Method for testing trace moisture in dimethyl sulfoxide

A dimethyl sulfoxide, trace moisture technology, applied in the preparation of test samples, material electrochemical variables, etc., can solve the problems of test result interference, unstable test results, and overall data decline.

Active Publication Date: 2014-07-23
XIAN KANGBEN MATERIAL
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

A large number of experimental results show that the Karl Fischer Coulomb method measures the water content in the solution with stable data and reliable results. However, when testing the water content of the dimethyl sulfoxide solution, the test results are unstable with the prolongation of the test time. And there is the problem that the overall test result is lower than the true value; it is also found that when the Karl Fischer Coulomb method is used to measure the water content in a certain solution, the data is reliable and stable. After sulfone, when the water content of the solution was tested again, the overall data dropped sharply and became unstable, indicating that the presence of dimethyl sulfoxide in the Karl Fischer reagent would interfere with the test results

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  • Method for testing trace moisture in dimethyl sulfoxide
  • Method for testing trace moisture in dimethyl sulfoxide
  • Method for testing trace moisture in dimethyl sulfoxide

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Embodiment 1

[0026] The present embodiment is a kind of Karl Fischer coulometric method testing the method for trace moisture in dimethyl sulfoxide, and its specific process comprises the following steps:

[0027] Step 1, prepare ethanol aqueous solution. The ethanol aqueous solution is prepared from ethanol and pure water. The mass fraction of pure water in the ethanol aqueous solution is 0.9-1.2%. In this embodiment, the mass fraction of pure water in the ethanol aqueous solution is 1.2%. The specific configuration process is as follows: uniformly mix absolute ethanol and pure water to obtain ethanol aqueous solution. The prepared aqueous ethanol solution is divided into two parts, the first part of ethanol water solution is used to prepare the mixed solution with Karl Fischer reagent as a new Karl Fischer reagent; the second part of ethanol aqueous solution is used to test its water content under different conditions Comparison of results.

[0028] In step 2, the water content of the...

Embodiment 2

[0043] The present embodiment is a kind of Karl Fischer coulometric method testing the method for trace moisture in dimethyl sulfoxide, and its specific process comprises the following steps:

[0044] Step 1, prepare ethanol aqueous solution. The ethanol aqueous solution is prepared from ethanol and pure water. The mass fraction of pure water in the ethanol aqueous solution is 0.9-1.2%. In this embodiment, the mass fraction of pure water in the ethanol aqueous solution is 1.1%. The specific configuration process is as follows: uniformly mix absolute ethanol and pure water to obtain ethanol aqueous solution. The prepared aqueous ethanol solution is divided into two parts, the first part of ethanol water solution is used to prepare the mixed solution with Karl Fischer reagent as a new Karl Fischer reagent; the second part of ethanol aqueous solution is used to test its water content under different conditions comparison of results;

[0045] In step 2, the water content of the...

Embodiment 3

[0060] The present embodiment is a kind of Karl Fischer coulometric method testing the method for trace moisture in dimethyl sulfoxide, and its specific process comprises the following steps:

[0061] Step 1, prepare ethanol aqueous solution. The ethanol aqueous solution is prepared from ethanol and pure water. The mass fraction of pure water in the ethanol aqueous solution is 0.9-1.1.2%, and in this embodiment, the mass fraction of pure water in the ethanol aqueous solution is 1.0%. The specific configuration process is as follows: uniformly mix absolute ethanol and pure water to obtain ethanol aqueous solution. The prepared aqueous ethanol solution is divided into two parts, the first part of ethanol water solution is used to prepare the mixed solution with Karl Fischer reagent as a new Karl Fischer reagent; the second part of ethanol aqueous solution is used to test its water content under different conditions comparison of results;

[0062] In step 2, the water content ...

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Abstract

The invention provides a method for testing trace moisture in dimethyl sulfoxide. Prepared ethanol water is divided into two parts; a first part of the ethanol water is used for preparing a uniform transparent mixed system of dimethyl sulfoxide, hydroxylamine hydrochloride, the ethanol water and a Karl Fischer's reagent; and a second part of the ethanol water is used for comparison of moisture content with the uniform transparent mixed system of dimethyl sulfoxide, hydroxylamine hydrochloride, the ethanol water and the Karl Fischer's reagent. In the system where dimethyl sulfoxide and the Karl Fischer's reagent coexist, dimethyl sulfoxide has the capability of oxidizing I<-> ions and is reduced to be dimethyl thioether. According to the invention, since hydroxylamine hydrochloride in the Karl Fischer's reagent containing dimethyl sulfoxide is pre-oxidized by dimethyl sulfoxide, it is guaranteed that the I<-> ions are completely converted into I2 through an electrode, testing results are real, reliable and stable, and deficiency in testing of trace moisture in a dimethyl sulfoxide solution by using Karl Fischer coulometry is overcome.

Description

technical field [0001] The invention relates to the field of trace moisture testing, in particular to a method for testing trace moisture in dimethyl sulfoxide. Background technique [0002] Dimethyl sulfoxide is a sulfur-containing organic compound. It is a colorless, odorless, transparent liquid at room temperature. It is a hygroscopic flammable liquid. It has high polarity, high boiling point, good thermal stability, aprotic, and Water miscibility and other characteristics, can be dissolved in most organic substances such as ethanol, propanol, and chloroform, known as "universal solvent", widely used as solvents and reaction reagents, especially as processing solvents and spinning solvents, such as polyurethane Synthesis and spinning solvents, polyamide, polyimide and polysulfone resin synthesis solvents, aromatic hydrocarbons, butadiene extraction solvents and chlorofluoroaniline synthesis solvents, etc. In addition, it is also widely used in the pharmaceutical industry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/42G01N1/28
Inventor 郭香杨阳锋郭继荣郑桂宁徐永花吴斌
Owner XIAN KANGBEN MATERIAL
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