied remains unchanged. This replaces all parameters of the entire sample information file, excluding any collected data from the other file.

Each of the individual tabbed dialogs contains a push button if you wish only to replace specific parameters and not the entire contents.

Comments Enter comments about the sample or its analysis conditions. Comments entered here are printed in the header of the reports.

Save Saves the information you have specified for this sample file.

Close Closes the dialog. If a file containing unsaved changes is open, you are prompted to save before the dialog closes.

Basic Displays the sample information file in the basic format.

5-6 Feb 06


Basic

When you open an existing sample information file or create a new one using the Basic for-mat, all parts of the file are contained on a single dialog. With the Basic format, you can quickly create a sample information file using previously defined parameter files. This format also allows you to switch to the Advanced format to view or edit parameters. Refer to Basic and Restricted Formats, page 4-7 for step-by-step instructions for creating a Basic sample information file.

If you are creating a new file, this dialog displays the defaults you specified in Sample defaults. Chapter 8 explains how to establish sample defaults.

Sample Displays the description of the file you are opening. If this is a new file, the description specified in sample defaults is displayed. You may enter a new description or add to the existing one.

Range: 50 alphanumeric characters

Mass Enter the mass of the sample to be analyzed.

Density Enter the density of the sample to be analyzed. This value is used only for the Calculated free-space method. An approximate value (± 2%) will provide sufficient free-space correction in most cases.

Feb 06 5-7


Degas conditions Click the down arrow to display a list of previously defined degas conditions files supplied with the analysis program, as well as any you may have created. Choose the Degas conditions file you wish to use.

These files are pertinent only if using the SmartPrep for degassing samples.

Analysis conditions Click the down arrow to display a list of previously defined analysis conditions files supplied with the analysis program, as well as any you may have created. Choose the Analysis Conditions file you wish to use.

Adsorptive properties Click the down arrow to display a list of previously defined adsorptive properties files supplied with the analysis program, as well as any you may have created. Choose the adsorptive properties file you wish to use.

Report options Click the down arrow to display a list of previously defined report options files supplied with the analysis program, as well as any you may have created. Choose the Report options file you wish to use.

Add Log Entry Displays the Add Log Entry dialog.

Use this dialog to enter information pertinent to the sample file. For example, if you are not using the SmartPrep for automatic degassing, you may wish to enter external degassing information. Any information you enter here is printed as part of the sample log report. You may make multiple entries by selecting this push button as many times as you wish.

5-8 Feb 06


Restricted Format

The Restricted format is used when analysis parameters must remain constant. For example, in the pharmaceutical industry where consistency and accuracy are crucial. A password is required to enter and exit this format. Refer to Restricted, page 8-3 for additional information on the Restricted format.

When you open an existing sample information file or create a new one using the Restricted format, the sample file editor is displayed in the same manner as the Basic. Some menu func-tions, however, are disabled and you cannot switch to the Advanced format to edit file parameters.

Replace All Allows you to copy all parameters of an existing sample file’s values into the sample information file you are creating. An “open file” dialog is displayed so that you may select the desired file. You may edit the values in the new file; the file from which they were copied remains unchanged and ready for the next use.

Save Saves the information you have specified for this sample file.

Close Closes the dialog. If a file containing unsaved changes is open, you are prompted to save before the dialog closes.

Advanced Displays the sample information file in the advanced format, allowing you to view or edit parameters.

Feb 06 5-9


Degas Conditions

The information contained in this dialog is automatically applied during the degassing proce-dure if you are using the SmartPrep Degasser for degassing your sample. If you are not using the SmartPrep, you can use this dialog for storing degassing information used with an external degassing unit.

Be sure to save this file to the directory you specified as the Parameter Files directory if it is to be included in the drop-down list of the Basic Sample Information dialog (see Parameter Files Directory in Chapter 8).

Description Displays the description of the file you are opening. If this is a new file, the description specified in sample defaults is displayed. You may enter a new description or add to the existing one

Range: 40 alphanumeric characters (at least one character is required)

Replace Allows you to copy the values of an existing degas conditions file into the current file. A dialog is displayed so that you may select the desired file. After the values are copied into the file, you may edit them as desired; the file from which they were copied remains unchanged.

Conditions Table Allows you to enter up to five stages of degas conditions.

Soak Temperature Enter the temperature at which the sample is to soak while flowing gas.

5-10 Feb 06


Temperature Ramp Rate

Enter the rate at which the temperature is to change when advancing to the soak temperature.

Soak Time Enter the amount of time to soak the sample.

Insert Inserts a row into the conditions table. A row is inserted above the selected line; the cursor moves to the new line.

Delete Deletes the selected row from the conditions table.

Clear Clears the table of all but one entry; one is required. The rows do not have to be selected.

Feb 06 5-11


Analysis Conditions

This dialog allows you to specify the analysis conditions for your sample. An analysis condi-tions file can be created as an independent parameter file or as part of the sample information file.


Description Displays the description of the file you are opening. If this is a new file, the description specified in sample defaults is displayed. You may enter a new description or add to the existing one

Range: 40 alphanumeric characters (at least one character is required)

Replace Allows you to replace the values in the current file with those from an existing file. A dialog is displayed so that you may select the desired file. After the values are copied in to the file, you can edit them as desired; the file from which they were copied remains unchanged.

5-12 Feb 06


Pressure Table Edit the existing pressure table or clear the table and enter values for a new pressure table.

A pressure table is a table of relative pressure points (and possibly calculation assignments) at which data (isotherms) are to be collected. The relative pressures may span the entire range of 0.00000001 to 0.995 P/Po. There must be one adsorption branch followed optionally by one desorption branch.

Several analysis conditions files containing complete pres-sure tables are included with the software; they are located in the PARAMS subdirectory. These files (and all other parame-ter files) can be changed. If you want to use any of these files, it is recommended that you use the Save As option on the File menu to save the file as a different name; then make your changes.

The pressure table for automatically collected data includes the pressure points for data collection (when Use calculation assignments is selected) and identifies calculations through which the data are processed. Refer to Summary Report, page 5-22 for a summary of the types of data generated for the Gemini.

Insert Range Displays the Insert Pressure Range dialog.

This dialog allows you to specify the starting pressure, the ending pressure, the number of points to insert within the specified range, and whether you wish to have linear or geometric progression.

Linear Inserts evenly spaced points into your table.

Feb 06 5-13


Geometric from low pressure

Inserts geometrically spaced points from the low pressure range. For example, to insert 5 points with a pressure starting at 0.01 and ending at 0.16, the following points are inserted into the table:

0.010.020.040.080.16

Geometric towards saturation

Inserts geometrically spaced points from the saturation pressure. For example, to insert 5 points with a 0.99 starting pressure and a 0.84 ending pressure, the following points are inserted into the table:

0.990.980.960.920.84

Insert Predefined Displays the Insert Predefined Pressures dialog.

Choose predefined pressure points for surface area, t-Plot micropore and/or BJH adsorption/desorption.

Click on the down arrow of each field to choose the desired set of points. You can also specify Adsorption/desorption total pore volume and saturation.

Insert Inserts a row into the pressure table. A row is inserted above the selected line; the cursor moves to the new line.

5-14 Feb 06


Delete Deletes the selected row.

Clear Clears the table of all entries except one; one is required. The rows do not have to be selected.

Use calculation assignments

Select this option to assign the points to be collected for each type of report.

If this option is not selected, each report (with the exception of Langmuir and BET) uses a range of pressures as selected in the report options. The Langmuir and BET reports interpo-late to entered relative pressures on the report options.

The outlier points can be selected so that they will not be reported

Preparation Displays the Analysis Preparation dialog.

Evacuation rate Allows you to enter a rate at which evacuation is to occur.

Evacuation time This is the hold time that the sample remains evacuated after reaching the specified evacuation rate, as well as the preliminary evacuation which takes place prior to the free-space measurement.

Free Space Displays the Free Space dialog allowing you to specify the type of free-space measurement desired.

Feb 06 5-15


None Choose this option for no free-space measurement.

Previously measured Choose this option to use the measurement from the previous sample. This choice is recommended when you are measur-ing a series of samples with similar volumes.

Measure Choose this option to have the free space measured.

Calculate The free-space value is calculated using the value entered for the Volume Correction (entered on the Unit Configuation dialog) and the nonideality factor (entered on the Adsorptive Properties dialog).

Enter Enables the Free Space field allowing you to enter a value.

Po and T Displays the Po and Temperature Options dialog.

Entered When you choose this option, the Po field is displayed so that you can enter the desired saturation pressure.

Most recent measured Choose this option to use the most recently measured satura-tion pressure (obtained using the Start Po Measurement option on the Unit menu).

Measure po foreach point

The Gemini V and Gemini VI share the same software. This option is applicable only for the Gemini VI.

Entered temp Enables you to enter the analysis temperature. This value is used when producing Dubinin reports.

5-16 Feb 06


Analysis Method Displays the Analysis Method dialog allowing you to choose the method you wish to use for the analysis.

Equilibrate With this method, the analyzer increases pressure in steps to the next specified level for data collection. It maintains this pressure and monitors volumes (or quantities) adsorbed. When the rate of adsorption (volume adsorbed during equili-bration time divided by total volume adsorbed) falls below 0.1%, equilibraiton is assumed to have occurred. The instru-ment then instroduces the next adsorbate gas dose.

When you choose this method, the Equilibration time field is enabled allowing you to enter the number of seconds between successive pressure readings during equilibration.

Scan This method applies to adsorption only. This method allows the adsorbate gas pressure to be raised continuously at a constant rate based on the pressures to be achieved and the length of the analysis.

When you choose this method, the Scan rate field is enabled allowing you to enter the length of the analysis.

Feb 06 5-17


Adsorptive Properties

This dialog allows you to specify the characteristics of the gases used. An Adsorptive proper-ties file can be created as an independent parameter file or as part of the sample information file.


Adsorptive Displays the name of the adsorptive gas for the file you are opening. If this is a new file, this field contains the default specified in Sample defaults. Enter the name of the desired adsorptive gas; you can use up to 40 alphanumeric characters.

Replace Allows you to replace the values in the current Adsorptive properties file with those from another file. A dialog is displayed so that you may select the desired file. You may edit the values in the new file; the file from which they were copied remains unchanged.

Mnemonic The mnemonic name for the adsorptive gas; for example, N2 for nitrogen, CO2 for carbon dioxide, etc.

Non-ideality factor Enter a factor to compensate for the forces of attraction between molecules in a real gas.

Density conversion factor Enter the density conversion factor for the adsorptive. The density conversion factor is determined by obtaining the ratio of the gas volume (STP) to the liquid volume.

Molecular cross-sectional area

Enter the molecular cross-sectional area of the adsorptive.

5-18 Feb 06


Report Options

This dialog allows you to specify report options. A report options file can be created as an independent parameter file or as part of the sample information file.


Description If you are opening an existing file, this field displays a description of the report options file. You may change the name if you wish.

If this is a new file, the default report options description is displayed. Enter a name for this file.

Maximum number of characters: 40

Show report title This option enables you to have a title appear on your report and provides a field for entering the title.

If this is a new file, the title you specified as the default is dis-played. You can accept the default title or enter a new one using up to 50 characters.

If you deselect this option, a title will not display on the report.

Feb 06 5-19


Show graphic Select this option to have a graphic display above the report title. The graphic can be in a bitmap (bmp) or an enhanced metafile (emf) format. For example, you may wish to display your company logo.

Click Browse to choose the graphic, then enter the height and width in the appropriate fields. This image can be edited from the report window.

Replace Allows you to replace the values in the current report options file with those from an existing file. A dialog is displayed so that you may select the desired file. You may edit the values in the new file; the file from which they were copied remains unchanged.

Overlays Displays the Graph Overlay Samples dialog.

Choose the sample files you wish to overlay onto selected plots.

Click Browse to the right of the Sample [n] field to choose a file. You may select up to eight files. After choosing your file(s), be sure to select the Overlay samples option for each report type you plan to overlay. Refer to Generating Graph Overlays, page 4-26 for step-by-step instructions on generat-ing overlays.

5-20 Feb 06


Selected Reports Contains a list of available reports:

• Summary• Isotherm• BET Surface Area• Langmuir Surface Area• t-Plot• BJH Adsorption*• BJH Desorption*• Dubinin*• MP-Method*• Options• Sample Log

*Not available with the Gemini V 2365

Use the mouse pointer or the arrow keys to move to the desired report, then double-click the left mouse button, or press Spacebar. A report is selected when it is preceded with a check mark; it is deselected in the same manner.

You can find examples of some of these reports in Chapter 7 beginning on page 7-22.

Edit Displays an associated dialog for the selected report. Editing options for available reports are shown in subsequent sections.

This button is disabled for the Options and Sample Log reports; the parameters for these reports cannot be edited.

Feb 06 5-21


Summary Report

The Summary report provides a condensed listing of data results. The Summary Report Options dialog allows you to choose the data to be included in the report.

All options on the Summary Report are available for the Gemini 2380; some are not available for the Gemini 2365.

If you choose Adsorption or Desorption total Pore Volume data the P/Po field is enabled so that you can enter the relative pressure at which to calculate the total pore volume. If Use cal-culation assignments (Collected Data screen) is not selected, the isotherm is interpolated to this value and that point used for the Total pore volume calculation. Otherwise, the point selected with calculation assignment is used.

Select All Selects all choices on the dialog, which is applicable only to the Gemini 2380.

Deselect All Deselects all choices on the dialog.

5-22 Feb 06


Isotherm Report Options

The Isotherm report indicates adsorption (up to saturation pressure) and desorption (down from saturation pressure) of a gas by a solid held at constant temperature.

The Gemini 2365 can collect data only on the adsorption isotherm and, therefore, can report only on the adsorption isotherm.

Select Reports Lists the types of reports offered.

Choices: Tabular Report, Linear plot, Logarithmic plot, Linear Absolute plot, Logarithmic Absolute plot

Pressure Composition plot

When you select Pressure Composition plot, the Adsorbate Molecular Weight field is enabled so that you can enter a value for the adsorbate. This plot is useful for plotting pres-sure as a function of Weight % adsorbed; for example, H2 adsorbed on carbon.

Options Displays the related Plot Options dialog; this example shows the dialog for the Linear plot.

All plot dialogs contain the same options.

Feb 06 5-23


Options(continued)

You can plot the graphs as a curve, points, or both.

Select Overlay samples to overlay data from the current plot with data from other samples. The other sample files are selected by clicking Overlays on the Report Options dialog.Autoscale options enable you to have the X- and/or Y-axes automatically scaled.

Linear X-axes begin at zero, and logarithmic X-axes begin at an appropriate value. Y-axes begin at zero. The system uses the highest values collected during analysis as the ending points for axes ranges.

If you choose not to autoscale data, the From and To fields are enabled, allowing you to specify a range. Data collected outside these ranges are not included in the plot.

The value entered in the To field must be greater than the value entered in the From field.

The X-axis fields show the relative pressure.The Y-axis fields show the quantity of gas adsorbed

Tabular Options Enables you to have Run Time and/or Time Between Points reported. Run time reports the time elapsed from the beginning of the analysis to the finish. Time between points reports the time relapsed between each point.

Also enables you to report Weight % when plotting pressure composition.

Volume Adsorbed Enables you to choose the manner in which the volume adsorbed is reported. These data are reported by default as Per Gram (cm3/g). However, you can choose to report data Per BET Surface Area (cm3/m2) or Per other Surface Area (m2/g). If the latter field is selected, a field is enabled allowing you to enter a value.

Weight The Adsorbate Molecular Weight field is enabled when you choose Pressure Composition plot, allowing you to enter the molecular weight of the adsorbate.

5-24 Feb 06


BET/Langmuir Surface Area Report Options

The BET calculation obtains the sample surface area value by determining the monolayer vol-ume of adsorbed gas from the isotherm data.

The Langmuir calculation determines the surface area of a sample by relating the surface area to the volume of gas adsorbed as a monolayer.

Displays as Langmuir Surface Area Report Options if the Langmuir report is being edited.

The Langmuir and BET Surface Area dialogs include the same fields; the operating instructions for both are the same.

Tabular report Select this option to have a tabular report of the plotted data.

BET (or Langmuir) Transform plot

Generates a traditional BET (Langmuir) surface area plot that is used to determine monolayer volume and BET C constant.

BET (or Langmuir) Isotherm plot

Uses the BET (Langmuir) monolayer volume and constant to produce an isotherm.

Overlay samples Allows you to overlay data of the selected type from the current plot with data from other samples. Click Overlays on the Reports Options dialog to choose the other samples.

Feb 06 5-25


Autoscale x-axis Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled automatically.

Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.

The X-Axis Range fields show the relative pressure.

The Y-Axis Range fields show the quantity of gas adsorbed.

From/To fields Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot. The value entered in the To field must be greater than the value entered in the From field.

Pressures Displays the Report Pressure Table dialog so that you may edit or enter relative pressure points.

• If Use calculation assignments is not selected on the collected/Entered dialog, the isotherm is interpolated to these pressure points, and those interpolated values are used in the BET calculations.

• If Use calculation assignments is selected, collected data are used.

Unavailable for Langmuir

5-26 Feb 06


Insert Predefined Displays the Surface Area Report Pressure Selection dialog, allowing you to select predefined points.

Choices: None, 1 point, 3 point, 5 point, 5 point low pressure

Insert Inserts a row into the table above the selected line; the cursor moves to the new line.

Delete Deletes the selected row.

Clear Removes all but the one required entry from the table. The rows do not have to be selected. A warning message requesting confirmation is displayed before the table is cleared.

Feb 06 5-27


t-Plot Report Options

The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to micropores. Matrix area, the area external to micropores, is directly determined and often proves to be a valuable way of chacterizing complex mixed materials.

Thickness Curve Presents the type of thickness curves available.

• Reference• Kruk-Jaroniec-Sayari• Halsey• Harkins and Jura• Broekhoff-de Boer• Carbon Black STSA

You can also apply the Frenkel-Halsey-Hill thickness curve using the Halsey option, and entering the appropriate values in the equation. Use Edit to edit the values in the equation.

Edit Displays the equation for the selected thickness curve so that you may view or edit the values.

5-28 Feb 06


Reference Displays the Entered t-Curve dialog allowing you to define a t-curve by entering the relative pressure and thickness values.

This table can also be created in another application if desired and imported into this dialog using Open. When creating the table in another application, the file must be saved as ASCII text with a THK extension. Use a two-column format with the relative pressures in the first column and the thickness values in the second column. Columns must be separated by a space (or a tab).

InsertInserts a row above the selected row. A row cannot be inserted if the value in the selected row is at its lowest value; values must be strictly increasing. For example, in the table shown above the default value is 0.000000001. Therefore, you must use Ctrl + Down Arrow to insert rows.

DeleteDeletes the selected row.

ClearClears the table of all but one entry; one entry is required.

Feb 06 5-29


Reference(continued)

OpenEnables you to import the values from an existing t-curve. One predefined curve is shipped with the analysis program and is found in the Referenc directory. The Referenc directory is defaulted when you select this push button.

Save AsDisplays the Save as T Curve dialog allowing you to save the current table of values under a different name.

Kruk-Jaroniec-Sayari Displays the Kruk-Jaroniec-Sayari Thickness Equation dialog.

You can edit the values for the numerator, the first element of the denominator, and the exponent.The range for a selected field is shown in the information bar at the bottom of the dialog.

