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High carbon ferro-chrome sample dissolving method

A technology of high-carbon ferrochromium and samples to be tested, which is applied in the field of material analysis, can solve problems such as difficulty in grasping the time of smoking and affecting the accuracy of analysis results, etc., and achieves accelerated chemical reaction speed, rapid sample dissolution effect, and sample preparation technology easy effect

Active Publication Date: 2009-07-29
SHANGHAI ELECTRIC POWER GENERATION EQUIPMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to control the smoking time of this method. If the smoking time is too long, insoluble pyrosulfate will be generated, which will affect the accuracy of the analysis results.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 1 part of 0.0500g high-carbon ferrochromium sample to be tested, put it in a microwave digestion tank, add 10mL of a mixed solution of concentrated hydrochloric acid, concentrated nitric acid and hydrofluoric acid, wherein the concentration of concentrated hydrochloric acid, concentrated nitric acid and hydrofluoric acid The volume ratio is 1.1:1.0:0.9, then seal it, put it into the microwave digestion device, close the door, set the power to 400 watts, use the Ramp to Temperature control mode (this mode comes with the instrument), and use the two-step digestion method, The specific microwave digestion process is shown in Table 1.

[0016] The microwave digestion process of table 1 embodiment 1

[0017] steps

[0018] The sample is completely digested.

Embodiment 2

[0020] Weigh 4 parts of 0.1000g high-carbon ferrochromium samples to be tested, place them in 4 microwave digestion tanks respectively, add 15mL of a mixed solution of concentrated hydrochloric acid, concentrated nitric acid and hydrofluoric acid to each tank, in which concentrated hydrochloric acid, concentrated nitric acid and hydrogen The volume ratio of hydrofluoric acid is 1.2:1.1:1.0, then seal it, put it into the microwave digestion device, close the door, set the power to 800 watts, adopt the Ramp to Temperature control mode, and adopt the two-step digestion method. For the specific microwave digestion process, see Table 2

[0021] The microwave digestion process of table 2 embodiment 2

[0022] steps

[0023] The sample is completely digested.

Embodiment 3

[0025] Weigh 6 parts of 0.1500g high-carbon ferrochrome samples to be tested, place them in 6 microwave digestion tanks, add 20mL of a mixed solution of concentrated hydrochloric acid, concentrated nitric acid and hydrofluoric acid to each tank, wherein concentrated hydrochloric acid, concentrated nitric acid and hydrogen The volume ratio of hydrofluoric acid is 1.3:1.2:1.1, then seal it, put it into the microwave digestion device, close the door, set the power to 800 watts, adopt the Ramp to Temperature control mode, and adopt the two-step digestion method. For the specific microwave digestion process, see table 3.

[0026] The microwave digestion process of table 3 embodiment 3

[0027] steps

[0028] The sample is completely digested.

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Abstract

The invention relates to a material analysis method, in particular to an alloy chemical analysis method. A dissolution method of a high carbon ferrochrome sample comprises the following steps: firstly, placing the high carbon ferrochrome sample to be measured into a microwave digestion tank, then adding a mixture of concentrated hydrochloric acid, concentrated nitric acid and hydrofluoric acid, and finally sealing the microwave digestion tank and putting into a microwave digestor for dissolution, wherein, process parameters obtained during the dissolution in the microwave digestor are as follows: the power is 400-1600w, the temperature is increased from normal temperature to 195 DEG C and the digestion time is 65-110min. 10-25mL of the mixture of the concentrated hydrochloric acid, the concentrated nitric acid and the hydrofluoric acid are needed when 0.0500-0.2000g of the high carbon ferrochrome sample is added. As microwave digestion method is adopted in the alloy chemical analysis method, the microwave activation characteristic causes the sample to be dissolved more completely and the sample can be dissolved without high-temperature fuming or fusion.

Description

technical field [0001] The invention relates to a material analysis method, especially an alloy chemical analysis method. Background technique [0002] High-carbon ferrochromium is not easy to dissolve because of the particularly stable chemical properties of chromium carbide (Cr3C). Therefore, under normal pressure, the following two methods are mainly used to dissolve the sample at present. [0003] The first one is the alkali fusion method: weigh 0.5000g of the sample and place it in a porcelain crucible filled with 4-5g of sodium peroxide in advance, stir it evenly, then cover it with 1-2g of sodium peroxide, and heat it slowly to make the sample After the sample is melted, keep it at about 700°C for about 5 minutes, and shake it continuously to make it melt. After natural cooling, place the crucible in a 500mL beaker, add about 100mL of hot water to leaching the melt, take out the crucible, and wash it with water. However, due to the difficulty in controlling the mel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
Inventor 李虹李晓晴史文斌郭慧丽
Owner SHANGHAI ELECTRIC POWER GENERATION EQUIPMENT CO LTD
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