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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

 Place the weight & piston on the specimen in the barrel and start the preheat as per the tables below.  Charge the cylinder with the weighed portion of sample and place the piston and release the encoder.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.4/01/03/MFI confidential PP a) Automatic Extrusion plastometer capable of maintaining a temperature of 230 ± 0.1 mg or equivalent. Test Specimen Pelletized samples do not require special preparation unless drying is required./SE/4.  Remove the standard template and reinsert the die and the piston in the cylinder.  Drop the standard die into the barrel. b) Weighing balance-having least count 0.  Release the encoder. Table2: LLDPE.  Press F3 on the machine till the present position of the released encoder is registered as zero.1°C with necessary accessories (The apparatus should be in conformance with the requirement of ASTM D 1238 ) . Pellet Properties .4. Place the piston in the barrel over the template. Drop the standard template on top of the die.2 °C for PE & 230 ± 0. Test Method Setting Up the Instrument  Set the test temperature. 7. Table3: PP) given below. Procedure  Ensure that the barrel temperature has reached the set point (190 ± 0.HPL/HSE/TECH. 6. switch on the heater and allow sometime reaching the test temperature.

16 is carried out according to the following formulae:  F5400 : MFI@2.  For B6000.16kg = 0.16kg = 0. Table2 & Table3)  For P5200 & P4501.HPL/HSE/TECH.198 x MFI@5kg  F5600 : MFI@2. However for filled materials the MFR must be calculated manually by collecting the extrudates cuts obtained during the test (as per ASTM D 1238 . Remove the piston and die from the cylinder and clean all the parts. 9.6kg loads. Mitsui Method for MFR Conversion (only applicable for Mitsui HMHDPE) The conversion from I5 to I2. Calculation The software is designed to calculate the MFR from the MVR values obtained & the Melt Density.16 x MFI@5kg  P5200 : MFI@2.16 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. Machine Factor to be multiplied with the results obtained from the machine for final reporting./SE/4. while that employed for Polypropylene is 0. ASTM D1238). 11. the pellet MFI is evaluated and reported at 5kg & 21.Method A).16kg = 0.7386 g/cc (ref.16kg = 0. The melt density employed for Polyethylene is 0.4. the pellet MFI is evaluated and reported at 5kg load.16kg = 0.4/01/03/MFI  confidential Discharge the residual sample from the cylinder at the end of the test. Reference  ASTM D 1238  ISO1133  MA 17066 Pellet Properties .7636 g/cc.16 x MFI@5kg  B5500 : MFI@2.198 x MFI@5kg  B6000 : MFI@2.

35 Number of No.7636 0.5 1.35 6.7636 0.35 25.35 6.16 2.35 6.16 2.05 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 6.05 1.7636 0.75±0.35 6. F-5600 F-5400 B-6401 B-6000 B5500 M5018L M6007L B5201 E5201 Y-5401 R5801 P5200 HDT -6/7 Kg 5 5 2.75±0. of.35 6.16 21.05 1.16 2.HPL/HSE/TECH.75±0.05 1.4/01/03/MFI  confidential HZ-F-103-5 Guidelines for MFI testing: Table1: HDPE Pellets Grade Load Temp.85±0. 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 .7636 0.7636 0.4 6.35 6.7636 0.75±0.35 6.7636 0.7636 gm 1.05 1.5 4.16 5 2.7636 0.75±0.4.05 1.16 °C 190 190 190 190 190 190 190 190 190 190 190 190 190 190 Pellet Properties Melt Material Density Wt gm/cc 0.05 1.75±0.9±0.05 6.75±0.05 3±0.7636 0.35 6.1 1.7636 0.7636 0.16 2.7636 0.16 2.85±0.35 6.6 5 5 2.1 1.05 1.7636 0./SE/4.35 6.75±0.