Refer to Appendix B, page B-6, for additional information on all t-Plot calculations.

Halsey Displays the Halsey Thickness Equation dialog.

You can edit the values for the multiplier, numerator, and exponent. The range for a selected field is shown in the information bar at the bottom of the dialog.

You can also edit these values to use the Frenkel-Halsey-Hill thickness curve.

5-30 Feb 06


Harkins and Jura Displays the Harkins and Jura Thickness Equation dialog.

You can edit the values for the numerator, first element of the denominator, and exponent. The range for a selected field is shown in the information bar at the bottom of the dialog.

Broekhoff-de Boer Displays the Broekhoff-de Boer Thickness Equation dialog.

You can edit the values for the multiplier, numerator, and exponent. The range for a selected field is shown in the information bar at the bottom of the dialog.

Carbon Black STSA Displays the STSA Thickness Equation dialog.

All coefficients can be edited. The range for a selected field is shown in the information bar at the bottom of the dialog.

Surface Area group box Allows you to choose the surface area value used for thickness calculations. You can use BET (most commonly used), Langmuir, or enter one of preference.

Feb 06 5-31


Pressure Range Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report.

• If Use calculation assignments is not selected on the Collected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calculating the data for this report.

• If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Fitted Thickness Range Provides two fields, allowing you to enter the minimum and maximum thicknesses you wish to include in the thickness curve.

The values entered for the thicknesses can be expressed in angstroms or nanometers. Select Options > Data presentation to specify desired units.

Surface area correction factor

This value corrects for unsmoothed surface areas and brings the values for BET surface area and micropore surface area into accordance. For most samples, the default value of 1.000 is adequate.

Tabular report Select this option to have a tabular report generated.

t-Plot Select this option to have a graphical representation of data.

Overlay samples Allows you to overlay data from the current sample file with data from other sample file(s). Click Overlays on the Report Options dialog to choose the other samples.

5-32 Feb 06


.

Autoscale x-axis Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled automatically.

Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points.

If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.

From/To fields Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.

The value entered in the To field must be greater than the value entered in the From field.

The X-Axis Range fields show the relative pressure

The Y-Axis Range fields show the quantity of gas adsorbed

Feb 06 5-33


BJH Adsorption/Desorption Report Options

The BJH calculation determines the mesopore volume/area distribution which accounts for both the change in adsorbate layer thickness and the liquid condensed in pore cores. You can generate BJH reports from adsorption and desorption data.

BJH reports are not available for the Gemini V 2365.

This field does not display on the BJH Desorption dialog

The BJH Adsorption and Desorption dialogs include the same fields; the operating instructions for both are the same.

Thickness Curve Type Presents the type of thickness curves available.

• Reference• Kruk-Jaroniec-Sayari• Halsey• Harkins-Jura• Broekhoff-de Boer• Carbon Black STSA (ASTM D-6556-0lA)

You can also apply the Frenkel-Halsey-Hill thickness curve using the Halsey option, and entering the appropriate values in the equation. Use Edit to edit the values in the equation. Halsey is the default thickness curve and typically is used for BJH calculations.

5-34 Feb 06


An incomplete pore distribution may be generated if you select a thickness curve which is not a good match for your sample.

Edit Displays the equation for the selected thickness curve, allowing you to view and edit, if desired, the parameters. Refer to t-Plot Report Options, page 5-28 for an explanation of this push button.

Minimum/Maximum BJH Provides fields for entering the minimum and maximum size pore to be included in BJH reports.

The size can be reported in width (default), radius, or diameter. Select Options > Data Presentation > Units to specify desired unit.

Fraction of pores open at both ends

(not displayed on desorption dialog)

During adsorption calculations, the software assumes that all pores are closed at one end. Sometimes a percentage of pores may be open at both ends, causing disagreement in the adsorption and desorption data or in the values for total volume and total BJH pore volume. In this field, you may enter the fraction of pores open at both ends to compensate for this error.

This field is not shown on the BJH Desorption Report Options dialog.

Adsorptive Displays the BJH Adsorptive Options dialog.

The recommended adsorptives and their values are shown. You may specify up to six additional adsorptive/adsorbate property factor combinations.

Feb 06 5-35


Adsorptive(continued)

The adsorbate property factor is the combination of constants in the numerator of the BJH equation which is specific to the type of gas used. Adsorbate property factors may be specified in angstroms or nanometers. Select Options > Data presentation to specify units.

Smooth differentials Smooths all differential calculations, eliminating variations in the differential computation caused by noise in the input data.

BJH Correction Enables you to choose the type of correction to apply to calculations. The type you choose will be displayed in the report header.

Standard Uses original BJH models.

Kruk-Jaroniec-Sayari Good for reference thickness curves.

Faas Good for statistical thickness curves.

Pressure Range Displays the Report Relative Pressure Range dialog (example shown on page 5-32) so that you may enter the range of pressures to use with this report.

• If Use calculation assignments is not selected on the Collected/Entered dialog, all of the non-outlier points of the collected data within the specified range are used for calculating the data for this report


5-36 Feb 06


Selected Reports Contains a list of available BJH reports:

• BJH Tabular Report• Cumulative Pore Volume• dV/d* Pore Volume• dV/dlog(*) Pore Volume• Cumulative Pore Area• dA/d* Pore Area• dA/dlog(*) Pore Area

* = width, radius, or diameter

Choose a report by double-clicking on the report name or highlight the report name and press the Spacebar. A report is selected when it is preceded with a check mark. Reports are deselected in the same manner.

You can measure pore width (w), pore radius (R), or pore diameter (D) for BJH reports. Select Options > Data presentation from the Main Menu to choose the desired measurement.

Edit Allows you to edit the selected report. Editing options for available reports are shown in the subsequent sections.

Feb 06 5-37


Tabular Report

Click Edit for the BJH Adsorption/Desorption tabular report to specify the method of data reduction; the BJH Adsorption (or Desorption) Tabular Report Options dialog is displayed.

Fixed pore size table This option allows you to specify exact pore sizes for which volume or area data are reported. Only the pore sizes within the specified range are reported. Click Table to enter or edit a fixed pore size table.

Collected points Choose this option to include all relative pressure points collected by the system.

Columns Displays the BJH Adsorption (or Desorption) Tabular Report Column Options dialog.

The default column title appears next to the column number. Each column includes a pull-down list of the data types available for inclusion in the report. You can measure pore width, pore radius, or pore diameter.

5-38 Feb 06


Table Enabled when you choose Fixed pore size table. Displays the BJH Adsorption (or Desorption) Fixed Pore Size Table dialog so that you may enter or edit a fixed pore size table.

The fixed pore size table must contain a minimum of two points and may include as many as 1000. The points must be strictly decreasing.

Insert Inserts a row into the pressure table. The row is inserted above the selected row and the cursor moves to the new row.

Delete Deletes the selected row from the pressure table.

Clear Clears all points from the pressure table; none have to be selected.

Feb 06 5-39


Plot Options

Click Edit for BJH Adsorption/Desorption plots to specify plotting methods and to customize plots.

A dialog similar to the following is displayed when you select a BJH plot.

Plot Options Lists the data presentation styles available for BJH plots. You may choose to plot as a curve, points, or both.

X-axis Lists the scale options for the x-axis.

Linear/Logarithmic Choose whether you wish to have the X-axis on a logarithmic or linear scale.

Autoscale Select this option to have the x-axis scaled automatically. The lowest and highest values collected during analysis are used as the beginning and ending points.

When you deselect this option, the adjacent fields are enabled so that you can specify beginning and ending values.

Data ranges are displayed in the information bar across the bottom of the dialog when a cursor is in a numerical data field.

Y-axis Lists the options for the y-axis.

Variable Choose the desired variable for the Y-axis.

Valid ranges display here.

5-40 Feb 06


Overlay Displays a list of overlay choices. You may choose to overlay the current plot with data from other samples or with other plots from this sample.

Autoscale Select this option if you wish to have the y-axis scaled automatically. The lowest and highest values collected during analysis are used as the beginning and ending points.

When you deselect this option, the adjacent fields are enabled so that you can specify beginning and ending values.

Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data field.

Feb 06 5-41


Dubinin Report Options

The Dubinin report is not available for the Gemini V 2365.

Report Type Allows you to specify the type of report you wish to generate. At least one type of report must be selected.

Select Radushkevich to generate the Radushkevich report.

Select Astakhov to generate the Astakhov report. With this choice, you may select Optimize exponent. If you do not select this option, the Exponent value field is enabled so that you can enter a value.

Refer to Appendix B, page B-18 for additional information.

Fitted relative pressure range

Enables you to specify minimum and maximum limits on relative pressures included in the line fit. Data collected outside these limits are not included in the line fit.

Selected Reports Lists the available Dubinin reports. Choose a report by double-clicking on the report name or highlight the report name and press the spacebar. A report is selected when it is preceded with a check mark ( ).

The following reports are available:

• Dubinin Tabular Report• Transformed Isotherm• dV/dW Pore Volume (Astakhov only)

Displayed only if Astakhov is selected.

5-42 Feb 06


Adsorptive Allows you to specify up to eight adsorptive/affinity coefficient (beta) combinations. The Dubinin Adsorptive Options dialog is displayed.

Pressure Range Displays the Report Relative Pressure Range dialog (example shown on page 5-32) so that you may specify minimum and maximum relative pressures to use with this report.

• If Use calculation assignments is not selected on the Collected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calculating the data for this report.


Feb 06 5-43


Tabular Report

Selecting Dubinin Tabular Report from the Dubinin Report Options dialog enables you to customize your report with one to six columns of data for Astakhov reports and one to five columns of data for Radushkevich reports. The Dubinin Tabular Report Column Options dia-log is displayed.

The default column title appears next to the column number. Each column includes a drop-down list of the data types to include in the report.

*The value for n (shown in Column 5) is the optimized exponent if Optimized Astakhov exponent is selected on the Dubinin Report Options dialog. If not, then the value for n is the t value entered in the Exponent field.

5-44 Feb 06


Transformed Isotherm Plot

Selecting Transformed Isotherm from the Dubinin Plot Option dialog enables you to restrict the line fit to a portion of the isotherm. The Dubinin Transformed Isotherm Plot Options dia-log is displayed.

Overlay samples Select this option to overlay the current plot with data from other samples. Then click Overlays on the Report Options dialog to choose the sample files.

Autoscale x-axisAutoscale y-axis

Select these options to have the X- and/or Y-axes automatically scaled. Both axes begin at zero; the system uses the highest values collected during analysis as the ending points for axes ranges.

If you choose not to autoscale data for either (or both) axis, the corresponding fields are enabled so that you may enter a beginning and ending value.

The X-axis shows the quantity of gas adsorbed at standard temperature and pressure.

The Y-axis shows the log of relative pressure.

Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

Feb 06 5-45


Pore Volume Plot

When you select dV/dw Pore Volume from the Dubinin Report Options dialog, the Dubinin dV/dw Pore Volume Options dialog is displayed.

This plot is available only when Astakhov is selected o the Dubinin Report Options dialog.

Plot options Choose to plot curve, points, or both.

Overlay samples Select this option to overlay data from other samples. Then click Overlays on the Report Options dialog to choose the files.

Autoscale x-axisAutoscale y-axis

Select these options to have the X- and/or Y-axes automatically scaled. Both axes begin at zero; the system uses the highest values collected during analysis as the ending points.

If you choose not to autoscale data for either (or both) axis, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot.

Data ranges are displaye din the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.


5-46 Feb 06


MP-Method Report Options

The MP-Method report is not available for the Gemini V 2365.

Pore size can be expressed in Angstroms or nanometers. Select Options > Data Presentation > Units to secify desired unit.

Thickness Curve Select the thickness curve type from this group box. You must choose either the Halsey equation or the Harkins and Jura equation. Use Equation to edit the values in the equation.

Equation Displays the equation for the type of thickness curve selected.

Harkins and Jura Displays the Harkins and Jura Thickness Equation dialog.

You can edit the values for the numerator, first element of the denominator, and exponent.

Feb 06 5-47


Halsey Displays the Halsey Thickness Equation dialog.

You can edit the values for the multiplier, numerator, and exponent.

Selected Reports Lists the available MP-Method reports. Choose a report by double-clicking on the report name or highlight the report name and press the spacebar. A report is selected when it is preceded with a check mark ( ).

The following reports are available:

• MP Tabular Report • Cumulative Pore Volume• dV/dw Pore Volume • Cumulative Pore Area• dA/dw Pore Area

The data for these reports are measured in pore width only.

5-48 Feb 06


Tabular Report

Selecting MP Tabular Report from the MP-Method Report Options dialog enables you to customize your report with up to four columns of data; columns 1 and 2 are fixed. The MP-Method Tabular Report Column Options dialog is displayed.

The default column title appears next to the column number for columns three through six. Columns 3 through 6 include a pull-down list of the data types to include in the report.

The MP-Method reports hydraulic radius only. If you select Pore size in diameter from the Data presentation menu, the MP-Method still reports pore size in radius.

Feb 06 5-49


Plot Options

Selecting an MP-Method plot option from the MP-Method Report Options dialog enables you to specify the plotting method used for your report and to customize the plot. The following plots are available:

• Cumulative Pore Volume• dV/dw Pore Volume• Cumulative Pore Area• dA/dw Pore Area

When you select any of these plots from the MP-Method Report Options dialog, a dialog sim-ilar to the following one is displayed. The fields on all dialogs are the same.

Plot options Choose to plot a curve, points, or both.

X-Axis Choose Autoscale to have the x-axis scaled automatically. The X-axis begins at zero and the system uses the highest values collected during analysis as the ending point.

If you deselect Autoscale, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot.



5-50 Feb 06


Y-Axis Variable Click on the down-arrow to choose a variable for the Y-axis.

Overlay You can use the choices in this drop-down list to overlay plots. You can choose a different type of plot for the current sample to overlay with the listed Variable, or you can choose Samples to overlay the variable plot with the same type of plot from other samples. Click Overlays on the Reports Options dialog box to choose the samples.

Autoscale Choose this option to have the y-axis scaled automatically. Y-axes begin at zero. The system uses the highest values collected during analysis as the ending points for axes ranges.

If you deselect this option, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot.

Y-axis range fields show the volume of gas adsorbed.


Feb 06 5-51


Options Report

The Options report is a subset of the contents report; it provides pertinent information for the following:

• Degas conditions• Adsorptive properties• Analysis conditions• Free space• Saturation pressure (Po)• Analysis method• Isotherm collection

Sample Log Report

The Sample Log report displays the following:

• Information entered using Add Log Entry on the sample file editor• Warnings and/or errors which occurred during analysis

5-52 Feb 06


Collected/Entered Data

An “Entered” dialog is added to the Advanced Sample Information file when Manually entered is selected as the type of data.

The Collected Data dialog is displayed after an analysis has been completed.

Pressure table For collected data, columns for the following are displayed:

• absolute pressure• relative pressure• quantity adsorbed• outliers (if Use calculation assignments is not selected)• calculation assignments for each requested report option

(if Use calculation assignments is selected)

For entered data, columns for the following are displayed:

• absolute or relative pressure, depending on the selection in the Pressures group box

• quantity adsorbed

Insert Enabled only for entered data. Inserts a row into the pressure table.

Delete Enabled only for entered data. Deletes the selected row.

Feb 06 5-53


Clear Enabled only for entered data. Clears the entire table; rows do not have to be selected.

Use calculation assignments

If selected, allows you to assign the points to be collected for each report type.

If deselected, each report (with the exception of Langmuir and BET) uses a range of pressures as selected in the report options. The Langmuir and BET reports interpolate to entered relative pressures on the report options.

The outlier points can be selected so that they will not be reported.

Po and T Displays the Po and Temperature Options dialog.

This dialog allows you to edit the values for the saturation pressure and the analysis temperature. Refer to page 5-16 for an explanation of the options on this dialog.

Free Space Displays the Free Space dialog, allowing you to view the isotherm using a different value for the free space.

The isotherm is redrawn each time values are edited.

5-54 Feb 06


None Select this option to have no free space values appear on the printed report.

Measured Select this option to view the isotherm for a measured free space.

Calculated Select this option to use a calculated free space. The free-space value is calculated using the volume correction entered on the Unit Configuation dialog and the nonideality factor entered on the Adsorptive Properties dialog.

Entered Select this option to enter a free-space value for the isotherm.

Feb 06 5-55

Save Gemini V Windows

Save

Save enables you to save any changes you have made to the file in the active window. The file is saved under its current name.

Save As

Save As enables you to:

• save a sample or parameter file in the active window under a different name. This option is useful for making a duplicate copy of a file that you can modify as desired without changing the original one. The original file remains open when you use this function, so be sure to open the new file before making any changes.

• save a subset (parameter) of the sample file in the active window as a standalone parameter file. For example, select Analysis Conditions from the Save As menu to cre-ate a standalone parameter file of the analysis conditions portion of the active sample file.

• save as an ASCII file (t-Curve) the relative pressures and corresponding thicknesses. These data are derived by dividing the condensed volume of adsorptive by the selected surface area. The density conversion factor in the adsorptive properties file is used to convert quantity adsorbed to volume of condensed adsoptive.

A dialog similar to the one shown below is displayed when you select the Save As command.

Enter a file name (up to eight characters) in the File name field; the appropriate extension is appended automatically when you click OK. The new file is saved as specified, but does not remain in the active window. Be sure to open the new file before making any changes to the file.

5-56 Feb 06

Gemini V Windows Save All

When saving t-Curve files, the Save As t-Curve dialog is shown first, allowing you to select the type of curve.

Save All

Save All enables you to save all open files under their current names. This option provides a faster way to save all open files at one time and avoids having to perform a Save operation on each individual file.

Close

Close enables you to close the file in the active window. The following message is displayed if changes have been made to the file:

(File name) has been changed. Save changes before closing?

Yes No Cancel

Click Yes to save the changes and close the file.

Click No to discard the changes and close the file.

Click Cancel to return to the open file.

Close All

Close All enables you to close all open files under their current names. The message shown above for Close is displayed for each file in which changes have been made. The same actions apply.

Feb 06 5-57

Print Gemini V Windows

Print

Print enables you to print the contents of a sample or parameter file. You can choose multiple files by holding the Ctrl key while making your selections. Regardless of which file type you select, a dialog similar to the one shown below is displayed.

File name The name of the file you select from the Files list box is copied to this field.

Destination Contains a drop-down list of the available print destinations.

If you select Screen or Printer, the requested file is sent to that specified destination.

If you select File, the requested file is converted to a text file which can be viewed with a text editor or other text file manipulation tools. You also must enter a name in the File name field of the Settings group box (or accept the default).

Copies Enabled when you select Printer as the destination, enabling you to print up to four copies.

StatusDate RangeFilesDirectories

These options are explained in Selecting Files on page 3-6.

File name Enabled when you select File as the destination. A default name is displayed in the field; you may enter a new one if you wish.


5-58 Feb 06

Gemini V Windows List

List

List enables you to generate a listing of the following information on a selected sample or parameter file.

• File name• Date the file was created (or last edited)• Time the file was created (or last edited)• File identification• File status

The List dialog is common to all file types. The title bar displays the type of file on which you have requested a list.

File name If you select only one file from the Files list box, the name is copied to this field. If multiple files are selected, the last one selected displays in this field.

