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Method for determining content of sodium p-toluenesulfinate in reduction process of p-toluenesulfonyl chloride

A technology of sodium toluenesulfinate and p-toluenesulfonyl chloride, applied in the direction of color/spectral characteristic measurement, etc., can solve the problems of detection result error, analysis of sodium toluenesulfinate, difficulty in improving the reduction reaction process of toluenesulfonyl chloride, etc., and achieve The effect of meeting the needs of detection sensitivity

Inactive Publication Date: 2010-02-17
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This analysis method, because the conversion rate of the methylation reaction cannot reach 100%, thus brings great errors to the detection results
If the sodium p-toluenesulfinate cannot be accurately analyzed, it is difficult to improve or optimize the process of the reduction reaction of p-toluenesulfonyl chloride
At present, there is no method for determining the sodium p-toluenesulfinate in the mixture of sodium p-toluenesulfinate and sodium p-toluenesulfinate

Method used

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  • Method for determining content of sodium p-toluenesulfinate in reduction process of p-toluenesulfonyl chloride
  • Method for determining content of sodium p-toluenesulfinate in reduction process of p-toluenesulfonyl chloride
  • Method for determining content of sodium p-toluenesulfinate in reduction process of p-toluenesulfonyl chloride

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Experimental program
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Effect test

Embodiment 1

[0015] Preparation of standard solutions of sodium p-toluenesulfonate and sodium p-toluenesulfinate

[0016] Preparation of standard solution of sodium p-toluenesulfonate

[0017] Accurately weigh 0.3884g (0.002mol) of sodium p-toluenesulfonate, dissolve it in an appropriate amount of distilled water and carefully transfer it into a 100ml volumetric flask to prepare a 0.02mol / l sodium p-toluenesulfonate standard solution. Then take the above 0.02mol / l sodium p-toluenesulfonate standard solution 50ml, 25ml, 10ml, 5ml to 100ml volumetric flasks, and prepare 0.01mol / , 0.005mol / l, 0.002mol / l, 0.001mol / l Standard solution of sodium toluenesulfonate.

[0018] Preparation of standard solution of sodium p-toluenesulfinate

[0019] Accurately weigh 0.1782 g (0.001 mol) of purified sodium p-toluene sulfinate, dissolve it with an appropriate amount of distilled water, and transfer it into a 100 ml volumetric flask to prepare a 0.01 mol / l sodium p-toluene sulfinate standard solution.

Embodiment 2

[0021] Determination of Absorption Wavelength of Sodium p-Toluene Sulfinate Solution

[0022] Take 0.01mol / l, 0.005mol / l, 0.002mol / l, 0.001mol / l sodium p-toluenesulfonate standard solution and 0.01mol / l sodium p-toluenesulfinate standard solution in Example 1, respectively, with distilled water For blank sample, carry out UV full-wavelength scanning at 200-400nm with UV2500 UV / Vis spectrophotometer, and the resulting spectrum is as follows figure 1 shown. It can be seen from the figure that the maximum absorption wavelengths of the two substances, sodium p-toluenesulfonate and sodium p-toluenesulfinate, are not very different, so the maximum absorption wavelength cannot be used to analyze the content of these two substances. like figure 2 , 3, at the wavelength of 282nm, sodium p-toluenesulfonate has no absorption, but sodium p-toluenesulfinate still has a strong absorption, so 282nm is selected as the best measurement wavelength for sodium p-toluenesulfinate.

Embodiment 3

[0024] Drawing of standard curve of sodium p-toluenesulfinate solution

[0025] The measurement conditions of UV / Vis spectrophotometer are as follows: wavelength is fixed at λ=282nm; bandwidth=2nm; integration time=10s; temperature during measurement is 20±2°C;

[0026] Accurately draw 20ml, 15ml, 12.5ml, 10ml and 5ml of the standard solution of sodium p-toluenesulfinate solution in Example 1 into a 100ml volumetric flask, and dilute to the mark with distilled water to obtain concentrations of 0.002mol / l, 0.0015mol / l, 0.00125 The standard solutions of mol / l, 0.001mol / l and 0.0005mol / l, under the wavelength of 282nm of UV2500 ultraviolet / visible light spectrophotometer, use a 1cm cuvette, take distilled water as a reference solution, read the absorbance and draw a standard curve ( See Figure 4 ), the regression equation is y=0.01688+392.83612×X, the corresponding correlation coefficient R=0.99865, and the accuracy of the experimental data is good.

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Abstract

The invention relates to a method for determining the content of sodium p-toluenesulfinate in a reduction process of p-toluenesulfonyl chloride. A wavelength of 282 nm, which does not absorb sodium 4-toluenesulfonate and absorbs a great amount of sodium p-toluenesulfinate, is obtained by respectively scanning ultraviolet-spectrum full wavelengths of standard solutions of the sodium 4-toluenesulfonate and the sodium p-toluenesulfinate, not only can favorably determine the content of the sodium p-toluenesulfinate, but also can satisfy the needs on detection sensitivity. Under the wavelength, the method not only can differentiate the sodium 4-toluenesulfonate from the sodium p-toluenesulfinate which are contained in the solution, but also can simultaneously achieve the quantitative determination of the sodium p-toluenesulfinate.

Description

technical field [0001] The invention relates to a quantitative method for sodium p-toluene sulfinate, in particular to a method for quantifying sodium p-toluene sulfinate and sodium p-toluene sulfonate by ultraviolet spectrophotometry in a reduction process of p-toluenesulfonyl chloride. A method for distinguishing and quantifying sodium p-toluenesulfinate. Background technique [0002] Sodium p-toluenesulfinate is the product obtained by the reduction of p-toluenesulfonyl chloride, which is obtained by the reduction of p-toluenesulfonyl chloride in an aqueous sodium sulfite solution. Since this step reaction in the aqueous solution is accompanied by the hydrolysis of p-toluenesulfonyl chloride to generate a by-product—sodium p-toluenesulfonate, it is very necessary to monitor the progress of the hydrolysis reaction during the production process. However, because the two substances are very close in the peak time of liquid chromatography, and the content of sodium p-toluene...

Claims

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Application Information

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IPC IPC(8): G01N21/33
Inventor 吴建一缪程平邹玲宗乾收陶至芳
Owner JIAXING UNIV
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