CN114062104A - Method suitable for quickly digesting and measuring molybdenum in molybdenum ore dressing material - Google Patents
Method suitable for quickly digesting and measuring molybdenum in molybdenum ore dressing material Download PDFInfo
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 110
- 239000011733 molybdenum Substances 0.000 title claims abstract description 110
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 239000000779 smoke Substances 0.000 claims abstract description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 4
- 239000012498 ultrapure water Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 31
- 239000012086 standard solution Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000011978 dissolution method Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 238000002137 ultrasound extraction Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 28
- 230000003595 spectral effect Effects 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003969 polarography Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method suitable for quickly digesting and measuring molybdenum in molybdenum beneficiation materials, which comprises the following steps: preparing a molybdenum standard grade difference solution; secondly, putting a weighed molybdenum ore dressing material sample into a polytetrafluoroethylene beaker, adding hydrochloric acid for dissolving, heating in an ultrasonic water bath instrument, adding nitric acid for continuous dissolution, adding hydrofluoric acid after dissolution, removing silicon at low temperature till the sample is nearly dry, adding perchloric acid, taking down and cooling after perchloric acid smoke is exhausted; adding nitric acid, placing in an ultrasonic water bath instrument to dissolve salts at low temperature, cooling after the sample is completely dissolved, and performing constant volume with ultrapure water to be detected; and step three, measuring and calculating the content of effective molybdenum in the molybdenum ore dressing material by using an inductively coupled plasma mass spectrometer. The invention adopts an acid dissolution method to digest the sample, and the sample is dissolved in an ultrasonic water bath instrument, the ultrasonic-assisted extraction method utilizes the cavitation action of ultrasonic waves to accelerate the extraction of the component to be detected, and the error caused by improper operation of personnel is reduced on the premise of ensuring the accuracy of the result.
Description
Technical Field
The invention relates to a method suitable for quickly digesting and measuring molybdenum in molybdenum beneficiation materials.
Background
Molybdenum is an important strategic resource with excellent performance, is widely applied to various fields such as agriculture, military, chemical industry, electricity, metallurgical machinery, medicine and the like, is also commonly used as an additive for producing various alloy steels, and has a lot of applications in electronic devices such as electronic tubes, transistors, rectifiers and the like. With the continuous development of the metallurgical industry and aerospace technology in China, the demand of molybdenum is increased year by year, and the search for molybdenum ore becomes a hotspot of mineral exploration projects. Molybdenum is one of refractory high-temperature metal elements, pure molybdenum has silvery white metallic luster, and powdered molybdenum is dark gray. Currently, about 30 kinds of molybdenum minerals are known in nature, and most of the molybdenum minerals exist in a sulfide form, and the rest molybdenum minerals exist in an oxide form. The molybdenum content in the ore is generally very low, on the order of a few thousandths or a few percent, and the molybdenum concentrate content can reach 50 percent. Molybdenum ore often accompanies tungsten, tin, copper, lead, zinc, gold, silver and other elements, so that the selection of a proper method is very important for quantitative analysis of molybdenum in the ore.
The molybdenum element is often measured by thiocyanate spectrophotometry, polarography, or the like.
The thiocyanate spectrophotometry and polarography are adopted, and the methods have the defects of complex operation, long analysis period, low efficiency and the like. The decomposition method of the ore sample can generally adopt alkali fusion or acid dissolution, the alkali fusion method can completely dissolve the sample, but more salts are introduced, the load of the power of the instrument is increased, and simultaneously a large amount of potassium and sodium elements can generate matrix interference.
Disclosure of Invention
The invention aims to provide a method suitable for quickly digesting and measuring molybdenum in molybdenum ore dressing materials, which solves the technical problem of how to accurately and quickly digest and measure a molybdenum ore, intermediate materials generated by the molybdenum ore and a sample in the process of extracting, enriching and refining molybdenum.
The invention aims to provide a method suitable for quickly digesting and measuring molybdenum in molybdenum ore dressing materials, and solves the technical problem of how to accurately and quickly digest and measure a sample.
