CN103308509A - Method for measuring gallium and scandium contents in blast furnace smoke dust - Google Patents
Method for measuring gallium and scandium contents in blast furnace smoke dust Download PDFInfo
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- CN103308509A CN103308509A CN2013102257896A CN201310225789A CN103308509A CN 103308509 A CN103308509 A CN 103308509A CN 2013102257896 A CN2013102257896 A CN 2013102257896A CN 201310225789 A CN201310225789 A CN 201310225789A CN 103308509 A CN103308509 A CN 103308509A
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Abstract
The invention provides a method for measuring gallium and scandium contents in blast furnace smoke dust. The method comprises the following step: measuring the spectral line intensity of a sample solution by using the conventional inductively coupled plasma atomic emission spectrometry, so as to obtain the corresponding gallium and scandium content values from a standard working curve of gallium and scandium according to the spectral line intensity; the method is characterized in that a sample solution is prepared by the following steps: adding sodium hydroxide into the sample for melting the sample at high temperature, leaching the molten sample to obtain a dissolution solution by using hot water, dissolving a sodium hydroxide precipitate in the dissolution solution by using hydrochloric acid, acidifying the test solution by using hydrochloric acid, and obtaining the sample solution to be tested. According to the method, after the sample is dissolved, the gallium and scandium contents in the blast furnace smoke dust can be directly measured, and the operation is convenient to operate; moreover, the measured gallium and scandium contents are high in accuracy rate, the measurement results have high stability, reproducibility and accuracy, and the daily requirements of measuring the gallium and scandium contents in the blast furnace smoke dust can be completely met.
Description
Technical field
The present invention relates to the assay method of a kind of gallium and scandium content, especially gallium in the blast furnace dust and scandium content are carried out method for measuring, belong to the analysis and testing technology field.
Background technology
The mensuration of gallium and scandium content in the blast furnace dust, also do not have at present the national standard analytical approach, the mensuration of gallium content is to adopt spectrophotometric method in other samples such as the steel, not only operates loaded down with trivial details, analyze, measure long flow path, efficient is low, but also will consume a large amount of chemical reagent, both contaminated environment, endanger again the healthy of operating personnel, and the increase cost, and being only applicable to the mensuration of Determination of Trace Gallium content, measurement range is 0.0005% ~ 0.010%.Although the mensuration of scandium content also is to use ICP-AES in the steel, but sample is with the acid dissolving, be not suitable for the mensuration of gallium and scandium content in the blast furnace dust, and be only applicable to the mensuration of Determination of Trace Scandium content, measurement range is 0.0002% ~ 0.010%.0.01% ~ 0.1%, also there not be the analytical approach energy Accurate Determining that is fit to for gallium in the blast furnace dust and scandium content great majority at present.And use ICP-AES; the method only needs after the sample dissolution; just can measure the gallium in the sample and scandium; save time and laborsaving; and need not to consume a large amount of chemical reagent, can reduce the pollution to environment, the protection operating personnel's is healthy; but larger because measuring difficulty, and be difficult to apply.Therefore, seeking a kind of effective method, measure gallium and scandium content in the blast furnace dust, is the important topic that the analytical test industry is badly in need of solution.
Summary of the invention
The object of the present invention is to provide a kind of can the Accurate Determining blast furnace dust in the method for gallium and scandium content.
The present invention is achieved through the following technical solutions: the assay method of gallium and scandium content in a kind of blast furnace dust, comprise line strength of measuring test liquid with conventional ICP-AES, in the standard working curve of gallium and scandium, obtain corresponding gallium and scandium content value according to this line strength, it is characterized in that test liquid makes through the following step:
A, in the blast furnace dust sample, by the amount of 4～6g/g sample, add NaOH, under 700～800 ℃ of temperature, heating and melting 10～20min gets molten sample;
B, in the molten sample of steps A, adding temperature by the amount of 30～40mL/g sample is 70～80 ℃ hot water, is stirred to molten sample dissolving, gets lysate;
C, in the lysate of step B, the volume ratio that adds hydrochloric acid and water is that hydrochloric acid solution to the NaOH sediment in the lysate of 1 ︰ 1 dissolves, and add again the hydrochloric acid solution 5～10mL of same concentrations, to 0.02g/mL, get concentrate at 100～110 ℃ of concentrated lysates of lower heating;
The concentrate of D, cooling step C is to room temperature, and by the amount of 20～30mL/g sample, the volume ratio that adds hydrochloric acid and water is the hydrochloric acid solution of 1 ︰ 1, with the dissolving concentrate, gets lysate; Hydrochloric acid solution with same concentrations dilutes this lysate to 0.01g/mL again, filters, and gets filtrate; Hydrochloric acid solution with same concentrations dilutes this filtrate to 0.002g/mL again, gets sample to be tested liquid.
