CN116046739A - Method for determining germanium content in mineral product - Google Patents
Method for determining germanium content in mineral product Download PDFInfo
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- CN116046739A CN116046739A CN202310047244.4A CN202310047244A CN116046739A CN 116046739 A CN116046739 A CN 116046739A CN 202310047244 A CN202310047244 A CN 202310047244A CN 116046739 A CN116046739 A CN 116046739A
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- germanium
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- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 35
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 30
- 239000011707 mineral Substances 0.000 title claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 claims abstract description 31
- 239000010949 copper Substances 0.000 claims abstract description 31
- 239000000779 smoke Substances 0.000 claims abstract description 17
- 239000012488 sample solution Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000004321 preservation Methods 0.000 claims abstract description 12
- 239000000523 sample Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 6
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims abstract description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 150000004678 hydrides Chemical class 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000005070 sampling Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
-
- 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
- G01N1/286—Preparing 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
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
-
- 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
- G01N1/286—Preparing 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
- G01N2001/2866—Grinding or homogeneising
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Life Sciences & Earth Sciences (AREA)
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- Immunology (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for measuring germanium content in mineral products, which relates to the field of germanium content measurement and comprises the following specific steps: step 1: heating 30g of copper ore in a drying oven for drying, and grinding the dried copper ore by a vibration grinder; step 2: taking 2-5g copper ore sample in a 400ml beaker, adding 20-30ml nitrohydrochloric acid, heating to 200-300 ℃ for heat preservation, generating yellow smoke in the heat preservation process, stopping heating when the yellow smoke disappears, and obtaining mineral sample solution; the method has the advantages of avoiding the processes of separating and extracting germanium by chemical means, reducing experimental procedures and experimental links introducing errors, improving the sampling efficiency and the instrument test precision and accuracy, effectively measuring the germanium content in copper ores, and having higher accuracy and precision of analysis results.
Description
Technical Field
The invention relates to the field of germanium content measurement, in particular to a method for measuring the germanium content in a mineral product.
Background
Germanium is a rare element and is widely distributed in nature. Copper ores, iron ores, sulphide ores, rock soil and spring water all contain trace germanium, and high-purity germanium is a good semiconductor material and is widely applied to the fields of physics and electronics; meanwhile, the positive effect of germanium on metabolism, cancer prevention and tumor cure is an important subject in the clinical medicine field research.
The existing method for measuring germanium element in copper concentrate is very expensive by means of wavelength dispersion X-ray fluorescence spectrometer according to national standard, and the wavelength dispersion X-ray fluorescence spectrometer conforming to the analysis method of national metallurgical products, so that the cost for measuring the germanium element content in copper concentrate by copper smelting units according to the X-ray fluorescence spectrometry specified by the national quality inspection administration is higher, and the method is not beneficial to being applied in copper production units.
Disclosure of Invention
The invention aims at: in order to solve the problem of high cost for measuring the content of germanium element in copper concentrate, a method for measuring the content of germanium in a mineral product is provided.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for determining the germanium content of a mineral product, comprising the steps of:
step 1: heating 30g of copper ore in a drying oven for drying, and grinding the dried copper ore by a vibration grinder;
step 2: taking 2-5g copper ore sample in a 400ml beaker, adding 20-30ml nitrohydrochloric acid, heating to 200-300 ℃ for heat preservation, generating yellow smoke in the heat preservation process, and stopping heating when the yellow smoke disappears to obtain mineral sample solution;
step 3: adding 10-25ml of mixed acid into the mineral sample solution, placing the beaker on an electric hot plate, heating to 300-350 ℃, stopping heating and cooling to room temperature when the space above the mineral sample solution in the beaker is filled with white smoke;
step 4: flushing the tank wall with water, adding water to 100mL, hot-dipping on an electric hot plate, slightly boiling for 10min, stopping heating and cooling to room temperature, adding 5mL of absolute ethyl alcohol, and standing for 1h;
filtering with slow quantitative filter paper, removing solid impurities by filtering, placing the filtrate in a 400mL volumetric flask, adding water to fix the volume, and standing for more than 10 hours;
step 6: absorbing the supernatant with the volume of 10-20mL in a volumetric flask, placing the supernatant in a 50mL colorimetric tube, adding an anti-interference agent, regulating acidity, keeping the volume fraction of the acid concentration to be 10-20%, generating hydride by adopting an atomic fluorescence spectrophotometer under the conditions of current carrying and reducing agent, measuring the corresponding fluorescence intensity, and obtaining the content of germanium by a working curve method.
