Geosynthetics Industrial Works DOCUMENT NO: WI-Q1-

027-4
WORK INSTRUCTIONS PAGE: 1 OF 10
TITLE: ASTM D3895 - OXIDATIVE-INDUCTION TIME DATE: 01/05

DEPARTMENT: Quality Control Laboratory

AUTHOR: MM

1. PURPOSE

1.1. This document provides the instructions for performing oxidative-induction

time (OIT) testing.

2. SCOPE

2.1. This document applies to all Quality Control Technicians.

3. SIGNIFICANCE AND USE

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. SUMMARY OF TEST METHOD

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

5.1. ASTM D3895-98, Standard Test Method for Oxidative-Induction Time of

Polyolefins by Differential Scanning Calorimetry.

6. DEFINITIONS

6.1. Oxidative-Induction Time (OIT)– time elapsed between the introduction of a

material to an oxidizing gas and the oxidation of the material under
isothermal conditions.

6.2. Differential Scanning Calorimetry (DSC)- a technique in which the difference

in heat flow inputs into a substance and a reference material is measured as
a function of temperature or time, while the substance and reference material
are subjected to a controlled-temperature program.

6.3. Polymer- a macromolecular material formed by the chemical combination of

monomers either having the same or different chemical composition.

6.4. Polymerization- a chemical reaction in which molecules of monomers are

linked together to form polymers.

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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6.5. Polyolefin – a polymer prepared by the polymerization of an olefin as the sole

monomer.

6.6. Flowmeter/Rotometer- a device for measuring the flow rate of a gas.

7. EQUIPMENT AND MATERIALS

7.1. Aluminum Weighing Dish.

7.2. Differential Scanning Calorimeter with High-Pressure Cell.

7.3. Gas Selector Accessory and Regulators.

7.4. Analytical Balance (Sartorius).

7.5. Forceps and Razor blade.

7.6. Flowmeter or Rotameter.

7.7. Oxygen and Nitrogen Gas (Ultra-high-purity grade, extra dry).

7.8. Indium and Tin (99.999% purity for calibration).

7.9. Aluminum Specimen Holders.

8. HEALTH AND SAFETY

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.

8.1.1. Oxygen is a very strong oxidizing agent and vigorously accelerates

combustion. Keep oil, grease and flame away from the equipment at
all times.

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. GENERAL INFORMATION

9.1.1. Testing is conducted in a standard laboratory environment of 23ºC

±3ºC and 20% ± 15% relative humidity.

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.

9.2. SPECIFIC PROCEDURES

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9.2.1. Sample Preparation

9.2.1.1. Obtain a sample (approx. 3 x 4 in.) of the material to be

analyzed.

9.2.1.2. Write the roll number on the sample using a correction pen.

9.2.1.3. Place an aluminum-weighing dish on the Sartorius balance.

9.2.1.4. Tare the balance.

9.2.1.5. Cut a small specimen using a razor blade.

9.2.1.6. Weigh the specimen.

9.2.1.6.1. NOTE: The specimen must weigh between 5.0

mg and 5.9 mg. If the specimen weighs more
than 5.9 mg, carefully trim the piece using a
razor blade and reweigh specimen until the
weight is acceptable. If the specimen weighs
less than 5.0mg, discard piece and cut a new
one. The specimen must be a whole piece.

9.2.1.7. Write the date and the weight on the sample with a correction
pen.

9.2.1.8. Remove the aluminum-weighing dish containing the sample

from the balance and take over to the DSC/OIT machine.

9.2.2. DSC Cell

9.2.2.1. Unscrew the 3 screws on the DSC cell (clockwise to loosen;

the screws are reverse thread) and remove the top cover of
the cell and place it gently next to the cell.

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.

9.2.2.4. Remove the old specimen pan using forceps. BE CAREFUL

not to scratch 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.

9.2.2.8. Replace the cell lid.

9.2.2.9. Replace the heat shield.

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9.2.2.10. Once you are sure all of the internal lids have been replaced
put the top cover on the DSC cell.

