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Preparation method of moisture test sample and test method

A technology for testing samples and detection methods, which is applied in the field of moisture test sample preparation, can solve the problems of high moisture meter load, waste of materials, and many abnormal situations, and achieve the effects of accurate moisture detection data, reduced costs, and reduced test data errors

Inactive Publication Date: 2016-07-13
GUIZHOU ANDA TECH ENERGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects in the existing technology that it is necessary to prepare blank samples every day, waste of time, waste of materials, inaccurate test data, many abnormal conditions and high load of the moisture meter, and provide a method that reduces costs, reduces test data errors, and improves work efficiency. Method of preparing moisture test samples for efficiency and improved service life of moisture meter

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] According to the method for preparing a moisture test sample provided by the present invention, the method comprises: under sample preparation conditions, adding a sample to a sample preparation bottle, and sealing the sample preparation bottle as a test sample;

[0014] Or, under sample preparation conditions, directly seal the sample preparation bottle as a blank sample;

[0015] Wherein, the sample preparation conditions include a substantially constant moisture content.

[0016] According to the present invention, the substantially constant moisture content means that the variation of the moisture content during the preparation process is small, and basically maintained within an imperceptible range. Moisture content refers to the ratio of the water weight in the air to the air weight, expressed in ppm. The unit "ppm" refers to the mass fraction of one millionth, that is, the weight of moisture contained in one million parts by weight of air, ppm=weight of moisture...

Embodiment approach

[0020] According to a preferred embodiment of the present invention, the sample preparation conditions include a moisture content below 10ppm (more preferably below 5ppm, such as 0.1-5ppm), a temperature of 0-30°C (more preferably 15-25°C), Oxygen content below 10ppm (more preferably below 5ppm, such as 0.1-5ppm), wherein, in the preparation process of moisture test sample, the absolute value of moisture content fluctuation≤0.2ppm (more preferably≤0.1ppm (such as 0.01-0.1ppm )), the absolute value of the temperature fluctuation is ≤2°C (more preferably ≤1°C (such as 0.1-1°C)).

[0021] According to the present invention, the sample preparation conditions can be provided by various conventional equipment capable of maintaining constant humidity (preferably constant temperature and / or constant oxygen) in the field. Preferably, the sample preparation conditions are provided by a vacuum glove box.

[0022] According to the present invention, when adding the sample, there is no sp...

Embodiment 1

[0037] Nitrogen is passed into the vacuum glove box, and the environmental conditions in the vacuum glove box are maintained at 0.4ppm ± 0.1ppm), the temperature is 20°C ± 1°C, and the oxygen content is 3ppm. Seal the sample preparation bottle in a vacuum glove box to obtain a blank sample. In addition, add 0.0782 g of sample to the sample preparation bottle and seal it to obtain a test sample. With the help of 860 cassette furnace and KF831 moisture meter, the absolute water content in the blank sample was measured by Karl Fischer titration to be 2.5 μg; the absolute water content in the test sample was 45.6 μg; the calculated water content in the sample was 551.2 ppm.

[0038]In the following three weeks, the method described in Example 1 was repeated once a week, and the quality of adding samples to the sample preparation bottle was respectively 0.0523g, 0.0674g and 0.0791g; The water contents were 2.4μg, 2.5μg and 2.5μg respectively; the absolute water contents in the test...

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Abstract

The invention relates to the field of moisture analysis and discloses a preparation method of a moisture test sample and a test method. The preparation method of the moisture test sample comprises steps as follows: a sample is added to a sample preparation bottle under a sample preparation condition, and the sample preparation bottle is sealed and serves as a test sample; alternatively, the sample preparation bottle is directly sealed under a sample preparation condition and serves as a blank sample, wherein the sample preparation condition comprises basically constant moisture content. The test method of the moisture test sample comprises steps as follows: the moisture detection sample is prepared with the preparation method, and the obtained moisture detection sample is subjected to moisture detection with a Karl-fischer potentiometric titration method. The preparation method of the moisture test sample and the test method have the advantages that the cost is reduced, the test data errors are reduced, the work efficiency is improved, and the service life of a moisture meter is prolonged.

Description

technical field [0001] The invention relates to the field of moisture analysis, in particular to a method for preparing and detecting a moisture test sample. Background technique [0002] With the development of scientific research and the progress of production technology, the quantitative analysis of moisture has been listed as one of the basic items in the physical and chemical analysis of various substances, as an important quality index of various substances. According to the different moisture contents in different forms of samples, different requirements for the determination of moisture are put forward. Moisture determination can be the control analysis of industrial production, or the quality signing of industrial and agricultural products; the moisture can be measured from tons of products, or the moisture analysis can be carried out in the laboratory with only a few microliters of test solution; Constant moisture analysis with a water content of a few percent to ...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N27/44
CPCG01N1/28G01N27/44
Inventor 陈明先雪峰郭刚强
Owner GUIZHOU ANDA TECH ENERGY CO LTD
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