Method for accurately and stably detecting purity of oxygen-linked bis (diphenylarsonic) by utilizing gas chromatography
A gas chromatography and stable detection technology, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of split discrimination and poor reproducibility, and achieve the effects of product quality control, accurate and stable measurement, and accurate quantification.
Pending Publication Date: 2022-04-01
中国人民解放军军事科学院防化研究院
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Problems solved by technology
[0004] The purpose of the present invention is to solve the problems of poor reproducibility and shunt discrimination when using gas chromatography to analyze oxygen-linked diphenylarsine, and to provide a method for accurately and stably detecting the purity of oxygen-linked bis-diphenylarsine by gas chromatography. Accurate and repeatable, can quickly and accurately determine the purity of oxygen-linked bis-diphenylarsine
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Embodiment 1
[0020] The method for accurately and stably detecting the purity of oxygen-linked bis-diphenylarsine by gas chromatography adopts the following experimental conditions:
[0021] 1. Experimental analysis instruments and conditions: GC 8000 TOP gas chromatograph, hydrogen flame ionization detector.
[0022] 2. Experimental sample: Oxydiphenylarsine standard product, synthesized in the laboratory, with a purity of 96.0%.
[0023] 3. Chromatographic conditions:
[0024] Chromatographic column: chrompack CP 8 type chromatographic column, 30m*0.25mm*0.25μm.
[0025] Carrier gas: The carrier gas is helium.
[0026] Column front pressure: 110kPa
[0027] Injection port temperature: 300°C
[0028] Column temperature rise program: initial temperature is 200°C, keep the temperature for 1 minute, then raise the temperature to 300°C at a rate of 10°C per minute, and keep the temperature for 12 minutes.
[0029] Injection volume: 1μL
[0030] Split: 30:1
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The invention relates to a method for accurately and stably detecting the purity of oxygen-linked bis (diphenylarsonic) by using gas chromatography, and belongs to the field of chemical detection of toxic agents. The method comprises the following steps: (1) preparing an oxydiphenylarsonic standard solution; (2) detecting by a gas chromatography hydrogen flame ionization detector; and (3) calculating by an area normalization method. According to the method, the purity of oxygen-linked bis-diphenylarsonic is detected by adopting a gas chromatographic method, the method has the advantages of being accurate in quantification, good in repeatability and the like, and relative standard deviations (n = 3) of analysis of samples with different concentrations are all smaller than or equal to 0.40%. The method can accurately and stably measure the purity of oxygen-linked bis (diphenylarsonic), overcomes the defects of shunting discrimination of a gas chromatography sample injection port on a target object and impurities and the like, realizes rapid and accurate measurement, and achieves control on the quality of a synthetic toxic agent product.
Description
technical field [0001] The invention relates to a method for accurately and stably detecting the purity of oxygen-linked bis-diphenylarsine by gas chromatography, which belongs to the field of poison chemical detection. Background technique [0002] Diphenylcyanarsine and diphenylchloroarsine are typical irritant poisons. During the Second World War, Japan equipped and used a large number of such poisons and abandoned them in China, posing a serious threat to public safety. The arsenic-chlorine (As-Cl) bond in diphenylchloroarsine and the arsenic-cyanide (As-CN) bond in diphenylcyanarsine are very active, and are prone to substitution reactions in protic solvents and then dehydration polymerization to generate oxygen. Bidiphenylarsine. As one of the main degradation products of dicyanoarsine and diphenylchloroarsine, this compound still has high toxicity, so the detection method of oxydiphenylarsine has application value for indirect identification of organic arsenic poison...
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Login to View More IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/68
Inventor 刘石磊吴姬娜杨旸张巧利袁铃
Owner 中国人民解放军军事科学院防化研究院