You may request a list of multiple files by holding down Ctrl while selecting the files. If no files are selected, a list is generated for all files in the Files window.




Feb 06 5-59

List Gemini V Windows



If you select File, the requested file is converted to a text file which can be viewed with a text editor or other text file manipulation tools. You also must enter a name in the File name field of the Settings group box (or accept the default).


File name Enabled when you select File as the destination. A default name is displayed in the field; you may enter a new one if you wish.

5-60 Feb 06

Gemini V Windows Export

Export

Export allows you to copy the isotherm data in a sample information file and reformat it in an ASCII format acceptable to other programs, such as spreadsheets. The output file consists of four columns containing the absolute pressure, relative pressure, specific quantity absorbed, and the elapsed time.

Select File > Export from the main menu; the Export Sample File dialog is displayed.

File name The name of the file you select from the Files list box is copied to this field. You can export multiple files by holding down Ctrl while selecting the files.





If you select File, the File name field is enabled so that you can enter a name for the exported file (or accept the default).


Feb 06 5-61

Export Gemini V Windows

File name Enabled when you select File as the destination. When you choose a file, its name is automatically inserted; however, you can edit the name if desired.

5-62 Feb 06

Gemini V Windows Convert

Convert

Convert enables you to convert StarDriver files (MGD extension) to a format compatible with the Gemini Windows program. The only files that will display in the Files window are those with the MGD extension.

Files window Displays the StarDriver files in the current directory (the current directory is shown just above the Directories window). Refer to page 3-8 for information on navigating to other directories.

Destination Displays the current directory and the name of the selected file with an SMP extension. If you wish to save the file in a different directory, be sure to enter (or navigate to) the desired directory. You can choose multiple files by holding down Ctrl while selecting the files.

Date RangeFilesDirectories


Feb 06 5-63

Exit Gemini V Windows

Exit

Exit enables you to exit the Gemini Windows program. If an analysis is in progress, it will continue until completion; analysis data are collected and stored in an embedded controller.

• If a window containing a modified file is open, the following message is displayed:

(File name) has been changed. Save changes before closing?

Yes No Cancel

Click Yes to save the changes and close the file.

Click No to discard the changes and close the file.

Click Cancel to return to the open file.

• If an analysis is in progress, the following message is displayed:

2459- An instrument is busy. A delay in restarting this applicaiton could result in loss of new data. Continue with program exit?

Yes No

Click Yes to exit the analysis program.

Click No to return to the analysis program and allow the analysis to continue.

Although data are stored in an embedded controller when you exit the program, data are not saved to disk in the computer until you reopen the program and save the data. If a power failure occurs and the analyzer does not have an Uninterruptible Power Supply (UPS), any unsaved data are lost.

5-64 Feb 06


6. UNIT MENU

The Unit menu contains the options for the operations which can be performed with the Gem-ini analyzer. A Unit menu is included for each attached analyzer. For example, if you have two analyzers, the main menu contains two Unit menus. For easy differentiation, the status dis-plays associated with each unit are displayed in different colors. The unit number and the serial number also are displayed in the title bar of the operational windows. This is especially convenient if you have more than one analyzer attached to the same computer. You can attach up to four Geminis to one computer.

Description

Listed below are brief descriptions of the Unit menu options. Detailed descriptions are found later in this chapter.

This menu does not appear on the menu bar if the analysis program is being used for offline data operations on a computer other than the one controlling the analyzer.

Start analysis Enables you to perform an analysis. Page 6-2.

Start Po measurement Allows you to measure the saturation pressure. Page 6-5.

Show Instrument Schematic

Displays a schematic of the Gemini analyzer, allowing you to monitor operation. Page 6-6.

Show Status Displays only the status portion of the operational window for the selected unit. Page 6-8.

Show instrument log Displays a log of recent analyses and error messages. Page 6-9.

Unit configuration Displays software version and the hardware configuration. Also allows you to enter a value for the volume correction. Page 6-11.

Feb 06 6-1

Start Analysis Gemini V Windows

Start Analysis

Use this command to begin an analysis. When you select this option, the Analysis dialog is displayed with all fields disabled (greyed) and the Start Analysis dialog positioned on top. This allows you to select a sample file for your analysis or to create a new one.

After a sample file has been selected, the Analysis dialog is displayed. The fields contain the values for the selected file or, if creating a file, the specified defaults.

You can continue to schedule analyses by clicking Next (appears after the current analysis is finished) on the analyzing view of the Analysis dialog.

View Allows you to choose the view you wish to display in the window.

Operation displays the current mode of operation.

Instrument Log displays a list of recent analyses and mes-sages (or errors). Refer to Show Instrument Log, page 6-9 for additional information.

Instrument Schematic displays a schematic of the Gemini analyzer. Refer to Show Instrument Schematic, page 6-6 for additional information.

Browse Click to choose a different sample information file; the Open Sample Information dialog is displayed allowing you to select the file.

Sample Displays an identification of the sample file.

6-2 Feb 06

Gemini V Windows Start Analysis

Mass Displays the value entered for the sample’s mass; this value can be edited if desired.

Density Displays the density of the sample specified in the sample information file. This value is applicable only if using a mea-sured free space; it is ignored for other types of free space.

Po Displays the entered, or most recently measured, saturation pressure.

Evacuation rateEvacuation time

Displays the evacuation rate and time specified in analysis conditions.

Free space Displays the applicable Free space value. If the Free space was entered, this field is enabled allowing you to edit the value if desired.

Report After Analysis Enables you to have a report generated automatically after the analysis; displays the Report Settings dialog so that you may specify output options.

Start Starts the analysis. After data points start to collect, displays an analyzing view of the Analysis dialog.

Feb 06 6-3

Start Analysis Gemini V Windows

Cancel Cancels an analysis; enabled only when an analysis is in progress.

Start On this view of the Analysis dialog box, this push button changes to Next when analysis finished.

Next Returns you to the first view of the Analysis dialog box so that you may start another analysis.

Close Closes the Analysis dialog.

6-4 Feb 06

Gemini V Windows Start Po Measurement

Start Po Measurement

Use this command to measure the saturation pressure; the P0 Measurement dialog is displayed.

As prompted in the dialog, verify that a sample tube is attached to the sample port and that it does not contain a filler rod, then simply click Start to begin the measurement.

At the end of the measurement, the dialog closes automatically. The value obtained is stored and recorded on the Unit Configuration dialog as the most recently measured Po, which is available for subsequent sample analyses. The Po option is selected from the Analysis Condi-tions dialog (Advanced format).

Feb 06 6-5

Show Instrument Schematic Gemini V Windows

Show Instrument Schematic

Select this option to display a schematic of the Gemini analyzer. This schematic is a graphic representation of the plumbing system, including system valves, the analysis and balance tube stations, and the Dewar/elevator position.

Represent system valves; refer to the table below. The state of the valve can also be determined quickly by color, where:

white = closedgreen = open

Valve Description1 Vacuum valve2 Adsorptive valve3 Helium valve4-s Analysis reservoir valve4-b Balance reservoir valve5-s Analysis port valve5-b Balance port valve

Open Closed

6-6 Feb 06

Gemini V Windows Show Instrument Schematic

The lower portion of the schematic also displays analysis details (refer to Show Status in the following section).

Represents the reservoir; one for the Balance tube (left side) and one for the sample tube.

Represents the servo valve; one for the balance port (left side) and one for the sample port.

Represents the Volume Adsorbed transducer (upper) and the differential pressure transducer.

The reading for the Volume Adsorbed transducer is dis-played just above its symbol.

The reading for the sample pressure transducer is displayed just below the analysis servo valve (5-s).

Represents the balance volume adjustment. The balance volume can be adjusted only by a Micromeritics service representative.

Represents the pressure relief valve. This valve prevents excessive pressure build-up in the event of abnormal operation.

Represents the balance tube (left side) and the sample tube.

Represents the position of the elevator/Dewar.

Feb 06 6-7

Show Status Gemini V Windows

Show Status

A status window is shown across the bottom of all operational dialogs as well as the instru-ment schematic. The Show Status option enables you to show only the status window. This frees up your computer screen allowing you to perform other tasks (such as creating or editing sample files), while still monitoring the progress of your analysis.

If you have multiple instruments attached to your computer, the status window for each instru-ment is displayed in a different color.

Analysis status bar Shows the progression of the analysis. This bar contains three stages:

• Preliminary: evacuation and free-space measurement; displays green during progression

• Analysis: data are collected; displays blue during pro-gression

• Termination: the Dewar lowers and analysis terminates; displays grey during progression.

Analysis details The following analysis details are displayed:

Sample: Sample file nameStage: Stage of the analysis (as in status bar)Last Point: Last point and number of points requestedP: Absolute pressure of last pointP/Po: Relative pressure of last pointQ: Quantity adsorbedPo: Absolute pressure of last measured or entered saturation pressure (Po)Run Time: Elapsed time since the start of analysis

Step details Provides details of the current step of the analysis.

6-8 Feb 06

Gemini V Windows Show Instrument Log

Show Instrument Log

Displays a log of recent analyses and messages (or errors). This information is logged for a period of 30 days.

Analysis Message

These options allow you to choose which entries are displayed in the window.

Add Log Entry Enables you to enter information to include in the sample log that is not automatically recorded by the system.

Report Displays the Log Report Settings dialog so that you can specify report output options.

Use the Start Date field to specify a date at which to start the printout. You can specify a date using one of the following methods:

• Highlight the field (or press F2 to clear the field) and type in the desired date

• Double-click in the field (or press F4) to display a calen-dar to choose a date

• Press F2 to clear the field, then F3 to insert the current date

Feb 06 6-9

Show Instrument Log Gemini V Windows

Report(continued)

Select the number of reports desired in the Number of Reports field; you may print up to 4. This field is disabled if you are printing to a File or to the Screen.

Choose the report destination in the Destination field. If you choose File as the destination, the File name field is enabled, allowing you to enter a name for the printed file (or you may accept the default).

6-10 Feb 06

Gemini V Windows Unit Configuration

Unit Configuration

Select this option to display hardware/software configurations and the volume correction for the selected analyzer. When you select this option from the Unit menu, the Unit Configuration dialog is displayed.

Configuration Displays the number of the port being used to control the analyzer and the serial number of the selected analyzer.

Software Versions Displays the version of the software card and the version of the application software.

Last measured Po Displays the value for the last measured saturation pressure.

Volume Correction Displays the volume correction of the attached Gemini analyzer. If a different value is entered in this field, it is stored with sample data at the beginning of the analysis. The value is this field is used in a calculated free space.

Init BB-RAM Deletes all stored analysis data and resets instrument parameters to factory defaults. It does not affect sample and parameter files.

Feb 06 6-11


7. REPORTS MENU

This chapter describes:

• how to start reports, page 7-3• how to close and open reports, page 7-5• the appearance of reports, page 7-14• manipulation tools for onscreen reports, page 7-14

It also contains examples of some of the reports available, page 7-22.

Reports can be generated for data:

• collected on a sample that has completed analysis

• collected on a sample that is currently being analyzed (includes only the information collected up to the time of the report)

• that is manually entered

Description

Listed below are brief descriptions of the commands contained on the Reports menu. Detailed descriptions follow this section.

Start report Allows you to generate a report on a completed sample analysis or on the data collected thus far for an analysis in progress. Page 7-3.

Close reports Closes all open report window(s). Page 7-5.

Open Report Enables you to open a report that was saved from the report window.

Feb 06 7-1

Description Gemini V Windows

SPC Report Options Allows you to specify the sample data to be included in SPC reports. Page 7-6.

Regression Report Allows you to generate a regression report. Page 7-7.

Control Chart Allows you to generate a control chart report. Page 7-11.

7-2 Feb 06

Gemini V Windows Start Report

Start Report

Select this option to generate a report on a sample analysis; the Start Report dialog is displayed.

File name The name of the sample file you select from the Files list window is copied to this field. If you select multiple files, the last one selected is displayed. If you have a sample file open, its name defaults to this field.

• If you select multiple files on which to have reports gen-erated, the reports specified in each sample file are printed to the output destination.

• If you choose a single file, the Select Reports dialog con-taining the available reports is displayed. This dialog allows you to choose the reports you wish to generate.

Feb 06 7-3

Start Report Gemini V Windows

File name(continued)

Select (or deselect) reports by double-clicking on the desired report (reports are selected when they are preceded with a check mark). Alternatively, you can hightlight the report and press the Spacebar.

Status This drop-down list determines what type of sample files are displayed in the Files list window in the specified directory for all dates, or within the specified range of dates (using push button).

Choices: All, Analyzing, Complete, Entered

Refer to Table 3-2. File Status and Description, page 3-8 for a description of the status types.

Date Range Displays the Select Dates dialog so that you may specify a range of dates. Refer to Selecting Files, page 3-7 for a description of this push button.

Copies Enabled when the Printer destination is chosen, allowing you to print up to four copies of the selected report(s).

Destination Displays a drop-down list of output destinations. You can print to a printer, to the screen, or to a file.

If you select Printer, requested reports are printed to the selected printer. This option also enables the Copies field allowing you to print up to four copies of each report.

If you select Screen, reports are displayed onscreen. Using this option allows flexibility for manipulating and customiz-ing reports. Refer to Onscreen Reports, page 7-14.

If you select File, the tabular reports of the requested file are converted to a text file which can be viewed with a text editor or other text file manipulation tool.

File name Enabled when you select File as the destination. Allows you to enter a name, or you may accept the default.

Files list box Displays a list of the available sample files for the choice shown in the Status field and within the range of dates specified in the Date Range dialog.

Directories Displays a list of available drives and directories. The drive and directory last accessed is displayed immediately above the Directories list box. Refer to page 3-8 for information on navigating to other directories.

7-4 Feb 06

Gemini V Windows Close Reports

Close Reports

This option enables you to close all open report windows at one time. This avoids having to select close on each report window.

Open Report

This option enables you to open a report that was saved from the Report window; the Report window opens with an Open dialog positioned on top.

After you navigate to the desired directory, select your file, and click Open, your report is dis-played in the Report window.

Report Window

Feb 06 7-5

SPC Report Options Gemini V Windows

SPC Report Options

When you select SPC Report Options, the SPC Calculations dialog is displayed.

The SPC Calculations dialog lists the variables available for SPC reporting. You can check as many as desired. However, for efficiency, it is best to select only the variable you actually intend to us. All variables selected must be computed for each sample file used in an SPC report.

Some SPC report parameters are not available for the Gemini V 2365; for example, the Dubinin reports.

7-6 Feb 06

Gemini V Windows Regression Report

Regression Report

Select this option to generate a regression report. The regression report is used to determine the interdependency between two variables. Up to three dependent variables (Y-axis) may be plotted against a single independent variable (X-axis). The degree of correlation between the variables also is reported. The graphs for the regression report are scaled so that all three fit on a single page. If you choose less than three, the graphs are scaled to fill most of the page.

Show report title Select this option to have a title display on your report. Accept the default or enter a new title. You can enter up to 40 alphanumeric characters.

Deselect this option to omit the report title.

Show graphic Select this option to have a graphic display above your report title. For example, you may wish to display your company logo. The graphic must be a bitmap (bmp) or enhanced meta-file (emf).

Click Browse to choose the file, then use the Height and Width fields to specify a size. This image can be edited in the report window (when printed to the screen), or removed if desired.

Feb 06 7-7

Regression Report Gemini V Windows

X- and Y-Axes Variable fields

Allows you to designate the X- and Y-axes variables. Click on the down arrow to display a list of variables. The vari-ables in this list are the ones you specified in the SPC report options.

With this option, you can plot the regression of up to three Y-axis variables against the X-axis variable. The X-axis speci-fies the independent variable for the regression, while the Y-axes provide the dependent variables.

Axis Range Enables you to specify the beginning and ending values for the X- and Y-axis ranges. Data collected outside these ranges are not included in the plot. These fields are disabled if you choose Autoscale.

Autoscale Allows you to have the X- and/or Y-axes scaled automati-cally. When scaled automatically, both axes begin at zero. The analysis program uses the highest values collected during analysis as the ending points.

Tabular report Enables you to generate tabular, as well as graphical, data of the included samples. A tabular report contains the numeric values contributed by each sample.

Label data Allows you to label the points on the plot to correspond with the values in the sample files.

Samples Displays the Regression Report Sample Selection dialog, allowing you to choose the sample files you wish to have reported.

7-8 Feb 06

Gemini V Windows Regression Report

File name Use this field to limit the files displayed in the Available Files pane. For example; enter a*.smp to display only the files beginning with an a.

Status This drop-down list determines the type of sample files that display in the Available Files pane in the selected directory for all dates, or within the specified range of dates (using Date Range push button). Refer to Table 3-2. File Status and Description, page 3-8 for an explanation of the Status types.

Date Range Displays the Select Dates dialog so that you can specify a range of dates. Refer to Selecting Files, page 3-7 for an explanation of this dialog.

Use all files inthis directory

Select this option to include all files from the selected direc-tory in the report.

Directories Lists the current directory. Use the directory window to nav-igate to a different directory. Refer to page 3-8 for information on navigating to other directories.

Add Moves the selected file in the Available Files pane to the Selected Files pane. Alternatively, you can simply double-click on the desired file(s). You can select multiple files by holding down Ctrl while making your selections. You can include up to 200 sample files.

Feb 06 7-9

Regression Report Gemini V Windows

Remove Removes the selected file from the Selected Files pane and places it back into the Available Files pane.

Save As Default Saves the current definition of the report as the default.

Recalculate archived SPC results

Select this option to have archived SPC values recalculated. This ensures that any changes made to the SPC Report Options are included in the new report; however, it does lengthen the time required to generate the report.

Report Settings The options in this group box enable you to choose output criteria.

The Copies field is enabled when you choose Printer as the destination, enabling you to print up to four copies of the report.

Report Generates the report.

7-10 Feb 06

Gemini V Windows Control Chart

Control Chart

This option enables you to generate a control chart report which plots the changes in a statistic.

Show report title Select this option to have a title display on your report. Accept the default or enter a new title. You can enter up to 40 alphanumeric characters.

Deselect this option to omit the report title.

Show graphic Select this option to have a graphic display above your report title. For example, you may wish to display your company logo. The graphic must be a bitmap (bmp) or enhanced meta-file (emf).

Click Browse to choose the file, then use the Height and Width fields to specify a size. This image can be edited in the report window (when printed to the screen), or removed if desired.

X-axis Order By Enables you to choose the order in which X-axis statistics are placed. You can have them placed by Time, File name, Date, Minutes, and Days.

Feb 06 7-11

Control Chart Gemini V Windows

Graph [n] Displays the Control Chart Graph [n] Options dialog, allowing you to define the Y-axis of each graph.

Statistic This drop-down list displays the SPC variables selected on the SPC Report Options dialog. The variable you choose will be plotted against time.

Autoscale Allows you to have the Y-axis scaled automatically. If you wish to specify a range, deselect this option and enter a range in the From and To fields.

Center Line Displays placement options for the variable’s optional value. Choose Entered to specify placement of the line.

Limit Lines Displays the options available for limiting lines. You can have the lines placed at some multiple of the standard devi-ation or at specified positions (Entered).

When you select Entered, the High limit and Low limit fields are enabled, allowing you to enter appropriate values.

Tabular report Allows you to generate tabular, as well as graphical, data of the included samples. A tabular report contains the numeric values contributed by each sample.

