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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, material analysis, chemical analysis by titration, etc., can solve problems such as system errors and achieve good uniformity and stability

Inactive Publication Date: 2018-02-27
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] The present invention provides a solid moisture standard substance and a preparation method thereof, including the following steps:

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

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

[0042]

[0043] In the above formula:

[0044] m 2 ——The quality of sodium tartrate dihydrate;

[0045] m 1 ——The quality of p-methoxybenzoic acid;

[0046] x——The target moisture content of the solid moisture standard material;

[0047] x 1 ——The moisture content of p-methoxybenzoic acid; ...

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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, and 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 for moisture detection in food, medicine and petrochemical products. Karl Fischer titration includes Karl Fischer coulometric method and Karl Fischer volumetric method. Regardless of the coulometric method or the volumetric method, calibration with reference materials with known moisture content is required. Although the coulometric method can directly calculate the moisture content of the sample based on the electrolysis power, due to the system error caused by the electrolysis efficiency and the side reaction of the Karl Fischer reaction, the directly calculated moisture has a certain deviation from...

Claims

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Application Information

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Patent Type & Authority Patents(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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