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Rapid analysis and detection method for trace bismuth in high-purity niobium or niobium oxide

A rapid analysis and detection method technology, applied in thermal excitation analysis, material excitation analysis, preparation of test samples, etc., can solve problems such as long analysis period, complicated operation process, and large environmental pollution, and achieve shortened analysis period, heavy weight, etc. Good performance and stable results

Inactive Publication Date: 2012-06-20
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complex operation process such as extraction and co-precipitation, the analysis period is long, and the pollution to the environment is large, it is difficult to meet the requirements of rapid analysis in the production process
Such as GB / T4324.2-1984 Tungsten Chemical Analysis Method Potassium Iodide-Strychnine Spectrophotometric Determination of Bismuth Quantity, needs to use chloroform to extract bismuth complexes, causing pollution to the environment, the detection limit of the actual sample can only reach 0.00008 %

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Determination of bismuth in high-purity niobium oxide (sample S-1)

[0018] The preparation of standard solution (each embodiment is all the same)

[0019] According to GB / T602-2002 "Preparation of Standard Solutions for Determination of Impurities in Chemical Reagents", a 0.1 mg / mL bismuth standard solution was prepared.

[0020] Preparation of standard solution series: Pipette 0, 0.1mL, 0.3mL, 0.5mL, 0.7mL of bismuth standard solutions with a mass concentration of 0.1mg / mL into 100mL volumetric flasks, add 2mL of nitric acid, dilute with water to 100mL, mix well , that is, 0.1 μg, 0.3 μg, 0.5 μg, 0.7 μg of bismuth per mL.

[0021] The processing of cation exchange resin (each embodiment is all the same)

[0022] Dry the cation exchange resin (such as 732 strong acid cation resin) in the air, grind it finely, wash it several times with water, soak it in 4mol / L nitric acid for 24 hours, wash it with ultrapure water until neutral, then soak and wash it repea...

Embodiment 2

[0030] Example 2: Determination of bismuth in high-purity niobium oxide (sample S-2)

[0031] Preparation of cation exchange column

[0032] Measure 2.5mL of the treated cation exchange resin and pour it into a polyethylene tube with a length of 150mm and an inner diameter of 5mm in a slurry form. Both ends are sealed with acid-washed medical cotton, and a filter plug is inserted. Peristaltic pump tubing.

[0033] Weigh 1g of high-purity niobium oxide sample into a closed digestion tank, add 3mL of hydrofluoric acid, and microwave until the solution is clear, dilute to 50mL, control the acidity of hydrofluoric acid to 6%, and shake well. Connect the cation exchange column and the peristaltic pump, adjust the peristaltic pump to drive the sample solution to flow through the cation exchange column at a speed of 12.6 rpm, and discard the effluent. Then rinse the cation exchange column with 15 mL of 1% hydrofluoric acid and 15 mL of ultrapure water, and discard the effluent. Th...

Embodiment 3

[0035] Example 3: Determination of bismuth in high-purity niobium (sample S-3)

[0036] Preparation of cation exchange column

[0037] Measure 2.5mL of the treated cation exchange resin and pour it into a 150mm-long, 5mm-diameter polypropylene tube in the form of slurry. Both ends are sealed with acid-washed medical cotton, and a filter plug is inserted. Peristaltic pump tubing.

[0038] Weigh 0.5g of high-purity niobium sample into a plastic cup, add 3mL of hydrofluoric acid and 1mL of nitric acid to dissolve, dilute to 50mL, control the acidity of hydrofluoric acid to 6%, and shake well. Connect the peristaltic pump and the cation exchange column, adjust the peristaltic pump to drive the sample solution to flow through the cation exchange column at a speed of 9.6 rpm, and discard the effluent. Then rinse the cation exchange column with 15 mL of 1% hydrofluoric acid and 10 mL of ultrapure water, and discard the effluent. Then use 28 mL of nitric acid with a concentration o...

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Abstract

The invention discloses a rapid analysis and detection method for trace bismuth in high-purity niobium or niobium oxide, which sequentially comprises the steps of: dissolving high-purity niobium oxide test samples by using hydrofluoric acid and dissolving metallic niobium by using hydrofluoric acid and nitric acid; adjusting a peristaltic pump to drive test sample solution to conduct ion exchange through a cation exchange column, wherein bismuth ions in the test sample solution are adsorbed on the column and are separated from matrix niobium and impurity elements; using hydrofluoric acid and ultra-pure water to sequentially wash the cation exchange column, using nitric acid or hydrochloric acid to elute bismuth element adsorbed on the exchange column, collecting eluent, fixing volume and shaking evenly; and using an inductive coupling plasma emission spectrometer to determine the emission intensity of the bismuth element in the eluent, and then calculating and analyzing the result according to a formula as shown the in accompanying drawing. The rapid analysis and detection method for the trace bismuth in the high-purity niobium or niobium oxide has the advantages that the method is simple, convenient and rapid, the accuracy is high, the analysis cycle is shortened and is approximately only 20 minutes, the actual sample detection lower limit reaches 0.00002 percent, the result is stable and the repeatability is good.

Description

technical field [0001] The invention relates to the rapid analysis and detection of bismuth element, especially the rapid analysis and detection method of trace bismuth in high-purity niobium or niobium oxide. Background technique [0002] Among the existing bismuth elemental analysis and detection methods, the determination of bismuth content in the GB / T15076.11-1994 chemical analysis method for tantalum and niobium uses DC arc atomic emission spectrometry, and the measurement range is 0.0001% to 0.030%. The accuracy of this method completely depends on the accuracy of the calibration curve of the standard sample, the standard sample must be traced to the certified reference material, wherein the determination of the amount of bismuth is still the use of chemical analysis methods. For the detection of micro or trace amounts of bismuth, in order to improve the sensitivity, it is generally necessary to use more cumbersome chemical separation methods, such as extraction, co-pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/34
Inventor 张颖
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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