Recalculate archived SPC results

Select this option to have archived SPC values recalculated. This ensures that any changes made to the SPC Report Options are included in the new report. It also lengthens the time required to generate the report.

Samples Displays the Control Chart Sample Selection dialog, allowing you to choose the sample files on which you wish to report.

7-12 Feb 06

Gemini V Windows Control Chart

This dialog functions in the same manner as the Regression Report Sample Selection Dialog explained earlier in this chapter. Refer to page 7-9 if you need assistance on the fields of this dialog.

Save as Default Saves the current definition of the report as the default.

Report Settings The options in this group box enable you to choose output criteria.

The Copies field is enabled when you choose Printer as the destination, enabling you to print up to four copies of the report.

Report Generates the report.

Feb 06 7-13

Printed Reports Gemini V Windows

Printed Reports

Header

All printed reports (either to the screen or to a printer) contain a header displaying file statistics.

• Tabular and graphical reports contain sample and instrument statistics such as date and time of analysis, analysis conditions, and so forth.

The headers for these reports also contain notes of any changes to the sample file that occur after analysis.

• Summary report headers contain the same type of information displayed in tabular and graphical reports with the exception of notes.

Onscreen Reports

The report window containing onscreen reports provides many options for customizing and manipulating reports:

• a tool bar• shortcut menus• zoom feature• axis cross hairs

When reports are printed to the screen, they are printed in a window like the one shown below. Each requested report is listed in the Reports window on the tool bar; they are also indicated by selectable tabs across the top of the report header. To view a specific report, select its tab or select the report in the Reports window and click Show.

Tabs display for each type of report you choose to generate.

Options on Tool Bar

List of reports requested

Header

Displays graphical (or tabular) data

7-14 Feb 06

Gemini V Windows Printed Reports

Tool Bar

Reports Contains a list of all requested reports.

Show Shows the selected report in the report window. If the report has been hidden, it and its associated tab will become visible.

Delete Deletes the selected report. A deletion confirmation dialog is displayed since this function cannot be undone. The deleted report(s) will have to be regenerated if deleted in error.

Hide Hides (removes) the selected report from the report window. The report’s associated tab is also removed.

Open Allows you to open a previously saved report file.

Print Displays a print dialog so that you can choose an appropriate printer for report output. A list of available reports is displayed in the window on the right side of the dialog.

Feb 06 7-15


Print(continued)

For convenience in selecting which reports to print, push buttons are provided beneath the report window. Or, you can make your selection by clicking on the desired reports.

Current selects the report displayed in the report window.

Shown selects only the shown reports; any unhighlighted reports indicate they are hidden. You can still select hidden reports from this window to print.

All selects all reports, including those that may have been hidden.

Clear clears all selections.

Save Saves all reports of the currently open file in a report format using the same name as the sample file, only with an rep extension. If you wish to specify a name and/or specific reports to save, use the Save As push button.

Save As Saves all or specified reports from the currently open file. The push buttons displayed on this dialog perform in the same manner as the print dialog (explained above).

Reports can be saved in three different formats:

Report system (*.rep): Saved in a format which allows you to reopen the file using the push button on the Report win-dow tool bar.

Spreadsheet (*.xls): Saved in a format which can be imported into most spreadsheet programs.

Ascii Text (*.txt): Saved in ASCII text which can be imported into programs accepting this type of file.

7-16 Feb 06


Default Style Displays the Default Style dialog so that you can specify default parameters for report fonts and curve properties.

Font Contains a list of report elements for which the font can be edited. Simply highlight the desired element and click Edit; a font dialog is displayed, enabling you to specify the desired font and attributes.

Curve The items in this group box enable you to specify a thickness for report curves and, when using histograms, the type of fill to apply.

Graph borderline thickness

Enables you to specify a thickness for the border of the graph.

Load Loads the last saved defaults.

Save Saves the changes as the defaults. If you do not click Save, the changes will apply to the current report set only. The next reports will revert to the defaults.

Close Closes the Default Style dialog and applies the changes. If you clicked Save, the changes become the defaults. If you did not click Save, the changes apply to the current report set

Close Closes the report window.

Feb 06 7-17


Shortcut Menus

Shortcut menus are accessed when you right-click on the tabular or graphical portion of a report.

Tabular Reports

Resize column Displays a dialog so that you can specify the width of the selected column (in inches).

Rename column Displays a dialog so that you can edit the name of the selected column. Use Ctrl + Enter to insert line feeds.

Move column Allows you to move the location of the selected column to the left or to the right.

Align column Enables you to right-align, left-align, or center the data in the selected column.

Hide column Displays a list of all columns, enabling you to select the one you wish to hide.

Show column Displays a list of all hidden columns, enabling you to select the one you wish to have shown again.

Column font Displays a Font dialog, allowing you to change font attributes for the tabular data in the current report.

Header font Displays a Font dialog, allowing you to change font attributes for column headers in the current report.

Edit title Allows you to edit the table title and font.

Copy table as text Enables you to copy the entire table (column headers and data) and then insert it into another program. Colums are tab-delimited, allowing easy alignment.

7-18 Feb 06


Graphs

Autoscale Autoscales all axes of the graph. This function is useful for returning to a full view after having zoomed in.

Redraw Sets axis boundaries to its original view. You can also use this function to remove cross-hairs.

Show curve Shows any curve(s) that has been hidden. This option is disabled (greyed) if no curves have been hidden.

Hide curve Hides (removes from view) any unwanted curve(s).

Edit curve Displays the Curve Properties dialog, allowing you to edit curve properties.

Title Displays the title of the curve you are editing.

Feb 06 7-19


Style Drop-down list containing styles in which collected data can be displayed.

Choices: Curve, Histogram, Points, Curve and Points

Curve group box Contains options for curves and points. You can edit the curve interpolation, the style of curve and/or points, as well as the pen color. The options in this group box are disabled if Histogram is chosen in the Style drop-down list.

Histogram group box Allows you to specify the type of fill as well as the color if Histogram is chosen as the style for collected data.

Edit axis Displays the Axis Properties dialog, allowing you to edit axis properties.

Title Enables you to edit the name and/or of the title for the selected axis.

Scale Enables you to edit the scale and its properties.

Gridlines Enables you to edit the gridlines for the selected axis.

Edit legend Displays the Legend Properties dialog, allowing you to edit the placement of the legend.

7-20 Feb 06


Zoom Feature

A zoom feature is included with the report system so that you can zoom in to examine fine details. To use this feature, simply hold down the left mouse button and drag the mouse cursor (drawing a box) across the area you wish to view; then release the button. The enlarged area immediately fills the graph area. Right-click in the graph area and choose Autoscale or Redraw from the shortcut menu to return to the normal view.

Axis Cross Hair

A cross-hair function is available so that you can view axis coordinates. To use this feature, simply left-click in the desired area of the graph.

Right-click in the graph area and choose Autoscale or Redraw from the shortcut menu to remove cross-hair lines and return to the normal view. Or, you can click outside of the graph area.

Edit title Displays the Title Properties dialog, allowing you to edit the current graph’s title and font.

Copy as metafile Copies the graph and places it on the clipboard, allowing you to paste it into other applications accepting Windows metafiles.

Copy as text Copies the data used to generate the graph as a series of tab-delimited columns of text.

X-axis position

Point of Coordination Y-axis position

Feb 06 7-21

Report Examples Gemini V Windows

Report Examples

The remainder of this section contains samples of some of the reports which may be generated by the Gemini Windows program. Most of the reports can be varied through entries on the report options screens.

Isotherm Plot

7-22 Feb 06

Gemini V Windows Report Examples

BET Surface Area Report

Feb 06 7-23


t-Plot Report

7-24 Feb 06


BJH Adsorption Pore Area

Feb 06 7-25


BJH Adsorption Pore Volume

7-26 Feb 06


Options Report

Feb 06 7-27


Summary Report

7-28 Feb 06


Sample Log Report

Feb 06 7-29


OPTIONS MENU

The Options menu contains options which allow you to configure the system to your labora-tory’s requirements. With the options on this menu, you can:

• Choose between basic, advanced, or restricted mode, page 8-12• Edit program defaults, page 8-6• Specify data presentation modes, page 8-4• Specify a directory for predefined parameter files, page 8-12

Description

Listed below are brief descriptions of the options contained on the Options menu. Detailed descriptions follow this section.

Option presentation Allows you to display the sample file dialog in Advanced, Basic, or Restricted format. Page 8-12.

Units Allows you to choose the types of units to use for measurement, pressure, and temperature. Page 8-4.

Graph Grid Lines Enables you to choose the types of grid lines to display for the X- and Y-axes. Page 8-5.

Sample defaults Allows you to specify defaults for the parameters contained in the sample information and parameter files. Page 8-6.

Parameter files directory Allows you to specify a location for the predefined parameter files used by the Basic and Restricted formats. Page 8-12.

Service Test Mode Enables you to perform certain troubleshooting procedures. This option is available only under the direction of a Micromeritics service representative. Page 8-2.

Feb 06 8-1

Option Presentation Gemini V Windows

Option Presentation

The sample editing dialogs for the Gemini Windows program may be presented in three differ-ent formats: Advanced, Basic, or Restricted.

Each format displays sample information and menu options differently.

• Advanced: displays all parts of the sample information file in a tabbed dialog similar to that of an index card file. Clicking on each tab opens an associated dialog. Use this format to edit parameter files or create customized sample files.

• Basic: displays all parameters of the sample file in a single dialog. Use this format to create sample files using previously created parameter files. The Basic format also allows you to switch to the Advanced format to view or edit file parameters.

• Restricted: displays in the same manner as the Basic format. This format also is used to create sample files using previously created parameter files. However, you cannot switch to the Advanced format to edit parameters. You must also use a password for entering and exiting this format.

Advanced

The Advanced format presents all parts of the sample information file in a tabbed dialog. For example, if you wish to open or create a sample file using the Advanced format, the following dialog is displayed.

The Advanced format is used to create customized sample files — easily and quickly. You can also switch to the Basic format, if desired, by clicking Basic. Refer to Advanced, page 5-5 for a description of the fields on this dialog.

If you are opening a Completed (used in an analysis) file, this dialog also contains a tab for Collected or Entered Data.

8-2 Feb 06

Gemini V Windows Option Presentation

Basic

The Basic format presents the sample information file and its parameter files in a single dia-log. For example, if you wish to open or create a sample information file using the Basic format, the dialog is displayed in this manner.

The Basic format is used to create sample information files using previously defined parame-ter files. You can easily switch to Advanced format, if desired, by clicking Advanced. Refer to Basic, page 5-7 for a description of the fields on this dialog.

Restricted

The Restricted format is identical to the Basic format, except that certain menu options are disabled, and you cannot switch to the Advanced format. This format is password-protected and is typically used in laboratories where analysis conditions must remain constant, for exam-ple, in the pharmaceutical industry.

When you select Restricted, a dialog requesting a password is displayed:

Any password (up to 31 characters) can be used to enable the Restricted format. The same password, however, must be used to exit the Restricted format. For example, if you enter “password” to enable the Restricted format, then you must use “password” to exit. If you for-get the password, open the system INI file and navigate to the Private section. The current password will be shown immediately following “OptionPresentationPassword.” Make a note of the password, exit the INI file, and enter the password where requested. Do not attempt to delete the password in the INI file.

This push button does not display when in the Restricted format.

Feb 06 8-3

Units Gemini V Windows

Units

This menu command displays the Units Selections dialog which allows you to choose the manner in which to display units of measurement, pressure, and temperature.

The choices default to the standard IUPAC units.

8-4 Feb 06

Gemini V Windows Graph Grid Lines

Graph Grid Lines

Graph Grid Lines enables you to choose the type(s) of grid lines to show on your reports; the Graph Grid Lines dialog is displayed.

X-AxisY-Axis

Enables you to choose Major and/or Minor lines to display in printed reports for the Logarithmic and Linear scales.

If you deselect these items (remove the check marks), your report will not display grid lines.

Grid Line Style Allows you to choose to the type of grid line to display if grid lines are being shown.

Feb 06 8-5

Sample Defaults Gemini V Windows

Sample Defaults

This option allows you to specify default parameters for sample information files. This option is presented in two formats: Advanced and Basic. Select Options > Option presentation to choose the format you wish to use. Alternatively, you can switch between the two formats using the Advanced / Basic toggle push button displayed on the lower right side of the screen.

Basic

When you select Sample defaults while using the Basic format, Basic Sample Defaults dialog is displayed.

The defaults you specify for the Basic format also serve as the defaults for the Restricted format.

Sequence Specify a default sequence for the sample file name. The number you specify is sequenced incrementally each time you create a sample file. It is the number that appears in the File name field when you select File > Open > Sample information.

• Use numbers, letters, or other printable characters, such as dashes. At least three numbers must be included.

• Use up to eight characters.

• The Gemini program prohibits using such characters as * or ?.

8-6 Feb 06

Gemini V Windows Sample Defaults

Sample Allows you to enter an additional identification that provides more information than the sample file name alone.

In the field on the left, edit the prompt for Sample if you wish. For example, you may prefer to use Test or Material. The maximum number of characters is 20.

In the field on the right, specify a format for the sample identification.

• Use numbers, letters, or other printable characters, such as dashes.

• Maximum number of characters is 42, plus the $ symbol.

• Include the automatically generated file name as part of the identification by using the $ symbol where you want the sequence number to appear.

For example, if the sequence number is 000-001, enter the sample identification as follows:

Lab #25 - $

The resulting sample identification for the first sample information file would be:

Lab #25 - 000-001

and the second:

Lab #25 - 000-002, and so on.

Mass Enter a default value for the sample mass (weight). This value can be edited in the sample information file.

Density Enter a default value for the density of the material you most commonly analyze.

Degas ConditionsAnalysis ConditionsAdsorptive PropertiesReport Options

Each parameter contains a drop-down list containing files of that type which were included with the software, as well as any you may have created. Choose the file you wish to use as the default.

Feb 06 8-7


Advanced

The Advanced Sample Defaults dialog resembles a set of index cards. The values you specify in the parameter portions of the sample file (Degas Conditions, Analysis Conditions, Adsorp-tive Properties, and Report Options) are saved as the defaults for newly created parameter files.

For example, after specifying defaults for a sample file in the Advanced format:

• Select File > Open > Sample Information, then click Yes to create the file, and the defaults you specify display for all parameters.

• Select File > Open > Analysis Conditions, then Yes to create the file, and the defaults you specify in the Analysis Conditions portion of the Advanced Sample Defaults dia-log display in the fields.

Replace all Allows you to replace all parameters of the default sample file you are creating with parameters from an existing sample file. For example, you may have an existing sample file that contains most (or all) of the parameters that you wish to use. You can even change the values in these files (if needed) without affecting the file from which they were copied.

Save Saves the specified defaults.

Close Closes the dialog.

8-8 Feb 06


Sequence Allows you to specify a default sequence for the sample file name. The number you specify is sequenced incrementally each time you create a sample file. It is the number that appears in the File name field when you select File > Open > Sample information.

• Use numbers, letters, or other printable characters, such as dashes. At least three numbers must be included.

• Use up to eight characters.

• The Gemini application prohibits using such characters as * or ?.

Sample Allows you to enter an additional identification that provides more information than the sample file name alone.

In the field on the left, edit the prompt for Sample if you wish. For example, you may prefer to use Test or Material. The maximum number of characters is 20.

In the field on the right, specify a format for the sample identification.

• Use numbers, letters, or other printable characters, such as dashes.

• Maximum number of characters is 42, plus the $ symbol.

• Include the automatically generated file name as part of the identification by using the $ symbol where you want the sequence number to appear.

For example, if the sequence number is 000-001, enter the sample identification as follows:

Lab #25 - $

The resulting sample identification for the first sample information file would be:

Lab #25 - 000-001

and the second:

Lab #25 - 000-002, and so on.

Feb 06 8-9


OperatorSubmitter

Allow you to enter the name (or other identification) of the operator performing the analysis and the name of the person, department, customer, etc. that submitted the sample for analysis.

The fields on the left can be edited to display something other than Operator and Submitter if desired.

The fields on the right allow you to specify default names or titles.

• Include the automatically generated file name (number) as part of the identification by using the symbol $ where you want the sequence number to appear. Refer to the example in the previous section.

• Maximum number of characters for the prompt is 20.

• Maximum number of characters for the identification is 42, including the $ symbol.

• Omit this item entirely from the sample information file by selecting Omit.

Mass Enter a default value for the sample’s mass. This value can be edited in the sample file.

Density Enter a default density; this value is used only when the calculated free-space method is used. This value can be edited in the sample information file.

Comments Allows you to enter comments about the sample or its analysis conditions. Anything you enter in this window is printed in the report header.

Add Log Entry Allows you to enter comments about the sample or its analysis conditions. Anything you enter using this option appears in the Instrument Log Report; it does not display in the report header.

8-10 Feb 06


Click on each remaining tab of the Advanced Sample dialog to establish parameter defaults. Refer to Chapter 5 beginning on page 5-10 for assistance on parameter dialogs.

Replace All Allows you to replace the contents of all parameter files contained in the current default sample file with those from an existing sample file. For example, you may have an existing sample file that contains most (or all) of the parameters that you wish to use. You can click this push button, choose the file, and then click OK. All parameter files of the file you choose are copied into the sample defaults dialog. You can edit the values if required without affecting the file from which they were copied.

Feb 06 8-11

Parameter Files Directory Gemini V Windows

Parameter Files Directory

This option allows you to select the location for the predefined parameter files displayed in the drop-down lists on the Basic Sample Information dialog.

When you select this option, the Parameter File Directory Selection dialog is displayed.

The directory specified here is the one you should use when creating parameter files to be included in the drop-down lists on the Basic sample information dialog. It is where the soft-ware goes to obtain the files for the drop-down lists. If parameter files are not saved to this directory, they are not included in the lists.

Service Test Mode

Various service tests are included in the Gemini operating program. These tests can be per-formed only with the assistance of a trained Micromeritics service representative. When you select Service Test Mode from the Options menu, a dialog box prompting you to enter a pass-word is displayed. This password will be provided by your service representative. You will not be able to perform these tests without his guidance.

8-12 Feb 06

Gemini V Windows Troubleshooting

9. TROUBLESHOOTING AND MAINTENANCE

This chapter describes common operational problems and their solutions, and maintenance procedures. If further assistance is needed after following the procedures in this chapter, con-tact a Micromeritics service representative.

Troubleshooting

Operating problems encountered with the analyzer are usually easily corrected. Typical prob-lems and the steps required to correct them are described in the following table.

Table 9-1. Common Operational Problems

What Happened Why What to Do

Unit does not work when power switch is turned on.

Power cord not fully inserted at one end or the other.

Insert power plug firmly into power source and analyzer power connector.

No power at outlet. Plug in lamp or small appliance to test outlet. If there is no power, contact electrician.

Plug prongs bent so that contact not made at outlet.

Gently move power plug at outlet while watching power indicator light. If indicator light comes on, have electrician replace outlet or plug.

Power cord damaged. Have electrician check cord using a test meter. Replace the cord if defective.

Loose internal connection or broken wire.

Call a Micromeritics service representative for repair or replacement information.

Specified pressure not reached or not maintained.

Sample or balance tube not properly attached.

Reattach sample and balance tubes, making sure both are securely attached to ports. Replace O-rings if they are defective (page 9-4).

