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Method for measuring total chlorine in methanesulfonic acid

A technology of methanesulfonic acid and a determination method, which is applied in the preparation of test samples, material analysis by observing the influence on chemical indicators, and analysis by chemical reaction of materials, etc., can solve the problem of no organic chlorine detection method. , did not explain the organic chlorine digestion method and other issues, to achieve the effect of high accuracy, easy operation and improved accuracy

Inactive Publication Date: 2014-05-21
SHANGHAI SINYANG SEMICON MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the analysis of inorganic chlorine, the national standard GB / T 9729-2007 general method for the determination of chloride, nitric acid acidification, silver chloride turbidimetry and the national standard GB / T 3050-2000 general method for the determination of chloride in inorganic chemical products - potentiometric titration There is no detection method for organochlorine in the two national standards, that is, the digestion method for organochlorine is not specified

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Accurately weigh 5 g of the sample into a polytetrafluoroethylene beaker, add 10 mL of electronic grade sodium hydroxide with a mass fraction of 50%, and slowly heat the sample on a heating plate until crystallization occurs.

[0042] After cooling, add 10mL of 25% nitric acid solution and 5mL of 17g / L silver nitrate solution, then add 2mL of 50% triethylene glycol solution, shake well, set the volume to 50g, let stand for 20min, and make a sample blank at the same time.

[0043] Measure the absorbance of the treated sample at 425nm on a UV-visible spectrophotometer with a 3cm cuvette, and measure the absorbance of the blank solution at the same time.

Embodiment 2

[0045] Accurately weigh 3 g of the sample into a polytetrafluoroethylene beaker, add 20 mL of electronic grade sodium hydroxide with a mass fraction of 25%, and slowly heat the sample on a heating plate until crystallization occurs.

[0046] After cooling, add 8mL of 25% nitric acid solution and 3mL of 17g / L silver nitrate solution, then add 5mL of 100% ethylene glycol solution, shake well, set the volume to 50g, let stand for 40min, and make a sample blank at the same time.

[0047] Measure the absorbance of the treated sample at 425nm on a UV-visible spectrophotometer with a 3cm cuvette, and measure the absorbance of the blank solution at the same time.

Embodiment 3

[0049] Accurately weigh 1 g of the sample into a polytetrafluoroethylene beaker, add 5 mL of electronic grade sodium hydroxide with a mass fraction of 10%, and slowly heat the sample on a heating plate until crystallization occurs.

[0050] After cooling, add 5mL of 25% nitric acid solution and 1mL of 17g / L silver nitrate solution, then add 10mL of 70% triethylene glycol solution, shake well, set the volume to 50g, let stand for 10min, and make a sample blank at the same time.

[0051] Measure the absorbance of the treated sample at 425nm on a UV-visible spectrophotometer with a 3cm cuvette, and measure the absorbance of the blank solution at the same time.

[0052] Draw the standard curve:

[0053] Take 0, 0.5, 1, 2, and 5 g of chloride ion standard solutions with concentrations of 100 μg / g respectively, add 10 mL of nitric acid with a volume fraction of 25% and 5 mL of silver nitrate solution with a volume fraction of 17 g / L, and then add 2 mL of triethylene glycol with a ma...

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Abstract

The invention discloses a method for measuring total chlorine in methanesulfonic acid. The method comprises the following steps: step 1, weighing a methanesulfonic acid sample of which the mass is 1-5 g, adding 5-20 ml of 10%-50% high-purity alkali solution, heating until crystal occurs, cooling, and then adding 5%-50% nitric acid to regulate the pH to be 1-4; step 2, adding 1-5 mL of 17g / L silver nitrate and 5-10 mL of 25% nitric acid solution, then adding 1-10 mL of 50%-100% polyalcohol as a dispersant, uniformly mixing silver chloride precipitate which is generated, standing for 10-40 minutes, and simultaneously preparing a blank solution; step 3, measuring the absorbancy of the sample solution and the blank solution; step 4, drawing a standard curve; and step 5, obtaining the content of the total chlorine in the sample solution according to the standard curve. The measurement method for measuring the total chlorine in the methanesulfonic acid provided by the invention has the advantages of being simple and easy to operate, good in reproducibility and high in recycle rate.

Description

technical field [0001] The invention relates to a method for analyzing and measuring organic chlorine in organic acids, in particular to a method for measuring total chlorine in industrial methanesulfonic acid. Background technique [0002] Methanesulfonic acid is also called methanesulfonic acid or methanesulfonic acid, referred to as MSA, and its molecular formula is CH 3 SO 3 H, is an organic strong acid, non-oxidizing acid. Methanesulfonic acid is an important intermediate in organic synthesis and medicine, and is often used in organic synthesis as a solvent, alkylation and lipidation reagent. In recent years, due to the excellent metal salt solubility, non-oxidation and environmental protection of methanesulfonic acid, its plating solution can obtain high-quality deposits, and can perform high-speed plating at high current densities. The field of electroplating has gradually become a mainstream solution. For example: the electroplating solution system of tin methane...

Claims

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Application Information

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IPC IPC(8): G01N1/44G01N21/78
Inventor 黄桂华李莎
Owner SHANGHAI SINYANG SEMICON MATERIALS
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