Method for analyzing components of mother solution of glyphosine

A technique for the analysis method of bisglyphosate, which is applied in the field of chemical analysis, and can solve problems such as large interference, inaccurate measurement results, and no analytical method established

Inactive Publication Date: 2011-04-27
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is very difficult to deal with diglyphosate mother liquor in production at present, the main reason is that the composition of the mother liquor is relatively complex, and there are no relevant reports on the comprehensive analysis of diglyphosate mother liquor, and the actual analysis of many components of diglyphosate mother liquor has not yet established analytical methods
At present, the determination of the content of iminodiacetic acid of a single component in the solution mainly adopts the acid-base titration method using methyl red as an indicator; the determination of the content of phosphorous acid, phosphoric acid and hydrochloric acid of a single component in the solution mainly adopts conventional methods Acid-base titration, directly titrate with alkali standard solution; for the determination of the content of diglyphosate in a single component in the solution, mainly use a buffer solution with a pH of 9.0, arsenazo (Ⅲ) as an indicator, and lead nitrate standard solution Complexometric titration; Mainly adopt sodium sulfite addition method etc. to the mensuration of formaldehyde content in the solution; To the mensuration of the nitrilotriacetic acid of single component, use nitrogen determination method to measure nitrilotriacetic acid content in the prior art, but in the mother liquor, nitrogen-containing compound is more There are many, large interference, and acid-base complexometric titration is also useful, that is, after dissolving nitrilotriace

Method used

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  • Method for analyzing components of mother solution of glyphosine
  • Method for analyzing components of mother solution of glyphosine
  • Method for analyzing components of mother solution of glyphosine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of analytical method of diglyphosate mother liquor composition, wherein nitrilotriacetic acid is determined by following method:

[0033] Instrument: Shimadzu high performance liquid chromatography (with UV detector)

[0034] Chromatographic column: Inertsil ODS--4,250×4.5mm, 5μm

[0035] Mobile phase: 0.15% KH 2 PO 4 , with H 3 PO 4 Adjust pH=2.0

[0036] Flow rate: 0.6mL / min

[0037] UV: 195nm

[0038] Injection volume: 20μL

[0039] Determination of standard solution:

[0040] Take nitrilotriacetic acid (AR) as the reference substance, weigh 0.1000g into a 50mL volumetric flask, add water to dissolve and dilute to the mark, shake well, accurately draw 1mL of the solution into a 100mL volumetric flask, add mobile phase to dilute to the mark, Shake well, filter through a microporous membrane, and inject the sample. The peak area of ​​nitrilotriacetic acid is 66428.

[0041] Sample determination:

[0042] Accurately draw 5mL of the mother solution int...

Embodiment 2

[0062] A kind of analytical method of diglyphosate mother liquor composition, wherein nitrilotriacetic acid is determined by following method:

[0063] Instrument: Shimadzu high performance liquid chromatography (with UV detector)

[0064] Chromatographic column: DIKMA ODS-3, 250×4.5mm, 5μm

[0065] Mobile phase: 0.1% H 3 PO 4 Aqueous solution, pH=2.0

[0066] Flow rate: 0.8mL / min

[0067] UV: 195nm

[0068] Injection volume: 20μL

[0069] Determination of standard solution:

[0070] Take nitrilotriacetic acid (AR) as the reference substance, weigh 0.1155g into a 50mL volumetric flask, add water to dissolve and dilute to the mark, shake well, accurately draw 1mL of the solution into a 100mL volumetric flask, add mobile phase to dilute to the mark, Shake well, filter through a microporous membrane, and inject the sample. The peak area of ​​nitrilotriacetic acid is 67886.

[0071] Sample determination:

[0072] Accurately draw 5mL of the mother solution into a 50mL vol...

Embodiment 3

[0092] A kind of analytical method of diglyphosate mother liquor composition, wherein nitrilotriacetic acid is determined by following method:

[0093] Instrument: Shimadzu high performance liquid chromatography (with UV detector)

[0094] Chromatographic column: DIKMA ODS-3, 250×4.5mm, 5μm

[0095] Mobile phase: 0.2% KH 2 PO 4 , with H 3 PO 4 Adjust pH=2.0

[0096] Flow rate: 1.5mL / min

[0097] UV: 195nm

[0098] Injection volume: 20μL

[0099] Determination of standard solution:

[0100] Take nitrilotriacetic acid (AR) as the reference substance, weigh 0.1155g into a 50mL volumetric flask, add water to dissolve and dilute to the mark, shake well, accurately draw 1mL of the solution into a 100mL volumetric flask, add mobile phase to dilute to the mark, Shake well, filter through a microporous membrane, and inject the sample. The peak area of ​​nitrilotriacetic acid is 66101.

[0101] Sample determination:

[0102] Accurately draw 5mL of the mother solution into a ...

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Abstract

The invention discloses a method for analyzing components of mother solution of glyphosine, in particular a method for analyzing the components of mother solution generated by preparing the glyphosine from iminodiacetonitrile serving as a main raw material. In the method, the contents of N-(phosphonomethyl) iminodiacetic acid, nitrilotriacetic acid and iminodiacetic acid in the mother solution are independently measured, and polyacids such as the N-(phosphonomethyl) iminodiacetic acid, phosphoric acid, phosphorous acid and the like are measured stepwise; meanwhile, calcium chloride is added to strengthen weak acid, quantitative inactive hydrogen is released, and the phosphoric acid, nitrilotriacetic acid and the N-(phosphonomethyl) iminodiacetic acid are measured; and according to reaction rules and interrelation of substances, the contents of the iminodiacetic acid, the N-(phosphonomethyl) iminodiacetic acid, the nitrilotriacetic acid, the phosphorous acid, hydrochloric acid and the phosphoric acid are skillfully measured. Through verification, the method is accurate, comprehensive, scientific, reasonable, and easy to operate, provides a reliable basis for recycling and comprehensively utilizing the mother solution of the glyphosine, and has high promotion value.

Description

technical field [0001] The invention relates to a method for analyzing the components of diglyphosate mother liquor, in particular to a method for analyzing the components of mother liquor produced when diglyphosate is produced by using iminodiacetonitrile as the main raw material, and belongs to the field of chemical analysis. Background technique [0002] Diglyphosate (N-(phosphomethyl)iminodiacetic acid) [0003] It is an intermediate for the production of glyphosate (N-phosphonomethylglycine) from iminodiacetonitrile (IDA method). Glyphosate is a widely used organic phosphine herbicide, which has the characteristics of high efficiency, broad spectrum, low toxicity and safety, and is very effective in the control of perennial deep-rooted weeds. In recent years, due to the large-scale promotion of glyphosate-resistant genetically modified crops, making its use more convenient, the market demand for glyphosate has grown rapidly, and it has continuously replaced other typ...

Claims

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Application Information

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IPC IPC(8): G01N21/79G01N21/31G01N30/02G01N30/60
Inventor 罗延谷董远萍何咏梅胡欣陈敬
Owner CHONGQING UNISPLENDOUR CHEM
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