The technical scheme of the invention is realized as follows: a method suitable for quickly digesting and measuring molybdenum in molybdenum ore dressing materials comprises the following steps: preparing a molybdenum standard grade difference solution; secondly, placing the weighed molybdenum ore dressing material sample in a polytetrafluoroethylene beaker, blowing water to moisten, adding hydrochloric acid to dissolve, heating in an ultrasonic water bath instrument, adding nitric acid to dissolve continuously, adding hydrofluoric acid after dissolving, removing silicon at low temperature till the sample is nearly dry, adding perchloric acid, taking down and cooling after perchloric acid smoke is exhausted; washing the wall of the cup with a small amount of deionized water, adding nitric acid, placing in an ultrasonic water bath instrument for dissolving salts at low temperature, cooling after the sample is completely dissolved, transferring to a volumetric flask, and performing constant volume with ultrapure water to be measured; and step three, measuring and calculating the content of effective molybdenum in the molybdenum ore dressing material by using an inductively coupled plasma mass spectrometer.
Preferably, before preparing the molybdenum standard deviation solution, preparing a molybdenum standard storage solution, then preparing a molybdenum standard solution, and then diluting the molybdenum standard solution to obtain the molybdenum standard deviation solution.
Preferably, the preparation method of the molybdenum standard storage solution comprises the steps of weighing spectrally pure molybdenum trioxide dried at 105-110 ℃ into a beaker, adding a sodium hydroxide solution for dissolving, and fixing the volume in a volumetric flask by water, wherein 1mL of the standard storage solution contains 1mg of molybdenum.
Preferably, the molybdenum standard solution is removed into a volumetric flask, and concentrated nitric acid is added, wherein 1mL of the solution contains 100ug of molybdenum respectively.
Preferably, the molybdenum standard storage solution or the molybdenum standard solution is respectively removed to prepare at least 6 molybdenum solutions with different molybdenum concentrations in the volumetric flask.
Preferably, the concentration gradient of the molybdenum standard deviation solution is as follows: 2ug/mL, 4ug/mL, 8ug/mL, 10ug/mL, 20ug/mL, 50 ug/mL.
Preferably, the temperature of the first heating in the ultrasonic water bath instrument is 100 ℃, and the time is 5-10 min.
Preferably, the wavelength of the analytical line of molybdenum is 202.3 nm.
Preferably, the operating conditions of the inductively coupled plasma mass spectrometer are that the rinsing pump speed is 45-55r/min, the analysis pump speed is 45-55r/min, the high-frequency power is 1140-1160W, and the auxiliary gas flow is 0.45-0.55L/min.
The invention has the beneficial effects that: the method for quickly digesting and measuring molybdenum in molybdenum ore dressing materials adopts an acid dissolution method to digest a sample, the sample is dissolved in an ultrasonic water bath instrument, ultrasonic-assisted extraction utilizes cavitation of ultrasonic waves to accelerate leaching and extraction of components to be measured, the diffusion and release of the extracted components can be accelerated by the secondary effect of the ultrasonic waves, the leaching speed is accelerated, the sample treatment time and the sample treatment process are shortened, and errors caused by improper operation of personnel are reduced on the premise of ensuring the accuracy of results. Effective molybdenum elements are extracted by acid, the concentration of the molybdenum elements in the solution is rapidly and accurately determined by utilizing the powerful analysis and test capability of an inductively coupled plasma emission spectrometer, and then the content of the effective molybdenum in the material is calculated. The method has the advantages of short sample processing flow, simple operation and high accuracy.
Detailed Description
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
1.1 Main instruments and working parameters
ICAP6000 model inductively coupled plasma atomic emission spectrometer (Thermo corporation, USA), ultrasonic water bath instrument.
1.2 Primary reagents
Hydrochloric acid, superior purity; nitric acid, superior grade purity; hydrofluoric acid, super pure; perchloric acid, superior grade purity; 150g/L of sodium hydroxide.
1.3 preparation of Standard solution
1.3.1 molybdenum standard storage solution, weighing 0.1500g of spectrally pure molybdenum trioxide dried at 105-110 ℃ into a 250mL beaker, adding 50mL of 150g/L sodium hydroxide solution for dissolving, transferring into a 100mL volumetric flask, fixing the volume with water, storing in a plastic bottle, and sealing. The molybdenum solubility of this standard stock solution, 1mL, contained 1mg of molybdenum.
1.3.2 molybdenum standard solution A: and (3) transferring 10.00mL of molybdenum standard solution into a 100mL volumetric flask, adding 10mL of concentrated nitric acid, diluting to a scale, and uniformly mixing. 1mL of this solution contained 100ug of molybdenum, respectively.
