MFI

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 230°C (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 190±0.1 °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 1


PP

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


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 ±

0.2°C 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.

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.

Pellet Properties 2


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 : [email protected] = 0.198 x MFI@5kg

F5600 : [email protected] = 0.198 x MFI@5kg

B6000 : [email protected] = 0.16 x MFI@5kg

B5500 : [email protected] = 0.16 x MFI@5kg

P5200 : [email protected] = 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

HZ-F-103-5

Pellet Properties 3


Guidelines for MFI testing:Guidelines for MFI testing:

Table1: HDPE Pellets

Grade Load Temp.Melt

Density

Material

Wt

Total

Preheat

time

Preheat

with Load

Measurin

g

Length

No. of.

measures

Number of

decimal

places (for

reporting)

Kg °C gm/cc gm s s mm

F-5600 5 190 0.7636 1.75±0.05 300 240 6.35 8 3

F-5400 5 190 0.7636 1.75±0.05 300 240 6.35 8 3

B-6401 2.16 190 0.7636 1.75±0.05 300 240 6.35 8 2

B-600021.6 190 0.7636 3±0.1 300 240 6.35 8 2

5 190 0.7636 1.75±0.05 300 240 6.35 8 3

B5500 5 190 0.7636 1.75±0.05 300 240 6.35 8 3

M5018L 2.16 190 0.7636 6.5 300 0 25.4 10 1

M6007L 2.16 190 0.7636 4.5 300 120 6.35 8 2

B5201 2.16 190 0.7636 1.75±0.05 300 240 6.35 8 2

E5201 2.16 190 0.7636 1.75±0.05 300 240 6.35 8 2

Y-5401 2.16 190 0.7636 1.9±0.1 300 240 6.35 8 2

R5801 2.16 190 0.7636 1.85±0.05 300 240 6.35 8 2

P5200 5 190 0.7636 1.85±0.05 300 240 6.35 8 3

HDT -6/7 2.16 190 0.7636 1.75±0.05 300 240 6.35 8 2

Pellet Properties 4


Table2: LLDPE Pellets

Grade

Load Temp. Melt

Density

Material

Wt

Total

Preheat

Time

Preheat

with Load

Measuring

LengthNo. of.

measures

Number of

decimal

places (for

reporting)


81401-S 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

81401W 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

81402S 2.16 190 0.7636 2.6±0.1 300 240 6.35 8 2

71601S 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

71601W 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

71602S 2.16 190 0.7636 2.6±0.1 300 240 6.35 8 2

72550M 2.16 190 0.7636 6.5 300 00 25.4 10 1

73005T /

73204T2.16 190 0.7636 4.5 – 5 300 120 6.35 8 2

72307E 2.16 190 0.7636 4.5 – 5 300 120 6.35 8 2

Pellet Properties 5


Table3: PP Pellets

GradeLoad Temp.

Melt

Density

Charge

Mass

Total

Preheat

Time

Preheat

Time with

Load

Measuring

LengthNo. of

Measures

Number of

decimal

places (for

reporting)

Kg. °C g/cc g s s mm

B200 2.16 230 0.7386 2.0 ± 0.1 300 240 6.35 8 2

B202S 2.16 230 0.7386 2.0 ± 0.1 300 240 6.35 8 2

R103 2.16 230 0.7386 3.0 ± 0.1 300 240 6.35 8 2

F103 2.16 230 0.7386 3.0 ± 0.1 300 240 6.35 8 2

M103 2.16 230 0.7386 3.0 ± 0.2 300 240 6.35 8 2

M304 2.16 230 0.73863.30 ±

0.1300 240 6.35 8 1

M106 2.16 230 0.7386 4.0 ± 0.2 300 120 6.35 8 1

M308 2.16 230 0.7386 4.0 ± 0.1 300 120 6.35 8 1

M110 2.16 230 0.7386 5.5 ± 0.1 300 60 25.4 10 1

F110 2.16 230 0.7386 5.5 ± 0.1 300 60 25.4 10 1

M312 2.16 230 0.7386 5.5 ± 0.1 300 60 25.4 10 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..

Pellet Properties 6


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.

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 190±0.1 °C with


ASTM D 1238 ) .

Weighing balance-having least count 0.1 mg or equivalent.

PP

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


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.

Pellet Properties 7


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 :

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 +/- 2ºC 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 ± 0.2°C for high MFI reactor sample).


as per the table No. 4.


the encoder.


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.



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

Pellet Properties 8


Table 4: Guidelines for Mitsui Plant Products

GradeSample Temp.

(ºC)

Load

(Kg).Melt

Density

(gm/cc)

Material

Wt.(gm)

Total

Preheat

time (Sec.)

Preheat

with Load

(Sec.)

