CN112432942A - Method for measuring contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore - Google Patents

Method for measuring contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore Download PDF

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CN112432942A
CN112432942A CN202011250335.0A CN202011250335A CN112432942A CN 112432942 A CN112432942 A CN 112432942A CN 202011250335 A CN202011250335 A CN 202011250335A CN 112432942 A CN112432942 A CN 112432942A
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molybdenum
tungsten
bismuth
metal ore
contents
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雷勇
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Hunan Shizhuyuan Nonferrous Metals Co Ltd
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Hunan Shizhuyuan Nonferrous Metals Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising

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Abstract

The invention discloses a method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore, which relates to the technical field of measuring the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore, in particular to a method for measuring the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore, and comprises the following steps: s1, crushing the tungsten, molybdenum and bismuth multi-metal ore; s2, weighing tungsten, molybdenum and bismuth multi-metal ore powder; s3, mixing the extraction solution; and S4, comparing and measuring the contents of the tungsten, the molybdenum and the bismuth. The method for measuring the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore has accurate analysis result; the analysis flow is simple and the speed is high; fills the domestic blank of analyzing the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore in an instrument analysis method; the method has wide application range, and has wide application value in exploration, mineral separation and smelting of tungsten, molybdenum and bismuth multi-metal ore beds because the influence of interference elements on the method is very small.