9.2.2.11. Hand tighten the 3 screws (counter-clockwise; the screws

are reverse threads). There should be about 1/8” gap
between the top of the cell and the lid.

9.2.2.12. Gently push down on the lid until it clicks.

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. Adjusting the gas flow.

9.2.3.1. Check the regulators for the Nitrogen and Oxygen lines.
They should read 10 psi.

9.2.3.2. Look at the Gas Switching Accessory box. There is a button

labeled “operation”. This button should be out. There will be
a red light. This light should be on “Gas 1”(Nitrogen).

9.2.3.2.1. NOTE: If the Gas 1 (Nitrogen) is not lit, you will

need to push the button under the operation
button in. Now the light should be lit.

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.

9.2.3.4. Look at the Gas Switching Accessory box. Push in the

button labeled “operation”. The red light should be on “Gas
2”(Oxygen).

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.

9.2.3.6. Make sure the button on the Gas Switching Accessory

labeled “operation” it is on “auto” (button is out). The red
light for Gas 1 should be lit.

9.2.4. Computer Set-up.

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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9.2.4.3. After waiting approximately one (1) minute, turn the

computer power back on.

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.

9.2.4.7.1. A box will appear that says UA. Click on this

box. The Universal Analysis screen will appear.
Press CTRL-ESC (hold down the control button
while pressing the escape button at the same
time). The Universal Analysis screen will
disappear.

9.2.4.7.2. You will now be back on the screen with the

rectangular box. Click on TA. A blue graph
screen will appear. Click on the box with the big
square () to make this a full screen.

9.2.4.8. Move the mouse arrow to the EXP PARAM (Experimental

Parameters) icon at the top of the screen. Click here. A box
will open.

9.2.4.9. In the space that is labeled SAMPLE NAME Enter the

[Roll Number] – [Lot Number] – [Railcar Number].

9.2.4.10. Move to the space that says SAMPLE SIZE  Enter the
Weight in mg.

9.2.4.11. Move to the space that says OPERATOR  Enter your

name.

9.2.4.12. Move to the space for COMMENTS  Enter the Resin

Type and the Masterbatch combination.

9.2.4.13. Verify: pan type  Aluminum.

9.2.4.14. Click on Gas 1 () Verify Nitrogen.

9.2.4.15. Click on Gas 2 ()Verify Oxygen.

9.2.4.16. Move to the space for the flow rate Verify 50 ml/min.

9.2.4.17. Move to the space for the method Verify “D3895-95.mth”.

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9.2.4.18. Move to save data file. After D:\TA\DSC\DATA\, type in the

roll #S.00x where x = number of tests run that day.

9.2.4.18.1. Example: D:\TA\DSC\DATA\1800251S.004

9.2.4.19. Close the experimental parameters screen by clicking on

the square with the () inside.

9.2.5. Running the test.

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.

9.2.5.1.1. NOTE: The test will take approximately 20

minutes to warm-up. Once this happens, the
test will automatically switch from Gas 1
(Nitrogen) to Gas 2 (Oxygen).

9.2.5.2. Check the flow rate of the gas every 15 minutes

(approximately) once the test switched from Nitrogen to
Oxygen to make sure the flow rate is between 70 and 80.
Adjust flow rate accordingly, if needed.

9.2.5.3. The test will take approximately 2.5 to 3 hours.

9.2.5.4. The Oxidative-Induction Time has been established once the

curve has crested the “hump” at approximately 150 minutes.

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.

9.2.5.6.1. NOTE: The instrument should be cleaned by

thermal desorption after every 3 or 4 tests to
remove any accumulated organic matter so as to
ensure safe operation.

9.2.6. Obtaining Test Results.

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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9.2.6.2. Press CTRL-ESC (hold down the control button while

pressing the escape button) to open the program list on the
screen.

9.2.6.3. Using the mouse, select UA.EXE (Universal Analysis).

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.

