CN111964990A - Method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag - Google Patents
Method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag Download PDFInfo
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- CN111964990A CN111964990A CN202010769993.4A CN202010769993A CN111964990A CN 111964990 A CN111964990 A CN 111964990A CN 202010769993 A CN202010769993 A CN 202010769993A CN 111964990 A CN111964990 A CN 111964990A
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- 239000011669 selenium Substances 0.000 title claims abstract description 42
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 40
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 38
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000002893 slag Substances 0.000 title claims abstract description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 13
- 239000010949 copper Substances 0.000 title claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 10
- 239000002184 metal Substances 0.000 title claims abstract description 10
- 239000002910 solid waste Substances 0.000 title claims abstract description 8
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000005485 electric heating Methods 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 5
- 238000004993 emission spectroscopy Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 7
- 238000009736 wetting Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 16
- 238000004458 analytical method Methods 0.000 abstract description 15
- 238000001514 detection method Methods 0.000 abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 5
- 238000009835 boiling Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 50
- 230000003595 spectral effect Effects 0.000 description 10
- 239000012086 standard solution Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000013582 standard series solution Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical class N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011978 dissolution method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Classifications
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- 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
-
- 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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems 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
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Engineering & Computer Science (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag, which comprises the steps of weighing a metallurgical slag sample, adding water to wet the sample, then adding aqua regia solution to dissolve the sample, placing the sample on an electric heating plate to carry out low-temperature heating reaction, washing the wall of a triangular beaker with distilled water, adding aqua regia solution, placing the triangular beaker on the electric heating plate to be heated to micro-boiling at low temperature, taking down and cooling to room temperature; and analyzing and measuring the contents of selenium and tellurium in the solution by adopting an inductively coupled plasma emission spectrometry. The invention explores the aqua regia solution dissolving sample prepared by concentrated hydrochloric acid and concentrated nitric acid, continuously determines the contents of selenium and tellurium in metallurgical slag by ICP-AES in aqua regia medium, and performs the method precision and accuracy tests under the determination condition. The sample can be guaranteed to be representative, and the accuracy of selenium and tellurium analysis results is improved; the method has the advantages of simple operation, low detection limit, small matrix effect, wide linear range, accuracy, reliability and the like.
Description
Technical Field
The invention belongs to a metallurgical analysis technology, and particularly relates to a method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag.
Background
Along with the improvement of living standard, waste residues with various metals and harmful elements coexisting are generated in the fields of urban mines and non-ferrous metal renewable resources and in the industrial metallurgy process, and the waste residues are various in types and complex in components. How to determine the content of the rare dispersion elements such as selenium, tellurium and the like in the metallurgical waste residues is an important link for determining the metallurgical process and the method, so that the establishment of an accurate, simple and rapid analysis method for determining selenium and tellurium has practical guiding significance.
At present, the determination of selenium and tellurium usually adopts an extraction separation spectrophotometry method, an atomic fluorescence spectrometry method and an ICP-AES method. Although the extraction separation spectrophotometry is accurate and reliable, the method uses more reagents, is complex in operation, time-consuming and labor-consuming, and cannot simultaneously measure multiple elements; the atomic fluorescence spectrometry has limitation on samples, and because the content of impurity metal ions in metallurgical slag is too high and too complex, the metallurgical slag is reduced into a solid state by potassium borohydride, a sample inlet pipe is blocked, the analysis and measurement results are influenced, and instrument failure is easily caused; the ICP-AES method has the advantages of high sensitivity, low detection limit, less interference and wide linear range.
Disclosure of Invention
The invention aims to solve the defects of large reagent dosage, complicated operation, low speed and easy instrument blockage of the existing method, and establishes an accurate, simple and rapid analysis method for determining the selenium/tellurium content in the complex copper-based multi-metal solid waste metallurgical slag.
