CN103776817A - Analyzing and detecting method for content of microelements in dedicated ferric oxide powder standard sample - Google Patents
Analyzing and detecting method for content of microelements in dedicated ferric oxide powder standard sample Download PDFInfo
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- CN103776817A CN103776817A CN201210414699.7A CN201210414699A CN103776817A CN 103776817 A CN103776817 A CN 103776817A CN 201210414699 A CN201210414699 A CN 201210414699A CN 103776817 A CN103776817 A CN 103776817A
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Abstract
The invention discloses an analyzing and detecting method for the content of microelements in a dedicated ferric oxide powder standard sample. The method comprises the following steps: taking low-quality ferric oxide powder as the sample, and controlling the content of each microelement in the sample; accurately weighing the sample, adding concentrated hydrochloric acid, heating to dissolve, removing into a volumetric flask, and diluting with water so as to obtain a sample liquid; weighing 5 parts of high-purity iron powder, adding concentrated hydrochloric acid, heating to dissolve, respectively removing into five volumetric flasks, respectively adding a standard solution of each microelement according to different amount into the five volumetric flasks, diluting with water, agitating uniformly, and respectively carrying out spectral line intensity measurement on each microelement so as to obtain a working curve; uniformly mixing the sample liquid and measuring the line strength of each microelement, and obtaining the content of each microelement in the sample through the working curve. The content of each microelement in the ferric oxide powder standard sample, obtained by the method, satisfies the requirement of the microelement analysis and detection in the ferric oxide powder, and the method can be used for performing quality control in ferric oxide powder analysis and detection and used for evaluating and revising detecting instruments, and effectively improves the efficiency of analysis and detection.
Description
Technical field
The present invention relates to the analyzing detecting method of micronutrient levels in a kind of special brown iron oxide standard specimen.
Background technology
Metallurgy industry is most important to the analyzing and testing of brown iron oxide, and it can adopt inductive coupling plasma emission spectrograph (ICP-AES) to implement analyzing and testing operation conventionally, for evaluating brown iron oxide quality and detecting the wherein content of trace element; Brown iron oxide standard specimen is the basis of reference during brown iron oxide detects, and can be used for the correction of detecting instrument and the supervision of brown iron oxide quality.Adopt at present ICP-AES to 14 micronutrient levels examinations in brown iron oxide, but lack the brown iron oxide standard specimen that contains 14 micronutrient levelss, therefore conventionally in brown iron oxide analysis and micronutrient levels detection, generally adopt the method that adds standard solution in pure zirconia iron powder or pure iron, adopt inductive coupling plasma emission spectrograph to measure line strength of each trace element in this test liquid, according to line strength of each trace element in test liquid, obtain the mass content of each trace element in sample through tabling look-up.The method has two large defects: 1. each operation all will add 14 element standard solution in pure zirconia iron powder test liquid, operates loaded down with trivial details, inefficiency.2. due to the matrix effect in standard solution, if the standard solution of Si is to have pure SiO
2formulated by anhydrous Na2CO3 melting, in the standard solution of its Si, just have Na ion, and Na ion is to need one of trace element of measuring, therefore can affect the measurement result of Na ion.
Summary of the invention
Technical matters to be solved by this invention is to provide the analyzing detecting method of micronutrient levels in a kind of special brown iron oxide standard specimen, utilize each micronutrient levels in the special brown iron oxide standard specimen that this method obtains, meet the requirement that in brown iron oxide, trace element analysis detects, can be used for the quality control in brown iron oxide analyzing and testing and evaluate brown iron oxide quality, correct detection instrument, effectively having improved the efficiency of analyzing and testing.
