F-3004 Peltier Sample Cooler...tions jack inside the sample cooler is firmly seated in the connection within the sample compartment. f Connect the 9-pin-female–9-pin-male’s female

Peltier Sample Cooler v. 1.0 (7 May 2004)

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F-3004 Peltier Sample Cooler

Operation Manual v. 1.0 http://jobinyvon.com

In the USA: Jobin Yvon Inc. 3880 Park Avenue, Edison, NJ 08820 In France: Japan: +81 (0) 3 58230140Tel:+1-732-494-8660 16-18, rue du Canal China: +86 (0) 10 6849 2216 Fax: +1-732-549-5157 91165 Longjumeau cedex Germany: +49 (0) 89 462317-0 E-Mail: [email protected] Tel: +33 (0) 1 64 54 13 00 Italy: +39 0 2 57604762 1-800-533-5946 Fax: +33 (0) 1 69 09 93 19 U.K.: +44 (0) 8204 8142


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Copyright 2001, 2004 by Jobin Yvon Inc. All rights reserved. No part of this work may be reproduced, stored in a retrieval system, or transmitted in any form by any means, including electronic or mechanical, photocopying and recording, without prior written permission from Jobin Yvon Inc. Requests for permission should be requested in writing. Information in this manual is subject to change without notice and does not represent a commitment on the part of the vendor. May 2004

Part Number 81049


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Table of Contents

0: Introduction ........................................................... 1 The Peltier effect ....................................................................................... 1 Symbols used in this manual..................................................................... 1

1: Requirements & Installation ....................................... 2 Requirements ............................................................................................ 2 Installation ................................................................................................. 3

2: System Operation .................................................... 9 Introduction................................................................................................ 9 To adjust the magnetic stirrer .................................................................. 10 To purge the sample holder..................................................................... 11 To adjust the basic Peltier-device parameters ........................................ 12 To run batch temperature-control experiments ....................................... 20

3: Troubleshooting .....................................................25 For further assistance… .......................................................................... 26

4: Specifications .......................................................27 Computer requirements........................................................................... 27 Software requirements ............................................................................ 27 Operating specifications .......................................................................... 27 Electrical and physical specifications ...................................................... 27

5: Index ..................................................................28


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Peltier Sample Cooler v. 1.0 (7 May 2004) Introduction

1

Warning:

Note:

0: Introduction The Peltier effect

Jean Peltier discovered a thermoelectric effect in 1834, in which electricity flowing through certain materials causes a temperature gradient across those materials. Specifically, Peltier noticed that an electric current moving through two different conductors can cause emission or absorption of heat. That is, when electricity flows through a substance such as bismuth telluride (Bi2Te3), heat is moved across the material, creating a warmer side and a colder side. Modern research on the “Peltier effect” shows that the charge carriers in doped semi-conductors push hear in the direction of their motion. Therefore, reversing the current’s di-rection changes the warm side to the cool side, so that the Peltier device may be used to heat a sample as well as cool it. Peltier devices are used to cool integrated circuitry, semiconductor photodetectors, and even food in picnic coolers. Their advantages over conventional cooling units are: no moving parts, small size, no refrigerant fluids, no vibration or mechanical noises, and high stability and long life. Their major disadvantage is their relative inefficiency. The Peltier Sample Cooler is an automated temperature controller for samples inside the SPEX® series of spec-trofluorometers. Thermoelectric heating and cooling controls the sample temperature faster than conventional water baths. A magnetic stirring system to keep your sample homogene-ously mixed, and a port for nitrogen gas purging (to reduce condensation on a chilled sam-ple) are included in the Peltier Sample Cooler.

Symbols used in this manual Certain symbols are used throughout the text for special conditions when operating the in-struments:

A hazardous condition exists, or danger exists that could damage the equipment. Jobin Yvon Inc., is not responsible for damage arising out of improper use of the equipment.

General information is given concerning operation of the equipment.

Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation

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1: Requirements & Installation Requirements

Computer requirements • Dedicated serial COM port • DataMax software • Windows™ 95 or higher • 973005 or equivalent PC computer

Electrical requirements • 115 VAC or 230 VAC ±15% (switch selectable), 60 or 50 Hz • 25 W average with output off; 55 W average with output on

Physical Requirements • Controller must be within 36" (90 cm) of Peltier Sample Cooler (communications cable

length)


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Note: Many public carriers do not recognize claims for concealed damage reported later than 15 days after delivery. For a shipping damage claim, inspection by the carrier agent normally is re-quired. Therefore, the original packing material should be kept as evidence. While Jobin Yvon is not liable for damage occurring during transit, the company will extend every effort to aid and ad-vise.

Installation 1 Unpack and inspect all components.

a The following Peltier Sample Cooler components should be included:

Quantity Description Part Number

1 Peltier Sample Cooler 400313 1 Sample-cooler cover 1 Control unit with 50-Ω BNC terminator LFI-3751 1 Peltier Sample Cooler Operation manual 81049 1 Wavelength Electronics™ User’s Guide with extra parts 1 9-pin-male-to-9-pin-female cable 400367 1 9-pin-to-25-pin RS-232 cable 35506 1 Power cord (115 V or 220 V) 98015 or 98020 4 #4-40 × 1¼" screw for FluoroMax® installation 600105 4 #4-40 × 1½" screw for Fluorolog® installation 600104 1 Magnetic stirring bar 53044 1 Certificate of Calibration for control unit 1 3.5" diskette (only if Peltier Sample Cooler was pur-

chased separately form the spectrometer)

b Inspect all the components for signs of damage that may have occurred during transit. If damage is evident, do not continue with the installation. Notify Jobin Yvon and the shipper at once.

2 Read this instruction manual thoroughly before installing the Peltier Sample Cooler.

3 Install the Peltier Sample Cooler:


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a Remove the existing sample holder from the sample compartment of the spectrofluorometer.

b Install the control unit as directed in the Wavelength Electronics™ User’s Guide (Chapter 1, “Preparing the Temperature Controller for Use,” steps A through F).

c Make sure that the 50-Ω BNC terminator is attached to the ANALOG INPUT on the back of the controller.

d Connect the 25-pin–9-pin adapter cable’s 25-pin female end to the RS-232 OUTPUT on the back of the control unit.

e Attach the 9-pin female end of the the 25-pin–9-pin adapter cable to the COM2 port on the host computer.


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Note: Be sure that the communica-tions jack inside the sample cooler is firmly seated in the connection within the sample compartment.

f Connect the 9-pin-female–9-pin-male’s female end to the OUTPUT jack on the back of the control unit.

g Attach the 9-pin-female–9-pin-male adapter cable’s male end to the jack on the front of the Peltier Sample Cooler.

h Insert the power cord into the jack on the control unit. Plug the other end of the power cord into a wall receptacle.

i Place the Peltier Sample Cooler into the sample compartment.


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Note: For installation in a Fluoro-Max®, use the shorter screws; for in-stallation in a Fluorolog®, use the longer screws.

j Attach the Peltier Sample Cooler to the front panel of the sample compartment using four #4-40 screws.

k (optional) If condensation may be a problem for the chilled sample, attach a dry-nitrogen gas line to the small metal purging inlet on the front of the sample cooler.

4 Install the software on the host computer. (only if the Peltier Sample Cooler was purchased separately from the spectrofluorometer)

5 Confirm that the upper and lower temperature limits are set correctly. a Start the instrument and computer, according to the instrument’s

instruction manual.

b Start DataMax.

c Choose a layout that includes a Peltier device.


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d Open Visual Instrument Setup.

e Click on the sample-holder icon.

The Sample Compartment Accessories dialog box opens.

f Choose the Temperature control option.

g Click on the thermometer icon.