Feb 06 9-1

Troubleshooting Gemini V Windows

Table 9-1. Common Operational Problems (continued)

What Happened Why What to Do

Helium or nitrogen drained from tank.

Leaks in the gas line connection. Pressurize the system. Close, then open the Shut-Off Valve on the gas bottle. If the needle on the pressure gauge on the gas bottle jumps abruptly, a leak in the gas line connection may be indicated. Check all gas line connections (refer to Setting up the Analyzer on page 2-2 for connection instructions).

Liquid nitrogen boils away too quickly to complete an analysis.

Dewar damaged. Replace Dewar.

Lengthy analysis. Refill Dewar about once an hour during analysis using the funnel provided.

9-2 Feb 06

Gemini V Windows Maintenance

Maintenance

Cleaning the Analyzer

The exterior casing of the analyzer may be cleaned using a clean cloth, dampened with isopro-pyl alcohol (IPA), a mild detergent, or a 3% hydrogen peroxide solution.

Recovering from a Power Failure

The analyzer has a battery back-up feature that saves entered data in case of power failure. Sample file parameters and any other data entered will still be present when power is restored. If an analysis was in progress when the power failure occurred, it will be canceled when the analyzer restarts. Any data collected during the analysis will still be present, but the analysis should be started again in order to produce complete results.

Do not immerse the analyzer or the power cord in any liquids. Doing so could result in electrical shock to personnel or damage to the unit.

Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in damage to the unit

Feb 06 9-3

Maintenance Gemini V Windows

Replacing Analysis Port Frit and O-Ring

A 40-µm frit is located in the analysis port of the analyzer. If the frit is contaminated, the con-taminant may adsorb or desorb during analysis, affecting the results. A contaminated frit on the analysis port may be indicated by a leak or by a free space reading much lower than nor-mal. The balance port also contains a frit, but it is a different size and does not need to be replaced.

A contaminated frit should be replaced as follows:

1. Remove the sample tube fitting from the analyzer using a wrench. Pry out the frit and O-ring.

2. Replace the frit and O-ring. Carefully reassemble the sample tube fitting and tighten by hand. Then tighten with a wrench to prevent leaks.

Do not interchange the frit from the balance (left) side because it is much more restrictive and the instrument will not run properly if these frits are not correctly placed.

40-µm Frit

Ο−ring

Sample Tube Fitting

To avoid degassing problems, the frit and O-ring should be clean and should not be touched with bare hands.

9-4 Feb 06

Gemini V Windows Maintenance

Performing a Blank Analysis for Diagnostic Purposes

A simple means of pinpointing operational problems in the Gemini is performing a blank anal-ysis. Leaks, as well as electronic problems will result in an unsatisfactory blank analysis. Perform this test before you begin detailed troubleshooting. The data produced during the blank analysis can be very helpful in identifying the cause of a problem. For this reason, we recommend that you perform this test, as described below, before calling your Service Repre-sentative and provide him a copy of the results.

1. Install blank, straight-wall sample tubes (free of cracks or chips) of the same size in the sample and balance ports. Be sure that the O-rings are present and are in good condition.

2. Place a Dewar of water at ambient temperature on the elevator.

3. Create a sample file for the blank tube analysis:

a. Select File > Open > Sample Information.

b. Click OK, then Yes to create the file; the Sample Information dialog is displayed.

c. Click Replace all; the Open Sample Information Dialog is displayed.

d. Choose the sample file titled, blankr.smp (Blank Tube Test), then click OK to display the Sample Information dialog box. For your convenience this sample file has been included with the analysis program and contains the appropriate values for a blank tube test.

The following procedure is performed using water at ambient temperature in the Dewar.

Blank Straight-Wall Sample Tubes

Dewar Containing Water

Feb 06 9-5

Maintenance Gemini V Windows

e. Edit the Description if desired; for example, you may wish to add the date to the current description of Blank Tube Test.

f. Click Save, then Close.

4. Select Unit > Start analysis; the Analysis dialog is displayed with the Start Analysis positioned on top.

5. Choose the sample file you created, then click OK; the Analysis dialog is fully displayed.

6. Click Report After Analysis and select Report after analysis. Choose Screen or Printer as the destination, then click OK.

7. Click Start on the Analysis dialog to begin the blank tube analysis.

8. Review the analysis results for acceptability. They should be within the tolerances shown in the following table. If these results are not achieved, call your Service Representative.

P/Po Tolerance in cm3

0.1 ±0.0080.2 ±0.0100.3 ±0.0120.4 ±0.0140.5 ±0.0160.6 ±0.0180.7 ±0.0200.8 ±0.0220.9 ±0.024

9-6 Feb 06

Gemini V Windows

10. ORDERING INFORMATION

The Gemini components and accessories can be ordered using one of the following method:

• Call our Customer Service Department at (770) 662-3636• Access our web site at www.micromeritics.com• Contact your local sales representative

When ordering, please use the information provided in this chapter to place your order:

Part Number Item and Description

060-00023-00 FlowPrep 060 Degasser (Requires gas regulator)

061-00023-00 VacPrep 061 Degasser (Requires a vacuum pump and gas regulator)

065-00000-00 SmartPrep 065 Degasser

004-61064-00 Dewar, 600 mL

240-25853-00 Powder Funnel, polypropylene

004-25846-00 Powder Funnel, aluminum

021-00000-00 Liquid Nitrogen Transfer System, Model 021

200-25879-00 Liquid Nitrogen Funnel

238-33001-00 Gemini Windows package; includes software and operator’s manual

238-42801-00 Operator’s manual

004-62230-58 Gas Regulator, CGA 580, 30 psig, for helium or nitrogen

004-33602-00 Pressure Relief Valve Kit, recommended for both gas supplies

236-61707-01 Sample Tube, 1.6 cm (5/8 in.) OD bulb x 1.35 cm (0.53 in.) ID x 1.52 cm (6 in.)

236-61702-00 Sample Tube, 1.9 cm (3/4 in.) OD bulb x 15.5 cm (6.1 in.) long - sample capacity: 6 cm3

236-61703-00 Sample Tube, 0.95 cm (3/8 in.) OD x 15.5 cm (6.1 in.) long - sample capacity: 2 cm3

004-27046-00 Frit, for sample tube, 40 µm

004-27024-00 Frit, for balance tube, 2 µm

236-14701-00 Sample Tube Rack

004-32004-00 Sample Tube Stopper

004-54611-00 Sample Tube Brush, 8-mm diameter, for straight wall sample tubes

004-54612-00 Sample Tube Brush, 25-mm diameter, for bulb sample tubes

Feb 06 10-1

Gemini V Windows

Part Number Item and Description

004-25022-00 Sample Port O-ring, Size 012, 3/8-in. ID

236-61704-00 Filler Rod, 7 mm (1/4 in.) x 146.1 mm (5.75 in.)

236-61705-00 Filler Rod, 7 mm x 101.6 mm (4 in.)

236-61706-00 Filler Rod, hanging, 7 mm (1/4 in.) OD

236-61708-00 Filler Rod, hanging, 13 mm (1/2 in.) OD

008-16045-00 High Vacuum Grease

062-00000-11 Vacuum Pump, 110/120 V

062-00000-23 Vacuum Pump, 220/240 V

062-33002-00 Oil Vapor Trap, for Vacuum Pump

004-16003-01 Vacuum Pump Oil, 1 Liter

280-32800-00 Weighing Support

004-16833-00 Reference Material, Carbon black, SA~23.8 m2/g

004-16818-00 Reference Material, Glass, SA~5.8 m2/g

004-61065-00 Glass Beads, 3 mm diameter, 90 grams

236-33601-00 Extended Operating Supplies

130-50000-00 Multivolume Pycnometer 1305

133-00000-00 AccuPyc 1330 Pycnometer, 10 cm3



236-33004-00 Hanging Filler rod Kit; contains two connectors with hooks, two filler rods, and installation instructions

236-33005-00 PrepSeal Accessory Kit; for degassing and transferring air-sensitive samples to an analysis port without contamination.

238-33011-00 CFR Part 11 Confirm; enables you to meet requirements which apply to the FDA 21 CFR Part 11 rule with regard to security, audit trails, etc. Includes software and operator’s manual

202-33024-00 DataMaster Program; for offline data reduction. Includes software and operator’s manual.

003-20616-03 RS-232 cable, 9-pin, female-to-female, straight-thru (a cable is required for each Gemini attached to the computer)

003-20690-00 USB Expander kit, for adding ports to accommodate multiple instruments being attached to one computer

10-2 Feb 06

Appendix A Gemini V Windows

A. ERROR MESSAGES

Error messages for the are listed numerically. If the Action response instructs you to contact your service representative, record the error message and make backup copies of any files involved in the operation.

2400 Series

2430- Error accessing file (file name), error code = (number).

2431- Error writing file (file name), error code = (number).

Cause A: Diskette may be damaged.

Action A: Clean the diskette drive. If this does not eliminate the problem, attempt operation using a backup copy of the file.

Cause B: Hard disk may be damaged.

Action B: Contact your service representative.

Cause C: A software error occurred when the file was accessed.

Action C: Contact your service representative.

Cause D: The name specified contains one or more invalid characters.

Action D: Enter a valid DOS filename (refer to your operating systems manual).

Cause: The hard disk does not have enough space left to perform the operation.

Action: Copy files not used regularly from the hard disk to diskette, delete them from the hard disk, and then try the operation again.

Feb 06 A-1

Gemini V Windows Appendix A

2432- Invalid response from MMI ‘FILE_READ’ request.

2433- New entries have been found in this directory. Refresh the directory information?

2434- File (file name) — Subset # (number) wrote wrong amount of data.

2436- Path specification (path name) is invalid.

2437- File (file name) does not exist.

Cause: An internal processing and/or hardware error has occurred.

Action: Contact your service representative if you continue to receive this error message.

Cause: Several files have been added to this directory by some function other than the Gemini program.

Action: Select Yes to update the directory information with data from each new file. This operation may take a minute.

Select No if you do not want to spend the time updating the directory information. This option may be feasible if a large number of files have been copied into the directory and you know the name of the file you wish to access.



Cause: You entered an invalid path name and/or extension.

Action: Type a valid path name (including the proper extension) and press Enter.

Cause: You entered a file specification that does not exist.

Action: Enter an existing file specification or select a file name from the list box.

A-2 Feb 06


2438- Disk drive (letter): is inaccessible.2439- Could not register file.2440- Subset not found.2441- Seek within file failed.2442- Bad header in subset file.2443- Subset owner denied access.2444- Not a valid file format.2445- Subset wrote the wrong amount of data.2446- Error reading data.2447- Error writing data.

2448- File directory (path name) is invalid. Resetting to the installation directory.

2449- This field does not contain a valid file specification.

2458- An instrument is performing a critical operation. Wait a few moments before exiting the application.

Cause: An unexpected error occurred when you tried to access a data file.

Action: Contact your service representative.

Cause: A working directory specified in the .INI file is invalid. The directory may have been deleted or moved to a different location.

Action: The installation directory will be substituted. The next time you open a file, use the Directories list to move to the correct directory.

Cause: You entered an invalid file name.

Action: See the description of file naming conventions in your DOS or Windows manual and re-enter the name.

Cause: You are attempting to exit the application while the instrument is per-forming a critical operation. This operation must be completed before the application can be stopped.

Action: Wait a short time and attempt to stop the application again.

Feb 06 A-3


2459- An instrument is busy. A delay in restarting this application could result in loss of new data. Continue with program Exit? (Yes, No)

2461- No instruments are in operation. This application will unconditionallyterminate.

2477- Unit n - S/N: nnnn did not properly initialize.

2480- File <name> cannot be analyzed. It is currently being edited.

Cause: You are attempting to exit the application while an analysis is in progress. While this is possible, the data collected while the application is inactive will not be permanently recorded until the application is re-started. A power failure to the instrument could cause some data to be lost.

Action: If you are not concerned with the potential for loss of data should a power failure occur, select Yes to continue; otherwise select No.

Cause: At least one instrument must be active for the application to operate. The initialization of all of the instruments configured with the Setup program has failed. The application stops.

Action A: Usually this message is preceded by another message giving the reason for the instrument’s failure to initialize. See the instructions for that mes-sage.

Action B: Ensure that the instrument is attached to the computer on the commu-nications port configured with the Setup program. Verify that the instru-ment has the power switch in the ON position. If the application continues to fail in its attempts to initialize the instrument, contact your service representative.

Cause: The software was unable to initialize this instrument; this is usually caused by one of the conditions listed in the error messages above.

Action: Correct the problem as described above, then restart the application.

Cause: You are trying to start an analysis using a file that is open for editing.

Action: Finish editing the file, save and close it, then start the analysis.

A-4 Feb 06


2481- Error accessing the sample information file <name>.

2484- The edit session for <name> must be saved before the analysis. Save changes and continue with the analysis? (yes, no)

2486- Could not construct (name) report type. Program will terminate.

2487- Could not start report generator. Error code (number). Program will terminate.

Cause: An unexplained error prevents you from accessing this file.

Action: The hard disk drive may be corrupt. Run diagnositics.

Cause: You attempted to start an analysis using a file that contains unsaved changes and is open for editing.

Action A Click Yes to save the changes and proceed with the analysis.

Action B: Click No to cancel the analysis and complete editing of the sample file.

Cause A: You may not have full rights to the application’s folders and files.

Action A: Contact your system administrator to have full rights granted.

Cause: B An internal processing and/or hardware error has occurred.

Action B: Contact your service representative if you continue to receive this error message.



Feb 06 A-5


2488- File (file name) cannot be opened for editing. It is already in use.

2489- File (file name) cannot be opened for writing. It is already in use.

2490- No ‘.INI’ file present. Application will terminate.

2492- This field’s entry is invalid.

2493- An entry is required for this field.

2494- Value is out of the valid range.

Cause: The file you specified is being used in another edit operation.

Action: Check the Windows list to locate the other edit session.

Cause: The file you specified in a Save As operation is already open for edit.

Action: Select a different file for the Save As operation.

Cause: The ASCII file containing initialization information and system options information used during program startup does not exist.

Action: Run the Setup program, select Change analyzer setup, and create the control file used by the Gemini.

Cause: The highlighted field contains an invalid entry.

Action: Check the entry and correct the error.

Cause: This field requires a valid entry for you to proceed.

Action: Enter or select an appropriate value.

Cause: The value you entered in the highlighted field is outside the valid range of values.

Action: Check the entry and enter or select an appropriate value.

A-6 Feb 06


2495- Value is out of the valid range. Enter a value between (value) and (value).

2496- Invalid number.

2497- This field contains an invalid character.

2498- The requested change to the Sample’s status is invalid at this time.

2499- Sequence number must contain at least 3 digits.

Cause: The value you entered in the highlighted field is outside the valid range of values.

Action: Check the entry and enter or select a value within the indicated range.

Cause: The number you entered in the highlighted field is invalid.

Action: Check the entry and enter or select a valid number.

Cause: You entered an invalid character in the highlighted field.

Action: Check the entry and enter valid characters.

Cause: A request to change the file’s status (for example, from automatically collected to manually entered) could not be done.

Action: Contact your service representative if you continue to receive this error message. Record the name of the sample file in which the problem occurred.

Cause: You tried to enter a sequence number that did not contain at least three digits.

Action: Enter a sequence number that contains at least three digits.

Feb 06 A-7


2500 Series

2500- All sample file names that can be created using the sequence number pattern already exist. You may want to modify the next sequence number.

2505- Error Logger cannot be initialized! Error code (number). Program will exit.

2506- (sample file) Output device (name) is not installed. Printing cannot be accomplished.

2508- (sample file) Overlay file (name) was not found. It will not be included in the reports.

2509- (sample file) Error opening file (name): (error). Reports cannot be produced.

Cause: No more sample information files can be created using the currently entered file name sequence number.

Action: Select Options > Sample defaults and enter another sequence number.


Action: Contact your service representative.

Cause: The selected output device is not installed in Windows.

Action: Select a different output device in the System Configuration dialog. Install the device using the Control Panel - Printers operation.

Cause: The specified overlay file could not be found.

Action: Ensure that the file specified as an overlay does exist.

Cause: An error occurred while the program was opening a file necessary to the report operation.

Action: Use the name given in the error message to investigate. Contact your service representative if you continue to receive this error message.

A-8 Feb 06


2510- (sample file) Error parsing reports from file (name). Reports cannot be produced.

2511- Print job (name) has been cancelled due to insufficient disk space. Delete unnecessary files and restart the report.

2512- Print job (name) cancelled.

Cause A: One or more data entry fields in the sample file may contain an invalid character (such as a single quote or double quotes).

Action A: Review the data entry fields (for example, the Sample field) and remove the invalid character.

Cause B: The system was unable to create the usual temporary files during the report, possibly due to insufficient disk space.

Action B: Check the space available on the hard disk.

Cause C: An internal processing error occurred.

Action C: Contact your service representative.

Cause: The disk drive does not have enough space for the temporary file required by the Windows Print Manager. Therefore, printing of the requested report has been canceled.

Action: Delete unnecessary files from the disk. You will require at least five megabytes of free space for normal operation.

Cause: The requested print job was canceled at your request.

Action: None required.

Feb 06 A-9


4000 Series

4003- Error Converting Pressures.4004- Error Computing Volume Adsorbed.

4006- Report Type Not Found.4007- Error Processing Report.

4008- Report requested on sample file with no data points.

4015- Error creating export file for sample <sample file name>.

Cause: An internal processing and/or hardware error occurred during report generation.


Cause: An internal processing and/or hardware error occurred during report generation.


Cause: You selected a file for reporting which contains no collected data.

Action: Select another file which contains collective data and restart the report.

Cause: A file error occurred during creation of an export output file.

Action: The output file name may be invalid. Ensure that the target directory exists. Ensure that the target diskette is not full or write protected. The target disk drive may be damaged or inoperative. Verify that other files may be created on the same drive. Contact your service representative if you continue to receive this error message.

A-10 Feb 06


4016- Sample <sample file name> has no data for export to ISO/DFT.

4023- The file <name> cannot be prepared for analysis. It is open for editing and contains errors.

4400- The communications port specified for the SmartPrep(s) is not physically installed in the Computer. Cannot initialize.

4401- The communications port specified for the SmartPrep(s) is already in use. Cannot initialize.

4402- The communications port specified for the SmartPrep(s) cannot be accessed. Cannot initialize.

4403- Cannot communicate with SmartPrep Unit n - S/N: nn.

Cause: The file selected for export has a status of No Analysis. No export file will be created.

Action: Select a file which contains analysis data.

Cause: You are trying to start an analysis using a file that contains errors and is open for editing.

Action: Finish editing this file, save and close it, then start the analysis.

Cause: The communications port associated with this unit is invalid.

Action: Run the setup program and specify a valid port.

Cause: The communications port associated with this instrument is in use by some other program in the system.

Action: Close the other program to release the port. Restart the Gemini applica-tion.


Action: Run the setup program and specify valid port.

Feb 06 A-11


4404- The application version of the SmartPrep Unit n - S/N: nn is invalid.

4405- Fatal communications error with SmartPrep Unit n - S/N: nn.

Cause: The controller software running on the designated instrument is invalid.

Action: Use the SmartPrep setup program to download the proper controller software to the instrument, or contact a service representative if unavail-able.

