Method for measuring trace amount of gold by heating solute ores through steam and adopting ICP-MS

A technology of dissolving ore and steam, applied in the direction of measuring devices, material analysis by electromagnetic means, instruments, etc., can solve the problems of result distortion, lower sensitivity, small detection limit, etc., and achieve reduced labor intensity, high test accuracy, and linearity wide range of effects

Inactive Publication Date: 2015-10-14
四川省地质矿产勘查开发局成都综合岩矿测试中心
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  • Abstract
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AI Technical Summary

Problems solved by technology

In production practice, the continuous measurement of 1% concentration of thiourea solution will reduce the atomization efficiency. As the measurement time increases, thiourea will continue to accumulate in the spray chamber, rectangular tube, and cone mouth, reducing sensitivity and finally distorting the results.
[0011] In summary, the method provided by "Rock and Mineral Analysis" cannot completely dissolve the gold in the sample, and the continuous measurement of thiourea solution will reduce the atomization efficiency. Accumulation reduces the sensitivity and finally distorts the results. The amount of foam used is large, which brings difficulties to the next step of thiourea release and removal of the foam. The detection limit is small, and the analysis speed, linear range and reproducibility of the results are poor.

Method used

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  • Method for measuring trace amount of gold by heating solute ores through steam and adopting ICP-MS

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Weigh 10g of the sample in a crucible, place it in a high-temperature furnace, and burn it from low temperature to 650°C for 2 hours, take it out and cool it, pour it into a 300mL polyethylene bottle, add 30mL (1+1) of newly prepared aqua regia, 1mL of Fe 3+ Mix the solution evenly, cover it and put it in a steam bath at 100°C, cover the steamer and keep it for 1 hour, take it out to cool, add 70mL of water, put a piece of foam plastic, put the polyethylene bottle on the shaker for 30min, take out the plastic foam, and water Wash it, squeeze it dry, put it into a colorimetric tube with a predetermined volume of 10mL thiourea solution, drain the air bubbles, keep it in a boiling water bath for 30 minutes, take out the foam plastic while it is hot, and obtain a gold thiourea solution, place it for clarification, and use ICP- For MS measurement, the reagents used are: gold standard solution: ρ(Au)=10ng / mL, thiourea solution (H 2NCSNH 2 )=5g / L, In internal standard solutio...

experiment example 1

[0030] (1) Selection of enrichment conditions for trace gold separation.

[0031] (2) Selection of working parameters for ICP-MS determination of gold.

[0032] (3) The detection limit and linear range of ICP-MS determination of gold.

[0033] (4) Sample verification.

[0034] Instruments and main reagents:

[0035] Graphite furnace atomic absorption spectrometer M6 (not used in "Rock and Mineral Analysis", deleted) (thermoelectric).

[0036] X Series II plasma mass spectrometer (thermoelectric).

[0037] Gold standard solution: ρ(Au)=10ng / L.

[0038] Thiourea solution: ρ(H 2 NCSNH 2 )=10g / L, 5g / L.

[0039] Sample pretreatment:

[0040] Weigh 10.0 g of the sample into a crucible, put it into a muffle furnace and raise it to 650° C., and keep it for 2 hours. After taking it out and cooling, pour it into a 300mL polyethylene bottle, add 30mL of freshly prepared aqua regia (1+1) and mix well, cover it and place it in a steam bath at 100°C, cover the steamer and keep the ...

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Abstract

The invention relates to a method for measuring trace amount of gold by heating solute ores through steam and adopting ICP-MS, and the method can be used for solving the problems that the existing method is low in efficiency, inconvenient to operate, low in accuracy, precision and analysis speed, narrow in linearity range, poor in result reproducibility and low in detection limit. The method provided by the invention is high in efficiency, convenient to operate, high in accuracy, good in precision, high in analysis speed, wide in linearity range, good in result reproducibility and high in detection limit. The method comprises the following steps: weighing 10g of a sample, placing the sample into a crucible, placing the crucible into a high temperature furnace, firing for 2h from low temperature to 650 DEG C, taking out, cooling, pouring the cooled sample into a 300mL polyethylene bottle, adding with freshly prepared 30mL (1+1) aqua regia and 1mL of Fe<3+> solution, mixing uniformly, capping, placing the polyethylene bottle into steam bath at 100 DEG C, covering with a steamer cover, keeping the temperature for 1h, taking out, cooling, adding with 70mL of water, placing a piece of foamed plastic into the polyethylene bottle, placing the polyethylene bottle into an oscillator for 30 min, taking out the foamed plastic, cleaning by water, squeezing the excessive water out, placing the foamed plastic into a colorimetric tube with 10mL of thiourea solution with volume metered in advance, removing air bubbles, placing into the colorimetric tube into boiling water bath for 30 min, taking out the foamed plastic while the temperature is high, thus obtaining a thiourea solution containing golden, standing for clarifying, and measuring by ICP-MS.

Description

Technical field: [0001] The invention relates to a method for measuring trace gold by ICP-MS. Background technique: [0002] The analysis of gold in geochemical samples is generally divided into two categories: fire assay gold enrichment-emission spectrometry and wet decomposition-atomic absorption method. Fire assay gold enrichment-emission spectrometry has been gradually eliminated by major laboratories due to factors such as high labor intensity, serious environmental pollution, and poor reproducibility of results. Wet decomposition-atomic absorption method has become the main analysis method. The plasma mass spectrometry disclosed in "Rock and Mineral Analysis" (Fourth Edition) uses aqua regia to dissolve the sample, foam plastic to adsorb gold, and thiourea to dissolve the sample for release. ICP-MS method is used to determine trace gold, with a detection limit of 0.15 ng / g. The instrument is an inductively coupled plasma mass spectrometer (U.S. Thermo Elemental x7 ty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62
Inventor 曾念华彭萌陈梅王君赵向阳
Owner 四川省地质矿产勘查开发局成都综合岩矿测试中心
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