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Sulfonic acid analog anion surfactants rapid checking method

A surfactant and detection method technology, applied in the field of analytical chemistry, can solve the problems of difficult sulfonic acid reduction, troublesome preparation, cumbersome steps, etc., and achieve the problem of effective component analysis and identification, good gas chromatography-mass spectrometry behavior, and reaction process fast effect

Inactive Publication Date: 2008-11-19
袁慧娟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But for sulfonic acid, the step of preparing methyl sulfonate is more loaded down with trivial details, need to prepare free sulfonic acid first
If the ammonium salt pyrolysis method is used, the chromatographic peaks obtained by cleavage of amines cause difficulties in the detection of sulfonic acid derivatives
[0007] Due to the stability of the sulfonic acid group, the derivatization effect of its silylation is not good, and it still has the disadvantage of troublesome preparation
[0008] The preparation of the same sulfonamide is even more cumbersome, it is necessary to obtain the sulfonyl halide first, and then react with the secondary amine to prepare
[0009] The preparation of sulfonyl halides is relatively convenient, but the aliphatic chain sulfonyl halides are easily decomposed and cannot be separated and analyzed by gas chromatography
[0010] The reduction of sulfonic acid is relatively difficult, so far there is no very mature derivatization reaction that can be chromatographically analyzed by reducing sulfonic acid to sulfhydryl through a one-step reaction

Method used

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  • Sulfonic acid analog anion surfactants rapid checking method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 5g of commercially available washing powders named Omiao, Baimao, and Jiamei, each containing sulfonic anionic surfactants, add 0.2g of potassium iodide, 10mL of N, N-dimethylformamide in turn, and shake until completely dissolved. Then add 0.7mL (about 5mmol) trifluoroacetic anhydride dropwise, the solution immediately turns dark red, and white smoke is generated, the reaction is violent, and elemental iodine is precipitated. After the color no longer deepens, the solution at this time is subjected to chromatic analysis.

[0022] The detection conditions of gas chromatography-mass spectrometry detection are as follows:

[0023] Detection instrument: Finnigan Voyager gas chromatography-mass spectrometer

[0024] Chromatographic column: DB-5 (30m×0.25mm, 0.25μm)

[0025] Column temperature: 90°C (hold for 2min) ~ 200°C (hold for 10min)

[0026] Heating rate: 15°C / min

[0027] Gasification chamber temperature: 250°C

[0028] Carrier gas (flow rate): He(1.0mL / m...

Embodiment 2

[0040] The invention is applied to the detection of sulfonic acid anionic surfactants in environmental water samples. Take 1L of washing wastewater, use 717 strong basic anion exchange resin (that is, quaternary ammonium styrene-divinylbenzene strong base anion exchange resin) to enrich and elute the anionic surfactant in the water. Dry the eluate with nitrogen, add 0.2 g of potassium iodide, 10 mL of N, N-dimethylformamide in sequence, and shake until completely dissolved. Then add 0.7mL (about 5mmol) trifluoroacetic anhydride dropwise, the solution immediately turns dark red, and white smoke is generated, the reaction is violent, and elemental iodine is precipitated. After the color no longer deepens, the solution at this time is subjected to chromatic analysis. The experimental results show that potassium iodide and N, N-dimethylformamide and trifluoroacetic anhydride derivative system are effective, combined with gas chromatography-mass spectrometry detection technology, ...

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Abstract

The invention discloses a fast detection method for detecting anionic surface active agent of sulfuric acids, which comprises: a potassium iodide is mixed with a sulfuric acid negative ion surface active agent by a molar ratio of 1:1-10:1, then N and N-dimethyl formamide having the amount of 5 to 20ml / mol of potassium iodide are added into the mixture, the mixture is agitated to reach complete dissolution, then trifluoroacetic anhydride with the molar ratio one to ten times the amount of potassium iodide is added into the solution, the solution turns into red and is taken for implementing the conventional gas phase chromatography-mass spectrum detection and then data processing analysis when the color stops darkening, thereby obtaining the detecting result. The detection method has advantages of fast and simple reaction process and easy control of conditions, and makes up defects that the traditional detection method has false positive easily and can not ensure detection results and has high requirements on sample pre-processing, and the method is particularly suitable for qualitative and quantitative analysis of all components in complex compounds such as anionic surface active agent.

Description

technical field [0001] The invention relates to a detection method of a surfactant, belonging to the field of analytical chemistry, in particular to a detection method of a sulfonic acid anionic surfactant. Background technique [0002] Sulfonic acid anionic surfactants are a class of compounds widely used in the fields of chemical industry and medicine, which have the characteristics of strong polarity and low volatility. Playing a great role in all aspects, sulfonic acid anionic surfactants have also brought serious environmental problems while being mass-produced and widely used. When they enter the water body, they will cause the water to produce foam, emulsification and particle suspension, which will isolate the exchange of oxygen in the water and oxygen in the air, affect the purification of the water body, cause the deterioration of the water quality, and pollute the environment. Therefore, the analysis and identification of sulfonic acid anionic surfactants are of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N1/28
Inventor 袁慧娟
Owner 袁慧娟
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