5 – 5 300 120 6.16 2.15 2.4/01/03/MFI confidential Table2: LLDPE Pellets Load Temp.16 190 0.5 s 300 300 300 300 300 300 300 s 240 240 240 240 240 240 00 mm 6. Pellet Properties Melt Charge Density Mass Total Preheat Measuring Preheat Time with Length No.35 6.15 2.35 25.35 6.35 8 2 2.95±0.16 190 0. 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.95±0.7636 gm 1./SE/4.7636 0.4.35 6.16 2.1 1.16 2.5 – 5 300 120 6.7636 0.16 2.6±0.15 1.7636 4.7636 0.6±0.7636 0.1 6.35 6.16 2.95±0.7636 0.16 2.95±0. of Number of Measures decimal .16 °C 190 190 190 190 190 190 190 gm/cc 0.35 6. measures decimal places (for reporting) Kg 2.7636 4. of.4 8 8 8 8 8 8 10 2 2 2 2 2 2 1 2.15 1.35 8 2 Table3: PP Pellets Grade Load Temp.HPL/HSE/TECH.7636 0.

16 230 0.16 2.30 ± 300 240 6. 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.1 5.4 25.1 2.35 8 1 M106 M308 M110 F110 M312 2. 2.0 ± 0.7386 0.4.7386 0.35 8 2 M103 2.7386 300 240 6.35 6.5 ± 0. B.7386 0.4/01/03/MFI confidential Time Load places (for reporting) B200 B202S R103 Kg. Determination of Melt Flow Index of Polyolefin Powder / Flake / Spheripol form Resin 1.2 3.16 230 0.1 300 240 6.16 230 0.5 minutes (as per ASTM D 1238) which is the sum total of waiting time & total preheating time during test. and piston position in the barrel as the timed measurement is being made.0 ± 0.4 8 8 10 10 10 1 1 1 1 1 0.1 5.7386 0.1 Note: Above test parameters are based on the total time requirement of 7 ± 0.35 6.1 3.35 25.7386 300 300 300 300 300 120 120 60 60 60 6.0 ± 0.2 4.16 230 230 230 230 230 0.16 °C 230 230 230 g/cc 0.16 2.1 s 300 300 300 s 240 240 240 mm 6.16 2. load.35 8 2 M304 2.5 ± 0.16 2.7386 0. Pellet Properties ./SE/4.35 6.16 2.1 5.0 ± 0.HPL/HSE/TECH.0 ± 0..0 ± 0.5 ± 0.7386 3.7386 3.0 ± 0.16 2.35 8 8 8 2 2 2 F103 2.4 25.7386 0.1 4.7386 g 2.

 Weighing balance-having least count 0.4/01/03/MFI confidential 2. safety goggles and safety shoes while carrying out the test. Safety  Care must be taken while handling and cleaning hot piston and orifice./SE/4.  Remove the standard template and reinsert the die and the piston in the cylinder. Drop the standard template on top of the die.  Automatic Extrusion plastometer capable of maintaining a temperature of 230 ± 0.4.1°C with PP necessary accessories (The apparatus should be in conformance with the requirement of ASTM D 1238 ) . Use of safety gloves.  Press F3 on the machine till the present position of the released encoder is registered as zero.1 °C with necessary accessories (The apparatus should be in conformance with the requirement of ASTM D 1238 ) .  Weighing balance-having least count 0. is solicited. Pellet Properties .  The material being extruded must not be touched with bare hands. Apparatus LLDPE & HDPE  Automatic Extrusion plastometer capable of maintaining a temperature of 190±0. switch on the heater and allow sometime reaching the test temperature.HPL/HSE/TECH. 5.1 mg or equivalent. 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. Test Method Setting Up the Instrument  Set the test temperature. 4.1 mg or equivalent.  Release the encoder. Place the piston in the barrel over the template.  Drop the standard die into the barrel. 3. Interference Moisture.

 Filter a suitable quantity of the sample under suction by adding 100ml hexane occasionally to eliminate the soluble low molecular weight fraction.4/01/03/MFI confidential Procedure : I.  During the preheat.2ºC under continuous Nitrogen gas purging inside the oven.  Thoroughly stir the slurry to make it homogeneous.  After proper drying.2 °C for PE dryer and reactor & 150 ± 0.  Turn off the switch for the vacuum line. 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.4.(gm) (gm/cc) Pellet Properties Total Preheat Measuring No.  MFI Testing procedure for dryer and reactor powder:  Ensure that the barrel temperature has reached the set point (190 ± 0. of measures decimal places(for . BD and for other testing also. 4.) Length (mm) No. take out the sample from the oven and cool it at ambient temperature. Density Wt. of. Preheat with Load time (Sec. 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.  Dry the sample in the constant temperature oven maintained at 100 +/.HPL/HSE/TECH./SE/4.  Discharge the residual sample from the cylinder at the end of the test.2°C for high MFI reactor sample). Remove the piston and die from the cylinder and clean all the parts. Load Melt Material (ºC) (Kg).  Charge the cylinder with the weighed portion of sample and place the piston and release the encoder.) (Sec.  This dried sample can be used for MFI. and then transfer the solid polymers in to the clean and dry aluminium pan.  Place the weight & piston on the specimen in the barrel and start the preheat as per the table No.  Weigh out the proper specimen size in accordance with the expected MFR of the polymer as per the table No. Table 4: Guidelines for Mitsui Plant Products Grade Sample Temp.4. crush and spread the polymers in the pan using the spatula.  Machine factor to be multiplied with the obtained result from machine for final reporting.

