HPL/HSE/TECH./SE/4.4.

4/01/03/MFI

confidential

Determination of Melt Flow Index of Polyolefin Powder & Pellet

A. Determination of Melt Flow Index of Polyolefin Pellet
1. Scope
This test method covers measurement of the rate of extrusion of molten resins through a die of
specified length and diameter under prescribed conditions of temperature, load, and piston
position in the barrel as the timed measurement is being made.
2. Summary
Using Extrusion Plastometer carries out the determination of MFI. MFI is the weight in grammes
of the material Extruded through a standard die under a fixed weight at 190 C (for Polyethylene)
or 230C (for Polypropylene) for ten minutes.
3. Interference
Moisture, solvents or other contaminants that could cause gassing and inadequate compaction of
the sample in the barrel can lead to incorrect melt flow rate determination.
4. Safety

Care must be taken while handling and cleaning hot piston and orifice.

The material being extruded must not be touched with bare hands. Use of safety gloves,
safety goggles and safety shoes while carrying out the test, is solicited.

5. Apparatus
LLDPE & HDPE

a)

Automatic Extrusion plastometer capable of maintaining a temperature of 1900.1 C with

necessary accessories (The apparatus should be in conformance with the requirement of
ASTM D 1238 ) .

b)

Weighing balance-having least count 0.1 mg or equivalent.

Pellet Properties

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

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PP

a)

Automatic Extrusion plastometer capable of maintaining a temperature of 230 0.1C with

necessary accessories (The apparatus should be in conformance with the requirement of
ASTM D 1238 ) .

b)

Weighing balance-having least count 0.1 mg or equivalent.

6. Test Specimen
Pelletized samples do not require special preparation unless drying is required.

7. Test Method
Setting Up the Instrument

Set the test temperature, switch on the heater and allow sometime reaching the test
temperature.

Drop the standard die into the barrel. Drop the standard template on top of the die. Place
the piston in the barrel over the template.

Release the encoder.

Press F3 on the machine till the present position of the released encoder is registered as
zero.

Remove the standard template and reinsert the die and the piston in the cylinder.

Procedure

Ensure that the barrel temperature has reached the set point (190 0.2 C for PE & 230
0.2C for PP).

Weigh out the proper specimen size in accordance with the expected MFR of the polymer
as per the tables (Table1: HDPE, Table2: LLDPE, Table3: PP) given below.

Charge the cylinder with the weighed portion of sample and place the piston and release
the encoder.

Place the weight & piston on the specimen in the barrel and start the preheat as per the
tables below.

Pellet Properties

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

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Discharge the residual sample from the cylinder at the end of the test. Remove the piston
and die from the cylinder and clean all the parts.

9. Calculation
The software is designed to calculate the MFR from the MVR values obtained & the Melt Density.
The melt density employed for Polyethylene is 0.7636 g/cc, while that employed for
Polypropylene is 0.7386 g/cc (ref. ASTM D1238). However for filled materials the MFR must be
calculated manually by collecting the extrudates cuts obtained during the test (as per ASTM D
1238 - Method A). Machine Factor to be multiplied with the results obtained from the
machine for final reporting.

Mitsui Method for MFR Conversion (only applicable for Mitsui HMHDPE)
The conversion from I5 to I2.16 is carried out according to the following formulae:

F5400

: MFI@2.16kg = 0.198 x MFI@5kg

F5600

: MFI@2.16kg = 0.198 x MFI@5kg

B6000

: MFI@2.16kg = 0.16 x MFI@5kg

B5500

: MFI@2.16kg = 0.16 x MFI@5kg

P5200

: MFI@2.16kg = 0.16 x MFI@5kg

10. Reporting

Material Identification

Date of Test

Temperature employed for testing (C)

Load Employed for testing

Melt Flow Rate reported in grammes/10minutes (The number of decimal places to which a
result must be reported is specified in Table1, Table2 & Table3)

For P5200 & P4501, the pellet MFI is evaluated and reported at 5kg load.

For B6000, the pellet MFI is evaluated and reported at 5kg & 21.6kg loads.

