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GIW WI-HQ1-027 - ASTM D3895 OIT Testing
GIW WI-HQ1-027 - ASTM D3895 OIT Testing
GIW WI-HQ1-027 - ASTM D3895 OIT Testing
027-4
WORK INSTRUCTIONS PAGE: 1 OF 10
TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
AUTHOR: MM
1. PURPOSE
2. SCOPE
3.1. “The OIT is a qualitative assessment of the level (or degree) of stabilization of
the material tested. This test can be used as a quality control measure to
monitor the stabilization level in formulated resin.”1
4.1. “The sample to be tested and the reference material are heated at a constant
rate in an inert gaseous environment (nitrogen). When the specified
temperature has been reached, the atmosphere is changed to oxygen
maintained at the same flow rate. The specimen is then held at constant
temperature until the oxidative reaction is displayed on the thermal curve.
The time interval from when the oxygen flow is first initiated to the oxidative
reaction is referred to as the induction period.”2
5. RELATED DOCUMENTS
6. DEFINITIONS
1
ASTM D 3895-98, “Standard Test Method for Oxidative-Induction Time of Polyolefins by
Differential Scanning Calorimetry”. 1998.
2
ASTM D 3895-98, “Standard Test Method for Oxidative-Induction Time of Polyolefins by
Differential Scanning Calorimetry”. 1998.
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WORK INSTRUCTIONS PAGE: 2 OF 10
TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
8.1. This list is not all-inclusive and the user is advised to use extreme caution. If
there is any aspect of this testing procedure that is unclear to the Technician,
please see the Quality Control Lab Manager or the Quality Assurance
Specialist immediately.
8.1.2. This test requires the use of gas under high pressure. Extreme
caution will be exercised when changing the Nitrogen and Oxygen
tanks.
9. PROCEDURES
9.1.2. DO NOT open the DSC cell when the temperature is over 40ºC.
9.1.3. NEVER touch the DSC cell with your fingers or forceps. It is
extremely sensitive and it will scratch or break.
9.1.4. DSC should be calibrated every 2 weeks. See WI-Q1-058 for Indium
calibration instructions.
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TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.1.2. Write the roll number on the sample using a correction pen.
9.2.1.7. Write the date and the weight on the sample with a correction
pen.
9.2.2.2. Remove the heat shield and place it gently next to the cell.
9.2.2.3. Remove the cell lid and place it gently near the cell.
9.2.2.5. Leave the empty DSC aluminum pan in the back of the cell
for reference.
9.2.2.6. Place a new DSC aluminum pan in the front of the cell. The
pan should be centered on the raised circle in the front of the
cell.
9.2.2.7. Place the specimen into the front DSC aluminum pan. The
specimen should be centered in the pan.
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WORK INSTRUCTIONS PAGE: 4 OF 10
TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.2.10. Once you are sure all of the internal lids have been replaced
put the top cover on the DSC cell.
9.2.2.13. Hand tighten the 3 screws the rest of the way. The heads of
the screws should be approximately 1 thread above the cell
lid
9.2.3.1. Check the regulators for the Nitrogen and Oxygen lines.
They should read 10 psi.
9.2.3.3. Look at the flowmeter. There will be a silver ball inside the
column. The flow rate of the Nitrogen should be between 50
and 60. If the flow rate is not correct, adjust by turning the
screw on the Gas Switching Accessory for Gas 1 labeled
“module” until the ball reads between 50 and 60.
9.2.3.5. Look at the rotameter. The flow rate for Oxygen, measured
by the silver ball, should be between 70 and 80. If the flow
rate is not correct, adjust the flow rate by turning the screw
on the Gas Switching Accessory for Gas 2 labeled “module”
until the ball reads between 70 and 80.
9.2.4.1. If screen is black, simply move the mouse around and the
screen should appear
.
9.2.4.2. If the screen appears to be locked (unable to use the mouse
or buttons) turn the computer off using the white power
button and proceed.
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TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.4.4. The boot manager (blue box/screen) will appear. Make sure
the line that says Warp 3.0 Disk 1 D: Logical 619M HPFS is
highlighted in gray and hit ENTER.
9.2.4.5. A white box/screen will appear that says OS/2 Warp. Wait. A
dark screen will appear with the words: Current drive is: D:.
Wait. Computer will be searching the disk. Wait.
9.2.4.6. A small white clock will appear in the center of the screen.
Wait.
9.2.4.7. On the screen you will see icons on the left side and a long
rectangular box on the right. In this rectangle, you will see a
box marked TA with a bar that has an arrow. Click on this
bar.
9.2.4.10. Move to the space that says SAMPLE SIZE Enter the
Weight in mg.
9.2.4.16. Move to the space for the flow rate Verify 50 ml/min.
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TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.5.1. Begin the test by moving the mouse to the green arrow and
clicking. The green arrow is located in the upper left-hand
corner of the screen. It is the first button.
9.2.5.5. To stop the test, move the mouse to the red square in the
upper left-hand corner. This is next to the green arrow you
used to begin the test.
9.2.5.6. A message will come up on the screen and ask if you would
like to terminate the test. Click YES, to continue and
terminate the test.
9.2.6.1. If the test is not stopped already, you should stop it now.
See 9.2.5.5.
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TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.6.4. From the menu on the bottom of the screen, select FILE.
9.2.6.5. Click on the next empty row. If all rows are full, click on row 1
to reset the table.
9.2.6.15. Look at the graph. Adjust the limit for the stopping time, if
necessary.
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TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.8.2. The computer should show the time the Oxygen started.
9.2.10.1. With the mouse, select points (1) and (2) on the curve.
Move the mouse to the desired spot and click. These should
be on the flattest points of the horizontal portion of the curve.
9.2.10.2. With the mouse, select points (3) and (4) on the curve.
Move the mouse to the desired spot and click. These should
be on the flattest points on the vertical portion of the curve.
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TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
9.2.11.7. With the mouse, move the cross arrows to the upper left
quadrant of the screen to determine where the label should
go.
9.2.12.3. Once the graph is finished printing, the results are given to
the Quality Control Manager.
10.1. Possible sources of error include, but are not necessarily limited to:
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WORK INSTRUCTIONS PAGE: 10 OF 10
TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05
10.1.2. If specimen runs the full test period and does not peak, it is possible
that there was not enough oxygen reaching to the sample to cause it
to oxidize. In this case the Lab Manager should be informed with an
Equipment Problem Repair Form.
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