In order to achieve the purpose, the invention adopts the following technical scheme. A method for analyzing the content of selenium/tellurium in complex copper-based multi-metal solid waste metallurgical slag comprises the following steps:
1) weighing 0.2-0.3 g of a metallurgical slag sample, accurately weighing the metallurgical slag sample to 0.0001g, and placing the metallurgical slag sample in a 250mL triangular beaker;
2) adding 1-5 mL of water to the sample for wetting, then adding 20-30 mL of aqua regia solution to dissolve the sample, placing the sample on an electric heating plate for heating reaction at a low temperature of 75-100 ℃, evaporating the volume to 1-2 mL, and taking down a triangular beaker;
3) washing the wall of the triangular beaker with distilled water, adding 10-15 mL of aqua regia solution, placing the triangular beaker on an electric heating plate, heating the triangular beaker at a low temperature until the triangular beaker is slightly boiled, taking down the triangular beaker, and cooling the triangular beaker to room temperature;
4) transferring the cooled solution into a 100mL volumetric flask, diluting to 100mL scale marks by using distilled water, uniformly mixing, and standing or dry filtering;
5) and analyzing and measuring the contents of selenium and tellurium in the uniformly mixed solution by adopting an inductively coupled plasma emission spectrometry.
The invention explores the aqua regia solution dissolving sample prepared by concentrated hydrochloric acid and concentrated nitric acid through the sample treatment test, the determination medium test, the influence test of matrix and coexisting elements on the determination, the linear test of working curve and the like, uses ICP-AES to continuously determine the contents of selenium and tellurium in metallurgical slag in the aqua regia medium, and performs the method precision and accuracy test under the determination condition. The sample can be guaranteed to be representative, and the accuracy of selenium and tellurium analysis results is improved; the method has the advantages of simple operation, low detection limit, small matrix effect, wide linear range, accuracy, reliability and the like.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and is not to be construed as limiting the invention.
A method for analyzing the content of selenium/tellurium in complex copper-based multi-metal solid waste metallurgical slag comprises the following steps:
1) accurately weighing a metallurgical slag sample in a 250mL triangular beaker, and accurately measuring the metallurgical slag sample to 0.0001 g; the sample weighing amount of the metallurgical slag sample can be selected from 0.2-0.3 g, so that the uniformity of the sample can be ensured, and the accuracy of selenium and tellurium analysis results can be improved.
2) Adding water to the metallurgical slag sample for wetting, then adding aqua regia solution to dissolve the sample, placing the sample on an electric heating plate for heating reaction at low temperature, steaming the sample to a small volume, and taking down the triangular beaker; the dosage of the aqua regia is 20-30 mL. This makes it possible to sufficiently dissolve the sample.
3) Washing the wall of the triangular beaker with distilled water, adding aqua regia solution, heating on an electric heating plate at low temperature to slightly boil, taking down and cooling; the dosage of the aqua regia is 10-15 mL, so that salts can be fully dissolved, and higher precision and accuracy can be obtained.
4) And transferring the cooled solution into a 100mL volumetric flask, diluting the solution to a scale with distilled water, uniformly mixing, and standing or dry filtering.
5) And analyzing and measuring the contents of selenium and tellurium in the uniformly mixed solution by adopting an inductively coupled plasma emission spectrometry.
Therefore, the invention explores aqua regia solution dissolving samples prepared by concentrated hydrochloric acid and concentrated nitric acid through sample treatment tests, medium test, matrix and coexisting element influence tests, working curve linear tests and the like, continuously measures the contents of selenium and tellurium in metallurgical slag by ICP-AES in aqua regia medium, and performs method precision and accuracy tests under the measuring conditions.
The specific embodiment of the invention is described in detail below, and in order to quickly and accurately measure the selenium and tellurium content in the metallurgical slag, a sample dissolving method of aqua regia dissolving samples is selected, and the analysis results of selenium and tellurium obtained by measurement are relatively ideal.