Measuring

Length

(mm)

No. of.

measures

No. of

decimal

places(for

reporting)

F-5600Reactor 1 150

0.50.7636 7 300 Nil 25.4 10

Nearest to

00/05

Dryer 190 5.0 0.7636 3 300 240 6.35 8 03

F-5400Reactor 1 150

0.50.7636 7 300 Nil 25.4 10

Nearest to

00/05

Dryer 190 5.0 0.7636 3.5 300 240 6.35 8 03

B-6401

Reactor 1 190 2.16 0.7636 6 300 60 6.35 8 1

Reactor 2 190 5.0 0.7636 2.5 300 240 6.35 8 3

Dryer 190 2.16 0.7636 3 300 240 6.35 8 2

B-6000

Reactor 1 1902.16

0.7636 3 300 240 6.35 82

Dryer 1905

0.7636 2 300 240 6.35 82

B5500Reactor 1 190

2.160.7636 6 300 60 25.4 8

1

Dryer 190 5 0.7636 3 300 240 6.35 8 2

B5201Reactor-1 190 2.16 0.7636 7 300 Nil 25.4 10 Nil

Dryer 190 2.16 0.7636 3 300 240 6.35 8 2

E5201Reactor-1 190 2.16 0.7636 7 300 Nil 6.35 10 Nil

Dryer 190 2.16 0.7636 3 300 240 6.35 8 2

Y-5401

Reactor-1 190 2.16 0.7636 3 300 240 6.35 8 2

Reactor-2 190 2.16 0.7636 3 300 240 6.35 8 2

Dryer 190 2.16 0.7636 3 300 240 6.35 8 2

R5801/HDT6/

HDT7

Reactor-1 190 2.16 0.7636 7 300 Nil 25.4 10 1

Reactor-2 190 5 0.7636 2.5 300 240 6.35 8 3

Dryer 190 2.16 0.7636 3 300 240 6.35 8 2

P5200Reactor-1 150

0.50.7636 7 300 Nil 25.4 10

Nearest to

00/05

Dryer 190 5 0.7636 3 300 240 6.35 8 2

Pellet Properties 9


MFI Conversion Formulae:

Grade Sample Conversion Formula

F5400 Reactor1 [email protected]=12.6 * MFR@ 0.5kg

F5600 Reactor1 [email protected]=12.6 * MFR@ 0.5kg

P5200 Reactor1 [email protected]=12.6 * MFR@ 0.5kg

F5400 Dryer [email protected]=0.198 * MFR@5kg

F5600 Dryer [email protected]=0.198 * MFR@5kg

B6401 Reactor2 [email protected]=0.301*( MFR@5kg)y y=1.13

R5801/ Reactor2 [email protected]=0.301*( MFR@5kg)y y=1.13

HDT-6 Reactor2 [email protected]=0.301*( MFR@5kg)y y=1.13

Pellet Properties 10


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. Repeat steps a & b two more times.

MFI Testing procedure

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


as per the table No. 05.


the encoder.


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.






Table5: Guidelines for Spheripol Plant Products:

Grade SampleLoad(Kg.)

Temp.(°C)

Melt Density(gm/cc)

Charge Mass

(g)

Total Preheat

Time(s)

Preheat Time with

Load(s)

Measuring Length(mm)

No.of Measures

No. of decimal

places(for reporting

B200Dryer

2.16 230 0.7386 3.5 300 240 6.3510

2

B202SDryer

2.16 230 0.7386 3.5 300 240 6.3510

2

R103Dryer 2.16 230 0.7386 4.5 300 240 6.35 10 1

Reactor 2.16 230 0.7386 2.5 300 240 6.35 10 2

F103Dryer 2.16 230 0.7386 4.5 300 240 6.35 10 1

Reactor 2.16 230 0.7386 2.5 300 240 6.35 10 2

M103 Dryer 2.16 230 0.7386 4.5 300 240 6.35 10 1

M304Dryer 2.16 230 0.7386 5 300 240 6.35 10 1

F.drum. 2.16 230 0.7386 5 300 240 6.35 10 1

M106 Dryer 2.16 230 0.7386 5.5 300 120 6.35 10 1

M308Dryer 2.16 230 0.7386 5.5 300 120 6.35 10 1

F.drum 2.16 230 0.7386 7 300 120 6.35 10 1

M110 Dryer 2.16 230 0.7386 7 300 60 25.4 10 1

F110 Dryer 2.16 230 0.7386 7 300 60 25.4 10 1

M312 Dryer 2.16 230 0.7386 7 300 60 25.4 10 1



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 MFR/E >5

Zone No: 1 2 3 4 5 1 2 3 4 5

Body Temperature(ºC) of different zone: 180 190 190 190 190 170 180 180 180 180

Screw speed (rpm) 20 10

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 ±

0.2°C for GPR1 of HP-LLDPE grade.)


as per the table no.06.


the encoder.


table no.06.






Table 6: Guidelines for Spherilene Plant Products:

Grade

Load Temp. Melt

Density

Material

Wt

Total

Preheat

Time

Preheat

with Load

Measuring

LengthNo.of.

measures

Number of

decimal places

(for reporting)


81401-S 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

81401W 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

81402S 2.16 190 0.7636 2.6±0.1 300 240 6.35 8 2

71601S 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

71601W 2.16 190 0.7636 1.95±0.15 300 240 6.35 8 2

71602S 2.16 190 0.7636 2.6±0.1 300 240 6.35 8 2

72550M 2.16 190 0.7636 6.5 300 00 25.4 10 1

73005T /

73204T2.16 190 0.7636 4.5 – 5 300 120 6.35 8

1

72307E 2.16 190 0.7636 4.5 – 5 300 120 6.35 8 1

M5018L

(GPR1)2.16 190 0.7636 6 300 Nil 25.4 10

1

M5018L

(GPR2)2.16 190 0.7636 6 300 Nil 25.4 10

1

M6007L

(GPR1)2.16 190 0.7636 5 300 120 6.35 10

1

M6007L

(GPR2)2.16 190 0.7636 5 300 120 6.35 10

1


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