Method for preparing molybdenum iron glass fuse pieces

A technology of glass frit and ferromolybdenum, applied in the field of quantitative analysis of X-ray fluorescence spectroscopy, can solve the problems of large release dose, influence on test results, and failure to meet the production cycle, and achieve the effect of meeting the use requirements

Inactive Publication Date: 2017-05-10
SHANXI TAIGANG STAINLESS STEEL CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] Disadvantages: After nitric acid digestion, the drying needs to be carried out at a temperature of about 100°C. The process is very slow and takes a long time; sample loss
[0006] Disadvantages: First, the platinum-gold crucible needs to be wall-mounted, and the wall-mounting operation is strict. A slight mistake will cause serious corrosion of the precious platinum-gold crucible; The amount of mold release added is large, which affects the test results
[0008] Disadvantages: cumbersome operation; incomplete decomposition of graphite powder used to protect the crucible will affect the analysis results
The existing sample processing and analysis technology cannot meet the requirements of the actual production cycle

Method used

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Examples

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Embodiment Construction

[0020] A method for preparing ferromolybdenum glass fusing sheet, carried out according to the following steps

[0021] Step 1. Take 0.2g ferromolybdenum sample, crush the ferromolybdenum sample, and grind it through a 200-mesh sieve to make the diameter less than 0.074mm;

[0022] Step 2. Configure the oxidizing agent namely Li 2 CO 3 and NaNO 3 mixture, Li 2 CO 3 The mass of 1g, NaNO 3 The mass of is 0.6 grams;

[0023] Step 3. Spread 5-6 grams of mixed flux on the bottom and inner side of the platinum crucible, put the platinum crucible into the muffle furnace, raise the temperature of the platinum crucible to 300°C at a speed of less than 15°C / min, and then put the ferromolybdenum and oxidant After mixing evenly, put it into a platinum crucible to avoid direct contact between ferromolybdenum and oxidant and the platinum crucible. The mixed flux is mixed with lithium metaborate and lithium tetraborate according to the mass ratio of lithium metaborate: lithium tetrabor...

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Abstract

The invention relates to the technical field of quantitative analysis of X-ray fluorescence spectrums, and discloses a method for preparing molybdenum iron sample glass fuse pieces. The method includes the process steps: grinding samples; performing pre-oxidation for the samples; preparing glass molten mass. The method particularly includes the steps: paving the bottom with mixed flux of lithium tetraborate and lithium metaborate; directly mixing lithium carbonate, sodium nitrate and molybdenum iron samples; gradually rising the temperature and oxidizing at the temperature lower than 700 DEG C; adding ammonium bromide reagents; preparing the glass fuse pieces at the temperature of 1100 DEG C. According to the method, the excellent molybdenum iron glass fuse pieces are simply, conveniently and rapidly prepared, use requirements of an X-ray fluorescence analysis method are met, and large-batch actual production inspection is rapidly finished in a high-quality manner.

Description

technical field [0001] The invention relates to the technical field of X-ray fluorescence spectrum quantitative analysis. Background technique [0002] At present, ferromolybdenum is mainly determined by chemical analysis methods, especially the main element Mo, which has a long detection cycle and cumbersome steps, while X-ray fluorescence spectrometry can shorten the detection cycle and is easy to operate. However, the determination of ferromolybdenum by X-ray fluorescence spectrometry is limited to the preparation of samples by the tablet method. Due to the influence of the sample matrix effect and particle size effect, the accuracy of the analysis results is poor; The accuracy is comparable to that of chemical analysis methods, but ferromolybdenum is placed in the crucible and directly added with flux for high-temperature melting. During the melting process, it is very easy to form an alloy with a low melting point with the platinum crucible, which will severely corrode ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/22G01N23/223
CPCG01N23/2202G01N23/223G01N2223/076G01N2223/1016
Inventor 刘伟王珺王小花任维萍
Owner SHANXI TAIGANG STAINLESS STEEL CO LTD
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