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Method for detecting trace impurity elements in tungsten carbide powder

A technology for trace impurities and impurity elements, applied in the field of trace impurity element analysis of high-purity materials, can solve the problems of inability to completely dissolve tungsten carbide, inaccurate determination of elements, inability to digest free carbon, etc. The effect of removing the inhibitory effect

Active Publication Date: 2019-10-22
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] CN105823772A Chinese patent discloses "a detection method for measuring impurity elements in tungsten carbide". , magnesium, vanadium, chromium, copper, and molybdenum. This method uses strong acids such as hydrofluoric acid and nitric acid to digest samples, which cannot digest free carbon in tungsten carbide, and cannot accurately determine elements less than 0.0001%;
[0008] CN103529015A Chinese patent discloses the "analysis and detection method of cobalt, nickel, iron, titanium and chromium in tungsten carbide", which uses sulfuric acid-ammonium sulfate to dissolve tungsten carbide samples, and uses citric acid to complex tungsten. The blank of the reagent is high, and it is not suitable for trace impurities. determination
The analysis device is complex and not suitable for tungsten carbide samples;
[0016] "Determination of 26 trace impurity elements in high-purity tungsten by inductively coupled plasma mass spectrometry" disclosed on pages 309-314, Volume 31, Issue 05, 2014 of "Cemented Carbide" uses H 2 o 2 Dissolve high-purity tungsten samples, but cannot completely dissolve tungsten carbide

Method used

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  • Method for detecting trace impurity elements in tungsten carbide powder
  • Method for detecting trace impurity elements in tungsten carbide powder
  • Method for detecting trace impurity elements in tungsten carbide powder

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Determination of eighteen kinds of impurities such as magnesium, aluminum, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, arsenic, molybdenum, cadmium, tin, antimony, lead, bismuth in 02 type ultrafine tungsten carbide powder samples amount of elements.

[0051] (1) Preparation of reagents and standard solutions

[0052] Ammonia water (ρ0.90g / mL), MOS grade;

[0053] Analysis water is ultrapure water (≥18.3MΩ cm);

[0054] Single-element standard storage solution of 18 impurity elements: 1000μg / mL, prepared with reference substances respectively.

[0055] Mixed standard solution A: containing calcium, molybdenum and lead, the mass volume concentration is 50 μg / mL, and the medium is 2.5% nitric acid (volume fraction).

[0056] Mixed standard solution 1: Contains calcium, molybdenum, lead 1μg / mL, medium is 2.5% nitric acid, and is prepared by diluting mixed standard solution A.

[0057] Mixed standard solution B: containing aluminum, a...

Embodiment 2

[0074] Determination of 18 kinds of impurity elements such as magnesium, aluminum, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, arsenic, molybdenum, cadmium, tin, antimony, lead, bismuth in 06 type tungsten carbide powder samples , and measure the precision.

[0075] (1) Preparation of reagents and standard solutions

[0076] Ammonia water (ρ0.90g / mL), high purity;

[0077] Analysis water double distilled water (≥18.3MΩ cm);

[0078] Below with embodiment 1.

[0079] (2) Digestion of samples

[0080] Weigh 0.5g tungsten carbide sample, place it in a 100mL beaker, and oxidize it in a muffle furnace at 700°C for 12min. After cooling, add 10mL of water and 10mL of ammonia water, and heat to dissolve on a 150°C electric heating plate. Take it out and cool it slightly, then transfer it into a volumetric flask, dilute the solution to 20mL with water, and mix well. Pipette 1000μL of the test solution into a volumetric flask, dilute to 50mL wit...

Embodiment 3

[0090] Determination of 18 kinds of impurity elements such as magnesium, aluminum, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, arsenic, molybdenum, cadmium, tin, antimony, lead, bismuth in 02 type tungsten carbide powder samples , and compared with the results determined by DC arc atomic emission spectrometry (AES).

[0091] (1) Preparation of reagents and standard solutions

[0092] With embodiment 1.

[0093] (2) Digestion of samples

[0094]Weigh 0.1g tungsten carbide sample, place it in a crucible, and oxidize it in a muffle furnace at 800°C for 15min. After cooling, add 10 mL of water and 1 mL of ammonia water, and heat to dissolve on a 100°C electric heating plate. Take it out and cool it slightly, then transfer it into a volumetric flask, dilute the solution to 20mL with water, and mix well. Pipette 10mL of the test solution into a volumetric flask, dilute to 100mL with water, mix well, and test. Make a reagent blank along with t...

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Abstract

The invention discloses a method for detecting trace impurity elements in tungsten carbide powder. The method specifically comprises the steps of: adopting an inductively coupled plasma mass spectrometry method for determining 18 impurity elements such as magnesium, aluminum, calcium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, arsenic, molybdenum, cadmium, tin, antimony, lead and bismuth simultaneously and quickly, wherein the determination lower limits of the impurity elements are all less than 0.0001%. The method effectively solves the problem of interference of large amount of insoluble free carbon during wet decomposition of tungsten carbide through oxidizing a tungsten carbide sample into tungsten trioxide in a high-temperature furnace and then digesting the sample with aqueous ammonia, eliminates the matrix suppression effect by adopting a tungsten matrix matching working curve, and carries out determination by adopting an inductively coupled plasma mass spectrometer. The method is simple in operation, detects many elements, has fast detection speed, is low in determination lower limit, achieves the trace amount level, is high in analysis precision, and is suitable for mass production analysis of high quality or high purity tungsten carbide.

Description

technical field [0001] The invention relates to the technical field of analysis of trace impurity elements in high-purity materials, in particular to a detection method for trace impurity elements in tungsten carbide powder, and in particular to the determination of magnesium, aluminum, calcium and titanium in tungsten carbide powder by using an inductively coupled plasma mass spectrometer , vanadium, chromium, manganese, iron, cobalt, nickel, copper, arsenic, molybdenum, cadmium, tin, antimony, lead, bismuth eighteen impurity elements. Background technique [0002] Tungsten carbide powder is the main raw material for cemented carbide production, and the content of impurity elements is an important indicator for quality control of cemented carbide products. At present, the testing standards for the content of trace impurity elements in tungsten carbide powder are: industry standard YS / T559-2009 and national standard GB / T4324.1~30-2012. [0003] "YS / T 559-2009 Tungsten Emiss...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N1/40G01N1/44G01N27/626
CPCG01N27/626G01N1/44G01N1/4044
Inventor 张颖李林元张蕾
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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