CN101832917A - Method for measuring arsenic in sulfate slag - Google Patents
Method for measuring arsenic in sulfate slag Download PDFInfo
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- CN101832917A CN101832917A CN201010200540A CN201010200540A CN101832917A CN 101832917 A CN101832917 A CN 101832917A CN 201010200540 A CN201010200540 A CN 201010200540A CN 201010200540 A CN201010200540 A CN 201010200540A CN 101832917 A CN101832917 A CN 101832917A
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Abstract
The invention relates to a method for measuring arsenic in sulfate slag. An aqua regia sample is adopted and the method comprises the following steps of: weighing pure iron equivalent to iron in the sample in quantity, performing matrix matching by adopting iron base, preparing standard solution of a working curve with effectively eliminating the base interference of the iron base, selecting an analysis spectral line of the arsenic in the sulfate slag by using the conventional inductive coupling plasma spectrograph in a control laboratory, measuring the working curve and the spectral intensity of the arsenic in the test solution on the inductive coupling plasma emitting spectrograph, and directly obtaining the analysis result of the sample by automatic regression calculation of a computer. The method solves the problems of fussy operating process of sample dissolution, absorption and color comparison in the conventional method, poor analysis and operation of high content arsenic and lower analysis result.
Description
Technical field
The present invention relates to technical field of analytical chemistry, refer more particularly to method for measuring arsenic in sulfate slag.
Background technology
Sulfate slag is the solid waste of sulfuric acid industry, is to adopt troilite or sulfur-bearing tailings to do raw material to produce a kind of waste residue of being discharged in the sulfuric acid process.The comprehensive utilization of sulfate slag can be eliminated its harm to environment, can utilize as resource again.China has millions of tons of sulfate slags to discharge every year, and some country has accomplished whole utilizations at present, and China's utilization has only about 50%.Sulfate slag can be used as iron-smelting raw material, reclaims non-ferrous metal and rare precious metal, makes cement etc., and therefore, it is a kind of of great value raw material, and the comprehensive utilization of sulfate slag is had crucial meaning.Through the sulfate slag after magnetic separation and the gravity treatment, iron-holder can reach 50%～65%, can be used as the iron-bearing material of ironmaking usefulness.But owing to secondary product sulfate slag as sulfuric acid industry, singularity and production technology because of its raw material troilite or sulfur-bearing tailings, cause sulfate slag to contain higher arsenic, and when smelting, arsenic almost all enters in the pig iron and the steel, cold short and the weldability of steel is degenerated, so the secondary ore deposit requirement arsenic of smelting iron is no more than 0.07%, high duty pig iron requires not contain arsenic, therefore the content of arsenic in sulfate slag is the leading indicator that sulfate slag detects, at present the detection of arsenic in sulfate slag content there is not corresponding standard both at home and abroad, majority is analyzed with reference to GB/T2464-1996 " arsenic Determination on content Ag-DDTC spectrophotometric method in troilite and the sulphur concentrate ", this method complicated operating process, the agents useful for same kind is more, flow process is longer, the analysis result of wanting consummate operative skill just can obtain, and analysis for high-load arsenic, operate bad, analysis result is on the low side easily, seek a kind of simple, fast, the analytical approach of easy-operating arsenic in sulfate slag, be the demand of the scientific research and the production of sulfate slag, the fair trade for sulfate slag simultaneously provides technical support.
Summary of the invention
Technical matters to be solved by this invention provides a kind of analytical approach of simple, quick, easy-operating arsenic in sulfate slag, molten sample, absorption and colorimetric are loaded down with trivial details in the former method the operating process and the analysis of high-load arsenic have been solved, operate badly, analysis result is problem on the low side easily.
For solving the problems of the technologies described above, the present invention adopts the molten sample of chloroazotic acid, utilize the condition of the existing inductively-coupled plasma spectrometer in laboratory, under suitable Instrument working parameter commonly used, recommend to select the optimized analysis spectral line of arsenic in sulfate slag, set up best working curve, on inductive coupling plasma emission spectrograph, measure the spectral intensity of arsenic in working curve and the test solution, directly draw the analysis result of sample by the automatic regression Calculation of computing machine.Specifically may further comprise the steps:
Step 1, sample are decomposed: take by weighing 0.1～1g sample, be accurate to 0.0002g, place and decompose vessel, add and be heated to sample behind the chloroazotic acid and dissolve fully;
The preparation of step 2, working curve standard solution: the massfraction that takes by weighing sample size is at least four parts of 30%～70% pure iron of measuring, place each beaker extremely fully respectively with the chloroazotic acid heating and decomposition, add a certain amount of arsenic standard solution respectively, make the working curve standard solution, the arsenic content of sample to be tested drops in the working curve scope;
Step 3, mensuration: on inductively-coupled plasma spectrometer, select arsenic analysis spectral line 189.042nm, 193.759nm, 197.262nm in this medium, working curve standard solution and test solution are measured the spectral intensity of arsenic simultaneously, and the automatic regression Calculation of computing machine goes out analysis result then.