Cause: There was a fatal error in the serial communications between the appli-cation and the SmartPrep Instrument Controller. All displays for that SmartPrep will be closed.

Action: Ensure that the SmartPrep is properly connected to the computer on the communications port configured in the Setup program. Stop and restart the application. If this error persists, contact your service representative.

A-12 Feb 06


6000 Series

6003- Serial write operation failed.6003- Serial write queue full.6004- Error opening communications port.

6005- Communications DCB error.6006- Communications state error.

6007- Error closing communications port.

6008- The sample has an invalid status and cannot be used for this analysis.

Cause: There was a fatal error in the serial communications between the appli-cation and the software. All instrument displays will be closed.

Action: Ensure that the analyzer is connected to the computer on the communi-cations port configured in the Setup program. Close the analysis pro-gram, then restart it. If this error persists, contact your service representative.


Action: Run the Setup program and specify a valid port.

Cause: There was a fatal error in the serial communications between the appli-cation and the software. All instrument displays will be closed.

Action: Ensure that the analyzer is connected to the computer on the communi-cations port configured in the Setup program. Close the analysis pro-gram, then restart it. If this error persists, contact your service representative.

Cause: You selected a sample file with a status other than No Analysis or Pre-pared.

Action: Select a sample file with a status of No Analysis or Prepared.

Feb 06 A-13


6009- Analysis: Evacuation timed out.

6010- Analysis: Dosing with Helium timed out.

6011- Analysis: Dosing with adsorptive timed out.

Cause: The analyzer failed to reach a pressure level of 10 mmHg within the user-specified evacuation time plus three minutes; or, the analyzer failed to reach a pressure level of 5 mmHg within an additional three minutes.

Action: Reattach the sample and balance tubes, making sure both are securely in the fitting. Verify that the vacuum pump is operating correctly. If these actions do not correct the problem, degas the sample again and repeat the analysis. If the analyzer continues to display this message, call a Micromeritics service representative.

Cause: The helium supply was depleted by the instrument during free-space measurement.

Action: Make sure the helium supply cylinder is not empty. Verify that the inlet valve on the gas supply cylinder is open. Verify that the gas pressure regulator setting is between 15 and 18 psig (103.4 and 124.1 kPa).

Cause A: The adsorbate gas supply was depleted by the instrument during analysis or temination.

Action A: Make sure the adsorbate gas supply cylinder is not empty. Verify that the inlet valve on the gas supply cylinder is open. Verify that the gas pres-sure regulator setting is between 15 and 18 psig (103.4 and 124.1 kPa).

Cause B: Sample has adsorbed the maximum amount of gas available.

Action B: If additional data points are needed, repeat analysis with a smaller amount of sample (to avoid exceeding 100 cm3 STP total volume adsorbed).

A-14 Feb 06


6012- Analysis: Operator cancelled operation.

6013- Analysis: Pressure overrange.

6014- Analysis: Volume adsorbed overrange.

6015- Analysis: Reference volume too large.

Cause: You clicked Cancel while an analysis or a Po measurement was being performed.

Action: Restart the analysis when ready.

Cause: Adsorbate gas pressure is too high.

Action: Verify that the gas inlet pressure regulator setting does not exceed 15 to 18 psi (103.4 and 124.1 kPa). If the analyzer continues to display this message, call a Micromeritics service representative.

Cause: The rate of adsorption by the sample exceeded the response capacity of the analyzer, preventing the normal refilling of the gas reservoirs.

Action: Repeat analysis with a smaller amount of sample in the tube.

Cause A: The analysis was canceled because the number of volume adsorbed A/D counts was less than 100 at the end of equilibration of free space or an analysis point.

Action A: Reduce volume of sample used or, if necessary, use filler rods in both the sample and balance tubes (see Appendix C).

Cause B: The analysis was canceled because the number of volume adsorbed A/D counts was less than 100 when volume adsorbed was recorded during a scanning run.

Action B: Reduce volume of sample used or, if necessary, use filler rods in both the sample and balance tubes (see Appendix C).

Feb 06 A-15


6016- Analysis: Pressure underrange.

6017- System: Power failure during analysis.

6018- Hardware: Pressure transducer failure.

6019- Hardware: Battery-backed memory has been reinitialized.

6020- Hardware: Valve I/O failure.

Cause: A test of the sample pressure transducer was made during evacuation. The test showed a low reading. The analysis will continue.

Action: Call a Micromeritics service representative.

Cause: A power failure occurred and, when power was restored, the automatic operation was canceled.

Action: Restart the automatic operation if desired.

Cause: A test of the sample pressure transducer was made during evacuation. The test showed that the transducer has failed. The analysis has been canceled.


Cause A: You clicked Init BB-ram on the Unit Configuration dialog. All previ-ously stored data have been deleted and all parameters have been reset to the initial default data.

Action A: Reset parameters if desired.

Cause B: Battery-backed RAM has failed.

Action B: Call a Micromeritics service representative.

Cause: An error in the valve control electronics has occurred.


A-16 Feb 06


6021- Hardware: Analog-to-Digital I/O failure.

6022- Hardware: Servo I/O failure.

6023- Desorption points in this sample file cannot be processed by this instrument.

6024- Some selected reports are invalid for this instrument.

Cause: An error in the pressure measurement electronics has occurred.


Cause: An error in the pressure balancing electronics has occurred.


Cause: You started an analysis using a sample file in which adsorption and des-orption points have been defined. Desorption data is not available on the Gemini 2365.

Action A: Continue with the analysis; only the adsorption points will be reported.

Action B: Cancel the operation and modify the sample file, or choose a different sample file for your analysis.

Cause: You have the Gemini 2365; some of the reports selected in the sample file cannot be produced by data collected on this instrument.

Action A: Continue with the operation. The reports unavailable for your instrument will not be produced; an error message is displayed.

Action B: Cancel the operation and modify the sample file, or choose a different sample file.

Feb 06 A-17


6026- Measure Po for each point is not supported by this model. Choose another sample file for analysis or change the Po options in the analysis conditions..

6027- Analysis: Po dosing failure.

Cause: You selected Measure po for each point as the saturation method, but this option is not available for the Gemini V; this option is available only for the Gemini VI.

Action: A Edit the Po options in the analysis conditions and select Entered or Most recent measured as the saturation pressure method.

Action: B Choose a sample file containing appropriate analysis conditions.

Cause: The Dewar does not contain enough cryogen to take accurate readings in the P0 tube.

Action: Refill the Dewar with cryogen and restart the analysis.

A-18 Feb 06

Gemini V Windows Appendix B

B. CALCULATIONS

This appendix contains the calculations used in reports available in the Gemini Windows program.

Free-Space Correction Algorithms

Free-space differential compensation for the Gemini is accomplished in two steps. First, the free-space correction, Cf (cc STP/mmHg) is determined. Second, the correction is applied to quantities adsorbed during analysis.

Determining the Free-Space Correction

The free-space correction Cf (cc STP/mmHg) is determined in one of two ways: Measured or Calculated.

Measured

Evacuate the sample and balance ports, charge the reservoirs with helium, and dose to 760 mmHg. Measure the gas quantity differential, Vh (cc STP), and the absolute sample pressure, Ph (mmHg). Record the free space correction:

Calculated

Measure the free-space correction as above, except use an empty sample tube of the same volume as that to be used during subsequent sample analyses. Calculate and record the sys-tem volume correction Vsys (cc STP):

Cf VhpH-------=

This method is calculated using a liquid nitrogen temperature. It should not be selected for free-space correction if a liquid nitrogen bath is not being used.

Vsys 760 mmHg VhPh-------×=

Feb 06 B-1

Appendix B Gemini V Windows

Calculate the sample volume Vsam (cc) from independently determined sample weight Wsam (g) and sample density Dsam (g/cc):

Calculate the quantity of gas displaced by the sample at liquid nitrogen temperature and stan-dard pressure:

Calculate the free-space correction due to both the system volume correction and the gas dis-placed by the sample in cc STP/mmHg:

Applying the Free-Space Correction to Quantities Adsorbed

Measure the uncorrected quantity adsorbed Vraw (cc STP) and the pressure at which this quantity is adsorbed Pads (mmHg). Use the independently determined adsorbate nonideality correction Cn (%/atm) and the free space correction Cf (cc STP/mmHg) to calculate the adsorbate quantity correction Vcor (cc STP) for this point:

Apply the correction to the uncorrected quantity adsorbed to obtain the corrected quantity adsorbed Vads (cc STP):

Vsam WsamDsam---------------=

Vgas Vsam 273.13 K77.15 K----------------------×=

Cf Vsys Vgas–760 mmHg-------------------------------=

Vcor Cf Pads 1 Pads Cn×

100% 760 mmHgatm

----------------------------×-------------------------------------------------

+××=

Vads Vraw Vcor–=

B-2 Feb 06


Surface Area Calculations

BET

For each point designated for surface area calculations, the BET1 transformation is calculated as follows:

where BI is in units of g/cm3 STP.

A least-squares fit is performed on the (PrelI ,BI) designated pairs where PrelI is the independent variable and BI is the dependent variable. The following are calculated:

a. Slope (S g/cm3 STP)

b. Y-intercept (YINT g/cm3 STP)

c. Error of the slope (SERR g/cm3 STP)

d. Error of the y-intercept (YIERR g/cm3 STP)

e. Correlation coefficient (Cc)

Using the results of the above calculations, the following can be calculated:

BET Surface Area (m2/g):

where

CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the Adsorptive Properties dialog

1. Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938).

B1Prel1

1.0 Prel1–( ) Nads1

×----------------------------------------------=

SABETCSA 6.023 1023×( )×

22414 cm3 STP( ) 1018 nm2/m2( ) S YINT+( )××---------------------------------------------------------------------------------------------------------------------=

Feb 06 B-3


BET C value:

Volume of the Monolayer (cm3/g STP):

Error of the BET Surface Area (m2/g):

Langmuir Surface Area

For each point designated for surface area calculations, the Langmuir2 transformation is cal-culated as follows:

where LI is in units of g/cm3 STP

A least-squares fit is performed on the (PrelI ,LI) designated pairs where PrelI is the inde-pendent variable and LI is the dependent variable. The following are calculated:

a. Slope (S g/cm3 STP)

b. Y-intercept (YINT g/cm3 STP)

c. Error of the slope (SERR g/cm3 STP)

d. Error of the y-intercept (YIERR g/cm3 STP)


C S YINT+YINT

-------------------=

VM1

C YINT×-------------------- 1

S YINT+-------------------= =

BETERRSABET SERR 2 YIERR 2+( )0.5×

YINT S+---------------------------------------------------------------------=

2. Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40, 1361 (1918); Phys. Rev 8, 149 (1916).

LIPrelI

NadsI

-----------=

B-4 Feb 06



Langmuir Surface Area (m2/g):

where

CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the Adsorptive Properties dialog

Volume of the Monolayer (cm3/g STP):

Langmuir b Value:

Error of the Langmuir Surface Area (m2/g):

SALANCSA 6.023 1023×( )×

22414 cm3 STP( ) 1018 nm2/m2( ) S××-----------------------------------------------------------------------------------------------=

VM1S---=

b YINT( ) VM( )=

LANERRSALAN SERR×

S-------------------------------=

Feb 06 B-5


t-Plot

For each point designated for t-Plot3 calculations, the following calculations are done:

Thickness for the Ith point (Å):

(Halsey4)

(Harkins and Jura5)

(STSA Carbon Black)

(Broekhoff-deBoer6)

where:

tI = thickness for Ith point HP1 = Halsey parameter #1HP2 = Halsey parameter #2HP3 = Halsey parameter #3HJP1 = Harkins and Jura parameter #1HJP2 = Harkins and Jura parameter #2HJP3 = Harkins and Jura parameter #3STSA1 = statistical thickness surface area parameter #1 (2.9800)STSA2 = statistical thickness surface area parameter #2 (6.4500)STSA3 = statistical thickness surface area parameter #3 (0.8800)BdB1 = Broekhoff-de Boer parameter #1 (-16.1100)BdB2 = Broekhoff-de Boer parameter #2 (0.1682)BdB3 = Broekhoff-de Boer parameter #3 (-0.1137)PrelI = relative pressure for the Ith point (mmHg)

Defaults for thickness curve parameters are shown in parentheses.

3. de Boer, J.H., et al, J. Catalysis 3, 32, 38, 44, 268 (1964); J. Catalysis 4, 319, 643, 649 (1965); Cranston, R. and Inkley, F., Adv. Catalysis 9, 143 (1957).

4. Halsey, G., J. Chem. Phys. 16, 931-937 (1948).5. Harkins, W.D. and Jura, G., J. Chem. Phys. 11, 431 (1943).6. Broekhoff, J.C.P. and de Boer, J.H., “The Surface Area in Intermediate Pores,” Proceedings of the Interna-

tional Symposium on Surface Area Determination, D.H. Everett, R.H. Ottwill, eds., U.K. (1969).

tI HP1 HP2PrelI

( )ln--------------------×

HP3=

tIHJP1

HJP2 PrelI( )log–

-------------------------------------------HJP3

=

tI STSA1 PrelI( )2 STSA2 PrelI

( ) STSA3+ +=

PrelI( )log BdB1

tI 2

-------------- BdB2 BdB3*tI( )exp+=

B-6 Feb 06


A least-squares analysis fit is performed on the (tI, NadsI) data pairs where tI is the indepen-dent variable and NadsI is the dependent variable. Only the values of tI between tMIN and tMAX, the minimum and maximum thickness, are used. The following are calculated:

a. Slope (S cm3/g-Å STP)

b. Y-intercept (YINT cm3/g STP)

c. Error of the slope (SERR cm3/g-Å STP)

d. Error of the Y-intercept (YIERR cm3/g STP)



External Surface Area (m2/g):

where

F = surface area correction factor, user-entered on the t-Plot Report Options dialog D = density conversion factor, user-entered on the Adsorptive Properties dialog

Micropore Surface Area (m2/g):

where SATOT is the BET surface area if the user enabled the BET report exclusively, or Lang-muir surface area if the user enabled the Langmuir report exclusively. If neither report has been selected, SATOT is the BET surface area value calculated using a set of default parameters.

Micropore Volume (cm3 liquid/g):

SAEXTS cm3/g A STP–( ) 1010 A/m( ) D( cm3 liquid/cm3 STP )××

F 106 cm3/m3( )×--------------------------------------------------------------------------------------------------------------------------------------------------------=

SAµP SATOT SAEXT+=

VµP YINT cm3/g STP( ) D cm3 liquid/cm3 STP( )×=

Feb 06 B-7


BJH Pore Volume and Area Distribution

For adsorption data, the relative pressure and volume adsorbed data point pairs collected dur-ing an analysis must be arranged in reverse order from which the points were collected during analysis. All calculations are performed based on a desorption model, regardless of whether adsorption or desorption data are being used.

The data used in these calculations must be in order of strictly decreasing numerical value. Points which do not meet this criterion are omitted. The remaining data set is composed of relative pressure (Pr), volume adsorbed (Va) pairs from (Pr1, Va1) to (PrN, VaN) where (PrN = 0, VaN = 0) is assumed as a final point. Each data pair represents an interval boundary (or des-orption step boundary) for intervals i=1 to i=N-1 where N = total number of (Pr, Va) pairs.

Generally, the desorption branch of an isotherm is used to relate the amount of adsorbate lost in a desorption step to the average size of pores emptied in the step. A pore loses its con-densed liquid adsorbate, known as the core of the pore, at a particular relative pressure related to the core radius by the Kelvin7 equation. After the core has evaporated, a layer of adsorbate remains on the wall of the pore. The thickness of this layer is calculated for a particular rel-ative pressure from the thickness equation. This layer becomes thinner with successive decreases in pressure, so that the measured quantity of gas desorbed in a step is composed of a quantity equivalent to the liquid cores evaporated in that step plus the quantity desorbed from the pore walls of pores whose cores have been evaporated in that and previous steps. Barrett, Joyner, and Halenda8 developed the method (known as the BJH method) which incor-porates these ideas. The algorithm used on the Gemini is an implementation of the BJH method.

Explanation of Terms

A pore filled with condensed liquid nitrogen has three zones:

a. The core - evaporates all at once when the critical pressure for that radius is reached; the relationship between the core radius and the critical pressure is defined by the Kelvin equation.

b. The adsorbed layer - composed of adsorbed gas that is stripped off a bit at a time with each pressure step; the relationship between the thickness of the layer and the relative pressure is defined by the thickness equation.

7. Kelvin, J. (published under the name of Sir William Thomson), Phil. Mag. 42, 448-452 (1871).8. Barrett, E.P.; Joyner, L.S.; and Halenda, P.P., J. Am. Chem. Soc. 73, 373-380 (1951).

B-8 Feb 06


c. The walls of the cylindrical pore - the diameter of the empty pore is required to determine the pore volume and pore area. End area is neglected.

Calculations

The volumes adsorbed (Va) are converted to the liquid equivalent volumes (V1, cm3/g):

where D is the Density Conversion Factor from the Adsorptive Properties dialog.

The relative pressure (Pr1) is assumed to be close to unity so that substantially all the pores in the sample are filled.

The corresponding Kelvin core radius is calculated. Only pores smaller than this size will be included:

where

A = adsorbate property factor (the BJH Adsorptive Options dialog)F = fraction of pores open at both ends (from the BJH Adsorption Report Options

dialog or the BJH Desorption Report Options dialog); assumed to be zero for desorption

This radius will be adjusted for the thickness of the adsorbed layer during subsequent calcu-lation steps.

adsorbed

layer

wallcore

Insignificant compared to core length

pore

VII VaI( ) D( )=

RcIA–

1 F+( ) PrI( )ln[ ]-----------------------------------------=

Feb 06 B-9


The thickness of the remaining adsorbed layer at this relative pressure is calculated:

where

HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey Thick-ness Equation dialog.

These calculations illustrate the use of the Halsey thickness equation. If the Harkins/Jura equation was selected, substitute the following wherever the thickness equation appears:

where

HJ1, HJ2, and HJ3 are Harkins and Jura Parameters 1, 2, and 3 (respectively) from the Har-kins and Jura Thickness Equation dialog.

The following calculations (a-c) are made for each relative pressure interval based on the increment of volume desorbed during that interval. The variable I refers to the interval num-ber, that is I=1 for the first interval from Pr1 to Pr2, and so on. J refers to each previous interval during which new pores were found. K refers to the total number of intervals in which new pores have been found. K is also the number of lines reported on the BJH table for collected data.

a. The thickness of the adsorbed layer at the end of the interval is calculated as follows:

(For the last pressure interval from the lowest PrI to zero relative pressure, TwI+1 = 0.)

For the first pressure interval, there are no previously opened pores so the volume desorbed from walls of previously opened pores is zero (Vd1 = 0), and the remainder of Step a is skipped.

The change in thickness of the wall layer due to desorption from preivously opened pores is calculated:

Tw1 HP1 HP2Pr1( )ln

------------------HP3

=

Tw1HJ1

HJ2 Pr1( )log–--------------------------------------

HJ3=

TwI 1+ HP1 HP2PrI 1+( )ln

------------------------HP3

=

∆Tw Tw1 TwI 1+–=

B-10 Feb 06


The annular cross-sectional area of the wall layer desorbed is calculated for all pre-viously opened pores:

The total volume of gas desorbed from walls of previously opened pores is calculated:

for all previously opened pores

where LPJ = length of previously opened pores as calculated in Step b(2).

b. The physical processes occurring for this pressure interval are determined as follows:

(1) If VdI is greater than the current increment of volume desorbed (VlI - VlI+1), desorption from walls only is occurring. Total surface of walls exposed thus far (cm2/g) is calculated as follows:

for all previously opened pores

where

DavgJ = weighted average pore diameter calculated below in Step b(2).

