CN102735516A - Method for measuring content of gallium in vanadium slag - Google Patents
Method for measuring content of gallium in vanadium slag Download PDFInfo
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- CN102735516A CN102735516A CN2012102552939A CN201210255293A CN102735516A CN 102735516 A CN102735516 A CN 102735516A CN 2012102552939 A CN2012102552939 A CN 2012102552939A CN 201210255293 A CN201210255293 A CN 201210255293A CN 102735516 A CN102735516 A CN 102735516A
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Abstract
The invention provides a method for measuring the content of gallium in vanadium extracted waste slag and vanadium slag. The method comprises the following steps adding hydrochloric acid, nitric acid and hydrofluoric acid to a sample to dissolve the sample; adding perchloric acid and diluted hydrochloric acid to dissolve the obtained sample solution to obtain a sample solution to be measured; measuring the spectral line intensity of the sample solution to be measured by adopting a conventional inductively coupled plasma atomic emission spectroscopy method; and obtaining a corresponding gallium content value in a standard working curve of the gallium according to the spectral line intensity. The method has the advantages of convenience in operation, high accuracy of the measured gallium content and good stability, reproducibility and accuracy of a measured result, so the requirement on measuring the content of the gallium in the vanadium extracted waste slag and the vanadium slag is met.
Description
Technical field
The present invention relates to a kind of assay method of gallium content, especially gallium content in vanadium extraction waste and the vanadium slag is carried out method for measuring, belong to the analysis and testing technology field.
Background technology
The mensuration of gallium content in vanadium extraction waste and the vanadium slag does not also have the national standard analytical approach at present, and the mensuration of gallium content is to adopt AAS in other samples such as the aluminium alloy; Not only operate loaded down with trivial detailsly, analyze, measure long flow path, efficient is low; But also to consume a large amount of chemical reagent; Both contaminated environment endangered health of operators again, and increased cost.The employing ICP-AES is measured; Though just can measure after the sample dissolution gallium element, time saving and energy saving, and need not consume a large amount of chemical reagent; Can reduce pollution to environment; The protection health of operators, but big because of measuring difficulty, and be difficult to apply.Therefore, also there is not efficient ways accurately to measure at present to gallium content in vanadium extraction waste and the vanadium slag.
Summary of the invention
The object of the present invention is to provide a kind of method that can accurately measure gallium content in vanadium extraction waste and the vanadium slag.
The present invention realizes through following technical scheme: the assay method of gallium content in a kind of vanadium extraction waste and the vanadium slag; Comprise line strength of measuring test liquid with conventional ICP-AES; In the standard working curve of gallium, obtain corresponding gallium content value according to this line strength, it is characterized in that test liquid makes through the following step:
A, the amount of pressing 10～12mL/g sample add nitric acid in vanadium extraction waste and vanadium slag sample, and press the amount of 30～36mL/g sample; In vanadium extraction waste and vanadium slag sample, add hydrochloric acid; By the amount of 2～4mL/g sample, in vanadium extraction waste and vanadium slag sample, add hydrofluorite, under 100～120 ℃ of temperature again; Heating for dissolving, the lysate of 4～5mL/g sample;
B, in the lysate of steps A; Amount by 2.5～3.5mL/mL lysate adds nitric acid; And adding hydrochloric acid by the amount of 7.5～10.5mL/mL lysate, the amount by 0.5～1.5mL/mL lysate adds hydrofluorite again, again under 100～120 ℃ of temperature; Heating for dissolving, the lysate of 4～5mL/g sample;
C, in the lysate of step B, add perchloric acid by the amount of 2.5～3.5mL/mL lysate, under 300～350 ℃, be heated to perchloric acid and smolder when bottleneck, continue heating 5～10min, cooling, lysate;
D, in step C gained lysate, add watery hydrochloric acid by the amount of 10～15mL/mL lysate, this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is heated to 100～150 ℃, is cooled to room temperature, and being diluted with water to concentration is 0.01g/mL, shakes up, and gets sample to be tested liquid.
The nitric acid of said steps A, hydrochloric acid and hydrofluorite are commercial analysis net product.
