Using a Tinius Olsen MP 987 Extrusion Plastometer Pgina 1 de 8

Using a Tinius Olsen MP 987 Extrusion Plastometer

Located in AT 141, Ball State University

This page was updated on 2/5/2015 and is located at: jcflowers1.iweb.bsu.edu/rlo/Plastometer.htm

Objectives:

By the end of this lesson, you should be able

to:

1. Identify and follow safe

procedures in using an extrusion
plastometer.

2. Clean and setup a plastometer

for testing and find critical values
to be used during a test.

3. Preheat a test sample and

conduct a test for melt flow index.

4. Clean the orifice and barrel of a

plastometer.

5. Calculate melt flow index from

measured values, conduct
subsequent tests, and leave the
area clean.

Introduction
This device allows you to perform a melt flow test (ASTM D1238) to determine the melt flow index for a
sample of thermoplastic pellets. By carefully heating a measured amount of resin at a specified
temperature, and then applying a measured force to extrude it through an orifice of a particular size, you
can collect the amount of plastic extruded in a given amount of time and determine the melt index (MI) or
melt flow index, often expressed in the number of grams per ten-minute period.

Plastics with higher MI values have less viscosity than those with lower MI values. Values under 1.00 for
MI are typically refereed to as fractional melt flow, since the numbers are fractions or decimals less than
1.00.

If other variables are not at play, then the following is a general comparison of
materials with lower and higher MI values.
Lower Melt Flow Index Higher Melt Flow Index
higher viscosity (thicker) at temperature lower viscosity (runnier) at temperature
higher molecular weight lower molecular weight
more difficult to flow fully past the gate of
flows more easily into an injection mold
an injection mold
may sag too much for some extrusion
better for extrusion
operations

Performing a test for melt flow index is helpful in validating the properties of plastic resin, determining if a
resin is a good candidate for extrusion, and even uncovering some instances where there had previously
been excessive heating (showing up as highly elevated MI values).

Notes

The following procedure is based on the Tinius Olsen MP 987 Instruction Manual, Instruction
Booklet # 87-10, ASTM D 1238 (Standard Test Method for Flow Rates of Thermoplastics by
Extrusion Plastometer), on existing laboratory materials, and on instruction from former
faculty in the Plastics area at Ball State University. Please consult ASTM D 1238 as needed.

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In some instances manufacturers have published specific procedures for melt flow tests for
resins (e.g., Polyox, see
http://msdssearch.dow.com/PublishedLiteratureDOWCOM/dh_0044/0901b803800443c9.pdf?
filepath=polyox/pdfs/noreg/326-00026.pdf&fromPage=GetDoc).

The plastometers located in AT 141 are used for instructional purposes rather than for
research, which would require them to have been recently certified for accuracy.

A. Safety
A1. Make sure you have received instruction on the use of this
plastometer before beginning. If you have any questions, ask
an instructor.

A2. Be sure to wear safety glasses and proper lab attire (no
loose clothing or hair, only closed-toed shoes.)

A3. When needed, wear gloves to avoid burns.

A4. Do not let hot plastic or hot metal come into contact with
your skin.

A5. Read this entire instructional sheet before beginning, and

familiarize yourself with the controls.

B. Setup
Background Research

B1. Write down an entry in the machine log sheet for your test. You should know which polymer you are
testing.

B2. Hygroscopic plastics may need to be dried in a dehumidification dryer prior to melt index testing. For
information on dehumidification drying, see http://jcflowers1.iweb.bsu.edu/rlo/DryerCD30.htm.

B3. Consult the table in Section 8.2 of ASTM D 1238 (copied below) to determine an acceptable
"condition" for the test of this particular polymer. This will be one of the pairs of values which indicates
that the testing temperature in C and the total mass including the 100g the piston would be 2.16 kg.
Write down the values for your polymer in your notes and on the plastometer log sheet.

Example

If we are using an extrusion grade of LDPE, then one of the standard conditions listed is
190/2.16. Therefore, the testing temperature would be 190C and the total load including the
100-gram piston would be 2.16 kg or 2160 grams. So you would need to add an additional
2060 grams of weight to the top of the piston.

