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Viscosity of polyamides Ted Brink

Polyamide viscosity measurement methods

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Different ways to express the molecular weight of polyamides

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Page 1: Polyamide viscosity measurement methods

Viscosity of polyamides

Ted Brink

Page 2: Polyamide viscosity measurement methods

Page 2

Effects of molecular weight

The molecular weight of a polymer influences:• melt viscosity (flow behaviour)• processing behaviour• mechanical properties• crystallization behaviour• optical properties

Page 3: Polyamide viscosity measurement methods

Page 3

Methods to measure molecular weight

• Melt viscosity as a function of shear rate• MFI (Melt Flow Index)• MVR (Melt Volume Rate)• RSV (Relative Solution Viscosity)• VN (Viscosity Number) • GPC (Gel Permeation Chromatography)• SEC (Size Exclusion Chromatography)

Page 4: Polyamide viscosity measurement methods

Page 4

MFI and MVRDisadvantages for polyamidecharacterization:• moisture

sensitivity• polymer reactivity

Units:• MFI in g/10 min• MVR in cm3/10 min

Capillary ( D = 2.0955 mm, L = 8.000 mm )

Barrel ( D = 9.5504 mm )

Piston( D = 9.4742 mm )

Temperature Control( ± 0.2oC )

Thermometeror PRT( ± 0.1oC )

Load (Wt + Piston = ± 0.5% )

Standardized test (ASTM D1238, ISO 1133)

Constant load test

Fixed die diameter

Fixed die L/D ratio

Mass / time measured

MFR 1/Viscosity

May be related to, but is not a strict function of Mw

Page 5: Polyamide viscosity measurement methods

Page 5

Limitations of MFI measurement

0.01 0.1 1 10 100 100010

01

00

01

00

00

γ

η

Two types of materials with the same MFI valuebut completely different rheological behaviorHygroscopic and chemical character of PA6 influence accuracy of measurement

melt indexconditions

A

B

Page 6: Polyamide viscosity measurement methods

Page 6

RSV and VN according to ISO 307

• solvents used:- 90 % formic acid- 96 % sulphuric acid- 100 % m-cresol- others

• concentration 1 g polymer/100 ml• measured at 25 °C• Ubbelohde capillary

RSV = Tsolution/TsolventVN = (Tsolution/Tsolvent)/c

Page 7: Polyamide viscosity measurement methods

Page 7

GPC/SEC

0

5

10

15

20

25

15 20 25 30 35

Ve (ml)

Raw

RI s

ign

al (

mV

)

0

0.2

0.4

0.6

0.8

1

1.2

3 3.5 4 4.5 5 5.5 6

LogMd

w/d

Lo

gM

Page 8: Polyamide viscosity measurement methods

Page 8

Methods to express molecular weight

η0 at

260

°C

MFI at

250

°C

Mn Mw VNRSV

H2SO4

RSV

HCOO

H

Pa.s g/10 ‘ g/mol g/mol cm3/g

1070 7.7 18000 35000 197 3.3 3.0

1280 7.1 20000 40000 210 3.6 3.2

2600 3.3 22000 47000 245 4.0 3.6

Page 9: Polyamide viscosity measurement methods

Page 9

Relation MFI and RSV (in formic acid)

2 2.2 2.4 2.6 2.8 3 3.2 3.4 3.6 3.8 40

10

20

30

Relative solution viscosity in formic acid

Melt

flow

in

dex [

g/1

0

min

]MFI measured at 235 °C and 2.16 kg

Page 10: Polyamide viscosity measurement methods

Page 10

Contact

Ted Brink

tel.: +31 (0) 651109899

email: [email protected]

internet: www.extrusionist.com