The Peltier Setup dialog box opens.

h Click Advanced. The Dialog window appears.


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i Switch on the controller’s POWER button.

j Turn knob to SET T. This setting adjusts the temperature limits.

k Push the TEMP LIMIT button once. Starting with the upper temperature limit, the upper and lower temperature limits are displayed alternately.

l Push the TEMP LIMIT button once to release this display.

If the green LED display shows the limits that match the values in the Safety Limits area of the Dialog window, no further action is needed. If the green LED display does not match these values, change the values in the Safety Limits area of the Dialog window.

Peltier Sample Cooler v. 1.0 (7 May 2004) System Operation

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2: System Operation Introduction

Aside from the magnetic stirrer and nitrogen purge port, operation of the Peltier Sample Cooler is entirely user-controlled from the computer. There are two ways to alter the opera-tion of the Peltier Sample Cooler:

To adjust the basic Peltier-device parameters: • maximum and minimum allowable temperatures, • maximum and minimum allowable electric current to the Peltier device, and • PID settings for rate of temperature change and sensitivity of the control unit to the

thermal inertia of the sample holder,

Use the Peltier Setup dialog box from the Visual Instrument Setup within DataMax.

To modify temperature-based experiments: • how many temperature points at which to set, • what temperatures they ought to be, and • batch experiments,

Use the Peltier Batch Scan dialog box. Enter this dialog box from the Collect... command of the DataMax toolbar.


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To adjust the magnetic stirrer 1 Place the magnetic stirring bar in the sample

cuvette. 2 Place the cover on the Peltier Sample Cooler. 3 Close the lid of the spectrofluorometer’s sample

compartment. 4 Turn the knob on the front of the Peltier Sample

Cooler from OFF to the desired stirring speed. “0” is the slowest speed, and “10” is the fastest speed.


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To purge the sample holder Purging the sample holder with dry nitrogen gas is usually done when the sample tempera-ture is below the ambient dew point, i.e., in a cold, humid environment. Purging with dry ni-trogen prevents water condensation on the cuvette, improving spectroscopic scan quality.

1 Attach the dry-nitrogen gas line to the purging port.

2 Start the gas.


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To adjust the basic Peltier Sample Cooler parameters

1 In Visual Instrument Setup, click on the sample-holder icon.

The Sample Compartment Accessories dialog box appears.

2 Choose the Temperature control option. Other options, such as a sample changer, might be present.

3 Click on the thermometer icon.

The Peltier Setup dialog box appears. Basic operations are displayed in this window.

Note: The Vis-ual Instrument Setup may dif-fer from that shown here, based on the accessories and model of instrument.


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4 Adjust the parameters. The Temperatures area displays current and desired temperatures. The Output area displays the electrical status of the Peltier Sample Cooler. Use the Advanced button to adjust heating and cooling parameters, and electrical and thermal limits of the Peltier device.

5 Click Apply. The parameters are updated.

6 Click OK. The Peltier Setup dialog box closes.

Note: Values are up-dated approximately every 5 seconds.


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To adjust the set-point of the sample The Temperatures area displays the current Sample Block, Immersion, and Setpoint temperatures. 1 Enter the desired

sample temperature here.

2 Click Apply.

Note: If the temperature entered is beyond the user-selectable, al-lowable range of the Peltier Sample Cooler, a warning mes-sage appears.


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Note: For safety reasons, the maximum allowable current is factory-set to ±5.0 A. The software re-fuses to accept any value greater than a magnitude of 5.0 A. The temperature limits of the Peltier device are –10 to +110°C.

To set electrical and thermal limits

1 Click Advanced. The Dialog window appears.

2 Enter the maximum and minimum allowable temperatures in these two fields.

3 Enter the maximum positive and nega-tive allowable cur-rents in these two fields.

4 Click OK. 5 Click Apply in the

Peltier Setup dialog box.