The nitric acid of said step B, hydrochloric acid and hydrofluorite are commercial analysis net product.
The perchloric acid of said step C is commercial analysis net product.
The present invention compared with prior art has advantage and effect: after adopting such scheme to process sample to be tested liquid; It is available ICP-AES of the prior art; Directly measure gallium content in vanadium extraction waste and the vanadium slag; Not only easy to operate, and the gallium content accuracy rate of measuring is high, and it measures the result has good stable property, reappearance and accuracy.The inventive method is reliable, practical, quick, can satisfy the needs of gallium content in daily mensuration vanadium extraction waste and the vanadium slag fully.
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe.
Embodiment 1
Prepare the gallium standard solution by routine:
1, the preparation of gallium standard solution:
1A, the amount of pressing the 30mL/g sample add watery hydrochloric acid in commercial 1.0000g gallium, this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 drips 10～15 pure nitric acid of commercial analysis again, in water-bath, is heated to the gallium dissolving, is cooled to room temperature, is diluted with water to the Gallium solution of 1mg/mL, gets the gallium standard solution;
Gallium standard solution 50.00 mL of 1B, removing step 1A are diluted with water to scale in 500 mL volumetric flasks, shake up, and per 1 mL of this solution contains 50 μ g galliums;
2, the preparation of iron standard solution:
2A, the amount of pressing 60mL/g high purity iron are put into 75mL watery hydrochloric acid with commercial 1.2500g pure iron, and this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is heated to the pure iron dissolving under 100 ℃ of temperature, drip 10 pure nitric acid oxidations of commercially available analysis; Under 100 ℃ of temperature, boil and drive most oxides of nitrogen, water flushing wall of cup, cooling solution is to room temperature; Thin up to solution concentration is 25mL/mL, gets the iron standard solution;
3, the preparation of the gallium standard solution of iron content:
0.00 mL that 3A, removing step 1B make, 0.50 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL gallium standard solution (massfraction is respectively 0.00%, 0.005%, 0.010%, 0.020%, 0.030%, 0.040%, 0.050%); Place seven 50mL volumetric flasks respectively; In seven volumetric flasks, add 5.00 mL iron standard solution and the 5 mL watery hydrochloric acid that step 2A makes respectively, this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is diluted with water to scale, and mixing obtains seven parts of standard solution of 50 mL faintly acid iron content respectively;
3B, with conventional ICP-AES of the prior art, respectively gallium line strength in seven parts of standard solution of determination step 3A is measured condition of work and is seen table 1, the wavelength and the progression of the element gallium in the standard solution are seen table 2;
3C, being horizontal ordinate with the massfraction of listed gallium standard solution among the 3A, is ordinate with gallium line strength in the step 3B gained standard solution, draws out the standard working curve of gallium.
Embodiment 2
The mensuration of gallium in the vanadium extraction waste to be measured:
1, the preparation of vanadium extraction waste test liquid to be measured:
1A, the amount of pressing 10 mL/g samples; In 0.5000 g vanadium extraction waste sample, add pure nitric acid 5 mL of commercial analysis; And adding commercial analysis pure hydrochloric acid 15 mL by the amount of 30mL/g sample, the amount by 2 mL/g samples adds pure hydrofluorite 1 mL of commercial analysis again, under 100 ℃ of temperature; Heating for dissolving gets lysate 2 mL;
1B, in the 2 mL lysates of step 1A; Amount by the 2.5mL/mL lysate adds pure nitric acid 5 mL of commercial analysis; And adding commercial analysis pure hydrochloric acid 15 mL by the amount of 7.5 mL/mL lysates, the amount by 0.5 mL/mL lysate adds pure hydrofluorite 1 mL of commercial analysis again, under 100 ℃ of temperature; Heating for dissolving gets lysate 2 mL;
1C, in the 2 mL lysates of step 1B, add pure perchloric acid 5 mL of commercial analysis by the amount of 2.5 mL/mL lysates, under 300 ℃, be heated to perchloric acid and smolder when bottleneck, continue heating 5min, cooling, lysate 1mL;
1D, in step 1C gained 1mL lysate, add watery hydrochloric acid 10 mL by the amount of 10 mL/mL lysates, this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is heated to 100 ℃ and treats the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 50mL, shakes up, and gets sample to be tested liquid;
2, the mensuration of gallium in the vanadium extraction waste sample:
2A, with the identical condition of work of embodiment 1 step 3B under; Measure line strength of present embodiment 2 step 1D gained sample to be tested liquid; According to measured line strength, on the working curve of embodiment 1 step 3C, gallium content is in the acquisition sample: 0.013%.
