Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same

An infrared spectrometer, a technology of solid matter, used in the determination of unsaturation of low-unsaturation rubber such as butyl rubber and EPDM rubber, and the field of sample holders, which can solve sample deformation, difficult to measure results, and affect infrared analysis. Results and other issues, to achieve the effect of saving time and cost, saving operation time, and simplifying the process

Active Publication Date: 2012-07-11
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

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  • Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same
  • Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same
  • Method for measuring unsaturation degree of sticky solid matter by infrared spectrometer and sample support for same

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Embodiment 1

[0061] 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.

[0062] Weigh 0.1850g of the butyl rubber sample to be tested, put it into a single-hole sample plate 2 with an aperture of 13mm and a thickness of 0.6mm, cover both sides with a polytetrafluoroethylene film 3, and then clamp two steel plates 4, put it into Tablets are compressed in a tablet press. 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 point, the sample can...

Embodiment 2

[0068] In this embodiment, the equipments such as hot tablet machine, balance and chromatograph used are the same as those in Embodiment 1 above.

[0069] Weigh 0.1850g of the EPDM sample to be tested, put it into a single-hole template 2 with an aperture of 13 mm and a thickness of 0.6 mm, cover both sides with a polytetrafluoroethylene film 3, and then clamp two steel plates 4, Put it into a tablet machine for 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 Image 6 The infrared spectrogram of the EPDM rubber to be tested is shown. Take 1687.6cm on the infrared spectrum -1 As the quantitative characteristic peak of unsaturation, manually select the range of the characteristic spectral region according to the actual situation, and obta...

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Abstract

The invention provides a method for measuring the unsaturation degree of sticky solid matter by an infrared spectrometer, comprising the following steps of: putting a sticky solid matter with a certain quantity into a hole of a single-hole sample preparation plate, tabletting in a tabletting machine to prepare a sample, and putting the sample preparation plate carried with the sample on a special sample support, so that the infrared measurement can be carried out on the infrared spectrometer. According to an obtained spectrum chart, and a standard curve obtained according to a standard sample with a known saturation degree, the unsaturation degree of the sticky solid matter to be detected can be directly obtained. The invention further relates to a sample support which can be used in the infrared measurement method.

Description

technical field [0001] The invention relates to a method for quantitatively analyzing the unsaturation of viscous solid substances, especially rubber polymers, by using an infrared spectrometer. 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, and infra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/35G01N1/28G01N21/01G01N21/3563
Inventor 孙秀霞邱迎昕王艳洁周新钦
Owner CHINA PETROLEUM & CHEM CORP
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