The hydrochloric acid solution of described step C, D is like this preparation: measures the commercially available analysis pure hydrochloric acid of 500mL, is diluted with water to 1000mL, and mixing, the volume ratio that gets hydrochloric acid and water is the hydrochloric acid solution of 1 ︰ 1.
Described NaOH and hydrochloric acid are commercial analysis net product.
The present invention compared with prior art has following advantages and effect: after adopting such scheme to make sample to be tested liquid, it is available ICP-AES of the prior art, directly measure gallium and scandium content in the blast furnace dust, not only easy to operate, and gallium and the scandium content accuracy rate measured are high, and its measurement result has good stability, reappearance and accuracy.The inventive method is reliable, practical, quick, can satisfy the needs of gallium and scandium content in the daily mensuration blast furnace dust fully.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1
Prepare routinely gallium and scandium standard solution
1, the preparation of gallium titer:
1A, the amount of pressing 300～400mL/g sample, in the pure gallium of commercially available 0.1000g, add dilute hydrochloric acid solution, commercially available analysis pure hydrochloric acid and the volume ratio of water are 1 ︰ 1 in the dilute hydrochloric acid solution, drip again 10～15 pure nitric acid of commercially available analysis, be heated to the gallium dissolving in water-bath, be cooled to room temperature, be diluted with water to the Gallium solution of 1mg/mL, get the gallium titer;
The gallium standard solution of 1B, removing step 1A is diluted to the gallium standard solution of 10 μ g/mL with the dilute hydrochloric acid solution of step 1A.
2, the preparation of scandium titer:
2A, with the pure scandium oxide of commercially available benchmark (more than 99.99%) in 800 ℃ of lower calcination 1h, the cooling, drying;
2B, the amount of pressing the 80mL/g sample, in the scandium oxide of the above-mentioned drying of 1.5338g, add dilute nitric acid solution, the commercially available pure nitric acid of analysis and the volume ratio of water are 1 ︰ 1 in the dilute nitric acid solution, dripping the commercially available pure hydrogen peroxide of analysis to sample dissolves fully, then boil and catch up with most hydrogen peroxide, be cooled to room temperature, be diluted with water to the scandium solution of 1mg/mL, get the scandium titer;
The scandium standard solution of 2C, removing step 2B is diluted with water to the scandium standard solution of 10 μ g/mL.
3, the preparation of ferrous solution:
3A, the amount of pressing the 3.2mL/g sample in the pure iron sample add commercially available analysis pure hydrochloric acid, under 150 ℃, are heated to the sample dissolving, get lysate;
3B, the amount of pressing the 0.5mL/1mL lysate in the lysate of step 3A gained drip the commercially available pure nitric acid of analysis, and under 100 ℃, slowly heating for dissolving is boiled 10min and removed oxides of nitrogen, gets lysate;
3C, the amount of pressing the 2.5mL/10mL lysate in the lysate of step 3B gained add the commercially available pure perchloric acid of analysis, and under 350 ℃, heating is smoldered to bottleneck and continued heating 5min, hot-cold lysis liquid;
3D, the amount of in the lysate of step 3C gained, pressing the 10mL/mL lysate, add hydrochloric acid solution, be heated to 100 ℃ and treat the salt dissolving, hot-cold lysis liquid is to room temperature, filter, merge cleansing solution and filtrate and dilute with water concentration to 10mg/mL, get the ferrous solution of 10mg/mL, concentration of hydrochloric acid solution is: commercially available analysis pure hydrochloric acid and the volume ratio of water are 1 ︰ 1.
