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Method for determining contents of monomers of ENB type ethylene-propylene-diene monomer rubber

A technology of EPDM rubber and monomer content, which is applied in the preparation of test samples and analysis by nuclear magnetic resonance, etc. It can solve the problems of single detection object, cumbersome experimental process, complicated sample preparation, etc., and simplify the experimental steps , easy to operate, and save testing costs

Inactive Publication Date: 2014-12-03
HUBEI INST OF AEROSPACE CHEMOTECH
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Problems solved by technology

[0004] The above public documents reflect the technical status of the determination of monomer content in ENB rubber, and its technical defects are: sample preparation is complicated, the experimental process is cumbersome, the test object is single, and the test cost is high

Method used

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  • Method for determining contents of monomers of ENB type ethylene-propylene-diene monomer rubber
  • Method for determining contents of monomers of ENB type ethylene-propylene-diene monomer rubber

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Embodiment Construction

[0009] Below in conjunction with embodiment the present invention is further described.

[0010] Step 1, determining the detection object: three monomers of ethylene, propylene and ethylidene norbornene in EPDM rubber are used as detection objects.

[0011] Step 2, preparing test samples: pre-weighing and cutting the test samples into fine pieces. Cut about 30mg of EPDM type ethylene propylene diene monomer into the size of sesame seeds, and fill it in the solid NMR rotor.

[0012] Step 3, select the detection conditions: the detection equipment used to collect the NMR experiment spectrum is a solid-state nuclear magnetic resonance spectrometer, and the collection method is a single-pulse hydrogen decoupling pulse sequence of carbon, wherein, in the process of selecting the detection conditions, the nuclear magnetic rotor rotation frequency No less than 10kHz, magnetic field strength of 9.4 Tesla, dual-channel magic-angle rotating probe; acquisition pulse delay time of 60 sec...

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Abstract

The invention discloses a method for determining the contents of monomers of an ENB (ethylidene norbornene) type ethylene-propylene-diene monomer rubber and for aviation fuel solid nuclear magnetic resonance analysis. The method comprises the steps of determination of detected objects, preparation of a detected sample, selection of detection conditions, implementation of nuclear magnetic detection, and processing of detection data, wherein ethylene, propylene and ethylidene norbornene of the ethylene-propylene-diene monomer rubber are taken as the detected objects; the detected sample is subjected to pre-weighing and small block cutting treatment; a solid nuclear magnetic resonance spectrometer is adopted, and an acquisition method is carbon monopulse and hydrogen-decoupled pulse sequences; and after belongingness of spectral peaks and integration of spectral peak areas, the detection data is obtained through formula calculation. With utilization of the solid nuclear magnetic resonance spectrometer, with the monomers of the ethylene-propylene-diene monomer rubber as the detected objects, and through sample preparation, spectrogram acquisition, spectral peak belongingness, integration processing and formula calculation, the mass percentage contents of the monomers of the sample are obtained. The method has the advantages of convenient operation, safe use, accurate detection data and scientific experimental method, simplifies the experimental steps, and saves detection costs.

Description

technical field [0001] The invention relates to a solid-state nuclear magnetic resonance analysis method for aerospace polymer thermal insulation materials, in particular to a method for measuring the content of each monomer of ENB-type ethylene-propylene-diene rubber. ENB is the abbreviation of ethylidene norbornene. Background technique [0002] The Chinese journal "Journal of Analytical Testing" in the second issue of volume 21 in 2002 reported the document "EPDM rubber 13 C-NMR Quantitative Analysis", this document uses the liquid nuclear magnetic resonance method to determine the content of each monomer of EPDM rubber. The sample preparation process of this method is cumbersome and requires the use of toxic reagents. [0003] Appendix C of the "ENB Type EPDM Specification" in the Chinese National Military Standard GJB5180-2003 reports "Determination of the Ethylene Content of ENB Type EPDM Rubber". This standard uses an infrared spectrometer to measure the absorbance o...

Claims

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Application Information

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IPC IPC(8): G01N24/08G01N1/28
Inventor 胡伟赵志刚聂海英马新刚庞爱民黄志萍
Owner HUBEI INST OF AEROSPACE CHEMOTECH
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