A new layer thickness (∆Tw) that will not overcompensate for the actual volume desorbed in this interval is calculated:

Since no cores are evaporated in this pressure interval, no new pores are revealed. Thus no ending Kelvin radius and average pore diameter are calculated for this interval. Note that this means the report may have fewer tabulated intervals on the collected data report than experimental pressure intervals.

CSAJ π Rcj ∆Tw+( )2 Rcj 2–[ ] 10 16– cm2/A2( )=

VdI LpJ( ) CSAaJ( )∑=

SAW π LPJ( ) DavgJ( ) 10 8– cm/A( )∑=

∆Tw V1I V1I 1+–( ) 108 A/cm( )SAwI

--------------------------------------------------------------=

Feb 06 B-11


(2) If VdI is less than the volume increment desorbed during this interval, the remaining volume is due to new pores with core evaporation taking place in this interval. K, the number of intervals with new pores exposed, is increased by 1. (For the interval from the lowest to zero relative pressure, no new pore volume is calculated and the rest of Step b is skipped.)

The volume desorbed from newly opened pores in this interval is calculated as follows:

The Kelvin radius for the end of the interval is calculated as follows:

All new pores opened in this interval are represented by one pore having a length-weighted average pore diameter and a corresponding length sufficient to account for the required volume of adsorbate. The weighted average pore diam-eter is calculated as follows:

DavgK is the diameter of a pore which would have a surface area that is the aver-age of the areas for pores with radius and , if its length was the mean of the lengths at those radii.

The relative pressure corresponding to is calculated as follows:

The thickness of the adsorbed layer at this pressure is calculated as follows:

The decrease in thickness of the wall layer by desorption from the walls of new pores during the lower portion of the pressure interval is calculated as follows:

VcI VII VII 1+–( ) VdI–=

RcK 1+A–

1 F+( ) PrI 1+( )ln[ ]-----------------------------------------------=

DavgK

2( ) RcK RcK 1++( ) RcK( ) RcK 1+( )RcK 2 RcK 1+ 2+

-------------------------------------------------------------------------------=

PavgK 1– 2A–

1 F+( ) DavgK( )

-----------------------------------ln=

TwavgKHP1 HP2

PavgK( )ln

----------------------HP3

=

∆Td TwavgKTWI 1+–=

B-12 Feb 06


The cross-sectional area of the newly opened pores is calculated as follows:

The length of the newly opened pores is calculated as follows:

c. Pore diameters and radii are adjusted for the change in thickness of the adsorbed wall layer during this interval. If new pores were opened during this interval, the average diameter is adjusted by the change in layer thickness during the second portion of the desorption interval as follows:

The layer thickness change during the whole interval is added to diameters of previ-ously opened pores as follows:

(not including DavgK)

The layer thickness change desorbed during this interval also is added to the radii corresponding to the ends of the pressure intervals as follows:

for all except RcK+1.

Steps a to c are repeated for each pressure interval.

After the above calculations have been performed, the diameters corresponding to the ends of the intervals are calculated as follows:

for all RcJ including RcK+1.

CSAcKDavgK

2---------------- ∆Td+

210 16– cm2/A2( )=

LPKVcI

CSAcK-----------------=

DavgKnewDavgKold

2 ∆Td( )+=

DavgJnewDavgJold

2 ∆( Tw )+=

RcJnew RcJold ∆Tw+=

DpJ 2 rcJ( )=

Feb 06 B-13


The remaining calculations are based on DP(I), Davg(I), and LP(I). These calculations are only done for Davg(I) values that fall between the Minimum BJH diameter and the Maximum BJH diameter specified by the operator on the BJH Adsorption Report Options dialog or the BJH Desorption Report Options dialog.

1) Incremental Pore Volume (VpI, cm3/g):

2) Cumulative Pore Volume (VpCUM(1), cm3/g):

3) Incremental Surface Area (SAI, m2/g):

4) Cumulative Surface Area (SACUM(I), m2/g):

5) dV/dD pore volume (dV/dDI, cm3/g-A):

6) dV/dlog(D) pore volume (dV/dlog(D)I, cm3g):

7) dA/dD pore area (dA/dDI, m2/g-A):

8) dA/dlog(D) pore area [dA/dlog(D)I, m2/g]:

VpI π LpI( )DavgI

2-----------

2

1016 cm2/A2=

VPCUM 1( )VpJ for J 1≤( )∑=

SAI π LPI( ) 10 2– m/cm( ) DavgI( ) 10 10– m/A( )=

SACUM10SAJ for J 1≤∑=

dV/dDIVPI

DpI DpI 1+–------------------------------=

dDv/d D( )I VPI/DpI

DpI 1+--------------- log=log

dA/dDISAI

DpI DpI 1+–------------------------------=

dA/d D( )Ilog SAI/DpI

DpI 1+--------------- log=

B-14 Feb 06


For fixed pore size tables (if selected), the following calculations are performed:

1) Average Fixed Pore Size (DFavgJ, A):

calculated for all intervals in the fixed pore size table.

For the intervals with between the Minimum BJH diameter and the Maximum BJH diameter.

2) Cumulative Pore volume (VpFCUMI, cm3/g):

where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y = VPCUMJ, using an AKIMA semi-spline interpolation.

3) Incremental Pore Volume (VpFI, cm3/g):

where VpFCUM0 = 0.

4) Cumulative Surface Area (SAFCUMI, m2/g):

where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y = SACUMJ.

5) Incremental Surface Area (SAFI, m2/g):

where SAFCUM0 = 0.

DFavgJ

DpFJDpFJ 1+

+2

---------------------------------=

VpFCUMIINTERP DpFI 1+( )=

VpFI VpFCUMIVpFCUMI 1–

–=

SAFCUMIINTERP DpFI 1+( )=

SAFI SAFCUMISAFCUMI 1–

–=

Feb 06 B-15


6) dV/dD pore volume (dV/dDpFI, cm3/g-A):

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dV/dDJ.

7) dV/dlog(D) pore volume [dV/dlog(DpF)I, cm3/g]:

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dV/dlog(D)J.

8) dA/dD pore area (dA/dDpFI, m2/g-A):

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dA/dDJ.

9) dA/dlog(D) pore area [dA/dlog(DpFI), m2/g]:

where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dA/dlog(D)J.

dV/dDpFI INTERP DpFI 1+( )=

dV/d D( pFI )log INTERP DpFI 1+( )=

dA/dDpFI INTERP DpFI 1+( )=

dA/d D( pFI )log INTERP DpFI 1+( )=

B-16 Feb 06


Compendium of Variables

Va = quantity adsorbed expressed as a volume (cm3/g STP)Vl = liquid equivalent volume of volume adsorbed (cm3/g)D = density conversion factor from the Adsorptive Properties dialog

(cm3/cm3 STP)Pr = relative pressureDp = pore (or core) diameter (A)Rc = Kelvin radius (A) of coreA = adsorbate property factor; from the BJH Adsorptive Options dialog F = fraction of pores open at both ends; from the BJH Adsorption Report

Options dialog box or the BJH Desorption Report Options dialog ∆Tw = thickness of adsorbed layer desorbed during interval (A)Tw = thickness of remaining adsorbed wall (A)

HP1, HP2, and HP3 are Halsey Parameters from the Halsey Thickness Equation dialog.

HJ1, HJ2, and HJ3 are Harkins and Jura Parameters from the Harkins and Jura Thickness Equation dialog.

Vd = volume of gas desorbed from walls of previously opened pores (cm3/g)Davg = average pore diameter (A)CSAa = annular cross-sectional area of the desorbed layer (cm2)CSAc = cross-sectional area of opening of newly opened pores (cm2)SAw = total surface area of walls exposed (cm2/g)∆Td = thickness of layer desorbed from walls of newly opened pores (A)Vc = volume desorbed from cores of newly opened pores (cm3/g)Lp = length of pore (cm/g)

Feb 06 B-17


Dubinin-Radushkevich

The Dubinin-Radushkevich9 equation is as follows:

where:

V = volume adsorbed at equilibrium pressure (cm3/g STP)Vo = the micropore capacity (cm3/g STP)Po = saturation vapor pressure of gas at temperature T (mmHg) P = equilibrium pressure (mmHg)B = a constantβ = the affinity coefficient of analysis gas relative to Po gas

(for this application β is taken to be 1)T = analysis bath temperature (K), from the Po and Temperature

Options dialog

For each point designated for Dubinin-Radushkevich calculations, the following calculations are done:

LV = log (V)

The intercept, log(Vo) can be found by performing a least-squares fit on the (LP,LV) desig-nated pairs where LP is the independent variable and LV is the dependent variable. Assuming the adsorption of gas is restricted to a monolayer, Vo is the monolayer capacity. Based on this assumption, the following are calculated:

a. Slope (S cm3/g STP)

b. Y-intercept (YI cm3/g STP)

c. Error of the slope (SERR cm3/g STP)

9. Dubinin, M., Carbon 21, 359 (1983); Dubinin, M., Progress in Surface and Membrane Science 9, 1, Aca-demic Press, New York (1975); Dubinin, M. and Astakhov, V., Adv. Chem. Ser. 102, 69 (1971); Lamond, T. and Marsh, H., Carbon 1, 281, 293 (1964); Medek, J., Fuel 56, 131 (1977); Polanyi, M., Trans. Faraday Soc. 28, 316 (1932); Radushkevich, L., Zh. fiz. Kemi. 33, 2202 (1949); Stoeckli, H., et al, Carbon 27, 125 (1989).

V( )log Vo( ) B T2× β

--------------- PoP

-------log×2

–log=

LP PoP

-------

2log=

B-18 Feb 06


d. Error of the y-intercept (YIERR cm3/g STP)



Monolayer Capacity (cm3/g STP):

Vo = 10YI

Error of Monolayer Capacity (cm3/g STP):

VoERR = Vo x (10YIERR - 1.0)

Micropore surface area (m2/g):

where

σ = molecular cross sectional area of gas (nm2)from the Adsorptive Properties dialog

SDP σ Vo 6.023 1023×( )××22414 cm3 1018 nm2/m2( )×--------------------------------------------------------------------=

Feb 06 B-19


Dubinin-Astakhov

The Dubinin-Astakhov equation is a follows:

where

V = volume adsorbed at equilibrium pressure (cm3/g STP)Vo = the micropore capacity (cm3/g STP)Po = saturation vapor pressure of gas at temperature T (mmHg) P = equilibrium pressure (mmHg)T = analysis bath temperature (K) R = the gas constant (0.0083144 kJ/mol)E0 = characteristic energy (kJ/mole)N = Astakhov exponent, may be optimized or user entered from the Dubinin

Report Options dialog β = the affinity coefficient of the analysis gas relative to the Po gas, from the

Dubinin Adsorptive Options dialog

For each point designated for Dubinin-Astakhov calculations, the following calculations are done:

LV = log(V)

A least-squares fit is performed on the (LP,LV) designated pairs where LP is the independent variable and LV is the dependent variable. If the user selected yes for the Optimize Astakhov Exponent prompt, a systematic search for the optimum value of N is conducted by recalcu-lating the linear regression and selecting the value of N that gives the smallest standard error of the y-intercept. The exponent N is optimized to within 10-4. If the optimum value for N is not found in this range, an exponent of 2 is used. The following are calculated:

a. Slope (S cm3/g STP)

b. Y-intercept (YI cm3/g STP)

c. Error of the slope (SERR cm3/g STP)

d. Error of the y-intercept (YIERR cm3/g STP)


f. Optimized Astakhov exponent (N)

V( )log Vo( ) RTβE0---------

N PoP

-------log×N

–log=

LP PoP

-------logN

=

B-20 Feb 06



Monolayer Capacity (cm3/g STP):

V0 = 10YI

Micropore Volume (cm3/g):

WI = (VI x D)

where

D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive Properties dialog

Limiting Micropore Volume (cm3/g):

W0 = (V0 x D)

where

D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive Properties dialog

Error of Limiting Micropore Volume (cm3/g):

W0ERR = W0 x (10YIERR - 1.0)

Characteristic Energy (KJ/mole):

Modal Equivalent Pore Diameter (Å):

where

β = affinity coefficient of the analysis gas relative to the Po gas from the Dubinin Adsorptive Options dialog

E 2.303 R T××β 2.303 S×( )1/N-------------------------------------=

Dmode 2 3N3N 1+----------------

1/N 103 nm3/Å3----------------------------×

1/3

×=

Feb 06 B-21


Maximum Differential Pore Volume (cm3/g-Å):

This value is also known as frequency of the mode

Mean Equivalent Pore Diameter (Å):

Micropore surface area (m2/g):

Γ is calculated by a polynomial approximation over the domain 0 ≤ x ≤ 1 as follows:

Γ(x+1) = 1+b1x + b2x2 + b3x3 + b4x4 + b5x5 + b6x6 + b7x7 + b8x8 + ε(x) | ε(x) | ≤ 3 x 10-7

where

b1 = -0.57719 1652b2 = 0.98820 5891b3 = -0.89705 6937b4 = 0.91820 6857b5 = -0.75670 4078b6 = 0.48219 9394b7 = -0.19352 7818b8 = 0.03586 8343

and where

dVdDmode-----------------Max 0.5 3N 1+( )× Wo× 3N 1+

3N----------------

1/3N×

β E⋅ 0

103 nm3/Å3( )---------------------------------×

1/3 3N 1+3N

----------------– exp×=

Dmean 2

103 nm3/Å3

β E⋅ 0----------------------------

1/3

Γ 3N 1+3N

----------------

---------------------------------------×=

SDA 1000 2.0 W0××E0

k-----

1/3

× Γ 3N 1+3N

---------------- ×=

x 1+ 3N 1+3N

---------------- =

B-22 Feb 06


Equivalent Pore Diameter (Å):

dV/dD Pore Volume (cm3/g-Å):

Di 2

103 nm3/Å3

β E⋅ 0----------------------------

N

–

W( i ) W0( )ln–ln-----------------------------------------×

1/3N

=

dVdwi-------- 0.5 W0 3N 103 nm3/Å3

β E⋅ 0----------------------------

N

×××Di

2-----

3N 1+( )–

× 103 nm3/Å3

β E⋅ 0----------------------------

N

Di

2-----

3N–

×–exp×=

Feb 06 B-23


MP-Method Calculations

For each point designated for MP-method10 calculations, the following calculations are done:

Thickness for the Ith point (Å):

(Halsey4)

or

(Harkins and Jura5)

where:

tI = thickness for Ith point H1 = Halsey parameter #1H2 = Halsey parameter #2H3 = Halsey parameter #3HJ1 = Harkins and Jura parameter #1HJ2 = Harkins and Jura parameter #2HJ3 = Harkins and Jura parameter #3PrelI = relative pressure for the Ith point (mmHg)

With the (tI,VI) data pairs, the Akima semi-spline interpolation method is used to interpolate volume adsorbed values based on thickness values that are evenly spaced 0.2 Angstrom apart starting at the first outlier point. Outliers are defined as those points have the maximum instantaneous slope within an iteratively shrinking subset of all points. The remaining pore surface area calculation result is the slope of the line defined by two consecutive interpolated points. The slopes of each pair of consecutive points from the origin to the last point must be monotonically decreasing and non-negative. With the interpolated points set the following can be calculated:

Average pore hydraulic radius (Å):

10. Mikhail, R., Brunauer, S. and Bodor, E., J. Colloid and Interface Sci. 24, 45 (1968)

tI H1 H2PrelI

( )ln--------------------×

H3=

tIHJ1

HJ2 PrelI( )log–

---------------------------------------HJ3

=

RItI tI 1–+

2------------------=

B-24 Feb 06


Remaining pore surface area for the Ith point (m2/g):

where

D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties dialog

Incremental pore surface area occluded for the Ith point (m2/g):

Cumulative pore surface area occluded for the Ith point (m2/g):

dA/dR pore surface area for the Ith point (m2/g-Å):

Incremental pore volume occluded for the Ith point (cm3/g):

Cumulative pore volume occluded for the Ith point (cm3/g):

dV/dR pore volume for the Ith point (cm3/g-Å):

SIVI VI 1––( ) D 10 6– m3/cm3×( )×

tI tI 1––( ) 10 10– m/A×-------------------------------------------------------------------------------=

SINCISI 1– SI–=

SCUMISINCI

SINCI 1–… SINC1

+ + +=

dAdRI--------

SINCI

tI tI 1––------------------=

VINCISINCI

104 cm2/m2×( ) RI 10 8– cm/Å×( )×=

VCUMIVINCI

VINCI 1–… VINC1

+ + +=

dVdRI--------

VINCI

tI tI 1––------------------=

Feb 06 B-25

Gemini V Windows Straight-Wall Sample Tubes

C. ANALYZING SAMPLES WITH TOTAL SURFACE AREA OF 1.0 m2 OR LESS

When analyzing samples with a surface area of 1.0 m2 or less, use filler rods in the balance and sample tubes to ensure optimum precision and accuracy. Two filler rods are included in the accessory kit. Insert them as described below. Refer to Preparing Samples, page 4-15 for instructions on cleaning and weighing sample tubes.

Straight-Wall Sample Tubes

1. Two filler rods are provided. Insert the longer filler rod into the balance tube by holding the balance tube horizontally and sliding the filler rod into the balance tube slowly.

Figure C-1. Inserting Filler Rod

2. After placing sample in the sample tube, insert the shorter filler rod into the sample tube as shown above.

3. Ensure that the filler rods are equidistant from the top of each tube. If they are not, add more sample or compact the sample until they are the same distance from the top of the tube.

Packing of some powders may restrict gas access to the powder and cause slower equilibration and/or lower results.

Feb 06 C-1

Straight-Wall Sample Tubes Gemini V Windows

Figure C-2. Balance and Sample Tubes with Filler Rods

4. Attach the balance tube to the balance port (refer to Installing the Sample Tube on page 4-20).

5. Attach the sample tube to the analysis port (refer to Installing the Sample Tube on page 4-20).

6. Perform the analysis as described Performing an Analysis, page 4-14. (Measure must be selected for Free Space.)

C-2 Feb 06

Gemini V Windows Bulb Sample Tubes

Bulb Sample Tubes

If the sample is bulky and of low surface area, the analysis may produce poor BET fit or poor reproducibility. If this occurs, we recommend using the following procedure:

1. Use the bulb sample tubes. Add sample to the sample tube and an equal volume of glass beads to the balance tube.

2. Slowly add a long filler rod to each tube (the filler rods should be the same size and should be equidistant from the top of each tube). Then, follow steps 4 through 6 in the preceding section of this appendix.

Figure C-3. Balance and Sample Tubes with Glass Beads and Filler Rods

Measure must be selected for free space option.

Make sure the filler rods reach all the way to the bottom of both tubes. It may be necessary to gently shake the tubes until the rods reach the bottom. If the rods do not reach the bottom of the tubes, refer to the next section, Hanging Filler Rods.

