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Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide

A detection method, a chromium carbide technology, applied in thermal excitation analysis, material excitation analysis, preparation of test samples, etc., can solve the problems of difficult decomposition, unsuitable measurement, unfavorable accuracy, etc., and achieve stable and accurate results. High and precise effect

Active Publication Date: 2010-04-07
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, chromium carbide is an insoluble compound, which is difficult to decompose completely. Although it can be decomposed by potassium pyrosulfate melting method, or dissolved with a large amount of sulfur and phosphorus mixed acid, the blank test solution of the above-mentioned melting (solvent) agent may introduce a large amount of impurity elements. It is not suitable for the determination of inductively coupled plasma atomic emission spectrometer, nor is it conducive to ensuring the accuracy of the analysis and determination of impurity elements in chromium carbide

Method used

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  • Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide
  • Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide
  • Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: Determination of elements such as aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten in chromium carbide (sample S-1)

[0041] Take 0.1000 g of chromium carbide sample and place it in a polytetrafluoroethylene sample dissolving cup, first use 1 to 2 mL of deionized water to rinse the cup wall, then add in turn the purity to be high-purity (MOS grade, the same as in the following examples), mass concentration It is 1.0mL of hydrofluoric acid of 1.14g / mL, and the purity is high-grade pure, and the mass concentration is 1.5mL of sulfuric acid 1.84g / mL, and the purity is high purity (MOS level, the following examples are the same), and the mass concentration is 1.42g / 0.8 mL of nitric acid, mix well, cover the cup, put the sample dissolving cup into the high-pressure tank, and seal the high-pressure tank. Place the high-pressure tank in the microwave digestion apparatus, and perform the first microwave digestion according to the working condition...

Embodiment 2

[0048] Embodiment 2: Determination of elements such as aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten in chromium carbide (sample S-2)

[0049] Take 0.1000 g of chromium carbide sample and place it in a polytetrafluoroethylene sample dissolving cup, first rinse the cup wall with 1-2 mL of deionized water, and then add high-purity hydrofluoric acid with a mass concentration of 1.14 g / mL in sequence 1.5mL, 2.0mL of sulfuric acid with a purity of 1.84g / mL, 0.8mL of high-purity nitric acid with a mass concentration of 1.42g / mL, mix well, cover the cup, and dissolve the sample The cup is put into the high-pressure tank, and the high-pressure tank is sealed. Place the high-pressure tank in the microwave digestion apparatus, and carry out the first microwave digestion according to the working conditions shown in Table 1 above. After the first microwave digestion is completed, remove the high-pressure tank from the microwave digestion device. After the high-pressure ...

Embodiment 3

[0055] Embodiment 3: Determination of elements such as aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten in chromium carbide (sample S-3)

[0056] Take 0.1000 g of chromium carbide sample and place it in a polytetrafluoroethylene sample dissolving cup, first rinse the cup wall with 1-2 mL of deionized water, and then add high-purity hydrofluoric acid with a mass concentration of 1.14 g / mL in sequence 2.0mL, 2.0mL of sulfuric acid with a purity of 1.84g / mL, 0.8mL of high-purity nitric acid with a concentration of 1.42g / mL, mix well, cover the cup, and dissolve the sample The cup is put into the high-pressure tank, and the high-pressure tank is sealed. Place the high-pressure tank in the microwave digestion apparatus, and carry out the first microwave digestion according to the working conditions shown in Table 4. After the first microwave digestion is completed, remove the high-pressure tank from the microwave digestion device, and wait for the high-pressure tank...

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Abstract

The invention discloses an analysis and detection method for impurity elements such as aluminum, calcium, ion, molybdenum, niobium, titanium, tungsten and the like in chromium carbide. The method comprises adding a chromium carbide sample into a dissolving cup, adding hydrofluoric acid, sulphuric acid and nitric acid sequentially, stirring, charging into a sealed high-pressure jar; putting the sealed high-pressure jar into a microwave extinguishing instrument for two times of microwave extinguishment; taking the high-pressure jar out of the microwave extinguishing instrument for cooling, transferring the dissolved chromium carbide liquid sample into a volumeric flask, diluting to a predetermined index, stirring; preparing a chromium substrate matched mixed standard solution series of aluminum, calcium, iron, molybdenum, niobium, titanium and tungsten; measuring element emission power of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten or the like in a blank liquid sample, a chromium carbide liquid sample and the prepared series mixed standard solution by an inductively coupled plasma atomic emission spectrometer in the same time, obtaining the analysis result by checking a standard working curve or by linear equation calculation. The invention adopts two times of microwave extinguishment using the mixed acid, solves the problem of hardness in chromium carbide decomposition, having a measurement range from 0.010% to 1.00%, which is high in accuracy, and good in precision.

Description

technical field [0001] The present invention relates to the analysis and detection of seven elements such as aluminum, calcium, iron, molybdenum, niobium, titanium and tungsten, especially the analysis and detection of seven elements such as aluminum, calcium, iron, molybdenum, niobium, titanium and tungsten in chromium carbide method. Background technique [0002] In the existing chemical analysis methods of chromium carbide, only the main content of chromium is determined, and there is no corresponding chemical analysis method for the impurity elements therein. However, when chromium carbide is added to the alloy as a cemented carbide additive, the content of impurity elements in chromium carbide directly affects the performance of the cemented carbide. In order to ensure the quality of cemented carbide products, seven impurity elements such as aluminum, calcium, iron, molybdenum, niobium, titanium, and tungsten in chromium carbide must be analyzed and detected. , It is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73G01N1/44
Inventor 熊静
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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