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LMI Melt Flow Rate Test: Applications and Calculations

The document discusses melt flow rate (MFR) testing methods using a melt flow rate tester. It describes Method A which involves manually cutting and weighing extrudate over time, and Method B which uses volumetric displacement measurements and a digital encoder to automatically time flow rate. It also discusses converting between Methods A and B to calculate melt density, using different test loads to measure flow rate ratios, and applications like measuring shear thinning behavior.

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Aliraza Aliraza
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0% found this document useful (0 votes)
56 views14 pages

LMI Melt Flow Rate Test: Applications and Calculations

The document discusses melt flow rate (MFR) testing methods using a melt flow rate tester. It describes Method A which involves manually cutting and weighing extrudate over time, and Method B which uses volumetric displacement measurements and a digital encoder to automatically time flow rate. It also discusses converting between Methods A and B to calculate melt density, using different test loads to measure flow rate ratios, and applications like measuring shear thinning behavior.

Uploaded by

Aliraza Aliraza
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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LMI Melt Flow Rate Test

Applications & Calculation


Azadeh Farahanchi
Rheological Scientist

38 Forge Parkway, Franklin, MA 02038


Tel: 508.541.9582
Cell: 774.287.2366
[email protected] 1
Proprietary & Confidential
Outline

 Melt Flow Rate Test Applications

 LMI Melt Flow Rate Tester

 Method A

 Method B

 Method A to B Conversion

 Operation Points

 Other Applications (Shear thinning behavior, intrinsic viscosity, and thermal stability)

Proprietary & Confidential


Melt Flow Rate Test Applications & Benefits
Standardized measure of flow characteristic of
polymer melts at a single point specific condition Quality control / lot to lot consistency

ASTM D1238
ISO 1133 https://www.slideshare.net
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Minimizing waste

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LMI Melt Flow Rate Tester

Weight
Weight
Digital encoder ±0.5%

Thermometer Piston
Piston ±0.1 °𝐶𝐶 D: 9.474 mm

Capillary die Barrel…

Capillary die
D: 2.095 mm, L/D:3.818

4
Proprietary & Confidential
Standardized Testing Condition
ASTM D1238 / ISO 1133 to specify:
 Testing conditions
(temperature and weight)
 Testing time
 Sample mass
 Piston travel
 Die dimensions
 Precision

5
Proprietary & Confidential
Method A
Mass measurement for MFR

Method A Upper scribe


Manual Operation
2.54
 Mass measurement of extrudate collected over time cm
Lower scribe
 Cut-n-weigh method
 Piston in proper position at end of pre-heating time
 Results:
𝟏𝟏𝟏𝟏 𝑴𝑴
𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴 𝑨𝑨 =
𝒕𝒕𝑨𝑨
where
𝑀𝑀𝑀𝑀𝑀𝑀 𝑔𝑔⁄10𝑚𝑚𝑚𝑚𝑚𝑚 : 𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑓𝑓𝑓𝑓𝑓𝑓𝑓𝑓 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟
Enter sample weights
𝑀𝑀 𝑔𝑔 : 𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚
𝑡𝑡𝐴𝐴 𝑚𝑚𝑚𝑚𝑚𝑚 : 𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 Samples

6
Proprietary & Confidential
Method B
Method B
Automatically Timed Flow Rate Measurement
 Volumetric displacement of polymer melt over time Volumetric displacement measurements for MVR
 No cutting and weighing (simpler method)
 More precise for routine analysis Upper scribe
 Piston in proper position at end of pre-heating time to
activate calibrate encoder
 Results: Lower scribe
𝟏𝟏𝟏𝟏𝝅𝝅𝑹𝑹𝟐𝟐 𝑳𝑳
𝑴𝑴𝑴𝑴𝑴𝑴 =
𝒕𝒕𝑩𝑩
where Digital encoder
3
𝑀𝑀𝑀𝑀𝑀𝑀 𝑐𝑐𝑐𝑐 �10𝑚𝑚𝑚𝑚𝑚𝑚 : 𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣 − 𝑓𝑓𝑓𝑓𝑓𝑓𝑓𝑓 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 (measuring time)
𝑅𝑅 (𝑐𝑐𝑐𝑐): 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 (0.477 𝑐𝑐𝑐𝑐)
𝐿𝐿 𝑐𝑐𝑐𝑐 : 𝐿𝐿𝐿𝐿𝐿𝐿𝐿𝐿𝐿𝐿𝐿 𝑜𝑜𝑜𝑜 𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡(0.635 𝑐𝑐𝑐𝑐)
𝑡𝑡𝐵𝐵 𝑚𝑚𝑚𝑚𝑚𝑚 : 𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡

𝑴𝑴𝑴𝑴𝑴𝑴 = 𝑴𝑴𝑴𝑴𝑴𝑴 × 𝝆𝝆𝒎𝒎


where
ρ𝑚𝑚 𝑔𝑔�𝑐𝑐𝑐𝑐3 : 𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑 𝑎𝑎𝑎𝑎 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 7
Proprietary & Confidential
Method A to B Conversion
Mass measurement for MFR

Method A/B Enter sample weights


For calculation of apparent melt density
Samples
 Measuring melt mass-flow rate (MFR) and melt
volume-flow rate (MVR) on the same charge of sample
 The ratio of the two values is a measure of the melt
density of the polymer in 𝑔𝑔/𝑐𝑐𝑐𝑐3
Volumetric displacement measurements for MVR
 Piston in proper position at end of pre-heating time to
activate calibrate encoder
 Results:
𝑴𝑴𝑴𝑴𝑴𝑴
𝑴𝑴𝑴𝑴𝑴𝑴𝑴𝑴 𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅𝒅 (𝝆𝝆𝒎𝒎 ) =
𝑴𝑴𝑴𝑴𝑴𝑴 Digital encoder
(measuring time)

8
Proprietary & Confidential
Method C & Method D

Method D
Method C Multi-Weight Using Automatically Timed
Automatically Timed Flow Rate Measurement for Flow Rate Measurements
High Flow Rate Polyolefins Using “Half” Die
 Flow Rate Ratio (FRR) test
 Using a modified die (D: 1.048 mm, L/D: 3.818)  Using two/three different test loads on
 For testing POs with a MFR of 75 or greater one charge of material
 Improve the reproducibility of results by reducing  Results:
the flow rate 𝑴𝑴𝑴𝑴𝑴𝑴𝑯𝑯𝑯𝑯𝑯𝑯𝑯𝑯𝑯𝑯𝑯𝑯 𝒕𝒕𝒕𝒕𝒕𝒕𝒕𝒕 𝒍𝒍𝒍𝒍𝒍𝒍𝒍𝒍
 procedures same as Method B with 2.540 cm 𝑭𝑭𝑭𝑭𝑭𝑭 =
𝑴𝑴𝑴𝑴𝑴𝑴𝑳𝑳𝑳𝑳𝑳𝑳𝑳𝑳𝑳𝑳 𝒕𝒕𝒕𝒕𝒕𝒕𝒕𝒕 𝒍𝒍𝒍𝒍𝒍𝒍𝒍𝒍
length of piston travel
 For comparison of MWD (higher FRR
means broader MWD)

9
Proprietary & Confidential
Operation Points

 Stabilizing the temperature of barrel with piston and die


in place for ~ 15 min prior to testing

 Swabbing out the barrel using cotton patches and barrel


cleaning tool

 Cleaning the die using a proper die cleaning tool

10
Proprietary & Confidential
Operation Points

 Using a die plug for materials with very high MFR

 Properly drying the hygroscopic samples (e.g. PET, PA,


PC, PU, PBT, PEEK, ABS)

 Sufficient melting time (7 minutes)


420 s

11
Proprietary & Confidential
Other Applications
Shear thinning of the polymer melt Intrinsic/solution Viscosity of PET
MFR (g/10min)

MFR (g/10min)
Weight (kg) Intrinsic Viscosity (dl/g)
 Determinning of IV of PET at 285 °C by melt
 Measuring MFR using various weights
rheometer (avoid using of noxious solvents)
 Graph of MFR vs Weight
 Describing the polymer flow behavior
 Both viscosity/MFR and IV are related to the
 Higher slope more shear thinning
polymer molecular weight1. So, they can be
 For comparing the MWD
correlated to each other!
1Fox-Flory and Mark-Houwink relationships
12
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Other Applications

Thermal stability

 resistance of polymer to a change in MFR at the


test temperature over specific period of time
MFR (g/10min)

 Can show the presence of moisture or reactive


chemicals in polymer.
 can measure the degradation rate or reactivity
of polymer
 Repeating the test at various temperatures to
give “processing window” of the polymer
Time (min)

13
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“Everything Flows”-Heraclitus
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Thank You !

14

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