Geosynthetics Industrial Works DOCUMENT NO:WI-HQ1-

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WORK INSTRUCTIONS PAGE: 1 of 9
TITLE: HIGH-PRESSURE OXIDATIVE-INDUCTION TIME DATE: 01/05

DEPARTMENT: Quality Control Laboratory

AUTHOR: MM
REVISED BY:

1. PURPOSE

1.1. This document provides the procedure for performing High-Pressure

Oxidative-Induction Time testing.

2. SCOPE

2.1. This document applies to all Quality Control Laboratory Technicians.

3. RELATED DOCUMENTS

3.1. ASTM D5885-97, Standard Test Method for Oxidative Induction Time of
Polyolefin Geosynthetics by High-Pressure Differential Scanning Calorimetry.

4. DEFINITIONS

4.1. 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.

4.2. Oxidative-Induction Time (OIT) – the time elapsed between the introduction
of a material to an oxidizing gas and the oxidation of the material under
isothermal conditions.

4.3. High-Pressure Differential Scanning Calorimetry (HPDSC) – differential-

scanning calorimetry in which the substance and reference material is
exposed to a controlled superambient atmosphere.

4.4. Geosynthetic – a planar product manufactured from polymeric material used

with rock, soil, earth or other geotechnical engineering-related material as an
integral part of a man-made project, structure or system.

5. EQUIPMENT AND MATERIALS

5.1. Aluminum Weighing Dish.

5.2. Differential Scanning Calorimeter with High-Pressure DSC Cell.

5.3. Analytical Balance (Sartorius).

5.4. Forceps and Razor blade.

5.5. Oxygen Gas (99.5% purity).

5.6. Aluminum Specimen Holders.

5.7. Indium (99.999% purity, for calibration).

5.8. Data Presentation Device (computer and printer).

6. PROCEDURES

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6.1. GENERAL INFORMATION

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

3ºC and 20% ± 15% relative humidity.

6.1.2. DO NOT open the DSC Cell when the temperature is over 40ºC.

6.1.3. NEVER touch the DSC Cell with your fingers or forceps. It is
extremely sensitive and it will scratch or break.

6.1.4. The DSC should be calibrated every month. See WI-Q1-058 for
Indium calibration instructions.

6.2. SPECIFIC PROCEDURES

6.2.1. Sample Preparation.

6.2.1.1. Obtain a sample (approx.3 x 4 in.) to be analyzed.

6.2.1.2. Write the roll number, lot number and masterbatch number
on the back of the sample using a correction pen.

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

6.2.1.4. Tare the balance.

6.2.1.5. Cut a small specimen using a razor blade.

6.2.1.6. Weigh the specimen.

6.2.1.6.1. 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 specimen with a
razor blade and reweigh until the weight is
appropriate. If the specimen weighs less than
5.0 mg, discard the specimen and cut a new
one. The specimen must be a whole piece.

6.2.1.7. Remove the aluminum-weighing dish from the balance and

take over to the DSC/OIT machine.

6.2.2. The DSC Cell.

6.2.2.1. 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.

6.2.2.2. Remove the heat shield and place it gently next to the cell.

6.2.2.3. Remove the cell lid and place it gently next to the cell.

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

not to scratch the cell.

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6.2.2.5. Leave the empty DSC aluminum pan in the back of the cell
for reference. It should be centered on the back circle of the
cell.

6.2.2.6. Place a new DSC aluminum pan in the front of the cell. It
should be centered on the front circle of the cell.

6.2.2.7. Place the specimen into the front DSC aluminum pan. The
specimen should be centered in the pan.

6.2.2.8. Replace the cell lid and heat shield.

6.2.2.9. Once all the internal lids have been replaced put the top
cover on the DSC Cell.

6.2.2.10. Hand tighten the 3 screws (counter-clockwise to tighten;

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

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

6.2.2.12. Hand tighten the 3 screws the rest of the way. The heads of
the screws should be approximately 1 thread above the cell.

6.2.3. Setting up the DSC Cell for High-Pressure.

6.2.3.1. If the DSC is not already set up to run a High-Pressure OIT,

you will need to set up accordingly. If the cell is already set
up, proceed to 6.2.4. (Computer Set-up).

6.2.3.2. Close the Nitrogen and Oxygen valves on the wall next to the
DSC completely. Turn the 2 black knobs on the gas lines in
a clockwise manner until hand tight.