Embodiment 3
The mensuration of gallium in the vanadium slag to be measured:
1, the preparation of vanadium slag test liquid to be measured:
1A, the amount of pressing 12 mL/g samples; In 0.5000 g vanadium slag sample, add pure nitric acid 6 mL of commercial analysis; And adding commercial analysis pure hydrochloric acid 18 mL by the amount of 36mL/g sample, the amount by 4 mL/g samples adds pure hydrofluorite 2 mL of commercial analysis again, under 120 ℃ of temperature; Slowly heating for dissolving gets lysate 3 mL;
1B, in the 3 mL lysates of step 1A; Amount by the 3.5mL/mL lysate adds pure nitric acid 10.5 mL of commercial analysis; And adding commercial analysis pure hydrochloric acid 31.5 mL by the amount of 10.5 mL/mL lysates, the amount by 1.5 mL/mL lysates adds pure hydrofluorite 4.5 mL of commercial analysis again, under 120 ℃ of temperature; Slowly heating for dissolving gets lysate 4 mL;
1C, in the 4 mL lysates of step 1B, add pure perchloric acid 14 mL of commercial analysis by the amount of 3.5 mL/mL lysates, under 350 ℃, be heated to perchloric acid and smolder when bottleneck, continue heating 10min, cooling, lysate 1mL;
1D, in step 1C gained 1mL lysate, by the amount of 15 mL/mL lysates, add watery hydrochloric acid 15 mL, this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is heated to 150 ℃ and treats the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 50mL, shakes up, and gets sample to be tested liquid.
2, the mensuration of gallium in the vanadium slag sample:
2A, with the identical condition of work of embodiment 1 step 3B under; Measure line strength of present embodiment 3 step 1D gained sample to be tested liquid; According to measured line strength, on the working curve of embodiment 1 step 3C, gallium content is in the acquisition sample: 0.013%.
Embodiment 4
The mensuration of gallium in the vanadium extraction waste to be measured:
1, the preparation of vanadium extraction waste test liquid to be measured:
1A, the amount of pressing 11 mL/g samples; In 0.5000 g vanadium extraction waste sample, add pure nitric acid 5.5 mL of commercial analysis, add commercial analysis pure hydrochloric acid 16.5 mL, add pure hydrofluorite 1.5 mL of commercial analysis by the amount of 3 mL/g samples by the amount of 33mL/g sample; Under 110 ℃ of temperature; Slowly heating for dissolving gets lysate 2.5 mL;
1B, in the 2.5 mL lysates of step 1A; Add pure nitric acid 7.5 mL of commercial analysis, add commercial analysis pure hydrochloric acid 22.5 mL, add pure hydrofluorite 2.5 mL of commercial analysis by the amount of 3 mL/mL lysates by the amount of 1 mL/mL lysate by the amount of 9 mL/mL lysates; Again under 110 ℃ of temperature; Slowly heating for dissolving gets lysate 3 mL;
1C, in the 3 mL lysates of step 1B, add pure perchloric acid 9 mL of commercial analysis by the amount of 3 mL/mL lysates, under 320 ℃, be heated to perchloric acid and smolder when bottleneck, continue heating 7min, cooling, lysate 1mL;
1D, the amount of in step 1C gained 1mL lysate, pressing 12 mL/mL lysates add watery hydrochloric acid 12 mL, and this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is heated to 120 ℃ and treats the salt dissolving, and hot-cold lysis liquid is to room temperature, and dilute with water concentration is 50mL, shakes up, and gets sample to be tested liquid.
