Core Research Facilities University of Massachusetts Lowell

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Standard Operating Procedure:

TA Instruments – Discovery TGA

APPROVAL REQUIREMENTS

TITLE DEPT NAME (PRINTED) SIGNATURE DATE

Author RES Chris Kuncho 25-NOV-14

Reviewer RES Patrick Casey 25-NOV-14

DOCUMENT REVISION HISTORY

REV DESCRIPTION OF CHANGES RELEASED BY DATE

A Initial Release Patrick Casey 25-NOV-14

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TABLE OF CONTENTS

SAFETY ......................................................................................................................................................................3 INTRODUCTION ........................................................................................................................................................4

1.0 Purpose ........................................................................................................................................................4 2.0 Description ...................................................................................................................................................4 3.0 List of Related Internal Documents ..............................................................................................................5 4.0 List of Related External Documents .............................................................................................................5

OPERATION ...............................................................................................................................................................5 5.0 Safety ...........................................................................................................................................................5 6.0 Process Description .....................................................................................................................................8 7.0 Maintenance .............................................................................................................................................. 15 TA Instuments ...................................................................................................................................................... 16

TRAINING CERTIFICATION CHECK SHEET ........................................................................................................ 17

PRIOR TO OPERATION, READ THE SAFETY PROVISIONS AND REVIEW THIS STANDARD OPERATING PROCEDURE IN ITS ENETIRETY.

This document should only serve as a reference. The TA Instruments Discovery TGA should not be operated by anyone without express permission and proper training by approved personnel.

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SAFETY The subsections below outline some of the obvious / major hazards that could exist during the operation of the TA Instruments Discovery TGA, and are divided to bring a level of clarity to such hazards.

Electrical Hazards: Electrical equipment should be installed, operated, serviced, and maintained only by qualified personnel only. Do not block the main switch as potential risk of personal injury or equipment damage if the instrument cannot be turned off in an emergency.

Inhalation Hazards: All materials being used should have Safety Data Sheets (SDS). Confirm that the material does not pose an inhalation hazard for the extrusion parameters being used.

Burn Hazards: The Furnace will be very hot. Be careful of hot surfaces with exposed skin and clothing.

Mechanical Hazards: Keep hands and long hair away from moving parts and feed sections. All long hair should be tied back.

Personal Protective Equipment (PPE): All personnel should utilize and implement proper PPE per OSHA requirements. Refer to OSHA requirements for proper use and implementation of PPE. The following items are suggested as a minimum to avoid injury based on the operation procedure outlined in this manual.

- Safety glasses - Lab coat - Long pants - Close-toed shoes - Proper gloves (when required)

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INTRODUCTION

1.0 Purpose

1.1 The purpose of this Standard Operating Procedure is to guide the user in the basic use of the TA Instruments Discovery Thermogravimetric Analyzer (Discovery TGA).

2.0 Description

2.1 The TA Instruments Discovery TGA (Figure 1) is used in conjunction with a controller computer and associated software to make up a thermal analysis system.

The Discovery TGA measures the amount and rate of weight change in a material, either as a function of increasing temperature or isothermally as a function of time, in a controlled atmosphere. The TGA can be used to characterize any material that exhibits a weight change and to detect phase changes due to decomposition, oxidation, or dehydration. This information helps the scientist or engineer identify the percent weight change and correlate chemical structure, processing, and end-use performance.

The Pan Hook is VERY sensitive and precise. Under no circumstances should the hook ever be touched or manipulated by hand or with tools. Serious damage to the instrumentation could occur.

Figure 1 TA Instruments Discovery TGA

Discovery Common Cabinet

Furnace

Discovery TGA

Autosampler

Keypad

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3.0 List of Related Internal Documents

3.1 UMass Lowell Chemical Hygiene Plan

3.2 RES-07-001 ETIC Operations Manual

4.0 List of Related External Documents

4.1 OSHA Laboratory Safety Guidance

4.2 Discovery TGA Getting Started Guide

4.3 Cleaning the Discovery TGA Furnace

4.4 Discovery TGA – Maintaining the Heat Exchanger

4.5 Replacing the Discovery TGA Hang-down Wires

4.6 Replacing the Discovery TGA IR Bulbs

4.7 Replacing the Discovery TGA Lower Furnace Assembly (LFA)

4.8 Replacing the Discovery TGA Lower Furnace Assembly (LFA) Thermocouple

OPERATION

5.0 Safety

5.1 Safety glasses

5.2 Lab Coat

5.3 Long Pants

5.4 Close-toed shoes

5.5 Proper Gloves (when required)

5.6 UMass Lowell EEM CHP

5.7 Material Safety Data Sheet(s)

Before continuing all personnel should familiarize themselves with the TA Instruments Discovery TGA.

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Figure 2 TA Instruments Discovery TGA Keypad

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Ethernet Port

Power Switch

USB “A” Port Connect to TGA USB “B” Port

Furnace Power Port Connect to TGA Furnace Power Port

Low Voltage Port Connect to TGA CONTROL IN Port

Power Inlet

Figure 3 Common Cabinet Rear Panel Connections

Figure 4 Discovery TGA Rear Panel Connections

Return Line

24 VDC OUT USB “B”

Furnace Power

Control In

Supply Line

GAS 2 Port GAS 1 Port

AIR COOL

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6.0 Process Description

6.1 Instrument startup

6.1.1 The TGA and Common Cabinet should always be on. If the TGA is ever found off, check power connections in the back of the instrument. The common cabinet has a power toggle on its lower rear panel near the power connector (see Power Switch in Figure 3).