Preferably, the mixed acid in the step 3 comprises nitric acid, perchloric acid and hydrofluoric acid, and the preparation method comprises the step of mixing the nitric acid, the perchloric acid and the hydrofluoric acid in a ratio of 5:4:1.
Preferably, the anti-interference agent in the step 6 is AR-level thiourea with the concentration of 100g/L, and the adding amount is 3-5ml.
Preferably, the acidity adjustment in step 6 is performed by using a nitric acid solution with a mass percentage of 69% or more.
Preferably, the current carrying in the step 6 is a 10-20% nitric acid solution, and the reducing agent is a mixed solution consisting of 20g/L potassium borohydride and 5g/L potassium hydroxide.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, an absorbance curve is obtained in an atomic absorption spectrometer, the germanium content in a copper concentrate sample is obtained according to the data difference corresponding to the absorbance curve, and the equipment adopted in the test is cheaper, so that the cost of detecting the germanium content is lower, and the method is beneficial to popularization and application in copper production units;
2. the AR-level thiourea is adopted as the anti-interference agent, so that interference is eliminated, and the absolute error of a sample is small; the method can effectively measure the germanium content in the copper ore, has higher accuracy and precision of analysis results, is used for measuring the germanium content in copper ore or copper concentrate for a long time in our company, and has higher repeatability and reproducibility.
Detailed Description
Embodiment one:
a method for determining the germanium content of a mineral product, comprising the steps of:
step 1: heating 30g of copper ore in a drying oven for drying, and grinding the dried copper ore by a vibration grinder;
step 2: taking 2g of copper ore sample in a 400ml beaker, adding 20ml of nitrohydrochloric acid, heating to 200 ℃ for heat preservation, generating yellow smoke in the heat preservation process, and stopping heating when the yellow smoke disappears to obtain a mineral sample solution;
step 3: adding 10ml of mixed acid into the mineral sample solution, placing the beaker on an electric hot plate, heating to 300 ℃, stopping heating and cooling to room temperature when the space above the mineral sample solution in the beaker is filled with white smoke;
step 4: flushing the tank wall with water, adding water to 100mL, hot-dipping on an electric hot plate, slightly boiling for 10min, stopping heating and cooling to room temperature, adding 5mL of absolute ethyl alcohol, and standing for 1h;
filtering with slow quantitative filter paper, removing solid impurities by filtering, placing the filtrate in a 400mL volumetric flask, adding water to fix the volume, and standing for more than 10 hours;
step 6: absorbing the supernatant with the volume of 10mL in a volumetric flask, placing the supernatant in a 50mL colorimetric tube, adding an anti-interference agent, regulating acidity, keeping the volume fraction of the acid concentration to be 10%, generating hydride by adopting an atomic fluorescence photometer under the conditions of current carrying and reducing agent, measuring the corresponding fluorescence intensity, and obtaining the content of germanium by a working curve method.
In the invention, the mixed acid in the step 3 comprises nitric acid, perchloric acid and hydrofluoric acid, and the preparation method comprises the step of mixing the nitric acid, the perchloric acid and the hydrofluoric acid in a ratio of 5:4:1.
In the invention, the anti-interference agent in the step 6 is AR-level thiourea with the concentration of 100g/L, and the adding amount is 3-5ml.
In the invention, the acidity is regulated in the step 6 by adopting nitric acid solution with the mass percent of more than 69%.