Example (b): the specific method of the invention is as follows:
1. preparation of assay solutions:
accurately weighing 0.2-0.3 g of sample (accurate to 0.0001 g) and placing the sample in a 250mL triangular beaker (carrying out a blank test along with the sample), wetting the sample with water, adding 20-30 mL of aqua regia to cover a watch glass, completely dissolving the sample at low temperature, taking down the sample when the sample is steamed to a small volume, slightly cooling the watch glass and the wall of the beaker, slightly boiling the sample to dissolve salts, taking down the sample, cooling the sample, adding 10-15 mL of aqua regia, transferring the sample to a 100mL volumetric flask, diluting the sample to a scale with water, uniformly mixing the sample and measuring the sample under the working condition of a selected instrument.
2. Preparing a working standard solution:
standard solutions of selenium and tellurium single elements: selenium standard solution rho (Se) =1000 mug/mL; tellurium standard solution rho (Te) =1000 mu g/mL;
mix standard series solutions: respectively transferring 0mL, 0.25mL, 0.5mL, 1mL, 2mL and 5mL selenium standard solutions rho (Se) =1000 mu g/mL; placing the tellurium standard solution rho (Te) =1000 mu g/mL into a group of 250mL volumetric flasks, adding 25mL aqua regia, diluting to the scale with deionized water, and mixing uniformly.
3. And (3) determination:
and (3) simultaneously measuring the contents of selenium and tellurium by using the inductively coupled plasma spectrometry by using the analysis test solution and the standard series solution under the selected instrument working condition.
4. The influence of different factors on the assay results was investigated:
4.1 selection of analytical lines:
in order to systematically research the influence of coexisting elements in the sludge on the determination of selenium and tellurium, three spectral lines with stronger intensity are selected according to spectral line interference and spectral line intensity information of the elements to be determined, which are given by an instrument spectral line library. The spectral profile image displayed on the screen was observed by scanning each single-element standard solution, mixed standard solution, and sample solution in order at the analysis line of each selected element. By comparing the sensitivity and spectral interference of each spectral line of the measured elements, the spectral lines with small interference, low background and high signal-to-noise ratio are finally determined as analysis spectral lines, and the results are shown in table 1.
TABLE 1 elemental analysis lines
| Element(s) | Selenium | Tellurium |
| Analysis line/nm | 203.985 | 225.902 |
4.2 detection limit test of method:
under the selected analysis spectral line and instrument working conditions, a calibration curve is established by using a Se and Te mixed standard series solution, 11 times of reagent blank solutions are continuously measured, the detection limit is calculated by a method of 3 times of standard deviation, and the result is shown in Table 2.
TABLE 2 detection limits of selenium and tellurium elements
| Element(s) | Selenium | Tellurium |
| Detection limit (μ g/mL) | 0.06 | 0.119 |
4.3 sample dissolution method comparative test:
2 metallurgical slag samples are selected, and the comparative test is carried out by the following two sample dissolving methods:
a sample dissolving method: wetting a sample with water, adding 0.25-0.50 mL of saturated ammonium bifluoride solution, adding 20-30 mL of aqua regia and 5-10 mL of tartaric acid solution, covering a watch glass, dissolving at low temperature to a small volume, boiling with water, adding 10-15 mL of aqua regia to a constant volume, uniformly mixing, and measuring.
B, sample dissolving method: wetting a sample with water, adding 20-30 mL of aqua regia to dissolve at low temperature to a small volume, boiling with water, adding 10-15 mL of aqua regia to a constant volume, uniformly mixing, and measuring.
The results obtained for both sample dissolution methods are shown in table 3.
The table data shows that: A. the results of selenium and tellurium measurement by the two sample dissolving methods B are approximate, but in the method A, an ammonium bifluoride solution and a tartaric acid solution are added for sample dissolving, so that glassware is corroded, the analysis cost is increased, and therefore, the sample dissolving method B is selected.
4.4 influence of aqua regia dosage on assay results:
the influence of the amount of aqua regia on the measurement results was investigated according to the experimental method and the results are shown in Table 4.
The data in table 4 show that: the selenium and tellurium results are better when the concentration (volume fraction) of 10 percent aqua regia is measured, so the concentration (volume fraction) of the aqua regia is 10 percent.