Filler Rod

SampleGlass Beads

Filler Rod

Feb 06 C-3

Hanging Filler Rods Gemini V Windows

Hanging Filler Rods

The Hanging Filler Rod Kit contains the following:

• Two connectors with hooks attached• Two filler rods

To insert the filler rods:

1. Remove the balance connector using an 11/16-in. wrench.

2. Remove and inspect the frit and O-ring for contamination and wear; replace if needed.

Figure C-4. Hanging Filler Rod

3. Insert the sample connector, frit, and O-ring in the port. Tighten the connector using an 11/16-in. wrench. Do not overtighten.

4. Attach a filler rod to the support hook.

Do not interchange the 2-µm frit (fine texture) from the balance port with the 40-µm frit (coarse texture) on the sample side. The instrument will not function properly if this occurs.

O-ring

Frit

Balance Connector

Support Hook

Hanging Filler Rod

After inserting the balance connector, turn the attached hook clockwise to ensure that it fits snugly.

C-4 Feb 06

Gemini V Windows Hanging Filler Rods

5. Place the connector nut, ferrule and O-ring on the balance tube stem.

6. Attach the balance tube to the port. Make sure it is fully in the port. Secure it in place by screwing the connector nut into the port.

7. Repeat steps 1 through 6 for the sample port.


O-ring

Ferrule

Connector Nut

Sample Tube Stem

Measure must be selected for the free space option.

Feb 06 C-5

Gemini V Windows Index

INDEX

$ symbol, 8-7, 8-9

AAdd log entry, 8-10Add Log Entry dialog, 5-8Add Log Entry push button, 5-6Adding an analyzer, 2-16Adsorbate, 1-18Adsorbate property factor, 5-36Adsorbed layer, B-8Adsorptive gas, 5-18Adsorptive Properties dialog, 5-18Adsorptive properties file, 5-18

creating, 4-11listing file statistics, 4-24, 5-59opening, 3-3printing contents, 4-23, 5-58

Adsorptive push buttonBJH report, 5-35Dubinin report, 5-43

Advanced format, 5-4, 5-5, 8-2creating sample file, 4-5establishing sample defaults, 4-3sample defaults, 8-8sample information file, 8-2

All file status, 3-8Analysis

blank, 9-5canceling, 6-4Dewar, 1-18method, 5-17performing, 4-14, 4-21, 6-2port frit, replacing, 9-4preparing for, 4-14small surface area, C-1

Analysis Conditions dialog, 5-12Analysis conditions file, 5-12


Analysis dialog, 6-2Analysis Method dialog, 5-17Analysis Preparation dialog, 5-15Analysis program

exiting, 5-64installing upgrade, 2-15subsequent installation, 2-15

uninstalling, 2-22using, 3-1

Analyzeradding another, 2-16changing setup, 2-21cleaning, 9-3configurations, 6-11environment, 1-17installing multiple, 2-5location, 1-15moving to a different computer, 2-17physical dimensions, 1-18rear panel connections, 2-4removing, 2-20setting up, 2-2specifications, 1-17turning on, 3-1verifying operation of, 2-10See also Equipment

Analyzing file status, 3-8Astakhov report, 5-42Autoscale, 5-41

in Control Chart reports, 7-12selecting options, 7-8

Axiscoordinates, viewing, 7-21properties, editing, 7-20

Axis Properties dialog, 7-20

BBalance connector, C-4Balance tubes, 4-16, 4-20

cleaning, 4-16degassing, 4-15installing, 2-11

Basic format, 5-4, 8-2creating sample file, 4-7sample file defaults, 4-1, 8-6Sample information file, 5-7, 8-3

BET Surface Area report, 5-25calculations, B-3example of, 7-23

BET Surface Area Report Options dialog, 5-25Bitmap graphic, in report title, 5-20BJH Adsorption/Desorption Plot Options dialog, 5-40BJH Adsorption/Desorption report, 5-34

calculations, B-8examples, 7-25

Feb 06 Index-1

Index Gemini V Windows

plots, 5-40tabular, 5-38

BJH Adsorption/Desorption Report Options dialog, 5-34BJH Adsorption/Desorption Tabular Report Column

Options dialog, 5-38BJH Adsorption/Desorption Tabular Report Options

dialog, 5-38BJH Adsorption/Desorption)Fixed Pore Size Table

dialog, 5-39BJH Adsorptive Options dialog, 5-35BJH Adsorptive Property Factor dialog, 5-35BJH correction, 5-36Blank analysis, 9-5

performing, 9-5Bookmarks tab, 1-5, 1-8Broekhoff-de Boer equation, 5-31Broekhoff-de Boer thickness curve, 5-31, B-6Browse push button, 3-6, 6-2

CCalculated free space, 5-16, 6-11Calculation assignment, 5-15Cancel push button, 6-4Carbon Black STSA thickness curve

See STSA thickness curveCascade windows, 3-11Cautions, defined, 1-3Check box, 3-5Cleaning

analyzer, 9-3sample tubes, 4-16

Close All command, 5-57Close command, 5-57Close Reports command, 7-5Collected data, 5-53Columns, editing on onscreen reports, 7-18Comments window, 5-6, 8-10Communications cable, connecting, 2-5Complete file status, 3-8Computer requirements, 1-19Control Chart command, 7-11Control Chart dialog, 7-11Control Chart Graph Options dialog, 7-12Control Chart report, 7-11

defining the Y-axis, 7-12recalculating archived results, 7-12

Control Chart Sample Selection dialog, 7-12Conventions

file name, 3-9for operator’s manual, 1-3

Convert command, 5-63Convert StarDriver Sample Files dialog, 5-63Converting StarDriver files, 5-63

Coolant, 1-15verifying level, 4-14

Correctionfactor, surface area, 5-32volume, 6-11

Cross hair, axis, 7-21Cross-references, 1-8Cryogen, 1-15

verifying level, 4-14Curve Properties dialog, 7-19

DData

collected, 5-53entered, 5-53points, 1-11

Date format, changing, 3-7Date Range push button, 3-7Default Style dialog, 7-17Defaults

parameter files, 4-3sample files, 4-1

Degas Conditions dialog, 5-10Degas conditions file, 5-10

creating, 4-8listing file statistics, 4-24, 5-59printing contents, 4-23, 5-58

Degasser, 1-16, 2-6Degassing, 9-4Density

conversion factor, 5-18sample, 5-6, 5-7

Dewar, 1-18precautions, 4-14

Dialog boxes, using, 3-4Directory, 3-8Drying oven, 4-16Dubinin Adsorptive Options dialog, 5-43Dubinin report, 5-42

pore volume plot, 5-46tabular, 5-44transformed isotherm plot, 5-45types available, 5-42

Dubinin Report Options dialog, 5-42, 5-44, 5-46Dubinin Tabular Report Column Options dialog, 5-44Dubinin Transformed Isotherm Plot Options dialog, 5-45Dubinin-Astakhov calculations, B-20Dubinin-Radushkevich calculations, B-18

EElectrical requirements, 1-18Enhanced metafile, in report title, 5-20

Index-2 Feb 06


Entereddata, 5-53free space, 5-16t-Curve, 5-29

Entered file status, 3-8Entered t-Curve dialog, 5-29Environment, 1-17Equation push button, 5-47Equilibrate method, 5-17Equipment

cleaning, 9-3damaged or lost, 2-1description, 1-11dimensions and weight, 1-18installation, 2-2location, 1-15, 1-17return, 2-1specifications, 1-17unpacking, 2-1See also Analyzer

Error messages, A-1Exit command, 5-64Exiting the analysis program, 5-64Export command, 5-61Export Sample File dialog, 5-61Exporting sample files, 5-61

FFile

printing to, 7-4selecting, 3-6status, 3-7, 3-8

File menu, 5-1Close All command, 5-57Close command, 5-57Convert command, 5-63description, 5-1Exit command, 5-64Export command, 5-61List command, 5-59Open command, 5-3Print command, 5-58Save All command, 5-57Save command, 5-56

File namedefault extensions, 3-9, 5-3included as part of ID, 8-7, 8-9sequence, 8-6

Filler rod, 6-5hanging, C-4inserting, C-1

Find command, 1-9Fitted thickness range, 5-32

Flash card SeeSoftware card

Free space, 1-14, 5-16calculated, 5-16, 6-11calculations, B-1dialog, 5-15editing, 5-54entered, 5-16previously measured, 5-16push button, 4-10

Frenkel-Halsey-Hill thickness curve, 5-28Frequency requirements, 1-18Frit

See Port fritFunction keys

See Shortcut keys

GGas

behavior, 1-14connecting, 2-3purity, 1-15regulator, attaching, 2-2regulators, 1-15, 4-14requirements, 1-15

Gas bottle pressure, 2-3Graph

copying as metafile, 7-21editing onscreen, 7-19grid lines, 8-5legend, editing, 7-20overlays, 4-26

Graph Grid Lines command, 8-5Graph Grid Lines dialog, 8-5Graph Overlay Samples dialog, 5-20Graphic, in report title, 5-20Grid lilnes, 8-5

HHalsey Thickness Equation, 5-30, B-6Harkins and Jura equation, 5-47Harkins and Jura Thickness Equation, 5-31, B-6Helium purity, 1-15

IIndex, online, 1-8Insert Predefined Pressures dialog, 5-14Insert Pressure Range dialog, 5-13Instrument log, 6-9Instrument schematic, 6-6

Feb 06 Index-3


Isotherm data, exporting, 4-25Isotherm Plot Options dialog, 5-23Isotherm report, 5-23

example of, 7-22Isotherm Report Options dialog, 5-23

KKeypad, 1-1

version, updating from, 2-7Kruk-Jaroniec-Sayari Thickness Equation, 5-30

LLangmuir Surface Area report, 5-25

calculations, B-4Langmuir Surface Area Report Options dialog, 5-25Leak checking, 9-5Legend Properties dialog, 7-20Links, 1-7Liquid nitrogen, 1-15List command, 5-59List Sample Information dialog, 5-59List, generating, 5-59Loading a sample, 4-20Log entry, 5-8Log Report settings dialog, 6-9

MMain menu, 3-10Manual

See Operator manualMenu structure, 3-10Metafile, copying graphs as, 7-21Monitor resolution, 1-19MP-Method Plot Options dialog, 5-50MP-Method report, 5-47

calculations, B-24plots, 5-50tabular, 5-49types available, 5-48

MP-Method Report Options dialog, 5-47MP-Method Tabular Report Column Options dialog,

5-49

NNext push button, 6-4Nitrogen purity, 1-15No analysis file status, 3-8Non-ideality factor, 5-18Notes, defined, 1-3

Numerical fields, valid ranges, 3-4

OOnline manual

cross references, 1-8index, 1-8printing options, 1-10using, 1-5See also Operator’s manual

Open command, 5-3Open dialog, 7-5Open Report command, 7-5Open Sample Information File dialog, 3-6, 5-3Operation, verifying, 2-10Operator, specifying, 8-10Operator’s manual

conventions, 1-3online, 1-5organization, 1-1See also Online manual

Option Presentation command, 8-2Options menu, 8-1

Graph Grid Lines command, 8-5Option presentation command, 8-2Parameter Files Directory command, 8-12Sample Defaults command, 8-6Units command, 8-4

Options report, 5-52example of, 7-27

Ordering information, 10-1O-ring, replacing, 9-4Outlier points, 5-15Overlay

Graph overlay, 4-26multiple graphs, 4-30multiple samples, 4-27

Overlay samples, 5-25, 5-32Overlays push button, 5-20

PP0 Measurement dialog, 6-5Parameter File Directory Selection dialog, 8-12Parameter files, 4-8, 5-4

Adsorptive properties, creating, 4-11Analysis conditions, creating, 4-10creating, 5-3Degas conditions, creating, 4-8establishing defaults, 4-3, 8-8listing file statistics, 4-24printing contents of, 4-23Report options, creating, 4-12specifying location, 8-12

Index-4 Feb 06


Parameter Files Directory command, 8-12Parts, ordering, 10-1Password

restricted format, 8-3Service test mode, 8-12

Po and T push button, 5-16Po and Temperature Options dialog, 5-16Port frit, replacing, 9-4Power cord, connecting, 2-2Power failure, recovering from, 9-3Power requirements, 1-18Preparation push button, 5-15Prepared file status, 3-8Preparing file status, 3-8Preparing for analysis, 4-14Presentation options, 8-2Pressure

measurement, 1-17relief valve for gas regulator, 1-15, 2-2table, 5-13

Pressures push button, 5-36Print command, 4-23, 5-58Print dialog, 7-15Print Sample Information File dialog, 5-58Printing to a File

description, 5-58Push button, 3-5

Browse, 3-6Date Range, 3-7Free Space, 5-15Overlays, 5-20Po and T, 5-16Preparation, 5-15Replace, 3-6

RRadio button, 3-5Radushkevich report, 5-42Ramp rate, 5-11Ranges, for numerical fields, 3-4Rear panel connections, 2-2, 2-5Regression report, 7-7

recalculaing SPC values, 7-10selecting X- and Y-Axes variables, 7-8

Regression Report command, 7-7Regression Report Options dialog, 7-7Regression Report Sample Selection dialog, 7-8Regulators

attaching, 2-2gas, 1-15verifying pressure, 4-14

Relative pressure, B-8Removing an analyzer, 2-20

Replace All pushbutton, 5-6Replace push button, 3-6Report

BET Surface Area, 5-25BJH Adsorption/Desorption, 5-34closing, 7-5Control Chart, 7-11displaying company logo in title, 5-20Dubinin, 5-42examples, 7-22generating, 4-22, 7-3graphs, editing onscreen, 7-19header, 7-14Isotherm, 5-23, 7-22Langmuir surface area, 5-25legend, editing, 7-20MP-Method, 5-47onscreen, 7-14onscreen, shortcut menus for, 7-18opening, 7-5Options, 5-52Regression, 7-7Sample log, 5-52saving in other formats, 7-16Statistical Process Control (SPC), 7-6Summary, 5-22Tabular, editing onscreen, 7-18title, showing, 5-19Tool bar, 7-15t-Plot, 5-28window, 7-14zoom feature, 7-21

Report button, 7-10Report Options dialog, 5-19Report options file, 5-19


Report Pressure Table dialog, 5-26Report Relative Pressure Range dialog, 5-32Reports menu, 7-1

Close Reports command, 7-5Control Chart command, 7-11Open report command, 7-5Regression Report command, 7-7SPC Report Options command, 7-6Start Report command, 7-3

Restricted format, 8-2, 8-3creating sample file, 4-7default values, 4-1Sample information file, 5-9

Return Materials Authorization (RMA), 2-2RS-232 cable, connecting, 2-5

Feb 06 Index-5


SSample

degassing, 4-15density, 5-6, 5-7, 8-7information, defining, 4-5preparation, 1-16, 4-15weighing, 4-18weight accuracy, 4-17with surface area of 1.0 m2 or less, C-1

Sample Analysis command, 6-2Sample defaults

Advanced format, 8-8Basic format, 8-6Restricted format, 8-6specifying, 8-6

Sample Defaults command, 8-6Sample Defaults dialog

Advanced format, 8-8Basic format, 8-6

Sample file namespecifying default sequence, 8-9

Sample information dialogAdvanced format, 5-5Basic format, 5-7

Sample information file, 3-6, 5-4Advanced format, 4-5, 5-4, 5-5Basic format, 4-7, 5-4, 5-7creating, 4-5, 5-3Default values, 4-1defaults for Advanced format, 8-8establishing defaults for Advanced format, 4-3exporting, 5-61exporting isotherm data, 4-25generating a list, 5-59listing file statistics, 4-24opening, 3-3printing contents, 4-23Restricted format, 4-7, 5-4, 5-9specifying defaults, 4-1, 8-6status, 3-8

Sample Log report, 5-52example of, 7-29

Sample tubes, 1-18blank, 9-5bulb, C-3cleaning, 4-16straight wall, C-1

Saturation pressure, 5-16measuring, 6-5

Save All command, 5-57Save As command, 5-56Save as Default button, 7-13Save As t-Curve dialog, 5-57

Save command, 5-56Scan method, 5-17Schematic, 1-13

displaying, 6-6Screen resolution, 1-19Select Dates dialog, 3-7Select Reports dialog, 7-3Selecting files, 3-6Setup program

adding an analyzer, 2-16changing an analyzer setup, 2-21moving an analyzer to a different computer, 2-17reinstalling analysis program, 2-15removing an analyzer from the computer, 2-20uninstalling the software, 2-22using for other functions, 2-13

Shortcut keys, 3-2for Select Dates dialog, 3-7list of, 3-3

Shortcut menu, 3-2for graphs, 7-19for tabular reports, 7-18

Show Instrument Log command, 6-9Show Status command, 6-8Soak

temperature, 5-10time, 5-11

SoftwareAnalysis program, 2-7current version, 6-11installing, 2-7installing upgrade, 2-15using, 3-1using for offline data reduction, 2-7

Software card, installing and removing, 2-5SPC Calculations dialog, 7-6SPC report, 7-6SPC Report Options command, 7-6Specifications, 1-17Spreadsheet format

exporting isotherm data, 5-61saving reports, 7-16

StarDriver files, converting, 5-63Start Analysis dialog, 4-21Start Po measurement command, 6-5Start push button, 6-4Start Report command, 7-3Start Report dialog, 7-3Status window, 6-8Status, file, 3-8, 7-4STSA thickness curve, 5-31, B-6Submitter, specifying, 8-10Summary report, 5-22

example of, 7-28

Index-6 Feb 06


Summary Report Options dialog, 5-22Surface area correction factor, 5-32Surface Area Report Pressure Selection dialog, 5-27System requirements, 1-15

TTable of Contents, online, 1-7t-Curve

entered, 5-29saving, 5-57

Temperatureanalysis, 5-16soak, 5-10

Text, copy graph data as, 7-21Thermal

diffusion, 1-14gradient, coolant bath, 1-14

Thickness curve, 5-28Broekhoff-deBoer, 5-31Carbon Black STSA, 5-31Entered, 5-29Frenkel-Halsey-Hill, 5-28Halsey, 5-48Harkins and Jura, 5-31Kruk-Jaroniec-Sayari, 5-30

Thumbnails tab, 1-10Tile windows, 3-11Title Properties dialog, 7-21Tool bar, reports window, 7-15t-Plot report, 5-28

calculations, B-6example of, 7-24

t-Plot Report Options dialog, 5-28Transformed isotherm plot, 5-45Troubleshooting, 9-1

UUltrasonic cleaning unit, 4-16Unit configuration dialog, 6-11Unit menu, 6-1

Sample Analysis command, 6-2Show Instrument Log command, 6-9Show Status command, 6-8Start Po measurement command, 6-5Unit Configuration command, 6-11

Units command, 8-4Units Selections dialog, 8-4USB hardware, 2-5

ordering, 10-2Use calculation assignments, 5-15, 5-54

VVacuum pump, 1-16, 1-17

connecting, 2-5Vacuum, verifying, 4-14Valves

location of, 1-13system, 6-6

View drop-down list, 6-2Voltage requirements, 1-18Volume

adsorbed, B-8correction, 6-11

WWarnings, defined, 1-3Weighing the sample, 4-18Windows menu, 3-11

ZZoom feature, 7-21

Feb 06 Index-7

Documents

gemini v - Micromeritics...The Gemini Windows® program is designed to enhance the operation of the Gemini V ana-lyzer, allowing you to prepare sample files, perform analyses, and