Preferably, type of heating described in the described step 1 is to heat on microwave heating or the electric hot plate.
Arsenic analysis spectral line in the described step 3 is 189.042nm.
Beneficial effect of the present invention comprises:
(1) decomposition of sample: can adopt two kinds of methods, a kind of directly heating for dissolving sample on electric hot plate of chloroazotic acid reagent of using, another kind of with a spot of chloroazotic acid reagent employing micro-wave digestion method dissolved samples, both can both make the arsenic in the sulfate slag sample decompose fully, enter in the test solution.Former approach does not need the micro-wave digestion stove, operates simplyr, and latter's method is used the micro-wave digestion method, and agents useful for same is few, economy, environmental protection, and all more former method of two sample decomposition methods is simple, easy to operate in a word, decomposes fully the accuracy height.
(2) take by weighing with sample size in the suitable pure iron of iron amount adopt iron-based to carry out the matrix coupling effectively to eliminate the matrix of iron matrix and disturb.
(3) utilize the laboratory to have the condition of inductively-coupled plasma spectrometer now, under suitable Instrument working parameter commonly used, recommend to select the optimized analysis spectral line of arsenic in sulfate slag, set up best working curve, on inductive coupling plasma emission spectrograph, measure the spectral intensity of arsenic in the standard solution of working curve and the test solution, directly draw the analysis result of sample by the automatic regression Calculation of computing machine.Invented a kind of method of fast, accurately measuring the arsenic in sulfate slag element.
(4) recommending not to be subjected to the arsenic analysis spectral line of spectrum interference substantially is 189.042nm, 193.759nm, 197.262nm, and the optimized analysis spectral line is that 189.042nm measures, and has improved accuracy, the precision of method.
(5) make working curve with the arsenic standard solution preparing standard solution, have magnitude tracing.
(6) analyst coverage is wide, can be fit to 0.005%--5% arsenic Determination on content in the sulfate slag, and analysis precision is good, the accuracy height.
Embodiment
The present invention is further illustrated with embodiment below, and relevant percentage composition is the massfraction amount.
Step 1, sample decompose, and comprising:
Method one takes by weighing 0.1～1g sample, preferably takes by weighing 0.5g, be accurate to 0.0002g, place the 250mL beaker, add 100mL chloroazotic acid heating and decomposition sample on middle high-temperature electric heating plate, decomposition samples can be added chloroazotic acid 20mL～50mL, heating and decomposition sample to liquor capacity to about 15mL once more for the indissoluble sample, when on high-temperature electric heating plate, heating, gripping beaker immediately, reactionless around the residue at the bottom of the visual inspection cup, can think that arsenic decomposes fully in the sample, cooling is settled in the 50mL volumetric flask;
Method two takes by weighing 0.1～1g sample, preferably takes by weighing 0.5g, be accurate to 0.0002g, place the micro-wave digestion cup, add 6～12mL chloroazotic acid, select different suitable sample digestion conditions according to different micro-wave ovens, carry out the molten sample of micro-wave digestion, be settled in the 50mL volumetric flask.If take by weighing the sample of other mass number,, to guarantee simultaneously that the analytical accuracy of sample and precision can reach to analyze to require to get final product as long as the reagent that adds can decompose sample fully.
The preparation of step 2, working curve standard solution: take by weighing at least four parts of the pure iron of 30%～70% amount of sample size, use chloroazotic acid 15～20mL heating and decomposition respectively, move in the 50mL volumetric flask, add arsenic standard solution, make the standard solution of working curve to fully.The addition of arsenic standard solution is according to the amount of taking by weighing of sample in each working curve standard solution, and determined to comprise that each point arsenic content calculates on the working curve of sample arsenic content.The adding of series arsenic standard solution finishes, and is settled to scale with deionized water or distilled water.
For example, when the arsenic content in the sulfate slag sample was usually between 0.01%～1%, preparation arsenic content was respectively the standard solution of the working curve of 0%, 0.01%, 0.08%, 0.4%, 2.00%5 point.When taking by weighing sample 0.2000g, the addition of arsenic standard solution respectively is 0 μ g, 20 μ g, 160 μ g, 800 μ g, 4mg; When taking by weighing sample 0.5000g, the addition of arsenic standard solution respectively is 0 μ g, 50 μ g, 400 μ g, 2mg, 10mg.
Step 3, mensuration: on inductively-coupled plasma spectrometer, select that the arsenic analysis spectral line is 189.042nm, 193.759nm, 197.262nm in this medium, the optimized analysis spectral line is 189.042nm, to the spectral intensity that the standard solution and the test solution of working curve are measured arsenic simultaneously, the automatic regression Calculation of computing machine goes out analysis result.
Specific embodiment
Adopt technique scheme, arsenic in three sulfate slag samples is being taken by weighing the 0.5000g sample in the 250mL glass beaker, adding the 100mL chloroazotic acid, dissolved samples is complete on middle high-temperature electric heating plate, constant volume has carried out mensuration and mark-on recovery test in the 50mL volumetric flask, result such as following table 1.