For solving the problems of the technologies described above, in the special brown iron oxide standard specimen of the present invention, the analyzing detecting method of micronutrient levels comprises the steps:
Step 1, to get low-quality brown iron oxide be sample, and each micronutrient levels in Control Assay, in sample, each micro-mass content is controlled respectively as B:0.0005-0.003%, Mg:0.005-0.03%, Al:0.005-0.03%, Si:0.005-0.03%, SO
4 2-: 0.05-0.3%, Ca:0.005-0.03%, Mn:0.05-0.3%, Ti:0.0005-0.003%, Na:0.005-0.03%, K:0.0005-0.003%, P:0.005-0.03%, Ni:0.005-0.03%, Cr:0.005-0.03%, Cu:0.005-0.03%;
Step 2, accurately take 1.000 grams of samples, move in 150mL quartz beaker, add 10mL concentrated hydrochloric acid, cover surface plate, 80-100 ℃ of heating dissolved it, and sample dissolves in rear immigration 100mL volumetric flask completely, be diluted to full scale with high purity water, obtain test liquid;
Step 3, take 5 parts of 0.700 gram of high-purity iron powders, move into respectively in 5 150mL quartz beakers, add 10mL concentrated hydrochloric acid, cover surface plate, 150 ℃ of heating are dissolved it, and after sample dissolves completely, then equivalent moves in 5 100mL volumetric flasks respectively, in 5 volumetric flasks, adding respectively concentration is B, Ti, the K of 0.01mg/mL, the SO that concentration is 1mg/mL
4 2-, Mn0, concentration is Mg, Al, Si, Ca, Na, P, Ni, Cr, the Cu of 0.1mg/mL, and capacity is respectively the standard solution of 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, be diluted to full scale with high purity water, shake up, then adopt inductive coupling plasma emission spectrograph to measure respectively line strength of each trace element in 5 volumetric flasks, obtain respectively the mass content of each trace element in 5 volumetric flasks;
Step 4, take the mass content of each trace element as horizontal ordinate, take line strength of each determination of trace element as ordinate, draw the working curve of each micro-mass content line strength relation corresponding with it, in working curve, the related coefficient of each element mass content line strength corresponding with it is greater than 0.9990, and obtains regression equation;
Line strength of each trace element in the test liquid of step 5, employing inductive coupling plasma emission spectrograph determination step one, according to line strength of each trace element in test liquid, by horizontal ordinate corresponding to working curve ordinate, can obtain the mass content of each trace element in sample.
Because the analyzing detecting method of micronutrient levels in the special brown iron oxide standard specimen of the present invention has adopted technique scheme, getting low-quality brown iron oxide is sample, and each micronutrient levels in Control Assay; Accurately take sample and move in quartz beaker, adding heating after concentrated hydrochloric acid that it is dissolved, then moving into dilute with water in volumetric flask and obtain test liquid; Take 5 parts of high-purity iron powders, move into respectively in quartz beaker, after adding concentrated hydrochloric acid, heating makes its dissolving, equivalent moves in 5 volumetric flasks respectively again, in 5 volumetric flasks by difference amount add respectively each trace element standard solution dilute with water, shake up, then carry out respectively line strength of each trace element and measure, obtaining content is the working curve that horizontal ordinate, line strength are ordinate; In test liquid, each micro-line strength is measured, and is obtained the content of each trace element in sample by working curve.Each micronutrient levels in the special brown iron oxide standard specimen that this method obtains, meet the requirement that in brown iron oxide, trace element analysis detects, can be used for the quality control in brown iron oxide analyzing and testing and evaluate brown iron oxide quality, correct detection instrument, effectively having improved the efficiency of analyzing and testing.
