Method for simultaneously determining trace gold, silver and palladium in geochemical sample

A geochemistry and sample technology, applied in the field of analytical chemistry, can solve the problems of uncertainty in the accuracy of measurement results, limited processing quantity, low analysis efficiency, etc., and achieve the effect of reducing analysis cost, low detection limit, and fast analysis speed.

Inactive Publication Date: 2015-12-02
刘向磊 +2
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, this method does not separate or correct the main mass spectrum interference elements of silver and palladium, such as Zr, Nb, Y, etc., and the accuracy of the measurement results is uncertain; Loaded foam enrichment, low analysis efficiency and high cost
At present, using a loaded foam to selectively enrich gold, silver, and palladium while separating other major mass spectrometric interference elements, ICP-MS directly determines trace amounts of gold, silver, and palladium in geochemical samples. Literature report

Method used

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  • Method for simultaneously determining trace gold, silver and palladium in geochemical sample

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Rock standard reference samples GBW07104 (quartz amphibole andesite) and GBW07290 (peridotite) were purchased from the Geochemical Standard Materials Research Center. The contents of the measured and interfering elements are shown in Table 1.

[0039] Weigh 10.00g rock standard samples GBW07104 and 3 parts each of GBW07290 in parallel, put them in a porcelain ark, put the porcelain ark in a horse boiling furnace, raise the low temperature to 600-650°C and heat it for 1 hour, take it out, and transfer it to 400mL after natural cooling Add 20mL of 1:1 aqua regia to the polypropylene sample digestion bottle, cover and tighten, put it in a 100°C constant temperature water bath, seal and digest for 1 hour, take it out; add 50mL of distilled water to the above-mentioned 400mL polypropylene sample digestion bottle after digestion Let it cool naturally, then add a piece of loaded diphenylthiourea polyurethane foam, press it with a glass rod to make it soak evenly, cover it again...

Embodiment 2

[0043] Soil standard reference samples GBW07406 (yellow red soil) and GBW07288 (soil) were purchased from the Geochemical Reference Material Research Center. The contents of the measured and interfering elements are shown in Table 1.

[0044] Weigh 10.00g soil standard samples GBW07406 (yellow red soil) and GBW07288 (soil) respectively in 3 parts in parallel, put them in a porcelain ark, put the porcelain ark into a horse boiling furnace, heat it from a low temperature to 600-650°C and keep it warm for 1 hour, take out , after natural cooling, transfer it to a 400ml polypropylene sample digestion bottle, add 20mL of 1:1 aqua regia, cover and tighten, put it in a 100°C constant temperature water bath, seal and digest for 1 hour, take out the 400ml polypropylene sample digestion bottle; add 50mL Distilled water, let it cool down naturally, then add a piece of loaded diphenylthiourea polyurethane foam, press it with a glass rod to make it soak evenly, cover it again, shake it in t...

Embodiment 3

[0048] The standard reference samples of water system sediments GBW07329 (sediments in Tibet area) and GBW07289 (water system sediments) were purchased from the Geochemical Standard Material Research Center. The contents of the measured and interfering elements are shown in Table 1.

[0049] Weigh in parallel 10.00g of water system sediment standard samples GBW07329 (Tibet area sediment) and GBW07289 (water system sediment) 3 parts each, in the porcelain ark, put the porcelain ark into a horse boiling furnace, and heat it from a low temperature to 600-650°C Burn and keep warm for 1 hour, take it out, transfer it to a 400mL polypropylene sample digestion bottle after natural cooling, add 20mL of 1:1 aqua regia, cover and tighten it, put it in a 100℃ constant temperature water bath, seal and digest for 1 hour, take out 400mL poly Propylene sample digestion bottle; add 50mL distilled water, let it cool naturally, put a piece of loaded diphenylthiourea polyurethane foam into it, pr...

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Abstract

The invention provides a method for simultaneously determining trace gold, silver and palladium in a geochemical sample. The method comprises the following steps: firstly, digesting the geochemical sample by using 1:1 chloroazotic acid in a constant-temperature boiled water bath in a sealed manner; secondly, selectively enriching the trace gold, silver and palladium by using diphenylthiourea loaded polyurethane foam, and separating other interference elements; and finally, drawing a standard curve of Au197, Ag107 and Pd105 by adopting an inductively coupled plasma source mass spectrometer through a standard curve method, and simultaneously determining the trace gold, silver and palladium in the sample. According to the method provided by the invention, the problem that other main interference elements with the abundance of geochemical elements, which is hundreds, even thousands of times of that of the silver and the palladium, have interference on mass spectrums of the silver and the palladium is solved; and compared with a traditional emission spectrum and graphite furnace atomic absorption spectrometry, the sampling amount in analysis of the silver in the geochemical sample is increased by dozens of times, so that the influences caused by gold grain effect of the geochemical silver are effectively overcome.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a method for simultaneously determining trace amounts of gold, silver and palladium in geochemical samples. Background technique [0002] It is known that the abundance of gold, silver and palladium geochemical elements is about 0.74ppb, 0.055ppm and 0.43ppb in the upper continental crust, and about 1.4ppb, 0.080ppm and 0.65ppb in the soil. Gold, silver and palladium are all Trace elements are difficult to determine accurately. At present, the gold in geochemical samples mainly adopts emission spectrometry (AES), polyurethane foam enrichment-graphite furnace atomic absorption method (GF-AAS) and polyurethane foam enrichment-inductively coupled plasma mass spectrometry (ICP-MS). Determination. The detection methods of silver and palladium are mainly based on emission spectroscopy and graphite furnace atomic absorption method. Both methods are used to measure silver,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N27/626
Inventor 刘向磊文田耀孙文军詹晓军张维王腾飞李永新
Owner 刘向磊
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