Method for determining unsaturated degree of viscous solid substance by infrared spectrum and specimen rack used in method

A solid material and sample support technology, applied in the unsaturation determination of low unsaturation rubber such as butyl rubber and EPDM rubber, in the field of sample support, it can solve the problem of sample deformation, influence of infrared analysis results, easy deformation, etc. problem, to save time and cost, simplify the process and improve accuracy

Active Publication Date: 2012-10-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] In particular, it should be pointed out that for viscous solid substances, due to its high viscosity and easy deformation characteristics, when using the above tablet method to prepare samples, on the one hand, it is difficult to take it out from the mold due to its high viscosity; This removal operation also causes a large deformation of the sample, which affects the results of infrared analysis and leads to inaccurate analysis results
In addition, the above-mentioned tableting method cannot guarantee the thickness of the sample, but must be measured for the thickness of the sample. However, due to the high viscosity and easy deformation of the viscous solid substance, the measurement of its thickness is very difficult, so the above-mentioned tableting method cannot guarantee the thickness of the sample. accuracy, which will also affect the accuracy of infrared analysis results
[0017] In addition, potassium bromide was used to dilute the sample to be tested in the above tablet method, which may be feasible for the analysis of higher component content, but for low component content, such as as low as 0.5% to 3.3% (mol) Butyl rubber unsaturation, which is difficult to measure accurately by infrared analysis after further dilution with potassium bromide

Method used

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  • Method for determining unsaturated degree of viscous solid substance by infrared spectrum and specimen rack used in method
  • Method for determining unsaturated degree of viscous solid substance by infrared spectrum and specimen rack used in method
  • Method for determining unsaturated degree of viscous solid substance by infrared spectrum and specimen rack used in method

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Embodiment 1

[0063] In this embodiment, the hot tablet machine used is CARVER-3800 hot press machine (American Laboratory Equipment Company), and the balance used is METTLER AL-204 with an accuracy of 0.1 mg. The chromatograph used was Shimadzu FTIR-8201PC Fourier Transform Infrared Spectrometer.

[0064] Weigh 6 butyl rubber samples of 0.1850 g to be tested, put them into the 6 through holes 5 of the porous template 2 with an aperture of 13 mm and a thickness of 0.6 mm, cover the two sides with a polytetrafluoroethylene film 3, and then clamp Upper two steel plates 4 are put into a tablet press for tableting. The tableting conditions are: pressure of 7 tons, temperature of 150° C., and tableting time of 5 minutes. Optionally, you can add 1 ton of pressure before pressing the tablet, and then release the pressure, and repeat it twice to eliminate air bubbles. In addition, for thermoplastic polymers or plastic inorganic substances that do not undergo chemical changes near the softening po...

Embodiment 2

[0072] In this embodiment, the equipments such as hot tablet machine, balance and chromatograph used are the same as those in Embodiment 1 above.

[0073] Weigh 6 EPDM samples of 0.1850g to be tested, put them into 6 through-holes 5 of the porous template 2 with an aperture of 13mm and a thickness of 0.6mm respectively, cover both sides with a polytetrafluoroethylene film 3, and then Clamp two steel plates 4 again, put into the tablet press machine and carry out tablet compression. The tableting conditions are: pressure 7 tons, temperature 160° C., and tableting time 5 minutes. Next cooling step, infrared measuring step etc. are identical with the corresponding step about butyl rubber in the above-mentioned embodiment 1, thereby obtain as follows Figure 6 The infrared spectrum of the tested EPDM rubber for one of the samples is shown. Take 1687.6cm on the infrared spectrum -1 As the quantitative characteristic peak of unsaturation, manually select the range of the characte...

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Abstract

The invention provides a method for measuring unsaturated degree of a viscous solid substance by the use of an infrared instrument. The method provided by the invention comprises the following steps of: respectively putting a certain amount of at least one viscous solid substance into a plurality of through holes of a porous sample preparation plate, tabletting in a tablet press to prepare samples, placing the sample preparation plate carried with a plurality of samples onto a specially-produced specimen rack in order to carry out infrared detection on an infrared spectrometer, and contrasting the standard curve obtained in dependence on a standard sample with known saturation degree according to the obtained spectrogram so as to directly obtain the unsaturated degree of the viscous solid substance to be measured. The invention also relates to the specimen rack which can be used in the above infrared measurement method.

Description

technical field [0001] The invention relates to a method for quantitatively analyzing the degree of unsaturation of viscous solid substances, especially rubber polymers, by using infrared spectroscopy. The invention is especially suitable for the unsaturation determination of low unsaturation rubbers such as butyl rubber and EPDM rubber. The invention also relates to a sample holder for use in the above method. Background technique [0002] In the synthetic rubber industry, some rubbers have relatively low unsaturation, such as butyl rubber and EPDM rubber. For low unsaturation butyl rubber, its unsaturation is only between 0.5% and 3.3% (mol); for low unsaturation EPDM rubber, its unsaturation is usually below 10% (mol). The methods for determining the degree of unsaturation disclosed in the literature include online prediction method, iodine index method, epoxy titration method, nuclear magnetic resonance spectroscopy, gel permeation chromatography-ultraviolet method, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/35F16M11/20F16M3/00G01N21/3563
Inventor 孙秀霞邱迎昕王艳洁周新钦
Owner CHINA PETROLEUM & CHEM CORP
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