Embodiment
In the special brown iron oxide standard specimen of the present invention, the analyzing detecting method of micronutrient levels comprises the steps:
Step 1, to get low-quality brown iron oxide be sample, and each micronutrient levels in Control Assay, in sample, each micro-mass content is controlled respectively as B:0.0005-0.003%, Mg:0.005-0.03%, Al:0.005-0.03%, Si:0.005-0.03%, SO
4 2-: 0.05-0.3%, Ca:0.005-0.03%, Mn:0.05-0.3%, Ti:0.0005-0.003%, Na:0.005-0.03%, K:0.0005-0.003%, P:0.005-0.03%, Ni:0.005-0.03%, Cr:0.005-0.03%, Cu:0.005-0.03%;
Step 2, accurately take 1.000 grams of samples, move in 150mL quartz beaker, add 10mL concentrated hydrochloric acid, cover surface plate, 80-100 ℃ of heating dissolved it, and sample dissolves in rear immigration 100mL volumetric flask completely, be diluted to full scale with high purity water, obtain test liquid;
Step 3, take 5 parts of 0.700 gram of high-purity iron powders, move into respectively in 5 150mL quartz beakers, add 10mL concentrated hydrochloric acid, cover surface plate, 150 ℃ of heating are dissolved it, and after sample dissolves completely, then equivalent moves in 5 100mL volumetric flasks respectively, in 5 volumetric flasks, adding respectively concentration is B, Ti, the K of 0.01mg/mL, the SO that concentration is 1mg/mL
4 2-, Mn0, concentration is Mg, Al, Si, Ca, Na, P, Ni, Cr, the Cu of 0.1mg/mL, and capacity is respectively the standard solution of 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, be diluted to full scale with high purity water, shake up, then adopt inductive coupling plasma emission spectrograph to measure respectively line strength of each trace element in 5 volumetric flasks, obtain respectively the mass content of each trace element in 5 volumetric flasks; Its corresponding relation is as following table:
| Mass content (%) | 0.00mL | 0.50mL | 1.00mL | 2.00mL | 3.00mL |
| B | 0.0000 | 0.0005 | 0.0010 | 0.0020 | 0.0030 |
| Ti | 0.0000 | 0.0005 | 0.0010 | 0.0020 | 0.0030 |
| K | 0.0000 | 0.0005 | 0.0010 | 0.0020 | 0.0030 |
| SO 4 2- | 0.00 | 0.05 | 0.10 | 0.20 | 0.30 |
| Mn | 0.00 | 0.05 | 0.10 | 0.20 | 0.30 |
| Mg | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Al | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Si | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Ca | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Na | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| P | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Ni | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Cr | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
| Cu | 0.000 | 0.005 | 0.010 | 0.020 | 0.030 |
Step 4, take the mass content of each trace element as horizontal ordinate, take line strength of each determination of trace element as ordinate, draw the working curve of each micro-mass content line strength relation corresponding with it, in working curve, the related coefficient of each element mass content line strength corresponding with it is greater than 0.9990, and obtains regression equation;
Line strength of each trace element in the test liquid of step 5, employing inductive coupling plasma emission spectrograph determination step one, according to line strength of each trace element in test liquid, by horizontal ordinate corresponding to working curve ordinate, can obtain the mass content of each trace element in sample.
This method is through production testing and practical application, before having solved in the time analyzing brown iron oxide trace element with inductive coupling plasma emission spectrograph (ICP-AES) two large defects without standard model, in the time analyzing brown iron oxide trace element, analyze simultaneously a brown iron oxide standard model just can control analysis process and the work of inductive coupling plasma emission spectrograph whether accurately and reliably, both having can be used for brown iron oxide quality assessment and micronutrient levels detects, also can implement verification to detecting instrument, and can supervise at brown iron oxide testing process implementation quality, improve brown iron oxide and detected quality and efficiency, solve the problem of analyzing whole process quality control.Can form a special technology.That this method has is quick, easy, method is held wield feature, has very strong practicality, has using value and promotion prospect in similar industry.
