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Measurement of Spin Finish On Artificial Fibre Using The Weighing and Non Weighing Methods

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201 views

Measurement of Spin Finish On Artificial Fibre Using The Weighing and Non Weighing Methods

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Uploaded by

Anonymous PHCzwD8eAO
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© © All Rights Reserved
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SPIN

Measurement of Spin Finish on Artificial Fibre


using the Weighing and Non-Weighing Methods

Application Note 6

Summary

Up to 250 times faster than wet


chemistry methods

No hazardous solvents required; no


hazardous waste produced

Easiest, most reliable technique available


suitable for unskilled personnel

Reliable measurements down to low


concentrations

Ideal for high sample throughput

Method
Benchtop NMR detects the hydrogen signal of oil after the
signal from the solid fibre has decayed. Dividing this signal
by mass gives the hydrogen density of oil on the fibre which

Application
In the production of artificial fibres such as polyamide and
polyester, the fibres are sprayed with an oil-based coating to
reduce static electricity and friction as well as enhance certain
physical characteristics. This coating is variously known in
different countries as spin finish, oil pick-up (OPU) and finish
on yarn (FOY). Measurement of the applied spin finish using
the MQC analyser is fast, simple and solvent free. Like its
predecessor the MQA, the MQC supports a non-weighing
method which allows even faster measurements. The fast,
precise results obtainable with the MQC allow tighter control
of the manufacturing process which translates, in real terms,
to fewer out of specification products and lower production
costs due to less finish material being used.
Advantages of NMR
The traditional method of testing is to dissolve the coating
in an organic solvent and then determine the amount of
dissolved oil in the solvent either gravimetrically (following
distillation) or by use of infrared spectroscopy. All these
methods are time consuming, use hazardous solvents
and require skilled operators. Benchtop NMR provides an
alternative method which is quick and easy to perform, simple
to calibrate, and capable of determining finish levels below
those accurately measurable by solvent extraction.

correlates with the spin finish content. For some samples it is


possible to substitute mass with the total NMR signal from oil
and fibre thus removing the necessity to weigh the sample.
This is often called the ratio or non weighing method.

SPIN finish
xyle

Measurement of Spin Finish on


onArtificial
ArtificialFibre
Fibre
using the Weighing and Non-Weighing Methods

Weighing Method

Sample Name

Application Note 6

Given Spin
Finish Content

Measured
Finish Content

Difference

Determination of Xylene Solubles


in Polypropylene

Non Weighing Method

Sample Name

Application
ApplicationNote
Note16
6

Given Spin
Finish Content

Measured
Finish Content

Difference

1.335 1.330 -0.006

1.335 1.326 0.009

1.335 1.344 0.009

1.335 1.347 -0.012

0.877 0.869 -0.008

0.877 0.940 -0.063

0.877 0.897 0.020

0.877 0.928 -0.051

0.486 0.506 0.020

0.486 0.529 -0.042

0.486 0.531 0.045

0.486 0.540 -0.054

1.565 1.536 -0.029

1.565 1.548 0.017

1.565 1.559 -0.006

1.565 1.559 0.006

0.537 0.509 -0.028

0.537 0.497 0.040

0.537 0.500 -0.037

0.537 0.499 0.038

1.039 0.984 -0.055

1.039 0.979 0.060

1.039 1.063 -0.024

0.450 0.424 0.026

0.450 0.411 0.039

0.864 0.828 0.036

0.864 0.853 0.011

1.110 1.185 -0.075

1.110 1.095 0.015

0.623 0.670 -0.047

Figure 1: Calibration curve for the Weighing method


produced by the MQC (SD = 0.0325, r2 = 0.9962)

1.039 1.026 -0.013

0.450 0.440 -0.010

Calibration

0.450 0.433 -0.017

0.864 0.828 -0.036

0.864 0.862 -0.002

1.110 1.170 0.060

1.110 1.117 0.007

range of interest. NMR is a comparative technique therefore

0.623 0.674 0.051

its accuracy is only as good as that of the reference technique

1.005 0.952 -0.053

weighing method has the advantage of reducing the amount

1.005 0.957 0.048

against which it is being compared.

1.364 1.347 -0.017

of work required to carry out the analysis.