4, the preparation of the gallium of iron content and scandium standard solution:
4A, 0.00 mL that makes of removing step 1B and 2C respectively, 1.00 mL, 3.00 mL, 7.00 mL, 10.00 mL, 15.00 mL, 20.00 (massfraction is respectively 0.00% for mL gallium and scandium standard solution, 0.010%, 0.030%, 0.070%, 0.10%, 0.15%, 0.20%), place respectively seven 50mL volumetric flasks, in seven volumetric flasks, add respectively the 5.00 mL ferrous solutions that the 3D step makes, be diluted to scale with dilute hydrochloric acid solution, the concentration of dilute hydrochloric acid solution is with step 3D, mixing obtains respectively gallium and the scandium standard solution of seven part of 50 mL iron-containing acidic;
4B, with conventional ICP-AES of the prior art, seven parts of gallium standard solution of difference determination step 4A gained and line strength of seven parts of scandium standard solution, measure condition of work and see Table 1, the Ga Element in the standard solution and the wavelength of scandium and progression see Table 2;
4C, the massfraction of listed gallium and scandium standard solution is as horizontal ordinate in the 4A, and gallium and scandium line strength are drawn out respectively the standard working curve of gallium and scandium as ordinate in the step 4B gained standard solution.
Embodiment 2
Gallium and determination of scandium in the blast furnace dust to be measured
1, the preparation of blast furnace dust test liquid to be measured
1A, 1.0000g blast furnace dust sample is placed nickel crucible, press the amount of 4g/g sample, add the pure solid sodium hydroxide 4g of commercially available analysis, under 800 ℃ of temperature, heating and melting sample 10min gets molten sample;
1B, the molten sample of step 1A is taken off slightly cold, the amount of pressing the 30mL/g sample is put into the 30mL temperature and is 70 ℃ hot water leaching in molten sample, stirs until molten sample dissolving, and takes off with hot water and to wash crucible, merges and takes off washing lotion in lysate, gets lysate;
1C, in step 1B gained lysate, be that the hydrochloric acid solution of 1 ︰ 1 slowly neutralizes with the volume ratio of hydrochloric acid and water, until the NaOH sediment in the lysate just dissolves, and add again the hydrochloric acid solution 5mL of same concentrations, to 50mL, get concentrate at 100 ℃ of concentrated lysate volumes of lower heating;
1D, with step 1C gained concentrate cooling, the amount of press the 20mL/g sample, the volume ratio that adds hydrochloric acid and water is the hydrochloric acid solution 20mL of 1 ︰ 1, to dissolve concentrate, gets lysate; Hydrochloric acid solution with same concentrations dilutes this lysate to 100mL again, filters, and gets filtrate; Pipette 10.00mL filtrate, the hydrochloric acid solution with same concentrations dilutes this filtrate to 50mL again, gets sample to be tested liquid.
2, gallium and determination of scandium in the blast furnace dust sample
2A, with the identical condition of work of embodiment 1 step 4B under, measure line strength of the present embodiment step 1D gained sample to be tested liquid, according to measured line strength, on the working curve of embodiment 1 step 4C, obtain in the sample gallium content and be 0.026%, scandium content is 0.017%.
Embodiment 3
Gallium and determination of scandium in the blast furnace dust to be measured
1, the preparation of blast furnace dust test liquid to be measured
1A, 1.0000g blast furnace dust sample is placed nickel crucible, press the amount of 6g/g sample, add the pure solid sodium hydroxide 6g of commercially available analysis, under 700 ℃ of temperature, heating and melting sample 20min gets molten sample;
1B, the molten sample of step 1A is taken off slightly cold, putting into the 40mL temperature by the amount of 40mL/g sample is that 80 ℃ hot water leaches, and stirs until molten sample dissolving, and takes off with hot water and to wash crucible, merges and takes off washing lotion in lysate, gets lysate;
1C, in step 1B gained lysate, be that the hydrochloric acid solution of 1 ︰ 1 slowly neutralizes with the volume ratio of hydrochloric acid and water, until the NaOH sediment in the lysate just dissolves, and add again the hydrochloric acid solution 10mL of same concentrations, to 50mL, get concentrate at 110 ℃ of concentrated lysate volumes of lower heating;
1D, with step 1C gained lysate cooling, the amount of press the 30mL/g sample, the volume ratio that adds hydrochloric acid and water is the hydrochloric acid solution 30mL of 1 ︰ 1, to dissolve concentrate, gets lysate; Hydrochloric acid solution with same concentrations dilutes this lysate to 100mL again, filters, and gets filtrate; Pipette 10.00mL filtrate, the hydrochloric acid solution with same concentrations dilutes this filtrate to 50mL again, gets sample to be tested liquid.
