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Method for completely digesting manganese ore sample

A manganese ore and sample technology, applied in the field of completely digesting manganese ore samples, can solve the problems of sample loss, analysis element loss, rare earth element analysis difficulties, etc., and achieve the effect of reducing analysis cost, ensuring accuracy and avoiding loss

Active Publication Date: 2019-09-27
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] 1). Use H 2 SO 4 The solution is used as the extraction reagent, and the matrix of the analysis sample solution is H 2 SO 4 The solution will interfere with the mass spectrum peaks of ICP-MS analysis, making it difficult to analyze rare earth elements;
[0013] 2). The sample analysis volume needs to be 200mg, using H 2 SO 4 The volume of the solution also reaches 100mL, that is, there is a problem of large sampling volume and digestion reagent usage, which does not meet the analysis principles of green economy;
[0014] 3). This method uses filter paper to filter the sample extraction supernatant, indicating that the sample is not digested completely, and there is a problem of sample loss
Moreover, the residue will adsorb the elements to be analyzed, resulting in the loss of the analyzed elements, so the analysis results cannot truly reflect the rare earth element content of the sample.
[0015] In summary, with H 2 SO 4 It is not advisable to analyze rare earth elements by digesting manganese ore with sealed and shaken solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] A method for fully digesting a manganese ore sample, comprising the steps of:

[0058] 1. Manganese ore sample pretreatment processing:

[0059] 1) crushing the manganese ore sample into particles;

[0060] 2) Put the crushed manganese ore sample into the digestion tank, and add 0.5mLHNO to every 48mg-52mg manganese ore sample 3 , 1.0 mL HF, 1.5 mL HCl, and 0.7 μL HClO 4 , shake well, heat and steam the open digestion tank to a water content of 3%-7%, forming a wet-dry sample;

[0061] 3) Add 0.5mL HNO to every 48mg-52mg manganese ore sample in the digestion tank with wet and dry samples 3 , 0.5mL HF, 1.5mL HCl, 0.6μL HClO 4 , heat after sealing the lid, set the heating temperature to 180-190°C, after 45-52 hours, take the digestion tank out of the oven, and form a cooled sample after cooling;

[0062] 2. Post-processing of manganese ore samples:

[0063] 1) Open the upper cover of the above-mentioned digestion tank equipped with cooled samples, heat the digestion...

Embodiment 2

[0069] On the basis of Embodiment 1, there are the following alternatives:

[0070] A method for fully digesting a manganese ore sample, comprising the steps of:

[0071] 1. Manganese ore sample pretreatment processing:

[0072] 1) The manganese ore sample is crushed into particles with a particle size of less than 75 μm; this particle size ensures the uniformity of the sample and ensures that the following analysis samples are representative;

[0073] 2) Put the crushed manganese ore sample into the digestion tank, add 0.5mL HNO for every 49.5mg-50.5mg manganese ore sample 3 , 1.0 mL HF, 1.5 mL HCl, and 0.7 μL HClO 4 , shake well, heat the open digestion tank at 150-160°C, and steam until the water content is 3%-7%; this step is the sample pre-decompression process to prevent the reaction pressure from being too high during the next step of oven high-temperature digestion cause explosion and other safety hazards. Because the ore sample contains silicate, it is necessary t...

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PUM

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Abstract

The invention discloses a method for completely digesting a manganese ore sample, which comprises pretreatment and post-treatment, and the pretreatment comprises the following steps: 1) crushing the manganese ore sample into particles; 2) putting the crushed sample into a digestion tank, adding HNO3, HF, HCl and HClO4, uniformly shaking, and heating and steaming the digestion tank until the water content is 3%-7%; 3) adding HNO3, HF, HCl and HClO4, capping, putting into a drying oven, heating, and cooling to form a cooled sample; the post-treatment processing comprises the following steps: 1) opening the digestion tank filled with the cooled sample, and heating and steaming until the water content is 3%-7%; 2) adding HNO3 and HCl, and steaming until the water content is 3%-7%; 3) adding HNO3, and steaming until the water content is 3%-7%; 4) adding HNO3, sealing, putting into an oven, heating for 4 hours, and taking out; and 5) adopting an HNO3 solution with a volume ratio of 2% as a matrix, and adopting ICP-MS for element analysis to obtain an analysis result. The method can improve the accuracy of the analysis result of the manganese ore sample, and the relative standard deviation of the analysis result is less than 3.0%; the process complexity and the analysis cost are reduced, and the convenience of actual analysis work of ore prospecting is improved.

Description

technical field [0001] The invention belongs to the technical field of ore analysis and measurement, in particular to a method for completely digesting manganese ore samples. Background technique [0002] Manganese is the tenth most abundant element in the earth's crust, and it is also the most common metal element after iron. Manganese ore is one of the important metal resources in my country, the reserves rank fourth in the world, and it is one of the important raw materials for metallurgy, light industry and chemical production. For example, adding small amounts of manganese to steel increases hardness, ductility, toughness and wear resistance. Due to the uneven distribution of manganese ore in my country, the deep burial of ore bodies and the difficulty in mining and beneficiation, in order to meet the demand for manganese and its compounds in my country, it is necessary to conduct an in-depth analysis of the ore-forming causes of manganese mines to establish a metallog...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28G01N1/44G01N27/626
CPCG01N27/62G01N1/286G01N1/44
Inventor 谭细娟王柱命梁婷
Owner CHANGAN UNIV