6 Adjust the controller to match:


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a Turn knob to SET T. This setting adjusts the temperature limits.

b Push the TEMP LIMIT button once. Starting with the upper temperature limit, the upper and lower temperature limits are displayed alternately.

c When the upper temperature limit is displayed, turn the knob immediately to the desired value matching that in the Dialog window.

d Push the TEMP LIMIT button once to confirm.

e Push the TEMP LIMIT button once. Starting with the upper temperature limit, the upper and lower temperature limits are displayed alternately.

f When the lower temperature limit is displayed, turn the knob immediately to the desired value matching that in the Dialog window.

g Push the TEMP LIMIT button once to confirm.


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To start or stop the heating or cooling cycles The electrical output of the controller is displayed in this area.

1 Choose Enable to start the Peltier Sam-ple Cooler,

OR

2 Choose Disable to stop the Peltier de-vice.

3 Click Apply.

Note: If the Enable button does not engage and start operation of the Peltier, check connections and settings to the Peltier device.


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To change PID parameters Instructions

1 Click Advanced. The Dialog window appears.

2 Enter the new set-tings in the Peltier Device Control area.

3 Click Restore De-faults to return the PID values back to Jobin Yvon’s default settings.

4 Click OK. The Dialog window closes.

5 Click Apply in the Peltier Setup window.


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Note: Jobin Yvon has set the PID values for an op-timum response from the Peltier device. We do not recommend changing these default values.

About PID parameters P = Proportional Gain The “Error Voltage” is the difference between set-point voltage (the desired temperature) and measured thermocouple voltage (actual temperature). The proportional gain, P, supplies a current proportional to the Error Voltage. If P is large, the Peltier device approaches the desired temperature rapidly. This, however, may overshoot the desired temperature. As the Error Voltage drops to 0 when the actual temperature reaches the set-point, so does P, cut-ting off heating or cooling. Thus over- and undershoots of the set-point may happen without adjusting the next two parameters listed below.

I = Integrator The integrator charges up based on how close the Error Voltage is to 0. Rapid charging (small integrator time-constant, or Integrator Time Const.) occurs if the Error Voltage is large; slow charging (large time-constant) occurs if the Error Voltage is small. At Error Voltage = 0, no charging occurs, and the output current is run via the integrator. Try to keep the time-constant large enough to compensate for the thermal inertia of the sample holder and Peltier device, otherwise the temperature may oscillate.

D = Differentiator The Differentiator (or Differentiator Time Const.) uses the change in Error Voltage with time, dV/dt (the derivative). The faster the Error Voltage changes (the larger the slope of dV/dt), the larger the “opposing” current. Thus, the Differentiator opposes radical changes in the sample’s temperature.


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To run batch temperature-control experiments

1 In the DataMax toolbar, choose Collect. A drop-down menu appears.

2 Choose Temperature Scan…. This opens the Temperature Scan dialog box.

3 Choose a predeter-mined experimental setup or existing file with these buttons.

4 Adjust parameters related to the tem-perature during a scan.

5 Get help.


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To choose a single experimental setup Enter the full pathname for an experimental setup here,

OR Click on Exp. Browse to browse through a folder of experimental-setup files:

Choose the drive and directory in this area.

Click on Info to pre-view a file.

From the list, click on a file to use. It is highlighted in the space.

List all files of types *.exp or *.*


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To search for specific output files Output files from the spectrometer are of the form .spc

Enter a unique file name with the file path,

OR Click on File Browse. This opens the Select File Name dialog box, and selects a file for overwriting—all previous data in that file will be lost:

Choose the drive and directory in this area.

Click on Info to pre-view a file.

From the list, click on a file to use. It is highlighted in the space.