Description

Method for measuring contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore
Technical Field
The invention relates to the technical field of determination of tungsten-molybdenum-bismuth multi-metal ores, in particular to a method for determining contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ores.
Background
The existing colorimetric method and volumetric method are mostly adopted for the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore, multi-metal samples containing more mineral elements such as tungsten, molybdenum, bismuth, copper and arsenic must be separated in advance, otherwise, accurate analysis results are difficult to obtain, and great difficulty exists in operation for separating ore materials containing various interference elements one by one. While some methods adopting instrumental analysis can only detect one element singly, and the repeated treatment of samples wastes manpower and material resources.
In the analysis process of tungsten, molybdenum and bismuth in the polymetallic ore, samples need to be processed for many times, so that the operation labor intensity is higher; the method has no problem of good instrument analysis method for simultaneously detecting the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for measuring the contents of tungsten trioxide, molybdenum and bismuth in a tungsten-molybdenum-bismuth multi-metal ore, which solves the problems that some methods adopting instrument analysis can only detect one element singly, the repeated treatment of samples wastes manpower and material resources, and in the analysis process of tungsten, molybdenum and bismuth in the multi-metal ore, the samples need to be treated for multiple times, the operation labor intensity is higher, and no good instrument analysis method exists for simultaneously detecting the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore comprises the following steps:
s1, crushing the tungsten, molybdenum and bismuth multi-metal ore: putting the tungsten-molybdenum-bismuth multi-metal ore into a crusher for crushing and filtering to prepare tungsten-molybdenum-bismuth multi-metal ore powder A;
s2, weighing tungsten, molybdenum and bismuth multi-metal ore powder: sequentially weighing tungsten-molybdenum-bismuth multi-metal ore powder A by an electronic scale, and dividing the tungsten-molybdenum-bismuth multi-metal ore powder A into three parts, wherein the mass parts are 0-100g, 200g of ion-doped tungsten-molybdenum-bismuth powder and 500g of ion-doped tungsten-molybdenum-bismuth powder;
s3, mixed extraction solution: sequentially placing hydrochloric acid, nitric acid and perchloric acid into a reaction kettle, placing the tungsten-molybdenum-bismuth polymetallic ore powder A into the reaction kettle, and mixing for a period of time under the condition of a certain temperature range until the tungsten-molybdenum-bismuth polymetallic ore powder A is uniformly mixed to prepare a mixed solution B;
s4, comparing and measuring the contents of tungsten, molybdenum and bismuth elements: measuring a certain volume of the mixed liquid B in the steps, putting the measured mixed liquid B into a plasma spectrometer for excitation to generate a plasma spectrum, and determining the contents of tungsten, molybdenum and bismuth in the sample according to the intensity of the generated characteristic spectral line.
Optionally, in the step S1, in crushing the tungsten-molybdenum-bismuth polymetallic ore, the model of the crusher is CP-300X180, the feeding granularity is less than 80mm, the discharging granularity is 3mm-20mm, and the power is 1.5 KW.
Optionally, in the step S3, in the mixed extraction solution, the model of the reaction kettle is THS-50L, and the rotation speed is 0-600 rpm.
Optionally, in the step S3, mixing the extraction solution for 20-30min at 30-60 ℃.
The invention provides a method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore, which has the following beneficial effects:
the analysis result is accurate; the analysis flow is simple and the speed is high; fills the domestic blank of analyzing the tin in the tungsten-molybdenum-bismuth-tin polymetallic ore in an instrument analysis method; the method has wide application range, and has wide application value in exploration, mineral separation and smelting of tungsten, molybdenum, bismuth and tin polymetallic ore deposits because the interference elements have little influence on the method.
Detailed Description
In the following, technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Embodiment 1
The invention provides a technical scheme that: a method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore comprises the following steps:
s1, crushing the tungsten, molybdenum and bismuth multi-metal ore: putting the tungsten-molybdenum-bismuth multi-metal ore into a crusher for crushing and filtering to prepare tungsten-molybdenum-bismuth multi-metal ore powder A;
s2, weighing tungsten, molybdenum and bismuth multi-metal ore powder: sequentially weighing tungsten-molybdenum-bismuth multi-metal ore powder A by an electronic scale, and dividing the tungsten-molybdenum-bismuth multi-metal ore powder A into three parts, wherein the parts by mass are 50g, 150g and 250g respectively;
s3, mixed extraction solution: sequentially placing hydrochloric acid, nitric acid and perchloric acid into a reaction kettle, placing the tungsten-molybdenum-bismuth polymetallic ore powder A into the reaction kettle, and mixing for a period of time under the condition of a certain temperature range until the tungsten-molybdenum-bismuth polymetallic ore powder A is uniformly mixed to prepare a mixed solution B;
s4, comparing and measuring the contents of tungsten, molybdenum and bismuth elements: measuring a certain volume of the mixed liquid B in the steps, putting the measured mixed liquid B into a plasma spectrometer for excitation to generate a plasma spectrum, and determining the contents of tungsten, molybdenum and bismuth in the sample according to the intensity of the generated characteristic spectral line.
And step S1, in crushing the tungsten-molybdenum-bismuth multi-metal ore, the model of the crusher is CP-300X180, the feeding granularity is less than 80mm, the discharging granularity is 3mm-20mm, and the power is 1.5 KW.
And step S3, mixing the extraction solution, wherein the model of the reaction kettle is THS-50L, and the rotating speed is 200 rpm.
And step S3, mixing the extractive solution at 45 deg.C for 20 min.
Example II
A method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore comprises the following steps:
s1, crushing the tungsten, molybdenum and bismuth multi-metal ore: putting the tungsten-molybdenum-bismuth multi-metal ore into a crusher for crushing and filtering to prepare tungsten-molybdenum-bismuth multi-metal ore powder A;
s2, weighing tungsten, molybdenum and bismuth multi-metal ore powder: sequentially weighing tungsten-molybdenum-bismuth multi-metal ore powder A by an electronic scale, and dividing the tungsten-molybdenum-bismuth multi-metal ore powder A into three parts, wherein the parts by mass are 75g, 175g and 275g respectively;
s3, mixed extraction solution: sequentially placing hydrochloric acid, nitric acid and perchloric acid into a reaction kettle, placing the tungsten-molybdenum-bismuth polymetallic ore powder A into the reaction kettle, and mixing for a period of time under the condition of a certain temperature range until the tungsten-molybdenum-bismuth polymetallic ore powder A is uniformly mixed to prepare a mixed solution B;
s4, comparing and measuring the contents of tungsten, molybdenum and bismuth elements: measuring a certain volume of the mixed liquid B in the steps, putting the measured mixed liquid B into a plasma spectrometer for excitation to generate a plasma spectrum, and determining the contents of tungsten, molybdenum and bismuth in the sample according to the intensity of the generated characteristic spectral line.
And step S1, in crushing the tungsten-molybdenum-bismuth multi-metal ore, the model of the crusher is CP-300X180, the feeding granularity is less than 80mm, the discharging granularity is 3mm-20mm, and the power is 1.5 KW.
And step S3, mixing the extraction solution, wherein the model of the reaction kettle is THS-50L, and the rotating speed is 450 rpm.
And step S3, mixing the extractive solution at 55 deg.C for 25 min.
Example three
A method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore comprises the following steps:
s1, crushing the tungsten, molybdenum and bismuth multi-metal ore: putting the tungsten-molybdenum-bismuth multi-metal ore into a crusher for crushing and filtering to prepare tungsten-molybdenum-bismuth multi-metal ore powder A;
s2, weighing tungsten, molybdenum and bismuth multi-metal ore powder: sequentially weighing tungsten-molybdenum-bismuth multi-metal ore powder A by an electronic scale, and dividing the tungsten-molybdenum-bismuth multi-metal ore powder A into three parts, wherein the parts by mass are 100g, 200g and 500g respectively;
s3, mixed extraction solution: sequentially placing hydrochloric acid, nitric acid and perchloric acid into a reaction kettle, placing the tungsten-molybdenum-bismuth polymetallic ore powder A into the reaction kettle, and mixing for a period of time under the condition of a certain temperature range until the tungsten-molybdenum-bismuth polymetallic ore powder A is uniformly mixed to prepare a mixed solution B;
s4, comparing and measuring the contents of tungsten, molybdenum and bismuth elements: measuring a certain volume of the mixed liquid B in the steps, putting the measured mixed liquid B into a plasma spectrometer for excitation to generate a plasma spectrum, and determining the contents of tungsten, molybdenum and bismuth in the sample according to the intensity of the generated characteristic spectral line.
And step S1, in crushing the tungsten-molybdenum-bismuth multi-metal ore, the model of the crusher is CP-300X180, the feeding granularity is less than 80mm, the discharging granularity is 3mm-20mm, and the power is 1.5 KW.
And step S3, mixing the extraction solution, wherein the model of the reaction kettle is THS-50L, and the rotating speed is 600 rpm.
And step S3, mixing the extractive solution at 60 deg.C for 30 min.
In summary, when the method for determining the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore is used, firstly, the tungsten-molybdenum-bismuth multi-metal ore is placed into a crusher to be crushed and filtered to prepare tungsten-molybdenum-bismuth multi-metal ore powder A, then, the tungsten-molybdenum-bismuth multi-metal ore powder A is sequentially weighed by an electronic scale, and the tungsten-molybdenum-bismuth multi-metal ore powder A is divided into three parts, wherein the parts by mass are respectively 0-100g, 100-200g and 200-500 g; secondly, sequentially placing hydrochloric acid, nitric acid and perchloric acid into a reaction kettle, placing the tungsten-molybdenum-bismuth polymetallic ore powder A into the reaction kettle, and mixing for 20-30min at the temperature of 30-60 ℃ until the mixture is uniformly mixed to prepare a mixed solution B; then, the contents of tungsten, molybdenum and bismuth are measured in comparison: measuring a certain volume of the mixed liquid B in the steps, putting the measured mixed liquid B into a plasma spectrometer for excitation to generate a plasma spectrum, and determining the contents of tungsten, molybdenum and bismuth in the sample according to the intensity of the generated characteristic spectral line.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (4)