1.3.3 molybdenum standard deviation solution: respectively transferring 2.00mL, 4.00mL and 8.00mL of molybdenum standard solution A (1.3.2) and 1.00mL, 2.00mL and 5.00mL of molybdenum standard storage solution (1.3.1), adding 10mL of concentrated nitric acid into six 100mL volumetric flasks to dilute to the scale, and mixing uniformly. The concentration of molybdenum in the standard deviation solution is shown in Table 1 Standard concentration
1.4 preparation of sample solutions
Accurately weighing a certain amount of sample in a polytetrafluoroethylene beaker, blowing water to moisten, adding 15ml of hydrochloric acid to dissolve, heating in an ultrasonic water bath instrument at 100 ℃ for 5-10min, adding 5ml of nitric acid to dissolve the sample continuously, adding 2ml of hydrofluoric acid after heating to dissolve the sample, removing silicon at low temperature to be nearly dry, adding 3ml of perchloric acid to remove residual fluorine, and taking down the sample to be slightly cold after perchloric acid smoke is exhausted. Washing the wall of the cup with a small amount of deionized water, adding 10mL of nitric acid, placing the cup in an ultrasonic water bath instrument to dissolve salts at low temperature, keeping the volume at 30-40 mL, cooling the sample after the sample is completely dissolved, putting the sample into a 100mL volumetric flask, and metering the volume with ultrapure water to be detected. And the content is determined according to the dilution of the sample. Molybdenum ions of the solution enter an atomization system of an inductively coupled plasma mass spectrometer in the form of aerosol, target elements are gasified, ionized and excited in a plasma torch to radiate characteristic spectral lines, the concentration of effective molybdenum in the solution is calculated according to the Lambert-beer law, and then the content of the effective molybdenum in the ore dressing raw ore and the intermediate material is calculated.
1.5 on-machine assay
1.5.1 wavelength of analysis line according to selection principle of spectral analysis spectral line, selecting spectral line with high sensitivity, less spectral interference or no interference as analysis spectral line of molybdenum. The wavelength of the analytical line of molybdenum is 202.3 nm.
1.5.2 standard and sample measurement the standard solution of range difference, the reagent blank solution without sample, the unknown sample solution are measured under the set condition, and the result is obtained after the instrument directly calculates according to the standard curve.
TABLE 2 operating conditions of ICP spectrometer
1.5.3 partial sample results are given below
| Sample class | Mo test result (ω/%) n is 11 |
| Sample 1 | 0.016 |
| Sample 2 | 0.055 |
| Sample 3 | 0.074 |
| Sample No. 4 | 5.33 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method suitable for quickly digesting and measuring molybdenum in molybdenum ore dressing materials is characterized by comprising the following steps: preparing a molybdenum standard grade difference solution; secondly, placing the weighed molybdenum ore dressing material sample in a polytetrafluoroethylene beaker, blowing water to moisten, adding hydrochloric acid to dissolve, heating in an ultrasonic water bath instrument, adding nitric acid to dissolve continuously, adding hydrofluoric acid after dissolving, removing silicon at low temperature till the sample is nearly dry, adding perchloric acid, taking down and cooling after perchloric acid smoke is exhausted; washing the wall of the cup with a small amount of deionized water, adding nitric acid, placing in an ultrasonic water bath instrument for dissolving salts at low temperature, cooling after the sample is completely dissolved, transferring to a volumetric flask, and performing constant volume with ultrapure water to be measured; and step three, measuring and calculating the content of effective molybdenum in the molybdenum ore dressing material by using an inductively coupled plasma mass spectrometer.
2. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 1, characterized in that: preparing a molybdenum standard storage solution before preparing the molybdenum standard difference solution, preparing the molybdenum standard solution, and diluting the molybdenum standard solution to obtain the molybdenum standard difference solution.
3. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 2, characterized in that: the preparation method of the molybdenum standard storage solution comprises the steps of weighing spectrally pure molybdenum trioxide dried at the temperature of 105-110 ℃ into a beaker, adding a sodium hydroxide solution for dissolving, fixing the volume in a volumetric flask by water, wherein 1mL of the standard storage solution contains 1mg of molybdenum.
4. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 3, wherein: and transferring the molybdenum standard solution into a volumetric flask, and adding concentrated nitric acid, wherein 1mL of the solution contains 100ug of molybdenum respectively.
5. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 4, wherein: respectively transferring the molybdenum standard storage solution or the molybdenum standard solution into a volumetric flask to prepare at least 6 molybdenum solutions with different molybdenum concentrations.
6. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 5, wherein: the concentration gradient of the molybdenum standard deviation solution is as follows: 2ug/mL, 4ug/mL, 8ug/mL, 10ug/mL, 20ug/mL, 50 ug/mL.
7. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 1, characterized in that: the temperature of the first heating in the ultrasonic water bath instrument is 100 ℃, and the time is 5-10 min.
8. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 1, characterized in that: the wavelength of the analytical line of molybdenum is 202.3 nm.
9. The method for rapidly digesting and measuring molybdenum in molybdenum beneficiation materials according to claim 1, characterized in that: the working conditions of the inductively coupled plasma mass spectrometer are that the flushing pump speed is 45-55r/min, the analysis pump speed is 45-55r/min, the high-frequency power is 1140-1160W, and the auxiliary gas flow is 0.45-0.55L/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114660051A (en) * | 2022-03-11 | 2022-06-24 | 西部矿业股份有限公司 | Method for determining rare precious trace metal rhenium in molybdenite concentrate |
| CN114910467A (en) * | 2022-04-28 | 2022-08-16 | 中国第一重型机械股份公司 | Metallurgical slag on-line monitoring and analyzing method and system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108241037A (en) * | 2016-12-23 | 2018-07-03 | 北京有色金属研究总院 | The rapid analysis method of molybdenum in a kind of molybdenum concntrate |
| RU2756458C1 (en) * | 2021-01-21 | 2021-09-30 | Федеральное государственное учреждение науки "Федеральный научный центр гигиены им. Ф.Ф. Эрисмана" Федеральной службы по надзору в сфере зашиты прав потребителей и благополучия человека | Method for determining mass concentrations of heavy metals in soil by the method for mass spectrometry with inductively coupled plasma |
-
2021
- 2021-11-22 CN CN202111383474.5A patent/CN114062104A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108241037A (en) * | 2016-12-23 | 2018-07-03 | 北京有色金属研究总院 | The rapid analysis method of molybdenum in a kind of molybdenum concntrate |
| RU2756458C1 (en) * | 2021-01-21 | 2021-09-30 | Федеральное государственное учреждение науки "Федеральный научный центр гигиены им. Ф.Ф. Эрисмана" Федеральной службы по надзору в сфере зашиты прав потребителей и благополучия человека | Method for determining mass concentrations of heavy metals in soil by the method for mass spectrometry with inductively coupled plasma |
Non-Patent Citations (6)
| Title |
|---|
| 吴勇;: "电感耦合等离子体质谱法测定铁矿石中铊含量", 世界有色金属, no. 07, 5 April 2020 (2020-04-05) * |
| 孙朝阳;贺颖婷;戴雪峰;蒋宗明;包成林;: "密闭酸溶-电感耦合等离子体原子发射光谱法测定钼矿中钼和铜", 理化检验(化学分册), no. 11, 18 November 2011 (2011-11-18), pages 1299 - 1301 * |
| 张旺强;王春妍;李瑞仙;巨力佩;陈月源;余志峰;毛振才;: "电感耦合等离子体发射光谱法测定富镁铁橄榄岩类矿石中铜镍铁和氧化镁", 岩矿测试, no. 02, 15 April 2011 (2011-04-15) * |
| 薛静;: "极谱法测定钼矿石中的总钼氧化钼硫化钼", 岩矿测试, no. 06, 15 December 2012 (2012-12-15) * |
| 谈建安;余志峰;王建波;: "电感耦合等离子体发射光谱法测定多金属矿石中的钼", 岩矿测试, no. 04, 15 August 2011 (2011-08-15) * |
| 黄光明;薛蒙伟;韩鹏飞;闫鲜;: "密闭消解ICP-AES测定钨矿石和钼矿石中的9种组分", 光谱实验室, no. 02, 25 March 2013 (2013-03-25) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114660051A (en) * | 2022-03-11 | 2022-06-24 | 西部矿业股份有限公司 | Method for determining rare precious trace metal rhenium in molybdenite concentrate |
| CN114910467A (en) * | 2022-04-28 | 2022-08-16 | 中国第一重型机械股份公司 | Metallurgical slag on-line monitoring and analyzing method and system |
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