Procedural Conditions
[The following data is copied from Section 8.2 ASTM D 1238 listing different acceptable
procedural "Conditions" for specific polymers where the first number in the pair is the
temperature in degrees Celsius and the second is the total weight in kilograms, including
the 100-gram piston.]
Material Condition
Acetals (copolymer and homopolymer) 190/2.16 190/1.05
Acrylics 230/1.2 230/3.8
Acrylonitrile-butadiene-styrene 200/5.0 230/3.8 220/10
Acrylonitrile/butadiene/styrene/polycarbonate 230/3.8 250/1.2 265/3.8 265/5.0
blends
Cellulose esters 190/0.325 190/2.16 190/21.60 210/2.16
Ethylene-chlorotrifluoroethylene copolymer 271.5/2.16
Ethylene-tetrafluoroethylene copolymer 297/5.0
Nylon 275/0.325 235/1.0 235/2.16 235/5.0
275/5.0
Perfluoro(ethylene-propylene) copolymer 372/2.16
Perfluoroalkoxyalkane 37215.0
Polycaprolactone 125/2.16 80/2.16
Polychlorotrifluorethylene 265/12.5
Polyether sulfone (PES) 380/2.16 360/10 343/2.16
Polyethylene 125/0.325 125/2.16 250/1.2 190/0.325

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190/2.16 190/21.60 190/10 310/12.5

Polycarbonate 300/1.2
Polymonochlorotrifluoroethylene 265/21.6 265/31.6
Polypropylene 230/2.16
Polyphenyl sulfone (PPSU) 365/5.0 380/2.16
Polystyrene 200/5.0 230/1.2 230/3.8 190/5.0
Polysulfone (PSU) 343/2.16 360/10
Polyterephthalate 250/2.16 210/2.16 285/2.16
Poly(vinyl acetal) 150/21.6
Poly(vinylidene fluoride) 230/21.6 230/5.0
Poly(phenylene sulfide) 315/5.0
Styrene acrylonitrile 220/10 230/10 230/3.8
Styrenic Thermoplastic Elastomer 190/2.16 200/5.0
Thermoplastic Elastomer-Ether-Ester 190/2.16 220/2.16 230/2.16 240/2.16
250/2.16
Thermoplastic elastomers (TEO) 230/2.16
Vinylidene fluoride copolymers 230/21.6 230/5.06
For Tm = 100 use 120/5.0 or 21.6

B4. Using the value you just found for the total mass use the table below from Section 3.2 of the MP 987
manual to determine which weights are to be added to the 100-gram piston to achieve the total load.
Please use gloves to touch the weights, which protects them from the moisture on your skin that can
promote oxidation and change their mass.

Example

If we are using an extrusion grade of LDPE and have determined the condition is 190/2.16,
then we need a total mass of 2.16kg or 2160g. Subtracting the mass of the 100g piston, we
would need to add 2060g. Sometimes we would need to stack multiple weights, but in this
case the single weight marked 2060 will suffice.

[Weight Combinations
from Section 3.2 of the Tinius Olsen MP 987 Instruction Manual]
Total
Use Piston
+ = Load
Weights Weight
Grams
225 + 100 = 325
2,060 + 100 = 2,160
1,100 + 100 = 1,200
3,700 + 100 = 3,800
2,400 + 10,000 + 100 = 12,500
4,900 + 100 = 5,000
6,600 + 4,900 + 10,000 + 100 = 21,600
950 + 100 = 1,050
9,900 + 100 = 10,000
900 + 100 = 1,000

B5. Read about the material to determine a likely value for the melt
index (try www.matweb.com if you do not have information from the
manufacturer).

B6. Consult Table 2 in ASTM to find the suggested sample size in

grams, the time interval in minutes, and the factor.

