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Solid moisture standard substance and preparation method thereof

A standard substance and moisture technology, applied in the preparation of test samples, analysis of materials, chemical analysis by titration, etc., can solve problems such as system errors

Inactive Publication Date: 2016-09-21
NAT INST OF METROLOGY CHINA
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Problems solved by technology

Although the coulometric method can directly calculate the moisture content of the sample according to the electrolysis electric quantity, due to the systematic error caused by the side reaction of the electrolysis efficiency and the Karl Fischer reaction, the directly calculated moisture has a certain deviation from the real moisture of the sample, and it is necessary to use the moisture standard substance determination method The relative indication error and correction coefficient, in order to correct the moisture measurement results of unknown samples

Method used

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  • Solid moisture standard substance and preparation method thereof
  • Solid moisture standard substance and preparation method thereof
  • Solid moisture standard substance and preparation method thereof

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preparation example Construction

[0039] A kind of solid moisture standard material and preparation method thereof of the present invention, comprises the following steps:

[0040] ①Put the raw material p-methoxybenzoic acid into the three-dimensional motion mixer, mix it for 10 minutes and take it out. The moisture content of p-methoxybenzoic acid was measured by Karl Fischer coulometric method. The moisture content of sodium tartrate dihydrate was measured by Karl Fischer coulometric method.

[0041] ②Take about 2kg of p-methoxybenzoic acid and add a certain quality of sodium tartrate dihydrate to prepare solid moisture standard substance. The added quality of sodium tartrate dihydrate is calculated according to the following formula.

[0042] m 2 = m 1 · ( x - x 1 ...

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Abstract

The invention relates to a solid moisture standard substance and a preparation method thereof. The method consists of: (1) preparation of solid moisture standard substance candidates; (2) water standard substance and preparation method thereof, comprising the steps of: (1) solid water standard material candidate preparation; (2) homogeneity test of the standard substance candidates; (3) stability test of the standard substance candidates; (4) value setting of the standard substance; and (5) uncertainty evaluation. Compared with the prior art, the moisture content of the moisture standard substance provided by the invention can be controlled by regulating the mass ratio of low moisture content p-methoxybenzoic acid to high moisture content sodium tartrate dehydrate, the moisture content can be arbitrarily controlled in the range of 0.1%-5%, thus having flexibility. The solid moisture standard substance has good homogeneity and stability. The standard substance can be used for calibration of the Karl-Fischer titration method, and also can be used for verification of the Karl-Fischer moisture measurement method.

Description

technical field [0001] The invention relates to a solid moisture standard substance and a preparation method thereof, which is a uniform solid moisture standard substance with adjustable moisture content. Background technique [0002] Karl Fischer titration is used to measure the moisture of solid and liquid samples. It is a specific method for moisture measurement and is widely used in the moisture detection of food, pharmaceuticals and petrochemical products. Karl Fischer titration includes Karl Fischer coulometric and Karl Fischer volumetric. Both coulometric and volumetric methods require calibration of standard substances with known moisture content. Although the coulometric method can directly calculate the moisture content of the sample according to the electrolysis electric quantity, due to the systematic error caused by the side reaction of the electrolysis efficiency and the Karl Fischer reaction, the directly calculated moisture has a certain deviation from the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N1/28
CPCG01N1/28G01N31/16G01N2001/2893
Inventor 王海峰刘卫全灿苏福海戴新华
Owner NAT INST OF METROLOGY CHINA
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