11. Reference

ASTM D 1238

ISO1133

MA 17066

Pellet Properties

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

confidential

HZ-F-103-5

Guidelines for MFI testing:

Table1: HDPE Pellets

Grade Load Temp.

F-5600
F-5400
B-6401
B-6000
B5500
M5018L
M6007L
B5201
E5201
Y-5401
R5801
P5200
HDT -6/7

Kg
5
5
2.16
21.6
5
5
2.16
2.16
2.16
2.16
2.16
2.16
5
2.16

C
190
190
190
190
190
190
190
190
190
190
190
190
190
190

Pellet Properties

Melt

Material

Density

Wt

gm/cc
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636

gm
1.750.05
1.750.05
1.750.05
30.1
1.750.05
1.750.05
6.5
4.5
1.750.05
1.750.05
1.90.1
1.850.05
1.850.05
1.750.05

Total
Preheat
time
s
300
300
300
300
300
300
300
300
300
300
300
300
300
300

Preheat
with Load
s
240
240
240
240
240
240
0
120
240
240
240
240
240
240

Measurin
g
Length
mm
6.35
6.35
6.35
6.35
6.35
6.35
25.4
6.35
6.35
6.35
6.35
6.35
6.35
6.35

Number of
No. of.

decimal

measures places (for

reporting)
8
8
8
8
8
8
10
8
8
8
8
8
8
8

3
3
2
2
3
3
1
2
2
2
2
2
3
2

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

confidential

Table2: LLDPE Pellets

Load

Temp.

Grade

81401-S
81401W
81402S
71601S
71601W
71602S
72550M
73005T /
73204T
72307E

Melt

Material

Density

Wt

Total
Preheat
Time

Number of
Preheat

Measuring

with Load

Length

No. of.
measures

decimal
places (for
reporting)

Kg
2.16
2.16
2.16
2.16
2.16
2.16
2.16

C
190
190
190
190
190
190
190

gm/cc
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636

gm
1.950.15
1.950.15
2.60.1
1.950.15
1.950.15
2.60.1
6.5

s
300
300
300
300
300
300
300

s
240
240
240
240
240
240
00

mm
6.35
6.35
6.35
6.35
6.35
6.35
25.4

8
8
8
8
8
8
10

2
2
2
2
2
2
1

2.16

190

0.7636

4.5 5

300

120

6.35

2.16

190

0.7636

4.5 5

300

120

6.35

Table3: PP Pellets
Grade Load Temp.

Pellet Properties

Melt

Charge

Density

Mass

Total

Preheat Measuring

Preheat Time with

Length

No. of

Number of

Measures

decimal

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

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Time

Load

places (for
reporting)

B200
B202S
R103

Kg.
2.16
2.16
2.16

C
230
230
230

g/cc
0.7386
0.7386
0.7386

g
2.0 0.1
2.0 0.1
3.0 0.1

s
300
300
300

s
240
240
240

mm
6.35
6.35
6.35

8
8
8

2
2
2

F103

2.16

230

0.7386

3.0 0.1

300

240

6.35

M103

2.16

230

0.7386

300

240

6.35

M304

2.16

230

0.7386

3.0 0.2
3.30

300

240

6.35

M106
M308
M110
F110
M312

2.16
2.16
2.16
2.16
2.16

230
230
230
230
230

0.7386
0.7386
0.7386
0.7386
0.7386

300
300
300
300
300

120
120
60
60
60

6.35
6.35
25.4
25.4
25.4

8
8
10
10
10

1
1
1
1
1

0.1
4.0 0.2
4.0 0.1
5.5 0.1
5.5 0.1
5.5 0.1

Note: Above test parameters are based on the total time requirement of 7 0.5 minutes (as per
ASTM D 1238) which is the sum total of waiting time & total preheating time during test..

B. Determination of Melt Flow Index of Polyolefin Powder / Flake / Spheripol form Resin
1. Scope
This test method covers measurement of the rate of extrusion of molten resins through a die of
specified length and diameter under prescribed conditions of temperature, load, and piston
position in the barrel as the timed measurement is being made.

