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Infrared spectroscopic determination method of bound acrylonitrile content in nitrile rubber

A measurement method, infrared spectroscopy technology, applied in the direction of measuring devices, material analysis through optical means, instruments, etc., can solve the problems that the accuracy of standard samples is difficult to guarantee

Active Publication Date: 2017-05-10
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method discloses a method for measuring the content of acrylonitrile in liquid rubber. Its obvious defect is that the accuracy of the standard sample selected for making the standard curve is difficult to guarantee.

Method used

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  • Infrared spectroscopic determination method of bound acrylonitrile content in nitrile rubber
  • Infrared spectroscopic determination method of bound acrylonitrile content in nitrile rubber
  • Infrared spectroscopic determination method of bound acrylonitrile content in nitrile rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1 test steps

[0049] (1) Preparation of sample solution

[0050] ① Extract the added oil and antioxidant in the nitrile rubber test sample with absolute ethanol, and then dry the extracted nitrile rubber test sample in a vacuum oven at 90°C.

[0051] ② Weigh 0.3g of the sample to be tested obtained in step ①, and put it into a 20mL sample bottle;

[0052] ③ Add 10mL of acetone to the sample bottle in step ②, shake the sample bottle to completely dissolve the nitrile rubber to be tested.

[0053] (2) Film preparation

[0054] Apply the sample solution obtained in step (1) evenly on the potassium bromide sheet, and evaporate the acetone on the potassium bromide sheet to prepare the sample membrane to be tested.

[0055] (3) Determination of infrared spectrum

[0056] ① Put the diaphragm obtained in step (2) into the infrared spectrometer;

[0057] ② The scanning parameters of the infrared spectrometer are set to 400cm -1 and 4000cm -1 , measure the background spec...

Embodiment 2

[0069] 1 test steps

[0070] (1) Preparation of sample solution

[0071] ①Use n-propanol to extract the added oil and antioxidant in the nitrile rubber test sample, and then dry the extracted nitrile rubber test sample in a vacuum oven at 105°C.

[0072] ②Weigh 0.1g of the sample to be tested obtained in step ①, and put it into a 20mL sample bottle;

[0073] ③ Add 20mL of acetone to the sample bottle in step ②, shake the sample bottle to completely dissolve the nitrile rubber to be tested.

[0074] (2) Film preparation

[0075] Apply the sample solution obtained in step (1) evenly on the potassium bromide sheet, and evaporate the acetone on the potassium bromide sheet to prepare the sample membrane to be tested.

[0076] (3) Determination of infrared spectrum

[0077] ① Put the diaphragm obtained in step (2) into the infrared spectrometer;

[0078] ② The scanning parameters of the infrared spectrometer are set to 600cm -1 and 2500cm -1 , measure the background spectrum ...

Embodiment 3

[0090] 1 test steps

[0091] (1) Preparation of sample solution

[0092] ① Extract the added oil and antioxidant in the nitrile rubber test sample with methanol, and then dry the extracted nitrile rubber test sample in a vacuum oven at 100°C.

[0093] ②Weigh 0.4g of the sample to be tested obtained in step ①, and put it into a 20mL sample bottle;

[0094] ③Add 15mL methyl ethyl ketone into the sample bottle in step ②, shake the sample bottle to completely dissolve the nitrile rubber to be tested.

[0095] (2) Film preparation

[0096] Apply the sample solution obtained in step (1) evenly on the potassium bromide sheet, evaporate the methyl ethyl ketone on the potassium bromide sheet, and prepare the sample membrane to be tested.

[0097] (3) Determination of infrared spectrum

[0098] ① Put the diaphragm obtained in step (2) into the infrared spectrometer;

[0099] ② The scanning parameters of the infrared spectrometer are set to 600cm -1 and 4000cm -1 , measure the bac...

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Abstract

The invention relates to an infrared spectroscopic assay method of the content of bound acrylonitrile in nitrile butadiene rubber. With a substitute standard rubber of which the mass percentage content of the bound acrylonitrile is known with the range being 17.5-39.5%, a standard curve is drawn form 3-10 points within the range to establish a quantitative formula (I). By means of an infrared spectrometer, the absorbance of 1,4-trans-polybutadiene (A<trans>), the absorbance of 1,2-vinyl-polybutadiene(A<vinyl>), the absorbance of 1,4-cis-polybutadiene (A<cis>), and the absorption area of the bound acrylonitrile (S<acrylonitrile>) are measured and are respectively substituted into the formula (I) and a formula (II) to calculate the mass percentage content of the bound acrylonitrile.

Description

technical field [0001] The invention relates to an analysis method for rubber microstructure content, in particular to an infrared spectrum determination method for combined acrylonitrile content in nitrile rubber. Background technique [0002] Nitrile rubber (NBR) is a synthetic rubber produced by the copolymerization of butadiene and acrylonitrile. NBR contains polar nitrile groups, has good oil resistance, solvent resistance and heat aging resistance, and is widely used in automobiles, aerospace, petrochemicals, textiles, wire and cable, printing and food packaging and other fields. [0003] The content of combined acrylonitrile has an important impact on the quality and performance of NBR. The content of combined acrylonitrile affects the difficulty of rotation in the rubber molecular chain and the intermolecular force, thereby affecting the flexibility of the molecular chain and the physical and mechanical properties of the product. The combined acrylonitrile content i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/3563
Inventor 高杜娟赵家琳吴毅范国宁王芳耿占杰刘俊保杨芳贾慧青李晓银魏玉丽笪敏峰黄世英高东梅赵慧晖
Owner PETROCHINA CO LTD
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