6.2.3.3. The gases are now closed off.

6.2.3.4. Disconnect the flow meter from the cell-input connection.

Use a wrench to hold the inner nut in place and with another
wrench gently loosen the outer nut and remove the line.

6.2.3.5. Connect the high-pressure line to the DSC cell input

connection. Hand tighten the nut. Then tighten a quarter-
turn using one wrench to hold the inner nut in place. DO
NOT over tighten, as you can damage the input lines.

6.2.3.6. Close the pressure release valve to the left of the cell until it
is hand tight.

6.2.3.7. On the front of the cell there are 2 knobs: an IN valve and an
OUT valve. Close both of these valves until they are hand
tight (clockwise).

6.2.3.8. Next to the IN and OUT valves, there is a PURGE valve.

Move this from PURGE to FILL.
6.2.3.9. Turn off the Gas Switching Accessory. It will not be needed
for this experiment.

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6.2.4. Computer Set-up.

6.2.4.1. If the screen is black, simply move the mouse around and
the screen should appear.

6.2.4.2. If the screen appears to be locked (unable to use the mouse

or buttons) turn off the computer using the white power
button and proceed with the following:

6.2.4.2.1. After waiting approximately one (1) minute, turn

the computer power back on.

6.2.4.2.2. 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.

6.2.4.2.3. 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. The
computer will be searching the disk.

6.2.4.2.4. A small white clock will appear in the center of

the screen. Wait. You will hear music briefly.

6.2.4.2.5. 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 with TA with a bar
that has an arrow. Click on this bar

6.2.4.2.6. 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.

6.2.4.2.7. 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.

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

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

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

[Roll Number] - [Lot Number].

6.2.4.5. Click on the space that says SAMPLE SIZE  Enter the
weight in mg.

6.2.4.6. Click on the space that says OPEARTOR  Enter your

name.

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6.2.4.7. Click on the space that says COMMENTS  Enter Resin

Type / masterbatch combination.

6.2.4.8. Verify: pan type  Aluminum.

6.2.4.9. Clear the purge gases. (Remove the X’s from the boxes by
clicking on them).

6.2.4.10. Click on METHOD  Change method to D5885-95.mth.

6.2.4.11. Click on save data file. After D:\TA\DSC\DATA\  Enter

the roll#H.00x, where the x = number of tests run that day.

6.2.4.11.1. EXAMPLE: D:\TA\DSC\DATA\1800251H.002

6.2.4.12. Close the experimental parameters screen by clicking on

the square with the () inside.

6.2.5. Purging the DSC Cell with Oxygen.

6.2.5.1. There is a dedicated Oxygen tank for doing HPOITs. Open

the tank and confirm the pressure gage reads 600 psi. Open
the gas line on the wall using the black arrow knob. DO
NOT USE THE NITROGEN.

6.2.5.2. Very SLOWLY open the IN valve on the front of the DSC.

6.2.5.3. Watch the gage on the front of the DSC. When it reads 200
psi, close the IN valve hand tight.

6.2.5.4. SLOWLY open the pressure release valve, allowing the

gas to GENTLY escape.

6.2.5.5. When there is just a little bit of gas left in the cell, close the
pressure release valve hand tight.

6.2.5.6. Again, SLOWLY open the IN valve on the front of the DSC.

6.2.5.7. Again, watch the gage on the front of the DSC. When the
gage reads 200 psi, close the IN valve hand tight.

6.2.5.8. Again, SLOWLY open the pressure release valve, allowing

the gas to GENTLY escape.

6.2.5.9. When there is just a little bit of gas still in the cell, close the
pressure release valve hand tight.

6.2.5.10. The DSC Cell is now purged.

6.2.6. Starting the test.

6.2.6.1. SLOWLY open the IN valve on the front of the DSC. Watch
the computer screen. When the pressure reaches 3500 Kpa
to 3800 Kpa, close the IN valve.

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6.2.6.2. 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.

6.2.6.3. Close the Oxygen line on the wall by turning the black arrow
knob to point up.

6.2.6.4. The test will take approximately 4 to 6+ hours to complete,

except for formulations with K306, which may take more than
24 hours to complete.

6.2.6.4.1. If a sample with K306 is being run, you’ll need to

modify the method.