4.5 influence of copper and lead elements on the measurement results:
according to the experimental method, the influence of different contents of copper and lead on the measurement result (the copper content of the sample is 20%, and the lead content is 26%) is studied, and the result is shown in table 5.
The data in table 5 show that: the content of copper and lead in the sample does not obviously interfere with the measuring result, so that the copper and lead do not need to be separated when the Se and Te in the sample are measured.
5. And (3) verifying the reliability and feasibility of the method:
5.1 precision of method:
0.2000 g-0.3000 g of 1# and 2# metallurgical slag is accurately weighed, and the measurement is repeated for 7 times according to the test method, and the results are shown in Table 6.
The data in Table 6 show that the relative standard deviation of selenium measured by the method is 1.40-1.67%, and the relative standard deviation of tellurium measured by the method is 1.82-2.44%, which shows that the method has good stability.
5.2 accuracy test of method:
accurately weighing 0.2000 g-0.3000 g of metallurgical slag of No. 1 and No. 2, adding standard solutions of Se and Te with different contents, and carrying out experiments according to experimental methods, wherein the results are shown in Table 7.
The data in Table 7 show that the recovery rate of the sample after the standard selenium is added is 99.4-107.7, and the recovery rate after the standard selenium is added is 95.0-104.0%, so that the method is proved to meet the analysis and detection requirements of selenium and tellurium.
Claims (1)
1. A method for analyzing the content of selenium/tellurium in complex copper-based multi-metal solid waste metallurgical slag is characterized by comprising the following steps:
1) weighing 0.2-0.3 g of a metallurgical slag sample, accurately weighing the metallurgical slag sample to 0.0001g, and placing the metallurgical slag sample in a 250mL triangular beaker;
2) adding 1-5 mL of water to the sample for wetting, then adding 20-30 mL of aqua regia solution to dissolve the sample, placing the sample on an electric heating plate for heating reaction at a low temperature of 75-100 ℃, evaporating the volume to 1-2 mL, and taking down a triangular beaker;
3) washing the wall of the triangular beaker with distilled water, adding 10-15 mL of aqua regia solution, placing the triangular beaker on an electric heating plate, heating the triangular beaker at a low temperature until the triangular beaker is slightly boiled, taking down the triangular beaker, and cooling the triangular beaker to room temperature;
4) transferring the cooled solution into a 100mL volumetric flask, diluting to 100mL scale marks by using distilled water, uniformly mixing, and standing or dry filtering;
5) and analyzing and measuring the contents of selenium and tellurium in the uniformly mixed solution by adopting an inductively coupled plasma emission spectrometry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010769993.4A CN111964990A (en) | 2020-08-04 | 2020-08-04 | Method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag |
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| CN202010769993.4A CN111964990A (en) | 2020-08-04 | 2020-08-04 | Method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag |
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| CN202010769993.4A Pending CN111964990A (en) | 2020-08-04 | 2020-08-04 | Method for analyzing selenium/tellurium content in complex copper-based multi-metal solid waste metallurgical slag |
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| CN (1) | CN111964990A (en) |
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- 2020-08-04 CN CN202010769993.4A patent/CN111964990A/en active Pending
Non-Patent Citations (6)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《GB/T 23607-2009 铜阳极泥化学分析方法 砷、铋、铁、镍、铅、锑、硒、碲量的测定 电感耦合等离子体原子发射光谱法》" * |
| 卞大勇: "ICP-AES测定纯铜中的硒、碲", 《天津化工》 * |
| 周万峰等: "ICP-OES快速测定高纯度金饰品中金含量――差减法", 《贵州地质》 * |
| 杨开放等: "电感耦合等离子体发射光谱(ICP-OES)法在非金属元素测定中的应用", 《中国无机分析化学》 * |
| 熊晓燕等: "纯硒中杂质元素的ICP-AES测定", 《光谱实验室》 * |
| 马丽君: "电感耦合等离子体原子发射光谱法(ICP-AES)测定贵金属车间外排水中的铜、硒、碲", 《中国无机分析化学》 * |
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