1.364 1.373 -0.009

1.575 1.637 0.062

1.575 1.575 0.000

0.503 0.528 0.025

Conclusion

0.503 0.492 0.011

1.004 1.020 0.016

NMR is very stable over the long term and rarely needs

1.004 0.980 0.024

Ultimately only two well known standards are required to


calibrate the instrument. However, initially it is recommended
that the instrument is calibrated by 3-6, preferably more,
standards with known coating weights evenly spread over the

Thereafter Artificial Setting Up Samples (SUSs) are available for


restandardising calibrations to compensate for small drifts in
the instrument, thus improving performance and ease of use.
Given that SUSs are very stable, they can be used in the long
term thus avoiding having to recalibrate an instrument on a
regular basis using real samples.


Average 0.000%

Std. Dev. 0.033%
Table 1: Comparison of NMR vs. given spin finish
contents using the weighing method on the MQC

Measurement
Samples are first weighed (weighing method only), pushed

Results

into a sample tube, then compressed to the optimum height

Figures 1 and 2 show the calibration graphs produced, and

using a PTFE stopper. After a suitable conditioning time, either

Tables 1 and 2 show the results from the same calibration

at room temperature or 40C, the sample is inserted into the

samples measured, using weighing and non-weighing

instrument. Measurement time is approximately one minute

methods respectively.

per sample.

Both graphs show good correlations between the reference

Weights can either be entered manually or transferred

values supplied and the NMR signal, r2 = 0.996 and 0.995

automatically from the electronic balance into the application

respectively for the weighing and non-weighing methods.

software (weighing method at room temperature only).

They also show that the spin finish can be measured accurately

Figure 2: Calibration curve for the non-weighing method


produced by the MQC (SD = 0.0375, r2 = 0.9949)

by NMR with standard deviations of 0.033% and 0.038%


between the given and measured values for the weighing and
non-weighing methods respectively. Of the two methods, the
weighing method yielded fractionally better correlation and
accuracy than the non-weighing method; however, the non-

calibration adjustment. If required, this can be done simply


Average 0.000%

using stable Setting Up Samples which recreates the


Std. Dev. 0.038%

original calibration carried out during installation

NMR penetrates through the whole sample and is

insensitive to air voids, which means it provides the most


accurate measurement of the total amount of oil in a
given volume of sample

In general, NMR is insensitive to colour


The NMR technique is non-destructive so the same sample
may be measured several times before being analysed by
other techniques

Sample measurement time is rapid (typically 64 seconds)

Table 2: Comparison of NMR vs given spin finish content


using the non-weighing method on the MQC

Oxford Instruments Ready-to-Run Application Package


For accurate determination of low spin finish
levels, the MQC-23 with a 0.55 Tesla (23 MHz)
magnet, fitted with an 18 mm diameter
(8 ml sample) probe is ideal. The Spin Finish
on Fibre package comprises:

MQC-23 which can be controlled using its

own built-in computer operating Microsoft


Windows or via a stand-alone PC

MultiQuant software including RI

Calibration, RI Analysis, and the EasyCal


Spin Finish application

Test/tuning sample
18 mm glass tubes

PTFE stoppers (to seal the tubes)


Stopper insertion/removal rod
Installation manual
Method sheet

Oxford Instruments
Magnetic Resonance
For more information please email:
[email protected]
UK
Tubney Woods, Abingdon
Oxon, OX13 5QX, UK

In addition you may require:

Tel.: +44 (0) 1865 393 200

A dry block heater and

Fax: +44 (0) 1865 393 333

aluminium block with holes for

China

sample conditioning at 40C

Room 1/E, Building 1

A precision balance

Xiangzhang Garden

A set of four Spin Finish

Shanghai 201102, China

(weighing method only)

Setting-Up-Standards (SUSs)

No. 248 Donglan Road


Tel: +86 21 6073 2925
Fax: +86 21 6360 8535
USA
300 Baker Avenue, Suite 150
Concord, Mass 01742, USA
Tel: +1 978 369 9933
Fax: +1 978 369 8287

visit www.oxford-instruments.com for more information


This publication is the copyright of Oxford Instruments 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 be regarded as a 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 acknowledges all trademarks
and registrations. Microsoft and Windows are registered trademarks of the Microsoft Corporation in the United States and other countries.
Ref. SF-08-11

www.oxford-instruments.com

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