6.2.6.4.2. Start the test as usual and when the method gets
to the isothermal segment (approx. 10 min. after
starting), you can lengthen the test time.

6.2.6.4.3. Right-click on the white part of the screen and go

to Method  then Modify running method…

6.2.6.4.4. Enter 1700 min. in the field then hit Send

Changes.

6.2.6.4.5. The change will appear at the top of the screen.

Close the window and if the test seems like it’ll
need more time to finish, you can modify it again
by following the same steps above.

6.2.6.4.6. The changes made will only apply to the running

method so after the test is complete, it will
default back to the normal settings.

6.2.6.5. The Oxidative-Inductive Time has been established once the

curve has crested the “hump”. The time of this will vary
depending on the material.

6.2.6.6. To stop the test, move the mouse to the red square in the
upper left-hand corner. This is next to your green arrow that
you used to start the test.

6.2.6.7. A message will appear on the screen and ask if you would
like to terminate the test. Click  YES, to continue and
terminate the test.

6.2.6.7.1. NOTE: The instrument should be cleaned by

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

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6.2.6.8. Open the pressure release valve SLOWLY, allowing the gas
to GENTLY escape.

6.2.7. Obtaining the test results.

6.2.7.1. If the test is not already stopped, see 6.2.6.6.

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

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

6.2.7.3. Using the mouse select  UA.EXE (Universal Analysis).

6.2.7.4. From the menu on the bottom of the screen, select  FILE.

6.2.7.5. Click on the next empty row. If all rows are full, click on row
1 to reset the table.

6.2.7.6. Click  LOOKUP icon.

6.2.7.7. Select  [CORRECT FILE]: 180251H.002 for example.

6.2.7.8. Select  OK.

6.2.7.9. Select  OPEN FILE.

6.2.7.10. Select correct file and click  OK.

6.2.7.11. X-Axis  TIME.

6.2.7.12. Y-Axis  SIGNAL “A” (HEAT FLOW).

6.2.7.13. Select  OK.

6.2.7.14. Data Limits  NONE.

6.2.7.15. Look at the graph. You may want to adjust the area of the
graph, removing the area after the “hump”.

6.2.7.15.1. NOTE: It is not important to include the portion

of 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.

6.2.7.15.2. NOTE: Click  DATA LIMITS and enter the

START TIME  25.00 minutes and the STOP
TIME  500.00+. Your curve will look something

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like this:

6.2.8. Select  OK.

6.2.9. Select  ANALYZE.

6.2.9.1. Click on  ANALYSIS PARAMETERS.

6.2.9.2. Step Transition on Midpoint  INFLECTION.

6.2.9.3. Step Change Between  START and STOP.

6.2.9.4. Special Area  % CRYSTALLINITY.

6.2.9.5. Click on  SAVE.

6.2.10. Select  ANALYZE.

6.2.10.1. Click on  OXIDATION TIME.

6.2.10.2. OXIDATION TIME THRESH HOLD  15.0.

6.2.10.3. OXIDATION GAS START TIME  ZERO (0).

6.2.10.4. Click  OK.

6.2.11. Selecting four (4) points to analyze.

6.2.11.1. 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.

6.2.11.2. 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 of the vertical portion of the curve.

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

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6.2.11.4. The computer will calculate the OIT.

6.2.12. Select  GRAPH.

6.2.12.1. Select  ANNOTATE.

6.2.12.2. Select  B (red letters).

6.2.12.3. Line 1  OIT VALUE (rounded to the nearest minute).

6.2.12.3.1. EXAMPLE: 118.56 min = 119 min

6.2.12.4. Line 2  ROLL NUMBER.

6.2.12.5. Line 3  LOT NUMBER.

6.2.12.6. Line 4  AGING (1600 UV, 90 DAYS OVEN, etc…)

6.2.12.7. Select  OK.

6.2.12.8. With the mouse, move the cross arrows to the upper left
quadrant of the screen. This will determine where the label
will be on the graph.

6.2.12.9. Select  OK.

6.2.13. Printing the graph.

6.2.13.1. Select  PRINT.

6.2.13.2. Select  CANNON.

6.2.13.3. The graph will print.

6.2.13.4. Once the graph is finished printing, one copy goes into the
Formulation file and one goes into the Formulation Data
Binder.

6.2.13.5. Percent OIT are calculated by dividing the aged sample OIT
by the unaged sample OIT.

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