Pellet Properties

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

confidential

2. Interference
Moisture, solvents or other contaminants that could cause gassing and inadequate compaction of
the sample in the barrel can lead to incorrect melt flow rate determination.
3. Safety

Care must be taken while handling and cleaning hot piston and orifice.

The material being extruded must not be touched with bare hands. Use of safety gloves,
safety goggles and safety shoes while carrying out the test, is solicited.

4. Apparatus
LLDPE & HDPE

Automatic Extrusion plastometer capable of maintaining a temperature of 1900.1 C with

necessary accessories (The apparatus should be in conformance with the requirement of
ASTM D 1238 ) .

Weighing balance-having least count 0.1 mg or equivalent.

Automatic Extrusion plastometer capable of maintaining a temperature of 230 0.1C with

PP
necessary accessories (The apparatus should be in conformance with the requirement of
ASTM D 1238 ) .

Weighing balance-having least count 0.1 mg or equivalent.

5. Test Method
Setting Up the Instrument

Set the test temperature, switch on the heater and allow sometime reaching the test
temperature.

Drop the standard die into the barrel. Drop the standard template on top of the die. Place
the piston in the barrel over the template.

Release the encoder.

Press F3 on the machine till the present position of the released encoder is registered as
zero.

Remove the standard template and reinsert the die and the piston in the cylinder.

Pellet Properties

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

confidential

Procedure :
I. Procedure for Mitsui Plant Products

Treatment of slurry:

Turn on the switch for the vacuum line and set the funnel fitted with 325-mesh screen in
the suction bottle.

Thoroughly stir the slurry to make it homogeneous.

Filter a suitable quantity of the sample under suction by adding 100ml hexane
occasionally to eliminate the soluble low molecular weight fraction.

Turn off the switch for the vacuum line, and then transfer the solid polymers in to the clean
and dry aluminium pan, crush and spread the polymers in the pan using the spatula.

Dry the sample in the constant temperature oven maintained at 100 +/- 2C under
continuous Nitrogen gas purging inside the oven.

After proper drying, take out the sample from the oven and cool it at ambient temperature.

This dried sample can be used for MFI, BD and for other testing also.

MFI Testing procedure for dryer and reactor powder:

Ensure that the barrel temperature has reached the set point (190 0.2 C for PE dryer
and reactor & 150 0.2C for high MFI reactor sample).

Weigh out the proper specimen size in accordance with the expected MFR of the polymer
as per the table No. 4.

Charge the cylinder with the weighed portion of sample and place the piston and release
the encoder.

Place the weight & piston on the specimen in the barrel and start the preheat as per the
table No.4.

During the preheat, material will be forced from the barrel by using proper weight to
achieve proper positioning of the piston scribe marks for dryer and reactor samples.

Discharge the residual sample from the cylinder at the end of the test. Remove the piston
and die from the cylinder and clean all the parts.

Machine factor to be multiplied with the obtained result from machine for final reporting.

Table 4: Guidelines for Mitsui Plant Products

Grade

Sample Temp. Load Melt

Material

(C) (Kg). Density Wt.(gm)

(gm/cc)

Pellet Properties

Total

Preheat Measuring No. of.

Preheat with Load

time (Sec.)

(Sec.)

Length
(mm)

No. of

measures decimal
places(for

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

confidential
reporting)