2, the mensuration of gallium in the vanadium extraction waste sample:
2A, with the identical condition of work of embodiment 1 step 3B under; Measure line strength of present embodiment 4 step 1D gained sample to be tested liquid; According to measured line strength, on the working curve of embodiment 1 step 3C, gallium content is in the acquisition sample: 0.013%.
Table 1 instrument condition of work
| Power (W) | Atomizing pressure (psi) | Secondary air amount (L/min) | Pump speed (rpm) | Integral time (s) |
| 1150 | 26.06 | 0.5 | 130 | 10 |
Table 2 element wavelength to be measured and progression
| Element | Wavelength (nm) | Level |
| Ga | 294.364 | 114 |
Claims (1)
1. the assay method of gallium content in vanadium extraction waste and the vanadium slag; Comprise line strength of measuring test liquid with conventional ICP-AES; In the standard working curve of gallium, obtain corresponding gallium content value according to this line strength, it is characterized in that test liquid makes through the following step:
A, the amount of pressing 10～12mL/g sample add nitric acid in vanadium extraction waste and vanadium slag sample, and press the amount of 30～36mL/g sample; In vanadium extraction waste and vanadium slag sample, add hydrochloric acid; By the amount of 2～4mL/g sample, in vanadium extraction waste and vanadium slag sample, add hydrofluorite, under 100～120 ℃ of temperature again; Heating for dissolving, the lysate of 4～5mL/g sample;
B, in the lysate of steps A; Amount by 2.5～3.5mL/mL lysate adds nitric acid; And adding hydrochloric acid by the amount of 7.5～10.5mL/mL lysate, the amount by 0.5～1.5mL/mL lysate adds hydrofluorite again, again under 100～120 ℃ of temperature; Heating for dissolving, the lysate of 4～5mL/g sample;
C, in the lysate of step B, add perchloric acid by the amount of 2.5～3.5mL/mL lysate, under 300～350 ℃, be heated to perchloric acid and smolder when bottleneck, continue heating 5～10min, cooling, lysate;
D, in step C gained lysate, add watery hydrochloric acid by the amount of 10～15mL/mL lysate, this watery hydrochloric acid is following volume ratio: HCl:H
2O=1:1 is heated to 100～150 ℃, is cooled to room temperature, and being diluted with water to concentration is 0.01g/mL, shakes up, and gets sample to be tested liquid.
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Cited By (4)
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| CN103940806A (en) * | 2014-04-10 | 2014-07-23 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for measuring gallium element in zinc oxide powder |
| CN104007227A (en) * | 2014-06-24 | 2014-08-27 | 武钢集团昆明钢铁股份有限公司 | Method for testing total iron content in vanadium slag |
| CN105300974A (en) * | 2015-11-11 | 2016-02-03 | 武钢集团昆明钢铁股份有限公司 | Detecting method for manganese oxide content in vanadium slag |
| CN106226288A (en) * | 2016-07-12 | 2016-12-14 | 广西壮族自治区分析测试研究中心 | The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103940806A (en) * | 2014-04-10 | 2014-07-23 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for measuring gallium element in zinc oxide powder |
| CN103940806B (en) * | 2014-04-10 | 2016-06-15 | 中国航空工业集团公司北京航空材料研究院 | A kind of analysis method measuring gallium element in Zinc oxide powder |
| CN104007227A (en) * | 2014-06-24 | 2014-08-27 | 武钢集团昆明钢铁股份有限公司 | Method for testing total iron content in vanadium slag |
| CN104007227B (en) * | 2014-06-24 | 2016-06-01 | 武钢集团昆明钢铁股份有限公司 | The measuring method of all iron content in a kind of vanadium slag |
| CN105300974A (en) * | 2015-11-11 | 2016-02-03 | 武钢集团昆明钢铁股份有限公司 | Detecting method for manganese oxide content in vanadium slag |
| CN105300974B (en) * | 2015-11-11 | 2018-05-04 | 武钢集团昆明钢铁股份有限公司 | The detection method of manganese content is aoxidized in a kind of vanadium slag |
| CN106226288A (en) * | 2016-07-12 | 2016-12-14 | 广西壮族自治区分析测试研究中心 | The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target |
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Application publication date: 20121017 |