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High purity gold micro impurity element micro-extraction determination method

A technology for trace impurities and determination methods, which is applied in solvent extraction, separation methods, chemical instruments and methods, etc., can solve the problems of high sensitivity and achieve the effects of fast analysis speed, high detection sensitivity and reduced reagent consumption

Inactive Publication Date: 2010-12-29
YUXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the domestic ICP-MS method for the determination of impurity elements in pure gold has not been reported. The sensitivity of the ICP-MS method is high, which is 2 to 3 orders of magnitude higher than that of the plasma emission spectrometry (ICP-AES). The atomic absorption method (AAS) is also 1 to 2 orders of magnitude higher, with a wide measurement range and good selectivity, and can realize the characteristics of simultaneous analysis of multiple elements, which is very suitable for the determination of trace impurity elements in high-purity metals

Method used

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  • High purity gold micro impurity element micro-extraction determination method
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  • High purity gold micro impurity element micro-extraction determination method

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Accurately weigh a pure gold sample with a mass of about 0.1000g into a 10mL polytetrafluoroethylene microwave digestion bottle, add a volume of 1.0mL aqua regia, and digest it in a microwave digestion furnace at a power of 1000W for 10 minutes; after digestion, heat the digestion solution Evaporate to nearly dryness, dissolve with hydrochloric acid with a volume of about 2.0mL and a concentration of 3.0mol / L, transfer to a micro-extraction tube, add methyl isobutyl ketone (MIBK) with a volume of 5.0mL, and fully shake the extraction time for 2.0min , after standing for stratification, suck out (or pour out) the MIBK phase with a straw, transfer the water phase into the sample tube, heat and evaporate to dryness, dissolve it with 2.0 mL of nitric acid with a concentration of 5 (m / v), and press the selected instrument Conditional analysis, and corresponding blank experiments were done at the same time. Determination of impurity results is as follows in Table 2,

[0035] T...

Embodiment 2

[0038] Accurately weigh a pure gold sample with a mass of about 0.0500g into a 10mL polytetrafluoroethylene microwave digestion bottle, add a volume of 0.5mL aqua regia, and digest it in a microwave digestion furnace at a power of 1000W for 5 minutes; after digestion, heat the digestion solution Evaporate to near dryness, dissolve with hydrochloric acid with a volume of about 1.0mL and a concentration of 3.0mol / L, transfer to a micro-extraction tube, add methyl isobutyl ketone (MIBK) with a volume of 2.0mL, and fully shake the extraction time for 1.0min , after standing for stratification, suck out (or pour out) the MIBK phase with a straw, transfer the water phase into the sample tube, heat and evaporate to dryness, dissolve it with 1.0 mL of nitric acid with a concentration of 5 (m / v), and press the selected instrument Conditional analysis, and corresponding blank experiments were done at the same time. Determination of impurity results is as follows in Table 3,

[0039] Ta...

Embodiment 3

[0042] Accurately weigh a pure gold sample with a mass of about 0.1500g into a 10mL polytetrafluoroethylene microwave digestion bottle, add a volume of 0.5mL aqua regia, and digest it in a microwave digestion furnace at a power of 1000W for 15 minutes; after digestion, heat the digestion solution Evaporate to nearly dryness, dissolve with hydrochloric acid with a volume of about 2.5mL and a concentration of 3.0mol / L, transfer to a micro-extraction tube, add methyl isobutyl ketone (MIBK) with a volume of 8.0mL, and fully shake the extraction time for 3.0min , after standing for stratification, suck out (or pour out) the MIBK phase with a straw, transfer the water phase into the sample tube, heat and evaporate to dryness, dissolve it with a volume of 3.0 mL of nitric acid with a concentration of 5 (m / v), and press the selected instrument Conditional analysis, and corresponding blank experiments were done at the same time. Determination of impurity results is as follows in Table ...

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Abstract

The invention discloses a miniature extraction plant and a micro extraction determining method for trace impurity elements in high purity gold. The miniature extraction plant comprises a sleeve (1) and a dividing piston (2) which are hermetically matched, wherein, a capillary tube (3) is arranged on the center position of the dividing piston. The micro extraction determining method comprises the steps of microwave digestion, micro extraction separation of gold matrix, optimization of running parameters of an instrument, selection of an isotope and an internal standard, deduction of interference of common ions, semiquantitative scan, preparation of standard solution, determination with a plasma mass spectrometer and calculation of a result. The method adopts the micro extraction plant to extract the gold matrix with the single-time extraction yield reaching 98 percent and the coefficient of recovery of the impurities reaching 95 percent, so that the existence of gold is not the interference to the determination of the impurity elements with ICP-MS. The method has the advantages of high detection sensitivity, low detection limit, small sample amount and quick analyzing speed, thereby being a trace analysis method.

Description

technical field [0001] The invention belongs to the technical field of metallurgical analysis, and in particular relates to a method for determining six impurities of silver, copper, iron, lead, antimony and bismuth in high-purity gold by using microwave digestion samples, micro-extraction separation and inductively coupled plasma mass spectrometry (ICP-MS). Elemental analysis methods. technical background [0002] With the rapid development of the microelectronics industry, pure gold materials have been widely used, and the purity detection of gold has attracted more and more attention. The national standard (GB 11066.5-1989) stipulates that silver, copper, and iron in pure gold should be tested. , lead, antimony and bismuth 6 impurity elements are detected. The testing methods of pure gold materials are mostly determined by emission spectroscopy and direct reading spectroscopy, but the analysis elements and analysis accuracy are limited by the instrument itself, and the c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/00G01N27/64G01N1/40G01N1/34
Inventor 李银科胡秋芬黄章杰杨项军韦群艳杨光宇黄云
Owner YUXI NORMAL UNIV