1. A method for measuring the contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore is characterized by comprising the following steps:
s1, crushing the tungsten, molybdenum and bismuth multi-metal ore: putting the tungsten-molybdenum-bismuth multi-metal ore into a crusher for crushing and filtering to prepare tungsten-molybdenum-bismuth multi-metal ore powder A;
s2, weighing tungsten, molybdenum and bismuth multi-metal ore powder: sequentially weighing tungsten-molybdenum-bismuth multi-metal ore powder A by an electronic scale, and dividing the tungsten-molybdenum-bismuth multi-metal ore powder A into three parts, wherein the mass parts are 0-100g, 200g of ion-doped tungsten-molybdenum-bismuth powder and 500g of ion-doped tungsten-molybdenum-bismuth powder;
s3, mixed extraction solution: sequentially placing hydrochloric acid, nitric acid and perchloric acid into a reaction kettle, placing the tungsten-molybdenum-bismuth polymetallic ore powder A into the reaction kettle, and mixing for a period of time under the condition of a certain temperature range until the tungsten-molybdenum-bismuth polymetallic ore powder A is uniformly mixed to prepare a mixed solution B;
s4, comparing and measuring the contents of tungsten, molybdenum and bismuth elements: measuring a certain volume of the mixed liquid B in the steps, putting the measured mixed liquid B into a plasma spectrometer for excitation to generate a plasma spectrum, and determining the contents of tungsten, molybdenum and bismuth in the sample according to the intensity of the generated characteristic spectral line.
2. The method for determining the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore according to claim 1, which is characterized in that: in the step S1, in crushing the tungsten-molybdenum-bismuth multi-metal ore, the model of the crusher is CP-300X180, the feeding granularity is less than 80mm, the discharging granularity is 3mm-20mm, and the power is 1.5 KW.
3. The method for determining the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore according to claim 1, which is characterized in that: and S3, mixing the extraction solution, wherein the model of the reaction kettle is THS-50L, and the rotating speed is 0-600 rpm.
4. The method for determining the contents of tungsten trioxide, molybdenum and bismuth in the tungsten-molybdenum-bismuth multi-metal ore according to claim 1, which is characterized in that: and step S3, mixing the mixed extract solution for 20-30min at 30-60 ℃.
CN202011250335.0A 2020-11-10 2020-11-10 Method for measuring contents of tungsten trioxide, molybdenum and bismuth in tungsten-molybdenum-bismuth multi-metal ore Pending CN112432942A (en)

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CN102288595A (en) * 2011-07-29 2011-12-21 西北矿冶研究院 Method for continuously measuring tungsten and molybdenum by taking citric acid and hydrogen peroxide as complexing agents
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