List all files of types *.spc or *.*


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To adjust temperature-control parameters

1 Click Temp Control…. The Temperature Control dialog box opens.

2 Enter the ex-periment’s starting tem-perature in Start Temp.

3 Enter the experiment’s final tem-perature in End Temp.

4 Enter how many different temperatures the Peltier should reach in Number of Temps.


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5 Enter the Tolerance (how close, in °C, the heater must be to the desired temperatures).

6 Enter the Equilibration Time. Equilibration Time is how long, in min, the heater waits before moving to the next tem-perature.

7 Choose to Insert, Replace, or Add to End a new temperature into the list, then type the value into the field.

8 Choose Probe to measure an external thermo-couple’s tem-perature, or Bath for the Peltier device’s temperature.

9 Check this box to shut off the Peltier de-vice after the experi-ment.

10 Enter the Standby Tempera-ture (at which the Peltier holds af-ter the experi-ment ends).

11 Click OK. The Temperature Control dialog box closes.

Peltier Sample Cooler v. 1.0 (7 May 2004) Troubleshooting

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3: Troubleshooting Consult the Wavelength Electronics™ User’s Guide for any problems that may occur with the control unit. Below are listed some problems that might occur:

Problem Possible Cause Suggested Remedies

Disconnected power cord Connect power cord..

Faulty wall receptacle Check wall receptacle.

Control unit does not turn on.

Fuse is blown Check and replace fuse.

No Peltier layout available Peltier Sample Cooler will not operate

Communications cables have bad connection

Select layout with Peltier in Visual Instrument Setup.

Check communications cables.

Check connection between spectro-fluorometer and Peltier Sample Cooler inside sample compartment.

Check all software settings.

Peltier Sample Cooler v. 1.0 (7 May 2004) Troubleshooting

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For further assistance... Before contacting the service department, complete the following steps:

1 Reboot the system if this the first time the prob-lem has occurred. a Turn off the system and accessories.

b After a cool-down period, turn the system back on and see if the failure persists.

2 Make sure all accessories are properly config-ured and switched on as appropriate.

3 Check the Troubleshooting chart to see if the problem is duscussed.

4 Try to duplicate the problem. Write down the steps required to repeat the error. Our service engineers will attempt to do the same with a test system.

5 If a DataMax software error or Windows™ error is displayed, write down the exact error shown.

6 Determine the serial numbers. a Open

DataMax.

b In the Instrument Control Center, under Help, find the version of the software.

c Make a note of the instrument’s serial number and instrument configuration, including all the accessories.

7 If you require further assistance in the United States, call us at (732) 494-8660, fax us at (732) 549-5157, or send an e-mail to service. Outside the United States, contact your local distributor.

Peltier Sample Cooler v. 1.0 (7 May 2004) Appendix

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4: Specifications Computer requirements

• 973005 or equivalent PC computer with RS-232 port

Software requirements • Windows™ 9x or NT4 (SP3 or higher) • DataMax 2.2.10

Operating specifications • Ambient environment for controller: 0–55°C • Minimum Peltier temperature for samples = –10°C • Maximum Peltier temperature for samples = +110°C • Display update to software ~ 0.2 Hz (every 5 s)

Electrical and physical specifications • 115 VAC or 230 VAC ±15% (switch selectable), 60 or 50 Hz • 25 W average with output off; 55 W average with output on • 3 ⁄32" (2.4 mm) O.D. inlet for dry-nitrogen purging • Controller dimensions are 4¼" (10.8 cm) W × 7" (17.8 cm) H × 1211 ⁄16" (32.2 cm) D

(allow 2¾" [7 cm] extra clearance depth for cables) • Peltier Sample Cooler dimensions are 6¼" (15.9 cm) W × 7½" (19.1 cm) H × 9" (22.9

cm) D

Peltier Sample Cooler v. 1.0 (7 May 2004) Index

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5: Index Key to the entries: Times New Roman font ...........subject or keyword Arial font....................................command, menu choice, or data-entry field Arial Condensed Bold font .......dialog box