F-5600

Reactor 1 150

300

Nil

25.4

10

300

240

6.35

0.7636

300

Nil

25.4

10

0.7636
0.7636
0.7636
0.7636

3.5
6
2.5
3

300
300
300
300

240
60
240
240

6.35
6.35
6.35
6.35

8
8
8
8

0.7636

300

240

6.35

0.7636

300

240

6.35

Reactor 1 190

0.7636

300

60

25.4

Dryer
Reactor-1
Dryer
Reactor-1
Dryer
Reactor-1
Reactor-2
Dryer

0.7636
0.7636
0.7636
0.7636
0.7636
0.7636

3
7
3
7
3
3

0.7636
0.7636

3
3

300
300
300
300
300
300
300
300

240
Nil
240
Nil
240
240
240
240

6.35
25.4
6.35
6.35
6.35
6.35
6.35
6.35

8
10
8
10
8
8
8
8

0.7636
0.7636
0.7636

7
2.5
3

300
300
300

Nil
240
240

25.4
6.35
6.35

10
8
8

0.7636

300

Nil

25.4

10

0.7636

300

240

6.35

Dryer
F-5400

B-6401

190

Reactor 1 150
Dryer
Reactor 1
Reactor 2
Dryer

190
190
190
190

Reactor 1 190
B-6000
Dryer
B5500

190

0.7636

0.5
5.0 0.7636
0.5
5.0
2.16
5.0
2.16
2.16
5

2.16
5
2.16
B5201
2.16
2.16
E5201
2.16
2.16
2.16
Y-5401
2.16
R5801/HDT6/ Reactor-1 190 2.16
HDT7
Reactor-2 190
5
2.16
Dryer
190
0.5
Reactor-1 150
P5200
5
Dryer
190
190
190
190
190
190
190
190
190

MFI Conversion Formulae:

Grade
F5400
F5600
P5200
F5400
F5600
B6401
R5801/
HDT-6

Pellet Properties

Sample
Reactor1
Reactor1
Reactor1
Dryer
Dryer
Reactor2
Reactor2
Reactor2

Conversion Formula
MFI@2.16=12.6 * MFR@ 0.5kg
MFI@2.16=12.6 * MFR@ 0.5kg
MFI@2.16=12.6 * MFR@ 0.5kg
MFI@2.16=0.198 * MFR@5kg
MFI@2.16=0.198 * MFR@5kg
MFI@2.16=0.301*( MFR@5kg)y
MFI@2.16=0.301*( MFR@5kg)y
MFI@2.16=0.301*( MFR@5kg)y

y=1.13
y=1.13
y=1.13

Nearest to
00/05
03
Nearest to
00/05
03
1
3
2
2
2
1
2
Nil
2
Nil
2
2
2
2
1
3
2
Nearest to
00/05
2

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

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II. Procedure for Spheripol Plant Products

Sample preparation procedure for flake, powder or spheripol form of PP(Dryer &
Reactor) resin .

1. Weigh 50 g of flakes to be tested and place in a clean blender (mixer)

2. Weigh 0.75 gm of the fine grind BHT and place in the blender.
3. Mix the stabilizer and flake in a blender as follows
a. 15 seconds minimum at high speed.
b. Tumble by hand to redistribute the mixture (do not invert)
c.

Pellet Properties

Repeat steps a & b two more times.

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

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MFI Testing procedure

Ensure that the barrel temperature has reached the set point (230 0.2 C).

Weigh out the proper specimen size in accordance with the expected MFR of the polymer
as per the table No. 05.

Charge the cylinder with the weighed portion of sample and place the piston and release
the encoder.

Place the weight & piston on the specimen in the barrel and start the preheat as per the
table No.05.

During the preheat, material will be forced from the barrel by using proper weight to
achieve proper positioning of the piston scribe marks.

Discharge the residual sample from the cylinder at the end of the test. Remove the piston
and die from the cylinder and clean all the parts.

Machine factor to be multiplied with the obtained result from machine for final reporting.

Table5: Guidelines for Spheripol Plant Products:

Melt
Charge
Load Temp.
Grade Sample
Density Mass
(Kg.) (C)
(gm/cc)
(g)
B200
B202S
R103

Dryer
Dryer
Dryer

Total
Preheat
Time
(s)

Preheat
Measuring
Time with
Length
No.of
Load
(mm)
Measures
(s)