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[The following is from ASTM D 1238]

Table 2 Standard Test Conditions, Sample Mass, and Testing Time

Suggested Mass of Time Factor for Obtaining
Flow Range
Sample in Cylinder Interval Flow Rate
g/10 min g min g/10 min
0.15 to 1.0 2.5 to 3.0 6.00 1.67
>1.0 to 3.5 3.0 to 5.0 3.00 3.33
>3.35 to 10 4.0 to 8.0 1.00 10.00
10 to 25 4.0 to 8.0 0.50 20.00
>25 4.0 to 8.0 0.25 40.00

Example

If we are using an extrusion grade of LDPE, MatWeb shows the average value for the melt
flow to be 5.73 g/10 min at http://www.matweb.com/search/DataSheet.aspx?
MatGUID=8e92b9e66e214e1b8fc8222dbff6d480&ckck=1 . ASTM D 1238 Table 2 is then
consulted and this flow rate fits in the range listed as "<3.5 to 10". Following this row to the
right we see the suggested mass of the sample is 4.0 to 8.0 g, the time interval is 1.00 min.,
and the factor is 10.00. (Since this test provides a mass per 10-minute period, and the
interval is only 1/10 of ten minutes, the factor is 10.00. You can see where the interval is 3
minutes, which is one-third of ten minutes, that the factor would have been 3.33.)

Preparing the Melt Index Test Apparatus

B7. Do a preliminary cleaning of the barrel (also know as the cylinder) by using a small square of cleaning
cloth and the cylinder cleaning tool. Make sure the cloth does not remain in the cylinder. Do not use
lubricants, water, solvents, or abrasives. (Later, you will do a final cleaning after the cylinder has reached
temperature.)

B8. Make sure the orifice is clean. If necessary, clean it, but not with any steel tool or anything that will
damage the metal surfaces.

B9. Place the orifice into the bottom of the cylinder, where it should seat.

B10. Place the piston rod down the cylinder.

Pre-Heating

B11. Plug in the plastometer's power cord if it was unplugged.

B12. Turn the power switch to ON.

B13. Set the temperature to the value identified earlier from Section 8.2 of ASTM D 1238. Do this by
pressing the MODE button in the TEMPERATURE area until the word SET appears, and then using the
down arrow and up arrow buttons. When you've reached the correct setting, press the ENTER button.

B14. In order to monitor the actual temperature, press the MODE button until the word ACTUAL appears.
When you notice the LED heater light beginning to blink on and off, the device is at temperature.

Setting the Timer

Note

The Tinius Olsen MP 987 Extrusion Plastometer has

three timer modes. Use Mode 1 as a simple stopwatch
mode and Mode 3 as a countdown timer. It is
recommended that you set the Mode 3 countdown
timer for the time interval of the test.

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B15. In the TIME area, pres the MODE button until a 3 is

displayed above the word MODE.

B16. Use the up/down arrows to set the time for the test time. (In the example with LDPE noted above, the
test time is 1 minute, so this would be set to 60 seconds). Press enter to record the set time.

B17. Practice with the timer switches. Go to Mode 1 (stopwatch timer) and try starting, stopping, and
resetting the time. Then quickly switch to Mode 3 and start the countdown timer. Stop it and reset it.

Cleaning after Pre-Heating

B18. Put on gloves that protect your hands from burns.

B19. When the set temperature has been reached, remove the hot orifice.

B20. While it is hot, clean the orifice. You can very carefully use the drill bit to clean the hole, and the
copper scouring pad to clean the outside.

B21. Clean the barrel until a cleaning wipe picks up no visible foreign material. Make sure that you are
using the cleaning tool, shown on the left, rather than the tamping tool or orifice removal tool.

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B22. Place the orifice back down the barrel and make sure it is seated.

B23. Place the piston down the barrel without adding any plastic.

B24. Allow the temperature of the orifice and piston to rise and stabilize for 15 minutes.

Sample Preparation

B25. Use a scale to tare the weight of a small cup so the scale reads 0.00g with the cup on it.

B26. Add pellets of clean, dry polymer to the cup until the amount of plastic indicated previously from Table
2 in ASTM D 1238 is found. Remember that hygroscopic materials must have first been dried in a
dehumidifying dryer.

