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Method for determining elementary composition of cobalt pyrite concentrate, and digestion method for cobalt pyrite concentrate sample

A technology of sulfur-cobalt concentrate and element composition, which is applied in the field of detection and analysis, can solve the problems of increasing the concentration of solution salts, large sample consumption, complicated operation, etc., and achieve the effect of ensuring safety and avoiding excessive pressure increase

Active Publication Date: 2016-08-10
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method has disadvantages such as complex operation, volatile loss of silicon, sulfur, arsenic and other elements, large sample consumption, long analysis process and time-consuming, etc. Sulfur-cobalt concentrate produced by screening and enriching mineral resources, due to the coexistence of high content of refractory elements such as sulfur, carbon, chromium, titanium, aluminum, silicon, etc. in the form of sulfide or other forms, causes such Sulfur-cobalt concentrate samples are particularly difficult to quickly digest; the other is to use fire melting and digestion, that is, lithium tetraborate, sodium carbonate, boric acid, sodium peroxide and other basic fluxes are melted and digested in a muffle furnace at high temperature. Then dissolve and leach salts with hydrochloric acid and other solutions to carry out element content analysis.
This type of method introduces a large amount of alkali metal ions such as lithium or sodium, and greatly increases the salt concentration of the solution, resulting in matrix effects, background noise and other interference factors that seriously affect the accurate determination of element content.

Method used

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  • Method for determining elementary composition of cobalt pyrite concentrate, and digestion method for cobalt pyrite concentrate sample
  • Method for determining elementary composition of cobalt pyrite concentrate, and digestion method for cobalt pyrite concentrate sample
  • Method for determining elementary composition of cobalt pyrite concentrate, and digestion method for cobalt pyrite concentrate sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Digestion of sulfur cobalt concentrate samples

[0044] Weigh 0.2000g of sulfur-cobalt concentrate sample (hereinafter referred to as sample No. 1) into the inner tank of microwave digestion, add 10.0mL of water and 10.0mL of nitric acid along the wall of the container in sequence, then shake the container to evenly disperse the sample, and then add 2.0mL of hydrogen Hydrofluoric acid and 2.0mL hydrogen peroxide; put the outer tank on quickly, cover the lid and tighten it with a torque wrench to ensure a good seal, put the sealed digestion container into the microwave digestion furnace according to the instrument operation steps, connect the temperature and pressure Microwave digestion and complexation reactions were performed after the sensor. In this example, the microwave reaction method of ramping up the temperature is adopted, the pressure is controlled below 800 psi (1 psi = 6.895 KPa), and the digestion reaction is divided into three stages and the temperature i...

Embodiment 2

[0049] Weigh 0.5000g of sulfur-cobalt concentrate sample (hereinafter referred to as No. 2 sample), add successively the combined digestion reagent of 15.0mL water, 15.0mL nitric acid, 3.0mL hydrofluoric acid and 3.0mL hydrogen peroxide, then seal the container for Microwave digestion; the pressure is controlled below 800psi, and the microwave heating conditions are first to raise the temperature to 90°C for 5 minutes and keep it for 5 minutes for low-temperature digestion, then raise the temperature to 150°C for 10 minutes and keep it for 10 minutes for medium-temperature digestion, and finally raise the temperature to 200°C for 5 minutes and keep it for 7 minutes High-temperature enhanced digestion; after the microwave digestion solution is cooled to room temperature, it is directly diluted with water and fixed to volume in a 200mL plastic volumetric flask.

[0050] Besides, the sulfur-cobalt concentrate sample was digested in the same way as in Example 1, and the solution wa...

Embodiment 3

[0052] Weigh 0.3000g of sulfur-cobalt concentrate sample (hereinafter referred to as No. 3 sample), add successively the combined digestion reagent of 10.0mL water, 10.0mL nitric acid, 2.0mL hydrofluoric acid and 2.0mL hydrogen peroxide, then seal the container for Microwave digestion; the pressure is controlled below 800psi, and the microwave heating conditions are first to raise the temperature to 80°C for 4 minutes and keep it for 4 minutes for low-temperature digestion, then raise the temperature to 140°C for 7 minutes and keep it for 8 minutes for medium-temperature digestion, and finally raise the temperature to 190°C for 5 minutes and keep it for 6 minutes High-temperature enhanced digestion; after the microwave digestion solution is cooled to room temperature, it is directly diluted with water and fixed to volume in a 100mL plastic volumetric flask.

[0053] Besides, the sulfur-cobalt concentrate sample was digested in the same way as in Example 1, and the solution was ...

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Abstract

The invention relates to a method for determining elementary composition of cobalt pyrite concentrate and a digestion method for a cobalt pyrite concentrate sample, belonging to the field of detection and analysis technology. To overcome technical problems in the prior art, the invention provides the digestion method for the cobalt pyrite concentrate sample. The digestion method comprises the following steps: weighing the cobalt pyrite concentrate sample, putting the sample in a container, directly adding water, concentrated nitric acid, hydrofluoric acid and hydrogen peroxide in sequence and then enclosing the container; carrying out gradient heating in three stages by using microwave heating so as to realize digestion; and after completion of digestion, carrying out cooling and then carrying out diluting with water until a volume is fixed so as to obtain a sample detection solution. Compared with the prior art, the digestion method provided by the invention has the advantages that operation is simple and fast; sample digestion is rapid and complete; reagents are simple and low in consumption; few examination steps are needed; flow is short; ICP-OES realizes simultaneous determination of gas, metallic elements, major elements and trace elements; technological performance indexes are excellent; and the range of detection elements and contents is wide; etc.

Description

technical field [0001] The invention relates to a method for determining elemental components in sulfur-cobalt concentrate and a sample digestion method thereof, belonging to the technical field of detection and analysis. Background technique [0002] Cobalt concentrate is mainly used in the alloy industry to produce cobalt sulfate, cobalt chloride, cobalt carbonate, cobalt oxide, metal cobalt, tungsten-cobalt alloy, cobalt magnetic alloy, as well as in the electronics industry as positive electrode materials for cobalt-lithium batteries or in the chemical industry Used as a catalyst, etc. [0003] There are not many cobalt ore resources in China, and cobalt ore and cobalt concentrates have always relied on imports to meet the growing domestic demand. There are especially few independent cobalt deposits in my country, which are mainly produced together with iron, nickel, copper and other minerals as associated minerals. The sulfide ore belt of vanadium-titanium magnetite i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N21/73
CPCG01N1/44G01N21/73
Inventor 成勇
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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