In the invention, the current carrying in the step 6 is a 10-20% nitric acid solution, and the reducing agent is a mixed solution consisting of 20g/L potassium borohydride and 5g/L potassium hydroxide.
Embodiment two:
a method for determining the germanium content of a mineral product, comprising the steps of:
step 1: heating 30g of copper ore in a drying oven for drying, and grinding the dried copper ore by a vibration grinder;
step 2: taking 3g of copper ore sample in a 400ml beaker, adding 25ml of nitrohydrochloric acid, heating to 250 ℃ for heat preservation, generating yellow smoke in the heat preservation process, and stopping heating when the yellow smoke disappears to obtain a mineral sample solution;
step 3: adding 18ml of mixed acid into the mineral sample solution, placing the beaker on an electric hot plate, heating to 320 ℃, stopping heating and cooling to room temperature when the space above the mineral sample solution in the beaker is filled with white smoke;
step 4: flushing the tank wall with water, adding water to 100mL, hot-dipping on an electric hot plate, slightly boiling for 10min, stopping heating and cooling to room temperature, adding 5mL of absolute ethyl alcohol, and standing for 1h;
filtering with slow quantitative filter paper, removing solid impurities by filtering, placing the filtrate in a 400mL volumetric flask, adding water to fix the volume, and standing for more than 10 hours;
step 6: absorbing the supernatant with the volume of 10-20mL in a volumetric flask, placing the supernatant in a 50mL colorimetric tube, adding an anti-interference agent, regulating acidity, keeping the volume fraction of the acid concentration to be 10-20%, generating hydride by adopting an atomic fluorescence spectrophotometer under the conditions of current carrying and reducing agent, measuring the corresponding fluorescence intensity, and obtaining the content of germanium by a working curve method.
In the invention, the mixed acid in the step 3 comprises nitric acid, perchloric acid and hydrofluoric acid, and the preparation method comprises the step of mixing the nitric acid, the perchloric acid and the hydrofluoric acid in a ratio of 5:4:1.
In the invention, the anti-interference agent in the step 6 is AR-level thiourea with the concentration of 100g/L, and the adding amount is 3-5ml.
In the invention, the acidity is regulated in the step 6 by adopting nitric acid solution with the mass percent of more than 69%.
In the invention, the current carrying in the step 6 is 15% nitric acid solution, and the reducing agent is a mixed solution consisting of 20g/L potassium borohydride and 5g/L potassium hydroxide.
Embodiment III:
a method for determining the germanium content of a mineral product, comprising the steps of:
step 1: heating 30g of copper ore in a drying oven for drying, and grinding the dried copper ore by a vibration grinder;
step 2: taking 5g copper ore sample in a 400ml beaker, adding 30ml nitrohydrochloric acid, heating to 300 ℃ for heat preservation, generating yellow smoke in the heat preservation process, and stopping heating when the yellow smoke disappears to obtain mineral sample solution;
step 3: adding 25ml of mixed acid into the mineral sample solution, placing the beaker on an electric hot plate, heating to 350 ℃, stopping heating and cooling to room temperature when the space above the mineral sample solution in the beaker is filled with white smoke;
step 4: flushing the tank wall with water, adding water to 100mL, hot-dipping on an electric hot plate, slightly boiling for 10min, stopping heating and cooling to room temperature, adding 5mL of absolute ethyl alcohol, and standing for 1h;
filtering with slow quantitative filter paper, removing solid impurities by filtering, placing the filtrate in a 400mL volumetric flask, adding water to fix the volume, and standing for more than 10 hours;
step 6: absorbing the supernatant with the volume of 10-20mL of the volumetric flask, placing the supernatant into a 50mL colorimetric tube, adding an anti-interference agent, regulating acidity, keeping the volume fraction of the acid concentration to be 20%, generating hydride by adopting an atomic fluorescence photometer under the conditions of current carrying and reducing agent, measuring the corresponding fluorescence intensity, and obtaining the content of germanium by a working curve method.
