Preparation method for ferromolybdenum sample melting glass body

A fusion glass and sample preparation technology, applied in the field of chemical analysis, can solve the problems of not being able to meet the actual requirements, not having the value of popularization, strict operation, etc., and achieve the effects of saving costs, prolonging the life and service cycle, and being easy to control

Active Publication Date: 2012-04-04
ANGANG STEEL CO LTD
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Problems solved by technology

In the literature, there are no specific instructions on the length of time, speed of rotation speed and temperature setting in the melting process. The operation of the experimental process is very strict and d

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 0.3000 g of a ferromolybdenum sample with a particle size of 120 mesh. Put the weighed sample in a 50ml platinum crucible, add 10ml of deionized water, slowly add 8ml of concentrated nitric acid (analytical grade with a molar concentration of 16moL / L) dropwise, heat at 40°C at low temperature, and shake to dissolve the sample completely. The crucible is first placed in a high temperature zone at 200°C to concentrate the volume. When a little salt precipitates out of the solution, the temperature needs to be lowered by 150°C until the sample is completely dried, then removed and cooled to room temperature.

[0021] Add 4.5000 g of lithium tetraborate (analytical pure) flux into the oven-dried platinum crucible, and add 0.15 g of ammonium iodide (analytical pure) release agent. Tilt the platinum crucible by 30°, rotate the crucible to mix the flux in the crucible, and cover the inner wall of the platinum crucible where the sample is hung. Put the platinum crucible ...

Embodiment 2

[0025] Weigh 0.3500 g of a ferromolybdenum sample with a particle size of 200 mesh. Put the weighed sample in a 50ml platinum crucible, add 15ml of deionized water, dropwise add 10ml of concentrated nitric acid (superior pure with a molar concentration of 16moL / L), heat at 100°C at low temperature, and shake to dissolve the sample completely. The crucible is first placed in the high temperature zone at 400°C to concentrate the volume. When the solution has a slight salt precipitation, the temperature needs to be lowered by 100°C until the sample is completely dried, then removed and cooled to room temperature;

[0026] Add 5.0000 g of lithium tetraborate (analytical pure) flux into the oven-dried platinum crucible, and add 0.20 g of ammonium iodide (analytical pure) release agent. Tilt the platinum crucible by 30°, rotate the crucible to mix the flux in the crucible, and cover the inner wall of the platinum crucible where the sample is hung. Put the platinum crucible with mix...

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Abstract

The present invention discloses a preparation method for a ferromolybdenum sample melting glass body. The preparation method comprises the following process steps: preparation of a sample, acid digestion of the sample, preparation of a melting glass body sample, and preparation of a glass body in a shaped crucible by the melting glass body sample. According to the method of the present invention, nitric acid is adopted to digest the ferromolybdenum sample; a treatment of low temperature drying is performed; regents of lithium tetraborate and ammonium iodide are added, the melting glass body is prepared at the high temperature of 1100 DEG C by high temperature melting. According to the present invention, a new melting sample preparing approach is provided for the ferromolybdenum synthesis by the X-ray spectrometry; the difficulties in the ferromolybdenum melting glass body preparation in the prior art are solved; the method of the present invention has characteristics of convenient operation, rapidness, easy control; with the method, the platinum crucible is not damaged, the service life and the use period of the platinum crucible are prolonged, the cost for repeatedly repairing the crucible is saved; the formed ferromolybdenum melting glass body is bright and transparent, meets the requirements of the detection by the XRF method, and has a strong application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a method for preparing a ferromolybdenum sample molten glass body in a shaped crucible used in X-ray fluorescence spectrometry analysis. Background technique [0002] At present, ferromolybdenum is mainly analyzed by wet chemistry, and the element detection cycle is long and the operation is cumbersome. However, X-ray fluorescence spectrometry can shorten the detection cycle and simplify the operation. However, the determination of ferromolybdenum by X-ray fluorescence spectrometry is only limited to the sample preparation by the tablet method. The precision of the tablet method is affected by the effects of particle size and minerals, and the precision of the sample preparation by the fusion method is better than that of the tablet method. However, when ferromolybdenum is placed in a platinum crucible and directly added with a flux for high-temperature melting, it is v...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N23/223
Inventor 邓军华曲月华王一凌
Owner ANGANG STEEL CO LTD
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