9.2.6.6. Click  LOOKUP icon.

9.2.6.7. Select  [CORRECT FILE]: 180251S.003 for example.

9.2.6.8. Select  OK.

9.2.6.9. Select  OPEN FILE.

9.2.6.10. Select correct file and click  OK.

9.2.6.11. Verify  X-AXIS = TIME.

9.2.6.12. Verify  Y-AXIS = SIGNAL “A” (HEAT FLOW).

9.2.6.13. Select  OK.

9.2.6.14. Data Limits  NONE.

9.2.6.15. Look at the graph. Adjust the limit for the stopping time, if
necessary.

9.2.6.15.1. NOTE: It is not important to include data on the

graph after the “hump’ has been crested. By
adjusting the graph and isolating the needed
area, the portion of the graph we are concerned
with will be magnified, making the information
clearer and easier to obtain.

9.2.6.15.2. To isolate the area on the graph, click on DATA

LIMITS. Next, change the time. The start time
will remain at 0, and the technician will determine
the end time by looking at the graph where the
“hump” has crested and starts to fall.

9.2.7. Select  ANALYZE.

9.2.7.1. Click on  ANALYSIS PARAMETERS.

9.2.7.2. Verify Onset & Step Transition Units  MANUAL.

9.2.7.3. Step Transition Midpoint at  INFLECTION.

9.2.7.4. Step Change Between  START and STOP.

9.2.7.5. Special Area  % CRYSTALLINITY.

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9.2.7.6. Click on  SAVE.

9.2.8. Select  ANALYZE.

9.2.8.1. Select  CURVE VALUE.

9.2.8.2. The computer should show the time the Oxygen started.

9.2.8.3. Select  OK.

9.2.8.4. Time  YES.

9.2.8.5. Temperature  YES.

9.2.8.6. X-Axis Signal  NO.

9.2.8.7. Y-Axis Signal  NO.

9.2.8.8. Arrow to point  YES.

9.2.8.9. Click  SAVE.

9.2.8.10. Adjust the label as needed by clicking on the label and

moving to the desired location.

9.2.8.11. Click on  OK to save. This is the Oxidation Gas Start

Time that you will need later in the analysis.

9.2.9. Select  ANALYZE.

9.2.9.1. Click on  OXIDATION TIME.

9.2.9.2. Verify Oxidation Time Thresh hold  Enter 15.0.

9.2.9.3. Enter the OXIDATION GAS START TIME in minutes (see

6.2.7.11.).

9.2.9.4. Click  OK.

9.2.10. Selecting four (4) points to analyze.

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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9.2.10.3. Once these points have been selected, click  OK.

9.2.10.4. The computer will calculate the OIT.

9.2.10.4.1. NOTE: Serrot has a standard limit for OIT: 100

minimum and 300 maximum. If the value is not
within specifications, contact the Quality Control
Manager.

9.2.11. Select  GRAPH ANNOTATE.

9.2.11.1. Select  B (red lettering).

9.2.11.2. Draw an arrow to a reference point  NO.

9.2.11.3. Line 1: Enter  OIT VALUE ROUNDED TO THE

NEAREST MINUTE (118.56 = 119 min.).

9.2.11.4. Line 2: Enter  ROLL NUMBER.

9.2.11.5. Line 3: Enter  RESIN LOT.

9.2.11.6. Select  OK.

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.

9.2.11.8. Select  OK.

9.2.11.9. Adjust label if necessary or select  OK to save the results.

9.2.12. Printing graph.

9.2.12.1. Select  PRINT.

9.2.12.2. Select  CANNON PRINTER.

9.2.12.3. Once the graph is finished printing, the results are given to
the Quality Control Manager.

10. TROUBLE SHOOTING

10.1. Possible sources of error include, but are not necessarily limited to:

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10.1.1. “Noise” or chatter in the signal - may be caused by incomplete

contact of either pan or the sample. Try cleaning the equipment and
cell.

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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