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Detecting method for 2, 5-dyhydroxy-1, 4-dithiane content

A detection method and technology of dithiane, which can be applied in the direction of removing certain components for weighing and chemical analysis by titration, which can solve the problems of weighing deviation, gas chromatography injection volume deviation, chromatographic peak area deviation, etc. , to achieve the effect of parallel and stable data, less equipment investment, and low detection cost

Inactive Publication Date: 2018-07-31
WEIFANG HUITAO CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The traditional detection method of 2,5-dihydroxyl-1,4-dithiane content takes 2,5-dihydroxyl-1,4-dithiane standard substance as a reference, prepares a gas chromatography detection solution according to the standard, and passes Gas chromatography automatically injects samples, compares and detects solution concentration, product peak area, loss on drying, etc., and obtains the content of the sample. This method requires high conditions, and there is an impact of storage time on the content of the reference substance. Deviation, gas chromatography injection volume deviation, chromatographic peak area deviation and other shortcomings

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  • Detecting method for 2, 5-dyhydroxy-1, 4-dithiane content
  • Detecting method for 2, 5-dyhydroxy-1, 4-dithiane content
  • Detecting method for 2, 5-dyhydroxy-1, 4-dithiane content

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Effect test

Embodiment 1

[0031] Embodiment 1 A kind of detection method of 2,5-dihydroxyl-1,4-dithiane content

[0032] Add 0.2520g of 2,5-dihydroxy-1,4-dithiane sample with 0.16% loss on drying to a 250ml iodine flask, add 100ml of purified water and 10ml of 2% (w / w) sulfuric acid solution, and ultrasonically dissolve After 20 minutes, add 50ml 0.1N iodine solution after completely dissolving, mix well, titrate with 0.1040N sodium thiosulfate standard solution until light yellow, add 1ml (10g / L) starch indicator, continue titrating until colorless or white, consume 0.1040N sodium thiosulfate 17.20ml;

[0033] The blank test consumes 49.22ml of 0.1040N sodium thiosulfate.

[0034] The blank test: in a 250ml iodine measuring bottle, add 100ml purified water and 10ml 2% (w / w) sulfuric acid solution, then add 50ml 0.1N iodine solution, mix well, and titrate to 0.1040N sodium thiosulfate standard solution Light yellow, add 1ml (10g / L) starch indicator, continue to titrate until colorless or white, consu...

Embodiment 2

[0042] Embodiment 2 A kind of detection method of 2,5-dihydroxyl-1,4-dithiane content

[0043] Add 0.2481g 2,5-dihydroxy-1,4-dithiane sample with 0.21% loss on drying to a 250ml iodine flask, add 100ml purified water and 10ml 2% (w / w) sulfuric acid solution, and ultrasonically dissolve After 20 minutes, add 50ml 0.1N iodine solution after completely dissolving, mix well, titrate with 0.1040N sodium thiosulfate standard solution until light yellow, add 1ml (10g / L) starch indicator, continue titrating until colorless or white, consume 0.1040N sodium thiosulfate 17.65ml; blank test consumes 0.1040N sodium thiosulfate 49.22ml.

[0044] The blank test: in a 250ml iodine measuring bottle, add 100ml purified water and 10ml 2% (w / w) sulfuric acid solution, then add 50ml 0.1N iodine solution, mix well, and titrate to 0.1040N sodium thiosulfate standard solution Light yellow, add 1ml (10g / L) starch indicator, continue to titrate until colorless or white, consume 49.22ml of 0.1040N sodi...

Embodiment 3

[0052] Embodiment 3 A kind of detection method of 2,5-dihydroxy-1,4-dithiane content

[0053] Add 0.2484g 2,5-dihydroxy-1,4-dithiane sample with 0.18% loss on drying to a 250ml iodine flask, add 100ml purified water and 10ml 2% (w / w) sulfuric acid solution, and ultrasonically dissolve After 20 minutes, add 50ml 0.1N iodine solution after completely dissolving, mix well, titrate with 0.1040N sodium thiosulfate standard solution until light yellow, add 1ml (10g / L) starch indicator, continue titrating until colorless or white, consume 0.1040N sodium thiosulfate 17.64ml; blank test consumes 0.1040N sodium thiosulfate 49.22ml.

[0054] The blank test: in a 250ml iodine measuring bottle, add 100ml purified water and 10ml 2% (w / w) sulfuric acid solution, then add 50ml 0.1N iodine solution, mix well, and titrate to 0.1040N sodium thiosulfate standard solution Light yellow, add 1ml (10g / L) starch indicator, continue to titrate until colorless or white, consume 49.22ml of 0.1040N sodiu...

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Abstract

The invention provides a detecting method for 2, 5-dyhydroxy-1, 4-dithiane content. A 2, 5-dyhydroxy-1, 4-dithiane sample is added in an iodine flask, 100 milliliters of purified water and 10 milliliters of sulfuric acid solution are added, dissolution is performed for 20-30 minutes, 50 milliliters of iodine solution is added after complete dissolution of the purified water and sulfuric acid solution and mixed uniformly, titration is carried out with 0.1040 N of sodium thiosulfate standard solution until the color is pale yellow, 1 milliliter of starch indicator is added, and the titration iscontinuously carried out until the color is colourless and white to the end. Compared with a traditional gas chromatography detecting method that a 2, 5-dyhydroxy-1, 4-dithiane primary standard substance is taken as a contrast for comparison, the detecting method does not need gas chromatography, the primary standard substance is not needed, the method has the advantages that the equipment investment is less, the detecting is simple and convenient, the data is parallel and stable, the detecting cost is low, and the operation is easy, and the detecting method is applicable to production detection.

Description

technical field [0001] The invention relates to a method for detecting the content of 2,5-dihydroxy-1,4-dithiane, which belongs to the field of fine chemicals. Background technique [0002] The traditional detection method of 2,5-dihydroxyl-1,4-dithiane content takes 2,5-dihydroxyl-1,4-dithiane standard substance as a reference, prepares a gas chromatography detection solution according to the standard, and passes Gas chromatography automatically injects samples, compares and detects solution concentration, product peak area, loss on drying, etc., and obtains the content of the sample. This method requires high conditions, and there is an impact of storage time on the content of the reference substance. Deviation, gas chromatographic injection volume deviation, chromatographic peak area deviation and other shortcomings. Contents of the invention [0003] In order to solve the deficiencies in the prior art, the present invention provides a method for detecting the content ...

Claims

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Application Information

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IPC IPC(8): G01N5/04G01N31/16
CPCG01N31/16G01N5/04
Inventor 刘剑伟丁翔
Owner WEIFANG HUITAO CHEM
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