7636 0.301*( MFR@5kg)y MFI@2.4 6.35 10 8 8 0.7636 7 300 Nil 25.13 y=1.7636 7 2.35 6.7636 3 3 300 300 300 300 300 300 300 300 240 Nil 240 Nil 240 240 240 240 6.7636 0.35 8 0.HPL/HSE/TECH.16 2.16=0.7636 6 300 60 25.4.35 6.7636 3 7 3 7 3 3 0.35 8 10 8 10 8 8 8 8 0.16 HDT7 Reactor-2 190 5 2.4 10 0.5 5.13 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 .16 2.7636 2 300 240 6.4 8 Dryer Reactor-1 Dryer Reactor-1 Dryer Reactor-1 Reactor-2 Dryer 0.16=0.5 3 300 300 300 300 240 60 240 240 6.35 25.5 5.16=12.35 6.16 5.4 10 0.16 Y-5401 2.0 2.16 2.7636 0.16=0.35 6.16=12.7636 0.0 2.7636 0.16=0.198 * MFR@5kg MFI@2.16=0.7636 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 R5801/HDT6/ Reactor-1 190 2.35 8 0.0 0.35 6.7636 0.5kg MFI@2.5kg MFI@2.16 2.5kg MFI@2.16 B5201 2.7636 0.7636 0.7636 0.7636 3 300 240 6.301*( MFR@5kg)y y=1.198 * MFR@5kg MFI@2.6 * MFR@ 0.7636 0.7636 3 300 240 6.16 5 2.35 6.5 6 2.16 Dryer 190 0.7636 3.16 E5201 2.7636 7 300 Nil 25.16=12.301*( MFR@5kg)y MFI@2.13 y=1.35 8 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 0.16 5 2.7636 0.35 6.35 6.4/01/03/MFI confidential reporting) F-5600 Reactor 1 150 7 300 Nil 25.7636 0.6 * MFR@ 0.35 6.6 * MFR@ 0.4 10 3 300 240 6.5 3 300 300 300 Nil 240 240 25./SE/4.35 8 Reactor 1 190 0.4 6.35 8 8 8 8 0.

powder or spheripol form of PP(Dryer & Reactor) resin . 15 seconds minimum at high speed.75 gm of the fine grind BHT and place in the blender. 1. Tumble by hand to redistribute the mixture (do not invert) c.4/01/03/MFI confidential II. Pellet Properties Repeat steps a & b two more times. b.HPL/HSE/TECH. Mix the stabilizer and flake in a blender as follows a. 3. Weigh 50 g of flakes to be tested and place in a clean blender (mixer) 2./SE/4. Procedure for Spheripol Plant Products  Sample preparation procedure for flake.4. Weigh 0. .

7386 3.7386 3.16 230 0.  Weigh out the proper specimen size in accordance with the expected MFR of the polymer as per the table No.4.5 300 240 6. material will be forced from the barrel by using proper weight to achieve proper positioning of the piston scribe marks.35 2.16 230 0.  Discharge the residual sample from the cylinder at the end of the test. of decimal places(for reporting 2 10 2 10 10 1 ./SE/4.2 °C). Remove the piston and die from the cylinder and clean all the parts. Table5: Guidelines for Spheripol Plant Products: Melt Charge Load Temp.  Place the weight & piston on the specimen in the barrel and start the preheat as per the table No.HPL/HSE/TECH.05.7386 4.  Charge the cylinder with the weighed portion of sample and place the piston and release the encoder.5 300 240 6.5 300 240 6.16 230 0.35 Pellet Properties No.  Machine factor to be multiplied with the obtained result from machine for final reporting.of Load (mm) Measures (s) 2.  During the preheat. 05.) (°C) (gm/cc) (g) B200 B202S R103 Dryer Dryer Dryer Total Preheat Time (s) Preheat Measuring Time with Length No. Grade Sample Density Mass (Kg.4/01/03/MFI confidential  MFI Testing procedure  Ensure that the barrel temperature has reached the set point (230 ± 0.35 2.

