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Application method of ammonium fluoride as digestion reagent of geological sample

A technology of geological samples and application methods, applied in the field of chemical analysis, can solve problems such as complex and cumbersome operation procedures, dangerous hydrofluoric acid, and heavy workload, and achieve the effects of strong application prospects, high work efficiency, and small workload

Active Publication Date: 2015-03-04
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires the purchase of expensive high-pressure airtight equipment, the operation process is complex and cumbersome, the workload is very heavy and relatively time-consuming
Moreover, both the open acid digestion method and the closed high-pressure acid digestion method require the use of dangerous hydrofluoric acid
[0004] In summary, the pretreatment technology for trace element testing of geological samples has not yet appeared, which can completely and effectively digest insoluble accessory minerals, and ensure fast and efficient work efficiency, and is also suitable for modern high-end, precise, and advanced analytical instruments and equipment. Digestion method

Method used

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  • Application method of ammonium fluoride as digestion reagent of geological sample
  • Application method of ammonium fluoride as digestion reagent of geological sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The present invention provides a kind of application method of ammonium fluoride as the digestion reagent of geological sample, and it comprises the steps:

[0035] 1) Physically pulverize the granite (GSR-1) sample to 200 mesh (sieve: 0.074 mm) to obtain a powder test sample;

[0036] 2) Weigh 250 mg of ammonium fluoride and 50±1 mg of granite (GSR-1) sample powder, place them in a clean PFA sample dissolving bottle, tighten the PFA sample dissolving bottle, shake it manually for 30 seconds and put it into an electronic oven , the temperature is set to 255°C, and the time is set to 1 hour;

[0037] 3) When the time is up, wait for the PFA sample dissolving bottle to cool down. At this time, the geological sample in the PFA sample dissolving bottle and ammonium fluoride form a solid cake mixture. Take out the PFA sample dissolving bottle and place it on the electric heating plate, add 2 ml of nitric acid, and heat it Set the temperature of the plate at 160°C, heat unti...

Embodiment 2

[0041] The present invention provides a kind of application method of ammonium fluoride as the digestion reagent of geological sample, and it comprises the steps:

[0042] 1) Physically pulverize the shale (GSR-5) sample to 200 mesh (sieve: 0.074 mm) to obtain a powder test sample;

[0043] 2) Weigh 300 mg of ammonium fluoride and 50±1 mg of shale (GSR-5) sample powder, place them in a clean Teflon sample dissolving bottle, tighten the Teflon sample dissolving bottle, shake it manually for 30 seconds, and put it into the electronic In the oven, the temperature is set to 250°C and the time is set to 1 hour;

[0044] 3) When the time is up, wait for the Teflon sample dissolving bottle to cool down. At this time, the geological sample in the Teflon sample dissolving bottle is a solid cake mixture with ammonium fluoride. Take out the Teflon sample dissolving bottle and place it on the electric heating plate, add 2 ml of nitric acid, Set the temperature of the electric heating plate...

Embodiment 3

[0048] The present invention provides a kind of application method of ammonium fluoride as the digestion reagent of geological sample, and it comprises the steps:

[0049] 1) Physically pulverize the basalt (BHVO-2) sample to 200 mesh (sieve: 0.074 mm) to obtain a powder test sample;

[0050] 2) Weigh 300 mg of ammonium fluoride and 50±1 mg of basalt (BHVO-2) sample powder, place them in a clean Teflon sample dissolution bottle, tighten the Teflon sample dissolution bottle, shake it manually for 30 seconds, and put it into an electronic oven , the temperature is set to 230°C, and the time is set to 30 minutes;

[0051] 3) When the time is up, wait for the Teflon sample dissolving bottle to cool down. At this time, the geological sample in the Teflon sample dissolving bottle is a solid cake mixture with ammonium fluoride. Take out the Teflon sample dissolving bottle and place it on the electric heating plate, add 1 ml of nitric acid, Set the temperature of the electric heating...

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Abstract

The invention provides a pretreatment method of ammonium fluoride for digesting a geological sample, which comprises the following steps of 1) weighting ammonium fluoride and the geological sample according to the mass ratio of (4-6):1, placing the ammonium fluoride and the geological sample into a dissolution sample bottle, shaking, and then heating the dissolution sample bottle for 0.5-1 hours to achieve 230-255 DEG C; 2) adding acid into the dissolution sample bottle after the dissolution sample bottle is cooled down to a room temperature and then heating for removing silicon; and 3) after removal of all silicon, adding acid and water into the dissolution sample bottle, then heating for dissolving solid state residue in the dissolution sample bottle completely. The application method has the advantages of high efficiency, safety, low cost, flexibility, small work load and the like, is a significant innovation in digestion methods of geological sample and has very good application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to an application method of ammonium fluoride as a digestion reagent for geological samples. Background technique [0002] The determination of trace element content and isotope ratio in geological samples such as rocks, sediments or soils is of great significance for studying the formation and evolution of the crust and mantle and tracing other geochemical processes. At present, in analytical geochemical testing, whether using conventional ICP-MS to analyze whole-rock trace elements in rock samples or using TIMS or MC-ICP-MS to determine whole-rock isotope ratios, it is necessary to convert geological samples into a solution form. After the solid sample is processed and decomposed into a solution form, the elements are uniformly present in the solution in an ion state, eliminating the measurement errors caused by the occurrence state and physical characteristics of the el...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44
Inventor 胡兆初张文刘勇胜陈海红高山
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)