Rapid instrument analysis method for residual quantity of hydroxylamine in reaction solution

A technology of instrumental analysis and reaction solution, which is applied in the field of chemical analysis, can solve the problems of not meeting the detection requirements and small detection amount, and achieve the effects of high accuracy, fast analysis speed and strong specificity

Inactive Publication Date: 2018-01-26
合肥利夫生物科技有限公司
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Problems solved by technology

[0004] Application publication number CN102937577A discloses a method for detecting trace amounts of hydroxylamine in water by ABTS free radical fading spectrophotometry. The detection amount of this technology is small and cannot meet the detection requirements of production

Method used

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  • Rapid instrument analysis method for residual quantity of hydroxylamine in reaction solution
  • Rapid instrument analysis method for residual quantity of hydroxylamine in reaction solution
  • Rapid instrument analysis method for residual quantity of hydroxylamine in reaction solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1 linear equation and standard substance chromatogram

[0050] Using acetonitrile-water (60:40, V / V) as solvent, configure a series of standard solutions with benzaldoxime standard solution concentrations of 20, 15, 10, 5, 1, 0ug / ml respectively, and inject samples under the above-mentioned chromatographic conditions The peak area was measured and quantified by the external standard method. Standard solution chromatogram such as " figure 1 ", take the peak area y as the ordinate, and the concentration x as the abscissa to perform linear regression, and the results are shown in "Table 1".

[0051] Retention time, linear equation and correlation coefficient of benzaldoxime in Table 1:

[0052] Analyte

Embodiment 2

[0053] Embodiment 2 derivation process optimization

[0054] 2.1 Choice of derivatization solvent

[0055] During the experiment, the choice of solvent for the derivatization reaction directly affects whether the solution is uniform during the derivatization process, and affects the accuracy of the detection results. In order to obtain the most accurate measurement results possible, we must choose a solvent that will make the derivatization reaction solution homogeneous. After literature review and specific experimental process in the laboratory, ethanol-purified water (12:3.8; g / g) was selected as the derivatization reaction solvent, and it was found that the use of this derivation solvent was better than other derivation solvents (such as ethanol-purified water; 50 / 50; V / V) can make the derivatization reaction solution uniform and non-layered, which is convenient for weighing and testing.

[0056] 2.2 Method detection limit and precision

[0057] LOD and LOQ are compound ...

Embodiment 3

[0066] The detection of residual amount of hydroxylamine in the reaction solution of embodiment 3

[0067] This method and the 2015 edition of "Chinese Pharmacopoeia" were used to detect the residual amount of hydroxylamine in the reaction solution.

[0068] This method: Weigh 1.7325g of hydroxylamine reaction solution into a 25ml volumetric flask, add 0.9488g of benzaldehyde, add 11.6663g of absolute ethanol, add 1.9885g of purified water, place on a constant temperature magnetic stirrer and stir for 1 hour. Then weigh 114.1 mg of the above solution into a 25 ml volumetric flask filled with 5 ml of acetonitrile, add 60% acetonitrile aqueous solution (acetonitrile: water = 60:40, V / V) to dilute to the mark, and mix well. To be analyzed by liquid chromatography. Test result: the content of hydroxylamine in the hydroxylamine reaction liquid is 1.75% (mass percentage).

[0069] The 2015 edition of "Chinese Pharmacopoeia" method: pipette 0.5ml of hydroxylamine reaction solution ...

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Abstract

The invention discloses a rapid instrument analysis method for the residual quantity of hydroxylamine in a reaction solution. The method comprises the following steps: 1, carrying out a derivatizationreaction on the hydroxylamine-containing reaction solution and benzaldehyde to generate benzaldoxime; and 2, determining the content of the benzaldoxime in the above obtained derivatization solutionof the reaction solution through high performance liquid chromatography, and calculating the content of the hydroxylamine in the original reaction solution according to the content of the benzaldoxime. The analysis and detection method provided by the invention has the advantages of simplicity in operation, high accuracy, strong specificity, high sensitivity, fast analysis speed and high efficiency. Compared with the prior art, the method allows determination using a high performance liquid chromatograph to be carried out after the derivatization reaction, and realize accurate qualitative andquantitative determination in order to meet needs in researches and production.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and relates to a rapid instrumental analysis method for residual hydroxylamine in a reaction solution, in particular to a method for producing benzaldehyde oxime through the reaction of benzaldehyde and hydroxylamine, which can be accurately qualitatively determined by liquid chromatography. A rapid instrumental analysis method for quantifying the content of hydroxylamine in the reaction solution. Background technique [0002] Hydroxylamine is usually used as a reducing agent in organic synthesis. In industry, hydroxylamine hydrochloride is usually used to dissociate hydroxylamine into hydroxylamine, and then let hydroxylamine react with succinic anhydride to generate N-hydroxysuccinimide. In this reaction, hydroxylamine hydrochloride is usually excessive and unreacted The finished hydroxylamine is unstable and explosive in the reaction solution, so the residual amount of hydroxylamine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 余三喜张坤徐海曹胜男徐芬
Owner 合肥利夫生物科技有限公司
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