The analysis result of the molten sample sample of table 1-electric hot plate
| Sample number | The measured value (%) of test number (TN) n=5 As | Analysis spectral line (nm) | Relative standard deviation (%) | Addition (%) | The recovery (%) |
| ??1# | ??0.012 | ??193.759 | ??5.10 | ??0.030 | ??96.6 |
| ??2# | ??0.134 | ??197.262 | ??1.42 | ??0.200 | ??101.8 |
| ??3# | ??0.714 | ??189.042 | ??0.63 | ??1.00 | ??99.9 |
Simultaneously above three samples are taken by weighing 0.5000g, also carried out mensuration and mark-on recovery test, result such as following table 2 with the molten sample of micro-wave digestion.
The analysis result of the molten sample sample of table 2-micro-wave digestion
| Sample number | The measured value (%) of test number (TN) n=5 As | Analysis spectral line (nm) | Relative standard deviation (%) | Addition (%) | The recovery (%) |
| ??1# | ??0.012 | ??193.759 | ??5.10 | ??0.030 | ??96.6 |
| ??2# | ??0.134 | ??197.262 | ??1.42 | ??0.200 | ??101.8 |
| ??3# | ??0.714 | ??189.042 | ??0.63 | ??1.00 | ??99.9 |
From last table 1,2 as can be seen, the inventive method has higher accuracy and precision, can satisfy the analyze demands of scientific research and production well.
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (3)
1. a method for measuring arsenic in sulfate slag is characterized in that, may further comprise the steps:
Step 1, sample are decomposed: take by weighing 0.1～1g sample, be accurate to 0.0002g, place and decompose vessel, add and be heated to sample behind the chloroazotic acid and dissolve fully;
The preparation of step 2, working curve standard solution: the massfraction that takes by weighing sample size is at least four parts of 30%～70% pure iron of measuring, place each beaker extremely fully respectively with the chloroazotic acid heating and decomposition, move in the volumetric flask behind the constant volume, add a certain amount of arsenic standard solution respectively, make the working curve standard solution, the arsenic content of sample to be tested drops in the working curve scope;
Step 3, mensuration: on inductively-coupled plasma spectrometer, select arsenic analysis spectral line 189.042nm, 193.759nm, 197.262nm in this medium, working curve standard solution and test solution are measured the spectral intensity of arsenic simultaneously, and the automatic regression Calculation of computing machine goes out analysis result then.
2. method for measuring arsenic in sulfate slag according to claim 1 is characterized in that, type of heating described in the described step 1 is to heat on microwave heating or the electric hot plate.
3. method for measuring arsenic in sulfate slag according to claim 2 is characterized in that, the arsenic analysis spectral line in the described step 3 is 189.042nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102788760A (en) * | 2011-05-17 | 2012-11-21 | 北京有色金属研究总院 | Multi-element standard solution for aluminum alloy chemistry analysis, and preparation method thereof |
| CN106442363A (en) * | 2016-11-30 | 2017-02-22 | 大工（青岛）新能源材料技术研究院有限公司 | Method for determination of arsenic content in wastewater |
| CN107091840A (en) * | 2017-06-15 | 2017-08-25 | 南昌航空大学 | The analysis method of sodium gluconate in a kind of titanium alloy activating solution |
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| JP2007327797A (en) * | 2006-06-06 | 2007-12-20 | Dowa Holdings Co Ltd | High-frequency inductively coupled plasma emission spectrometric analysis method |
| CN101435775A (en) * | 2008-12-23 | 2009-05-20 | 二重集团（德阳）重型装备股份有限公司 | Method for measuring impurity elements arsenic, tin antimony in ferromolybdenum |
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| JP2007327797A (en) * | 2006-06-06 | 2007-12-20 | Dowa Holdings Co Ltd | High-frequency inductively coupled plasma emission spectrometric analysis method |
| CN101614657A (en) * | 2008-06-27 | 2009-12-30 | 上海宝钢工业检测公司 | The assay method of arsenic in the gas and dust discharged by roasting and burning furnace |
| CN101435775A (en) * | 2008-12-23 | 2009-05-20 | 二重集团（德阳）重型装备股份有限公司 | Method for measuring impurity elements arsenic, tin antimony in ferromolybdenum |
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Cited By (3)
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| CN102788760A (en) * | 2011-05-17 | 2012-11-21 | 北京有色金属研究总院 | Multi-element standard solution for aluminum alloy chemistry analysis, and preparation method thereof |
| CN106442363A (en) * | 2016-11-30 | 2017-02-22 | 大工（青岛）新能源材料技术研究院有限公司 | Method for determination of arsenic content in wastewater |
| CN107091840A (en) * | 2017-06-15 | 2017-08-25 | 南昌航空大学 | The analysis method of sodium gluconate in a kind of titanium alloy activating solution |
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Application publication date: 20100915 |