2, gallium and determination of scandium in the blast furnace dust sample
2A, with the identical condition of work of embodiment 1 step 4B under, measure line strength of the present embodiment step 1E gained sample to be tested liquid, according to measured line strength, on the working curve of embodiment 1 step 4C, gallium and scandium content are respectively in the acquisition sample: 0.026%, 0.017%.
Embodiment 4
Gallium and determination of scandium in the blast furnace dust to be measured
1, the preparation of blast furnace dust test liquid to be measured
1A, 1.0000g blast furnace dust sample is placed nickel crucible, press the amount of 5g/g sample, add the pure solid sodium hydroxide 5g of commercially available analysis, under 750 ℃ of temperature, heating and melting sample 15min gets molten sample;
1B, the molten sample of step 1A is taken off slightly cold, putting into the 35mL temperature by the amount of 35mL/g sample is that 75 ℃ hot water leaches, and stirs until molten sample dissolving, and takes off with hot water and to wash crucible, merges and takes off washing lotion in lysate, gets lysate;
1C, in step 1B gained lysate, be that the hydrochloric acid solution of 1 ︰ 1 slowly neutralizes with the volume ratio of hydrochloric acid and water, until the NaOH sediment in the lysate just dissolves, and add again the hydrochloric acid solution 7.5mL of same concentrations, to 50mL, get concentrate at 105 ℃ of concentrated lysate volumes of lower heating;
1D, with step 1C gained lysate cooling, the amount of press the 25mL/g sample, the volume ratio that adds hydrochloric acid and water is the hydrochloric acid solution 25mL of 1 ︰ 1, to dissolve concentrate, gets lysate; Hydrochloric acid solution with same concentrations dilutes this lysate to 100mL again, filters, and gets filtrate; Pipette 10.00mL filtrate, the hydrochloric acid solution with same concentrations dilutes this filtrate to 50mL again, gets sample to be tested liquid.
2, gallium and determination of scandium in the blast furnace dust sample:
2A, with the identical condition of work of embodiment 1 step 4B under, measure line strength of the present embodiment step 1E gained sample to be tested liquid, according to measured line strength, on the working curve of embodiment 1 step 4C, gallium and scandium content are respectively in the acquisition sample: 0.026%, 0.017%.
Table 1 instrument condition of work
| Power (W) | Atomizing pressure (psi) | Assisted gas flow (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 |
| Sc | 361.379 | 093 |
Claims (3)
1. the assay method of gallium and scandium content in the blast furnace dust, comprise line strength of measuring test liquid with conventional ICP-AES, in the standard working curve of gallium and scandium, obtain corresponding gallium and scandium content value according to this line strength, it is characterized in that test liquid makes through the following step:
A, in the blast furnace dust sample, by the amount of 4～6g/g sample, add NaOH, under 700～800 ℃ of temperature, heating and melting 10～20min gets molten sample;
B, in the molten sample of steps A, adding temperature by the amount of 30～40mL/g sample is 70～80 ℃ hot water, is stirred to molten sample dissolving, gets lysate;
C, in the lysate of step B, the volume ratio that adds hydrochloric acid and water is that hydrochloric acid solution to the NaOH sediment in the lysate of 1 ︰ 1 dissolves, and add again the hydrochloric acid solution 5～10mL of same concentrations, to 0.02g/mL, get concentrate at 100～110 ℃ of concentrated lysates of lower heating;
The concentrate of D, cooling step C is to room temperature, and by the amount of 20～30mL/g sample, the volume ratio that adds hydrochloric acid and water is the hydrochloric acid solution of 1 ︰ 1, with the dissolving concentrate, gets lysate; Hydrochloric acid solution with same concentrations dilutes this lysate to 0.01g/mL again, filters, and gets filtrate; Hydrochloric acid solution with same concentrations dilutes this filtrate to 0.002g/mL again, gets sample to be tested liquid.
2. assay method according to claim 1 is characterized in that described NaOH and hydrochloric acid are commercial analysis net product.
3. assay method according to claim 1, it is characterized in that: the hydrochloric acid solution of described step C, D is like this preparation: measure the commercially available analysis pure hydrochloric acid of 500mL, be diluted with water to 1000mL, mixing, the volume ratio that gets hydrochloric acid and water is the hydrochloric acid solution of 1 ︰ 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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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| JPS5837548A (en) * | 1981-08-31 | 1983-03-04 | Meidensha Electric Mfg Co Ltd | Analysis of ca in ge-ga alloy |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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 |
| 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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