2

25-pin–9-pin adapter cable................................ 4

9

9-pin-female–9-pin-male adapter cable............ 5

A

Add to End...................................................... 24 Advanced........................................7, 13, 15, 18 Analog Input ..................................................... 4 Apply ..............................................14, 15, 17, 18

B

batch..............................................................9, 20 Bath.................................................................. 24 bismuth telluride ................................................ 1 BNC terminator.................................................. 4

C

cable....................................................2, 3, 25, 27 Certificate of Calibration ................................... 3 Collect..........................................................9, 20 COM port ........................................................... 2 COM2................................................................. 4 computer...............................................2, 6, 9, 27 condensation.............................................1, 6, 11 controller ................................3, 4, 5, 8, 9, 15, 25 cover .............................................................3, 10 current temperature.......................................... 13

D

damage ........................................................... 1, 3

danger ................................................................. 1 DataMax.................................. 2, 6, 9, 20, 26, 27 derivative..........................................................19 Dialog ...........................................7, 8, 15, 16, 18 differentiator.....................................................19 dimensions........................................................27 directory......................................................21, 22 Disable.............................................................17 diskette................................................................ 3 drive............................................................21, 22 dV/dt..................................................................19

E

Enable..............................................................17 Equilibration Time .........................................24 Error Voltage....................................................19 exp ...................................................................21 Exp. Browse ...................................................21 external thermocouple .....................................24

F

File Browse.....................................................22 final temperature ..............................................23 fuse....................................................................25

H

hazardous condition ........................................... 1 Help ..................................................................26 host computer..................................................... 6

I

Immersion .......................................................14 Info..............................................................21, 22 Insert ............................................................5, 24 Instrument Control Center ...............................26


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integrator...........................................................19

J

Jean Peltier..........................................................1

L

layout ................................................................25

M

magnetic stirrer.........................................1, 9, 10

N

nitrogen...........................................1, 6, 9, 11, 27

O

OK...............................................................15, 18

P

pathname ..........................................................21 Peltier Batch Scan..............................................9 Peltier device ......................... 1, 9, 13, 17, 19, 24 Peltier effect........................................................1 Peltier Setup.......................... 7, 9, 12, 13, 15, 18 PID................................................................9, 18 power cord....................................................5, 25 preview .......................................................21, 22 Probe ...............................................................24 proportional gain ..............................................19 purge ...............................................1, 6, 9, 11, 27

R

reboot ................................................................26 Replace ...........................................................24 Restore Defaults............................................18 RS-232......................................................3, 4, 27

S

Safety Limits.....................................................8

Sample Block .................................................14 sample compartment..........................4, 5, 10, 25 Sample Compartment Accessories ............7, 12 sample temperature ................................1, 11, 14 sample-holder icon.............................................7 Select File Name..............................................22 serial number ....................................................26 SET T...........................................................8, 16 set-point ......................................................14, 19 Setpoint ...........................................................14 setup............................................................20, 21 software ....................................... 2, 6, 25, 26, 27 spc ...................................................................22 Standby Temperature ..................................24 starting temperature..........................................23 stirring speed ....................................................10 symbols...............................................................1

T

TEMP LIMIT ...............................................8, 16 Temperature control ...........................7, 12, 20 temperature limits.....................................6, 8, 16 Temperature Scan............................................20 thermal inertia...............................................9, 19 thermal limits..............................................13, 15 thermoelectric effect................. See Peltier effect thermometer icon .........................................7, 12 time constant.....................................................19 Tolerance ........................................................24 Troubleshooting .........................................25, 26

U

update................................................................27

V

Visual Instrument Setup ....................7, 9, 12, 25

W

Wavelength Electronics™ User’s Guide3, 4, 25 Windows™.............................................2, 26, 27


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Documents

F-3004 Peltier Sample Cooler...tions jack inside the sample cooler is firmly seated in the connection within the sample compartment. f Connect the 9-pin-female–9-pin-male’s female