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A kind of method for measuring methyl phosphine dichloride content

A technology for methyl phosphine dichloride and chloride ion content, which is applied in measuring devices, instruments, scientific instruments, etc., and can solve the problems affecting the accuracy of measurement values ​​of methyl phosphine dichloride, high sample preparation requirements, titration interference, etc. problem, to achieve the effect of low cost, high accuracy and less interference

Active Publication Date: 2021-10-12
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the hydrolysis process, HCl gas is easily lost due to volatilization, and the titration has clear requirements on pH, such as: mercury nitrate titration of chloride ions requires a pH of 3 to 4, silver nitrate titration of chloride ions requires a pH of 6 to 7; and, if If the concentration of methyl phosphate after hydrolysis in the sample is too high, it will interfere with the titration, thereby affecting the accuracy of the measured value of methyl phosphine dichloride;
[0007] 3. Using an infrared spectrophotometer to measure methylphosphine dichloride, mainly based on the fact that the infrared absorption value of methylphosphine dichloride is significantly lower than that of phosphorus trichloride, but this method has high requirements for sample preparation and is relatively cumbersome to operate

Method used

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  • A kind of method for measuring methyl phosphine dichloride content
  • A kind of method for measuring methyl phosphine dichloride content
  • A kind of method for measuring methyl phosphine dichloride content

Examples

Experimental program
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Effect test

Embodiment 1

[0063] A method for measuring methyl phosphine dichloride content, comprising the steps:

[0064] 1) Preparation of standard products

[0065] Weighing: Weigh the methyl phosphine dichloride standard and the phosphorus trichloride standard respectively, and set aside;

[0066] Standard pretreatment:

[0067] Put the aqueous sodium hydroxide solution in the reaction device, put the reaction device in an ice-water bath, and keep the temperature in the reaction device at 0°C; then, add the standard methyl phosphine dichloride dropwise into the reaction device through a constant pressure dropping funnel , stirring, chlorine ions are generated; finally, take the reaction solution in the reaction device and repeatedly wash the constant pressure dropping funnel to obtain the product Ⅰ containing chloride ions;

[0068] Put the sodium hydroxide aqueous solution in the reaction device, put the reaction device in an ice-water bath, and keep the temperature in the reaction device at 0°...

Embodiment 2

[0094] On the basis of embodiment 1, further,

[0095] The methyl phosphine dichloride standard product is superior grade, and the phosphorus trichloride standard product is analytical pure.

Embodiment 3

[0097] On the basis of embodiment 2, further,

[0098] In the step 1) and step 4), the sodium hydroxide aqueous solution is 30wt.%.

[0099] In the pretreatment process of step 1) and step 4), the sodium hydroxide aqueous solution is first placed in the reaction device, and the reaction device is placed in an ice-water bath to keep the temperature in the reaction device at 0°C; Add the standard methylphosphine dichloride, phosphorus trichloride standard or the sample to be measured dropwise into the reaction device from the dropping funnel; during the dropping process, ensure that the temperature in the reaction device is lower than 10°C; finally, take the reaction device The reaction liquid in the constant pressure dropping funnel is washed repeatedly to ensure full reaction.

[0100] Such as Figure 4 As shown: there are four openings on the reaction device, including opening I, opening II, opening III and opening IV, and opening I is set with a constant pressure dropping ...

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Abstract

The invention relates to a method for measuring the content of methylphosphine dichloride, which belongs to the technical field of chemical quantitative analysis. In the present invention, high performance liquid chromatography is used to measure chloride ions in the pretreated standard solution, a standard curve is established, and a linear regression equation is made. Then, the pretreated sample solution is measured, and finally the methyl Phosphine dichloride content. The determination method has reasonable design, high accuracy, little corrosion to the instrument, low cost, less interference and good data reproducibility.

Description

technical field [0001] The invention relates to a method for measuring compounds, in particular to a method for determining the content of methylphosphine dichloride, which belongs to the technical field of chemical quantitative analysis. Background technique [0002] In the preparation process of the herbicide glufosinate-ammonium, methyl phosphine dichloride is an essential intermediate for the synthesis of diethyl methyl phosphite, and there are three raw materials that cannot be completely consumed in the system of synthesizing methyl phosphine dichloride. Phosphorous chloride, in order to improve the yield of methyl phosphine dichloride, need to further grasp the content of two components respectively in the mixed system of methyl phosphine dichloride and phosphorus trichloride, so that add appropriate amount of aluminum trichloride and Methyl phosphine dichloride generates complexes, and the methyl phosphine dichloride is purified. [0003] Therefore, in order to opti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 张弦彭舟皮亚威
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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