Standard Operating Procedure: TA Instruments Discovery TGA

Size: px

Start display at page:

Download "Standard Operating Procedure: TA Instruments Discovery TGA"

Tracy Lindsey
5 years ago
Views:

Core Research Facilities University of Massachusetts Lowell One University Avenue Lowell, MA 01854

(PRINTED) SIGNATURE DATE Author RES Chris Kuncho 25-NOV-14 Reviewer RES Patrick Casey 25-NOV-14

1 Core Research Facilities University of Massachusetts Lowell One University Avenue Lowell, MA 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

2 TABLE OF CONTENTS SAFETY...3 INTRODUCTION Purpose Description List of Related Internal Documents List of Related External Documents...5 OPERATION Safety Process Description Maintenance TA Instuments TRAINING CERTIFICATION CHECK SHEET 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. RES A 2

3 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) RES A 3

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.

4 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. Discovery TGA Autosampler Discovery Common Cabinet Furnace Keypad Figure 1 TA Instruments Discovery TGA RES A 4

5 3.0 List of Related Internal Documents 3.1 UMass Lowell Chemical Hygiene Plan 3.2 RES ETIC Operations Manual 4.0 List of Related External Documents OPERATION 5.0 Safety 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 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. RES A 5

6 Figure 2 TA Instruments Discovery TGA Keypad RES A 6

Common Cabinet Rear Panel Connections Return Line Supply Line 24 VDC OUT USB B Control In

7 Ethernet Port 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 Switch Power Inlet Figure 3 Common Cabinet Rear Panel Connections Return Line Supply Line 24 VDC OUT USB B Control In Furnace Power GAS 1 Port GAS 2 Port AIR COOL Figure 4 Discovery TGA Rear Panel Connections RES A 7

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.

8 6.0 Process Description 6.1 Instrument startup 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) If the PC is off, start up the PC by normal means Power on the Tower Power on the Monitor Lower the TGA furnace if it is raised by pressing Furnace Up/Down button on the TGA keypad (see Figure 2 & Figure 5). Figure 5 Furnace Up/Down Icon 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 Using the PC, click TRIOS Icon (Figure 6) Figure 6 TRIOS Icon Select Discovery and click Connect (Figure 7). Figure 7 Discovery Instrument View RES A 8

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.

3 Taring the sample pan. 6.3.1 Remove cover of Autosampler and place each clean pan in Autosampler carousel well.

9 The experiment screen will appear by default. 6.2 Sample Preparation Pan Selection Determine the proper sample pan for the experiment by referencing Table 1. Table 1 Discovery TGA: Pan Selection Once the proper sample pan is selected clean it using a propane torch (Figure 8) Figure 8 Cleaning a Sample Pan 6.3 Taring the sample pan 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. RES A 9

6.3.2 Open the Calibration screen by clicking the sidebar on

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

4 Click all applicable carousel wells on the Tare screen that

10 6.3.2 Open the Calibration screen by clicking the sidebar on the lower left (Figure 9). Figure 9 Calibration Screen Click Tare on the upper left sidebar (Figure 10). Figure 10 Tare Icon Click all applicable carousel wells on the Tare screen that correspond to a physical pan (Figure 11). Figure 11 Autosampler Carousel Pan Location Selector RES A 10

11 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 Remove Autosampler cover and remove Carousel NOTE: Do not knock over pans, or damage Autosampler Carousel Take the Carousel to the analytical balance Using forceps move a pan to the analytical balance from the carousel Tare the balance Weigh out 20.0mg +/- 0.1mg of sample into pan Using forceps return pan to its position in the carousel Repeat steps to 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 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 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 RES A 11

12 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) Figure 13 Test Sample Experiment Information Under the procedure field set the following (Figures 14 20): Mode: Standard Test: (Select one of the following and input test parameters) Figure 14 Test Sample Experiment Information RES A 12

13 Curie Point: Heat and Hold: Figure 15 Curie Point Template Figure 16 Heat and Hold Template Hi-Res Constant Reaction Rate: Figure 17 Hi-Res Constant Reaction Rate RES A 13

14 Hi Resolution Dynamic: Figure 18 Hi Resolution Dynamic Template Ramp: Stepwise Isothermal: Figure 19 Ramp Template Figure 20 Stepwise Isothermal Template RES A 14

6.5.4 If additional runs are needed (Figure 21): 6.5.3.4 At the left side of the screen 6.5.3.4.1 Mouse over Run 1 6.5.3.4.2 Right Click 6.5.3.4.3 Select Append Run 6.5.3.4.4 Repeat steps 6.5.3.4 as needed per sample and experiment.

15 6.5.4 If additional runs are needed (Figure 21): At the left side of the screen Mouse over Run Right Click Select Append Run Repeat steps as needed per sample and experiment. Figure 21 Creating Additional Runs Click the Start icon to run the experiment(s) (Figure 22) 7.0 Maintenance Figure 22 Start Icon 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 RES A 15

16 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 RES A 16

17 TRAINING CERTIFICATION CHECK SHEET UCard ID NAME (LAST, FIRST) SIGNATURE DATE TRAINER TRAINEE OPERATION NUMBER OPERATION DESCRIPTION Can load software and add new experiment Can tare sample pans and load test material Can define test parameters and start test Understands the potential hazards associated with equipment Knows the location of the UML Chemical Hygiene Plan (CHP) TRAINER INITIAL* * TRAINER S INITIAL CONFIRMS THAT TRAINEE IS PROFICIENT * RES A 17

Standard Operating Procedure: TA Instruments Discovery DSC

Core Research Facilities University of Massachusetts Lowell One University Avenue Lowell, MA 01854 Standard Operating Procedure: TA Instruments Discovery DSC APPROVAL REQUIREMENTS TITLE DEPT NAME (PRINTED)