Determination of Xylene Solubles in Polypropylene

xyle
Determination of Xylene Solubles

in Polypropylene
Xylene solubles (XS) is a historically established term denoting
Application Note 16
the percentage of soluble species in polypropylene homo- and

co-polymers. This value is approximately proportional to the
amorphous content of the materials. In practice this measure is
widely used for product quality control and monitoring physical
properties of the polymer during synthesis and processing.
Method
The xylene extraction method (ASTM D5492, technically
equivalent to the standard ISO 16152) is commonly employed
to determine the xylene solubles content by weight. However,
this method requires dissolution of the products in a harmful
solvent, use of high temperatures (135 and 150C), large
Calibration and Results
sample sizes (to guarantee reliable reproducibility), highly
The calibration is generated using at least 6 samples of real
skilled analysts, and long measurement times.
products with predefined xylene solubles values spanning the
The xylene solubles can also be measured using a Fourier
range of concentrations of interest. Figure 1 shows a calibration
transform infrared technique (FTIR). Although this method
for polypropylenes with xylene solubles content ranging from
reduces significantly the analysis time, it requires delicate
0.9 to 4.9 % by weight (wt.-%). As seen in this figure, NMR
sample preparation and a highly skilled operator.
gives an excellent linear correlation between the NMR response
In contrast to the standard wet chemistry method and FTIR
and the concentration of xylene solubles in the products.
technique, low resolution Nuclear Magnetic Resonance

(NMR) provides a fast, direct and user friendly method for
determination of the xylene solubles content in polypropylene
products that can be operated by a non NMR expert user.
This technique is based on measurement of the NMR
response obtained from amorphous part of the material, and
quantification of the xylene solubles content by calibration.
Advantages of benchtop NMR
NMR is very stable over the long-term, therefore requires

little recalibration
The sample measurement time is short (typically 20 seconds)

Minimal sample preparation is required
The NMR technique is non-destructive, so repeatability
1
measurements can be made conveniently.
Samples require preconditioning at 60C for 20 minutes.
Figure 1: Calibration obtained for xylene solubles in polypropylenes;

standard deviation of the linear fit is 0.06 wt.-%, correlation coefficient
R2 = 1.00. Measurements were made using Oxford Instruments MQC23 benchtop NMR analyser fitted with an 18 mm diameter probe.
Oxford Instruments
Magnetic Resonance
Table 1. Results of instrument repeatability test
Given XS
Value,
wt.-%
Results (wt.-%) of Repeat Measurements
0.92
0.94 0.87 0.90 0.94 0.92 0.91 0.93 0.89 0.92 0.91
Mean XS Standard
Value,
Deviation
wt.-%
wt.-%
0.91
0.02
For more information please email:

magres@oxinst.com
UK
Tubney Woods, Abingdon
The instrument repeatability was tested
In addition to this package the following
by measuring one sample ten times. After
equipment is required:
every test measurement, the sample was
Dry block heater capable of maintaining
transferred from the magnet bore back to

the conditioning block for 20 min to be
conditioned at 60C and then measured again.
Table 1 shows the repeatability test results.
Recommended Instrument
Configuration
The MQC-23 with 0.55 Tesla magnet fitted
with an 18 mm diameter (8 ml) probe is ideal
for this application. The Xylene Solubles in
Polypropylene package comprises:
The MQC-23 which can be controlled using

its own built-in computer using Microsoft
Windows or via a stand-alone PC
MultiQuant software including

RI Calibration, RI Analysis, and the EasyCal
samples at 60C
Aluminium block with holes for 18 mm

diameter tubes
Oxon, OX13 5QX, UK

Tel.: +44 (0) 1865 393 200
Fax: +44 (0) 1865 393 333
China
Room 14-F, No. 1 Plaza
No. 800 Nanjing East Road
Shanghai 200001, China
The instrument offers

multiple advantages over
other instruments on the
market:
Tel: +86 21 6132 9678
High signal sensitivity

Small benchtop footprint
Specific Xylene Solubles in
Concord, Mass 01742, USA
Fax: +86 21 6360 8535

USA
300 Baker Avenue, Suite 150
Tel: +1 978 369 9933
Fax: +1 978 369 8287
Polypropylene Applications Software
Low maintenance
Minimal sample preparation
Xylene Solubles in Polypropylene application
Test / tuning sample

Sample tubes with an outer diameter
of 18 mm
Polytetrafluoroethylene (PTFE) stoppers

Stopper removal tool
Installation Manual
Method Sheet
visit www.oxford-instruments.com for more information
This publication is the copyright of Oxford Instruments Molecular Biotools Ltd. and provides outline information only, which (unless agreed
by the company in writing) may not be used, applied or reproduced for any purpose or form part of any order or contract or regarded as the
representation relating to the products or services concerned. Oxford Instruments policy is one of continued improvement. The company
reserves the right to alter, without notice the specification, design or conditions of supply of any product or service. Oxford Instruments
Molecular Biotools Ltd. acknowledges all trademarks and registrations. Oxford Instruments Magnetic Resonance is a trading name of Oxford
Instruments Molecular Biotools Ltd. Oxford Instruments Molecular Biotools Ltd., 2010. All rights reserved. Part no: XS-02-10
www.oxford-instruments.com

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xyle

Determination of Xylene Solubles

Xylene solubles (XS) is a historically established term denoting

the percentage of soluble species in polypropylene homo- and

Calibration and Results

sample sizes (to guarantee reliable reproducibility), highly

The calibration is generated using at least 6 samples of real

skilled analysts, and long measurement times.

products with predefined xylene solubles values spanning the

The xylene solubles can also be measured using a Fourier

range of concentrations of interest. Figure 1 shows a calibration

transform infrared technique (FTIR). Although this method

for polypropylenes with xylene solubles content ranging from

reduces significantly the analysis time, it requires delicate

0.9 to 4.9 % by weight (wt.-%). As seen in this figure, NMR

sample preparation and a highly skilled operator.

gives an excellent linear correlation between the NMR response

In contrast to the standard wet chemistry method and FTIR

and the concentration of xylene solubles in the products.

technique, low resolution Nuclear Magnetic Resonance

Advantages of benchtop NMR

NMR is very stable over the long-term, therefore requires

The sample measurement time is short (typically 20 seconds)

measurements can be made conveniently.

Samples require preconditioning at 60C for 20 minutes.

Figure 1: Calibration obtained for xylene solubles in polypropylenes;

Table 1. Results of instrument repeatability test

Results (wt.-%) of Repeat Measurements

For more information please email:

The instrument repeatability was tested

In addition to this package the following

by measuring one sample ten times. After

every test measurement, the sample was

Dry block heater capable of maintaining

transferred from the magnet bore back to

The MQC-23 which can be controlled using

MultiQuant software including

Aluminium block with holes for 18 mm

Oxon, OX13 5QX, UK

The instrument offers

Tel: +86 21 6132 9678

High signal sensitivity

Concord, Mass 01742, USA

Fax: +86 21 6360 8535

Polypropylene Applications Software

Xylene Solubles in Polypropylene application

Test / tuning sample

Polytetrafluoroethylene (PTFE) stoppers

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