Claims (1)
1. an analyzing detecting method for micronutrient levels in special brown iron oxide standard specimen, is characterized in that this method comprises the steps:
Step 1, to get low-quality brown iron oxide be sample, and each micronutrient levels in Control Assay, in sample, each micro-mass content is controlled respectively as B:0.0005-0.003%, Mg:0.005-0.03%, Al:0.005-0.03%, Si:0.005-0.03%, SO
4 2-: 0.05-0.3%, Ca:0.005-0.03%, Mn:0.05-0.3%, Ti:0.0005-0.003%, Na:0.005-0.03%, K:0.0005-0.003%, P:0.005-0.03%, Ni:0.005-0.03%, Cr:0.005-0.03%, Cu:0.005-0.03%;
Step 2, accurately take 1.000 grams of samples, move in 150mL quartz beaker, add 10mL concentrated hydrochloric acid, cover surface plate, 80-100 ℃ of heating dissolved it, and sample dissolves in rear immigration 100mL volumetric flask completely, be diluted to full scale with high purity water, obtain test liquid;
Step 3, take 5 parts of 0.700 gram of high-purity iron powders, move into respectively in 5 150mL quartz beakers, add 10mL concentrated hydrochloric acid, cover surface plate, 150 ℃ of heating are dissolved it, and after sample dissolves completely, then equivalent moves in 5 100mL volumetric flasks respectively, in 5 volumetric flasks, adding respectively concentration is B, Ti, the K of 0.01mg/mL, the SO that concentration is 1mg/mL
4 2-, Mn0, concentration is Mg, Al, Si, Ca, Na, P, Ni, Cr, the Cu of 0.1mg/mL, and capacity is respectively the standard solution of 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, be diluted to full scale with high purity water, shake up, then adopt inductive coupling plasma emission spectrograph to measure respectively line strength of each trace element in 5 volumetric flasks, obtain respectively the mass content of each trace element in 5 volumetric flasks;
Step 4, take the mass content of each trace element as horizontal ordinate, take line strength of each determination of trace element as ordinate, draw the working curve of each micro-mass content line strength relation corresponding with it, in working curve, the related coefficient of each element mass content line strength corresponding with it is greater than 0.9990, and obtains regression equation;
Line strength of each trace element in the test liquid of step 5, employing inductive coupling plasma emission spectrograph determination step one, according to line strength of each trace element in test liquid, by horizontal ordinate corresponding to working curve ordinate, can obtain the mass content of each trace element in sample.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062282A (en) * | 2014-07-05 | 2014-09-24 | 武钢集团昆明钢铁股份有限公司 | Method for measuring content of strontium carbonate in permanent magnetic ferrite mixture |
| CN114964976A (en) * | 2022-08-01 | 2022-08-30 | 北矿检测技术有限公司 | Rare earth oxide standard sample and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007097241A1 (en) * | 2006-02-22 | 2007-08-30 | Nippon Mining & Metals Co., Ltd. | Nickel crucible for melting of analytical sample, method of preparing analytical sample and method of analysis |
| CN101975771A (en) * | 2010-09-14 | 2011-02-16 | 常熟出入境检验检疫局综合技术服务中心 | Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder |
| CN102269719A (en) * | 2011-07-04 | 2011-12-07 | 河北钢铁股份有限公司邯郸分公司 | X-fluorescence film-pressing method for measuring content of components in ferric oxide powder |
-
2012
- 2012-10-26 CN CN201210414699.7A patent/CN103776817A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007097241A1 (en) * | 2006-02-22 | 2007-08-30 | Nippon Mining & Metals Co., Ltd. | Nickel crucible for melting of analytical sample, method of preparing analytical sample and method of analysis |
| CN101975771A (en) * | 2010-09-14 | 2011-02-16 | 常熟出入境检验检疫局综合技术服务中心 | Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder |
| CN102269719A (en) * | 2011-07-04 | 2011-12-07 | 河北钢铁股份有限公司邯郸分公司 | X-fluorescence film-pressing method for measuring content of components in ferric oxide powder |
Non-Patent Citations (2)
| Title |
|---|
| 刘爱坤 等: "电感耦合等离子体原子发射光谱法测定氧化铁粉中微量组分", 《理化检验-化学分册》 * |
| 闻向东 等: "ICP-AES法测定氧化铁粉中的硅、铝、钙、锰和硫", 《钢铁研究》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062282A (en) * | 2014-07-05 | 2014-09-24 | 武钢集团昆明钢铁股份有限公司 | Method for measuring content of strontium carbonate in permanent magnetic ferrite mixture |
| CN114964976A (en) * | 2022-08-01 | 2022-08-30 | 北矿检测技术有限公司 | Rare earth oxide standard sample and preparation method thereof |
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