16 230 0.7386 0.16 2.  200 gm product + 1500 ppm B215 (B215 is the combination of I-168 & I-1010 of 2 : 1 ratio.5 300 240 6.) + 400 ppm Cast.35 10 1 0.16 230 230 230 Dryer F103 confidential III.7386 5 300 240 F.16 230 0.35 2.drum 2.7386 0.35 10 10 10 2 1 1 240 6.35 2.35 Reactor Dryer Dryer 2.35 10 1 300 120 6. mix the blend for 1 minute. 2.7386 7 300 120 6.5 2.7386 0.5 300 120 6.16 230 230 0.5 4.5 300 240 6.7386 2. Procedure for Spherilene Plant Products  Sample preparation procedure for flake.16 230 0.16 230 0. powder or Spheripol form of resin.16 230 0.16 230 Dryer Dryer Dryer 2.35 10 10 1 1 0.35 6.5 300 300 240 240 6.7386 7 7 7 300 300 300 60 60 60 25.4.  Temperature profile and the screw rpm of the Brabender should be followed as per the following Table.4 10 10 10 1 1 1 2.35 5.drum.4 25.4 25.16 2.7386 4.HPL/HSE/TECH.7386 2.7386 F.7386 5 300 Dryer Dryer 2. MFR/E <5 Zone No: Body Temperature(ºC) of different zone: Screw speed (rpm) Pellet Properties 1 180 2 3 MFR/E >5 4 5 190 190 190 190 20 1 2 3 4 5 170 180 180 180 180 10 .4/01/03/MFI Reactor M103 M304 M106 M308 M110 F110 M312 10 2 10 1 6.7386 5.16 230 0./SE/4.16 2.

4 8 10 Pellet Properties decimal places 2 2 2 2 2 2 1 1 1 1 .of.6±0.95±0.35 25.1 1.16 190 190 0.2°C for GPR1 of HP-LLDPE grade.5 s 300 300 300 300 300 300 300 s 240 240 240 240 240 240 00 mm 6.35 6.  Machine factor to be multiplied with the obtained result from machine for final reporting.5 – 5 6 300 300 120 Nil 6.16 2.16 °C 190 190 190 190 190 190 190 gm/cc 0.4.7636 4. Table 6: Guidelines for Spherilene Plant Products: Load Temp.06.)  Weigh out the proper specimen size in accordance with the expected MFR of the polymer as per the table no. Remove the piston and die from the cylinder and clean all the parts.6±0. 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.7636 0.16 190 0.35 8 2.1 6.  MFI Testing procedure for GPR1 and GPR2powder :  Ensure that the barrel temperature has reached the set point (190 ± 0.16 2.7636 0.35 25.15 1.7636 4.15 1.35 6.35 6. 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.  Discharge the residual sample from the cylinder at the end of the test.5 – 5 300 120 6.16 2.  Discard first 100 gm of extruded material and then collect the material and cut it in granule shapes.  Place the weight & piston on the specimen in the barrel and start the preheat as per the table no.06.7636 0.16 2.HPL/HSE/TECH.7636 gm 1.7636 0./SE/4.95±0.16 2.35 6.2 °C for PE & 230 ± 0.95±0.15 2.95±0.16 2.35 6.7636 0.4/01/03/MFI  confidential After attaining the temperature.7636 0.4 8 8 8 8 8 8 10 2.7636 0.  Charge the cylinder with the weighed portion of sample and place the piston and release the encoder. measures (for reporting) Kg 2.15 2.16 2.

4 10 2.35 10 Pellet Properties 1 1 1 .7636 5 300 120 6.35 10 2.HPL/HSE/TECH.7636 5 300 120 6.4./SE/4.7636 6 300 Nil 25.16 190 0.16 190 0.4/01/03/MFI (GPR1) M5018L (GPR2) M6007L (GPR1) M6007L (GPR2) confidential 2.16 190 0.