Method for detection of arsenic content in pyrite or pyrite concentrate by atomic fluorescence spectrophotometry

A technique of atomic fluorescence spectrometry and pyrite, applied in fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of low accuracy of detection results, complicated operation process, easy loss of arsenic, etc., and achieve fast measurement speed and accurate measurement results , the effect of improving the degree of restoration

Active Publication Date: 2017-06-20
SICHUAN YINHE CHEM
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Problems solved by technology

At present, the national standard detection method of arsenic content in pyrite and pyrite concentrate adopts the Ag-DDTC spectrophotometric method, which is easy to lose arsenic, the operation process is complicated, and the accuracy of the detection result is low

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0030] A method for detecting arsenic content in pyrite by atomic fluorescence spectrometry, comprising the following steps:

[0031] Step 1, drying the pyrite sample at 100-105°C to constant weight, pulverizing it with a pulverizer, and passing it through a 150um test sieve;

[0032] Step 2. Take 0.2 g of the sieved sample in a 150 mL container, add 15 mL of hydrochloric acid, and heat to dissolve the sample; then add 5 mL of nitric acid, continue heating and steaming to a wet salt shape, and cool to obtain a wet salt sample;

[0033] Step 3. Add 5mL of hydrochloric acid with a volume ratio of 1:1 to the wet salt sample, dissolve the soluble salts, cool, transfer to a 100mL volumetric flask, add 10ml of thiourea-ascorbic acid mixture, and dilute with water to volume Carry out dry filtration, discard initial 20mL filtrate, pipette 1mL filtrate in 50mL volumetric flask, add water again and dilute constant volume, obtain sample solution; Described thiourea-ascorbic acid mixed so...

Embodiment 2

[0039] A method for detecting arsenic content in pyrite by atomic fluorescence spectrometry, comprising the following steps:

[0040] Step 1, drying the pyrite sample at 100-105°C to constant weight, pulverizing it with a pulverizer, and passing it through a 150um test sieve;

[0041] Step 2. Take 0.2 g of the sieved sample in a 150 mL container, add 15 mL of hydrochloric acid, and heat to dissolve the sample; then add 5 mL of nitric acid, continue heating and steaming to a wet salt shape, and cool to obtain a wet salt sample;

[0042] Step 3: Add 5mL of hydrochloric acid with a volume ratio concentration of 1:1 to the wet salt sample, dissolve the soluble salts, cool, transfer to a 100mL volumetric flask, add 10ml of thiourea solution, and then dilute with water to constant volume; Filter, discard the initial 20mL filtrate, pipette 1mL filtrate into a 50mL volumetric flask, and then dilute with water to obtain a sample solution; the concentration of the thiourea solution is 1...

Embodiment 3

[0048] Pyrite is replaced by sulfur concentrate, and the rest of the parameters and operating process are exactly the same as those in Example 1.

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Abstract

The invention discloses a method for detection of arsenic content in pyrite or pyrite concentrate by atomic fluorescence spectrophotometry. The method includes: (1) drying pyrite or pyrite concentrate to a constant weight, and conducting crushing and sieving; (2) taking 0.2g of a sieved sample and putting the sample into a 150mL container, adding 15mL of hydrochloric acid, and conducting heating and dissolving, then adding 5mL of nitric acid, and performing heating to a wet salt state; (3) adding 5mL of hydrochloric acid into a wet salt sample, performing cooling, then transferring the mixture into a 100mL volumetric flask, adding 10mL of a thiourea-ascorbic acid mixed solution or a thiourea solution, adding water for dilution to a constant volume, and performing dry filtration, discarding the initial 20mL of filtrate, shifting 1mL of filtrate into a 50mL volumetric flask, then adding water for dilution to a constant volume, thus obtaining a sample solution; and (4) using an atomic fluorescence spectrophotometer to measure the fluorescence intensity of the sample solution obtained in (3), and working out the content of arsenic in the pyrite or pyrite concentrate sample solution. The method provided by the invention can effectively improve the dissolution thoroughness of arsenic in pyrite and sulfur concentrate, improve the reduction degree of arsenic, reduce the loss rate of arsenic, and enhance the accuracy and precision of arsenic in pyrite and sulfur concentrate.

Description

technical field [0001] The invention relates to the field of mineral detection, in particular to a method for detecting the arsenic content of pyrite or sulfur concentrate by atomic fluorescence spectrometry. Background technique [0002] Arsenic is a harmful impurity element in sulfuric acid, so its composition needs to be tested from ore raw materials to products. At present, the national standard detection method of arsenic content in pyrite and sulfur concentrate adopts the Ag-DDTC spectrophotometric method, which is easy to lose arsenic, the operation process is complicated, and the accuracy of the detection result is low. Therefore, if the accuracy and precision are to be improved, the thoroughness of the dissolution of arsenic in pyrite and sulfur concentrate, the degree of arsenic reduction, and the reduction of arsenic loss rate should be improved as much as possible. Contents of the invention [0003] An object of the present invention is to solve at least the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 周中田陈宁谢友才赵汝鉴刘锋曾理
Owner SICHUAN YINHE CHEM
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