6.1.2 If the PC is off, start up the PC by normal means.

6.1.1.1 Power on the Tower.

6.1.1.2 Power on the Monitor.

6.1.3 Lower the TGA furnace if it is raised by pressing Furnace Up/Down button on the TGA keypad (see Figure 2 & Figure 5).

6.1.4 Start the software.

NOTE: The Discovery TGA can be run using the touch screen on the Discovery Common Cabinet or using the TRIOS Software on the PC.

6.1.1.3 Using the PC, click TRIOS Icon (Figure 6)

6.1.1.4 Select Discovery TGA @Lab and click Connect (Figure 7).

Figure 7 Discovery Instrument View

Figure 6 TRIOS Icon

Figure 5 Furnace Up/Down Icon

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6.1.1.5 The experiment screen will appear by default.

6.2 Sample Preparation.

6.2.1 Pan Selection.

6.2.1.1 Determine the proper sample pan for the experiment by referencing Table 1.

6.2.1.2 Once the proper sample pan is selected clean it using a propane torch (Figure 8)

6.3 Taring the sample pan.

6.3.1 Remove cover of Autosampler and place each clean pan in Autosampler carousel well. Make sure that the bottom of the pan is properly aligned with the recessed slots in the Autosampler.

Table 1 Discovery TGA: Pan Selection

Figure 8 Cleaning a Sample Pan

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6.3.2 Open the Calibration screen by clicking the sidebar on the lower left (Figure 9).

6.3.3 Click Tare on the upper left sidebar (Figure 10).

6.3.4 Click all applicable carousel wells on the Tare screen that correspond to a physical pan (Figure 11).

Figure 9 Calibration Screen

Figure 10 Tare Icon

Figure 11 Autosampler Carousel Pan Location Selector

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6.3.5 Click Start on the carousel image.

NOTE: The readout under the Start button gives an approximate time to completely tare all selected positions on the carousel.

6.4 Sample Loading

6.4.1 Remove Autosampler cover and remove Carousel

NOTE: Do not knock over pans, or damage Autosampler Carousel

6.4.2 Take the Carousel to the analytical balance.

6.4.3 Using forceps move a pan to the analytical balance from the carousel.

6.4.4 Tare the balance.

6.4.5 Weigh out 20.0mg +/- 0.1mg of sample into pan.

6.4.6 Using forceps return pan to its position in the carousel.

6.4.7 Repeat steps 6.4.3 to 6.4.6 for all positions on the carousel.

NOTE: Make sure you place experimental samples to the same location on the Autosampler from when they were tared.

6.4.8 Return carousel to Autosampler and replace cover

NOTE: There is a pin on the Autosampler that lines up with a hole on the carousel. These must be lined up for proper working use of the Autosampler. Also, care must be taken to not damage the Autosampler, or jostle the pans.

NOTE: The TGA Autosampler can accommodate 25 samples for testing. Each individual sample must follow steps 6.3 through 6.4 to be properly tested.

6.5 Running an experiment.

6.5.1 On the experiment screen click Empty in running queue, in the upper left section of the screen. This will populate the first run of the sequence (Figure 12).

Figure 12 Starting the Experiment

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6.5.2 Under the sample field input the following (Figure 13):

• Sample Name

• Pan Number

• Pan Type

• Operator

• Project

• Notes (Optional)

• File Name and Specified Path (Optional)

6.5.3 Under the procedure field set the following (Figures 14 – 20):

6.5.3.1 Mode: Standard

6.5.3.2 Test: (Select one of the following and input test parameters)

Figure 13 Test Sample Experiment Information

Figure 14 Test Sample Experiment Information

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Curie Point:

Heat and Hold:

Hi-Res Constant Reaction Rate:

Figure 15 Curie Point Template

Figure 16 Heat and Hold Template

Figure 17 Hi-Res Constant Reaction Rate

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Hi Resolution Dynamic:

Ramp:

Stepwise Isothermal:

Figure 18 Hi Resolution Dynamic Template

Figure 19 Ramp Template

Figure 20 Stepwise Isothermal Template

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6.5.4 If additional runs are needed (Figure 21):

6.5.3.4 At the left side of the screen

Mouse over Run 1 6.5.3.4.1

Right Click 6.5.3.4.2

Select Append Run 6.5.3.4.3

Repeat steps 6.5.3.4 as needed per sample and 6.5.3.4.4experiment.

6.5.5 Click the Start icon to run the experiment(s) (Figure 22)

7.0 Maintenance

7.1 Preventative Maintenance Instruction: please reference the External Documents below for Discovery TGA Maintenance:

• Cleaning the Discovery TGA Furnace • Discovery TGA – Maintaining the Heat Exchanger • Replacing the Discovery TGA Hang-down Wires • Replacing the Discovery TGA IR Bulbs

Figure 21 Creating Additional Runs

Figure 22 Start Icon

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• Replacing the Discovery TGA Lower Furnace Assembly (LFA) • Replacing the Discovery TGA Lower Furnace Assembly (LFA) Thermocouple

7.2 Vendor Information:

TA Instuments

159 Lukens Drive

New Castle, DE 19720

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TRAINING CERTIFICATION CHECK SHEET UCard ID NAME (LAST, FIRST) SIGNATURE DATE

TRAINER

TRAINEE

OPERATION NUMBER OPERATION DESCRIPTION

TRAINER INITIAL*

1 Can load software and add new experiment

2 Can tare sample pans and load test material

3 Can define test parameters and start test

4 Understands the potential hazards associated with equipment

5 Knows the location of the UML Chemical Hygiene Plan (CHP)

6

7

8

9

10

11

12

13

14

* TRAINER’S INITIAL CONFIRMS THAT TRAINEE IS PROFICIENT *