In the invention, the mixed acid in the step 3 comprises nitric acid, perchloric acid and hydrofluoric acid, and the preparation method comprises the step of mixing the nitric acid, the perchloric acid and the hydrofluoric acid in a ratio of 5:4:1.
In the invention, the anti-interference agent in the step 6 is AR-level thiourea with the concentration of 100g/L, and the adding amount is 3-5ml.
In the invention, the acidity is regulated in the step 6 by adopting nitric acid solution with the mass percent of more than 69%.
In the invention, the current carrying in the step 6 is a 20% nitric acid solution, and the reducing agent is a mixed solution consisting of 20g/L potassium borohydride and 5g/L potassium hydroxide.
Table 1 shows the results of the experimental determination of the germanium content in copper ores
TABLE 1
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (5)
1. A method for determining the germanium content of a mineral product, comprising the steps of:
step 1: heating 30g of copper ore in a drying oven for drying, and grinding the dried copper ore by a vibration grinder;
step 2: taking 2-5g copper ore sample in a 400ml beaker, adding 20-30ml nitrohydrochloric acid, heating to 200-300 ℃ for heat preservation, generating yellow smoke in the heat preservation process, and stopping heating when the yellow smoke disappears to obtain mineral sample solution;
step 3: adding 10-25ml of mixed acid into the mineral sample solution, placing the beaker on an electric hot plate, heating to 300-350 ℃, stopping heating and cooling to room temperature when the space above the mineral sample solution in the beaker is filled with white smoke;
step 4: flushing the tank wall with water, adding water to 100mL, hot-dipping on an electric hot plate, slightly boiling for 10min, stopping heating and cooling to room temperature, adding 5mL of absolute ethyl alcohol, and standing for 1h;
filtering with slow quantitative filter paper, removing solid impurities by filtering, placing the filtrate in a 400mL volumetric flask, adding water to fix the volume, and standing for more than 10 hours;
step 6: absorbing the supernatant with the volume of 10-20mL in a volumetric flask, placing the supernatant in a 50mL colorimetric tube, adding an anti-interference agent, regulating acidity, keeping the volume fraction of the acid concentration to be 10-20%, generating hydride by adopting an atomic fluorescence spectrophotometer under the conditions of current carrying and reducing agent, measuring the corresponding fluorescence intensity, and obtaining the content of germanium by a working curve method.
2. A method of determining the germanium content of a mineral product according to claim 1, wherein: the mixed acid in the step 3 comprises nitric acid, perchloric acid and hydrofluoric acid, and the preparation method comprises the step of mixing the nitric acid, the perchloric acid and the hydrofluoric acid in a ratio of 5:4:1.
3. A method of determining the germanium content of a mineral product according to claim 1, wherein: the anti-interference agent in the step 6 is AR-level thiourea with the concentration of 100g/L, and the adding amount is 3-5ml.
4. A method of determining the germanium content of a mineral product according to claim 1, wherein: and in the step 6, the acidity is regulated by adopting nitric acid solution with the mass percent of more than 69%.
5. A method of determining the germanium content of a mineral product according to claim 1, wherein: the current carrying in the step 6 is a 10-20% nitric acid solution, and the reducing agent is a mixed solution consisting of 20g/L potassium borohydride and 5g/L potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310047244.4A CN116046739A (en) | 2023-01-31 | 2023-01-31 | Method for determining germanium content in mineral product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310047244.4A CN116046739A (en) | 2023-01-31 | 2023-01-31 | Method for determining germanium content in mineral product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116046739A true CN116046739A (en) | 2023-05-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310047244.4A Withdrawn CN116046739A (en) | 2023-01-31 | 2023-01-31 | Method for determining germanium content in mineral product |
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| Country | Link |
|---|---|
| CN (1) | CN116046739A (en) |
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2023
- 2023-01-31 CN CN202310047244.4A patent/CN116046739A/en not_active Withdrawn
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