2.16

230

0.7386

3.5

300

240

6.35

2.16

230

0.7386

3.5

300

240

6.35

2.16

230

0.7386

4.5

300

240

6.35

Pellet Properties

No. of
decimal
places(for
reporting
2

10
2
10
10

HPL/HSE/TECH./SE/4.4.4/01/03/MFI
Reactor

M103
M304
M106
M308
M110
F110
M312

10

10

6.35

10
10
10

2
1
1

240

6.35

10

300

120

6.35

5.5

300

120

6.35

10
10

1
1

0.7386

300

120

6.35

10

0.7386
0.7386
0.7386

7
7
7

300
300
300

60
60
60

25.4
25.4
25.4

10
10
10

1
1
1

2.16

230

0.7386

2.5

300

240

6.35

2.16

230

0.7386

4.5

300

240

6.35

Reactor
Dryer
Dryer

2.16
2.16

230
230

0.7386
0.7386

2.5
4.5

300
300

240
240

6.35
6.35

2.16

230

0.7386

300

240

F.drum.

2.16

230

0.7386

300

Dryer
Dryer

2.16

230

0.7386

5.5

2.16

230

0.7386

F.drum

2.16

230

Dryer
Dryer
Dryer

2.16
2.16
2.16

230
230
230

Dryer
F103

confidential

III. Procedure for Spherilene Plant Products

Sample preparation procedure for flake, powder or Spheripol form of resin.

200 gm product + 1500 ppm B215 (B215 is the combination of I-168 & I-1010 of 2 : 1
ratio.) + 400 ppm Cast, mix the blend for 1 minute.

Temperature profile and the screw rpm of the Brabender should be followed as per the
following Table.
MFR/E <5

Zone No:
Body Temperature(C) of different zone:
Screw speed (rpm)

Pellet Properties

1
180

MFR/E >5
4

190 190 190 190

20

170 180 180 180

180

10

HPL/HSE/TECH./SE/4.4.4/01/03/MFI

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After attaining the temperature, start the extrusion of the above mixture in the hopper
by turn on the screw slowly up to the required rpm given in the above Table.

Discard first 100 gm of extruded material and then collect the material and cut it in
granule shapes.

MFI Testing procedure for GPR1 and GPR2powder :

Ensure that the barrel temperature has reached the set point (190 0.2 C for PE & 230
0.2C for GPR1 of HP-LLDPE grade.)

Weigh out the proper specimen size in accordance with the expected MFR of the polymer
as per the table no.06.

Charge the cylinder with the weighed portion of sample and place the piston and release
the encoder.

Place the weight & piston on the specimen in the barrel and start the preheat as per the
table no.06.

Discharge the residual sample from the cylinder at the end of the test. Remove the piston
and die from the cylinder and clean all the parts.

Machine factor to be multiplied with the obtained result from machine for final reporting.

Table 6: Guidelines for Spherilene Plant Products:

Load

Temp.

Grade

81401-S
81401W
81402S
71601S
71601W
71602S
72550M
73005T /
73204T
72307E
M5018L

Melt

Material

Density

Wt

Total
Preheat
Time

Preheat

Measuring

with Load

Length

Number of
No.of.

measures (for reporting)

Kg
2.16
2.16
2.16
2.16
2.16
2.16
2.16

C
190
190
190
190
190
190
190

gm/cc
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636
0.7636

gm
1.950.15
1.950.15
2.60.1
1.950.15
1.950.15
2.60.1
6.5

s
300
300
300
300
300
300
300

s
240
240
240
240
240
240
00

mm
6.35
6.35
6.35
6.35
6.35
6.35
25.4

8
8
8
8
8
8
10

2.16

190

0.7636

4.5 5

300

120

6.35

2.16
2.16

190
190

0.7636
0.7636

4.5 5
6

300
300

120
Nil

6.35
25.4

8
10

Pellet Properties

decimal places

2
2
2
2
2
2
1
1
1
1

HPL/HSE/TECH./SE/4.4.4/01/03/MFI
(GPR1)
M5018L
(GPR2)
M6007L
(GPR1)
M6007L
(GPR2)

confidential

2.16

190

0.7636

300

Nil

25.4

10

2.16

190

0.7636

300

120

6.35

10

2.16

190

0.7636

300

120

6.35

10

Pellet Properties

1
1
1