C. Conducting the Test (Manual Operation)

Sample Preheat and Purges

C1. With gloves on, remove the hot piston and place it on an insulated surface (such as an extra thermal
glove).

C2. In less than a minute, carefully put the measured amount of plastic into the cylinder, stopping to ram
the material as needed.

Caution

Do not add more pellets to the funnel than will flow down the cylinder. If necessary, remove
the funnel and gently ram down the material before adding the remainder of the pellets.

C3. Gently ram the material down, as shown on the left, below.

C4. Add the piston on top of the material and make sure it is seated.

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C5. Add the required amount of weight, as shown on the left, below.

C6. A small stop (the dowel shown below) is typically used to prevent the weight from traveling too far
down during the purge. After the purge at least one of the small index lines must be visible on the piston
above the collar. Notice how in the example at the right, below, the bottom of the dowel is resting on the
collar and the top will come into contact with the weight.

C7. Use the Mode 1 stopwatch timer and start timing how long the plastic is pre-heating. This pre-heating
should last for 7 +/- .5 minutes, which is a range of 6 minutes 30 seconds to 7 minutes 30 seconds. The
timer readout is in seconds, so this range is 390 seconds to 450 seconds. The purge should be completed
two minutes prior to the start of the test (i.e., in the first five minutes of this phase, or by the 300 second
mark.) As material is purged, remove it carefully with a small metal spatula.

Testing

C8. Remove any extrudate that has emerged using a small metal spatula.

C9. Place an empty metal cup under the nozzle.

C10. Switch the timer to countdown MODE 3.

C11. At the end of the sample pre-heating time, remove the stop (wooden dowel) to allow the weighted
piston to lower, extruding plastic.

C12. Immediately start the countdown timer, which should have been set last for the amount of time you
found in Table 2 of ASTM D 1238. (The example for LDPE was 1 minute.)

C13. Immediately at the end of the allotted time, neatly cut off the last of the plastic that has extruded,
placing it into the metal cup. If there are bubbles in the plastic, discard it and try again with a new sample
after cleaning all material from the cylinder.

D. Cleaning the Plastometer and Orifice

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D1. Finish extruding the plastic that is in the cylinder. You might want to gently press on the top of the
weight to add a bit more pressure and speed this up.

D2, With gloves, remove and clean the orifice, being careful not to damage it. Do not use abrasives paper
or steel wool. Use only the orifice drill and a copper scouring pad. (If this machine had been recently
calibrated and the test needed to be valid, then the orifice might need to be cleaned by pryolitic
decomposition of any residue in a chamber filled with nitrogen; solvent cleaning could also be used in
those instances, though only if no residue is left in the orifice that would interfere with results.)

D3. Clean the piston while it is hot using the copper scouring pad.

D4. Swab out the cylinder until a dry cotton patch comes out clean. Do not use solvents, water, the
scouring pad, the drill, or abrasives.

D5. After it is clean, return the orifice to the cylinder, return all plastometer tools, turn off the plastometer,
and unplug its power cord.

E. Calculating Melt Flow Index Values

Calculations

E1. After the plastic extruded during the test has cooled, find its mass to
the nearest 1 mg (0.001 g) if the scale allows. (Do not include the mass of
the metal cup, just the mass of the extrudate.)

E2. Multiply this mass by the corresponding factor in Table 2 of ASTM D

1238 that you used.

Example

For example, if the mass were 0.83 g and a factor of 10 were used
(because the time interval used was one minute), then the melt
index or melt flow index would be 10 x 0.83g per 10 minutes, or
8.3g/10min.

Iterative Testing

E3. Repeat this test as needed and find the average of several runs.

E4. Finish filling out the machine log sheet.

Leaving all in order

E5. Make sure the area is clean when you leave it and all tools have been replaced.

"Using a Tinius Olsen MP 987 Extrusion Plastometer"

All information is subject to change without notification.
Jim Flowers
Department of Technology, Ball State University

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