CN104597000A - Hydride generation-atomic florescence spectrometry method for determining trace quantity of antimony in galvanized steel sheet plating - Google Patents
Hydride generation-atomic florescence spectrometry method for determining trace quantity of antimony in galvanized steel sheet plating Download PDFInfo
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- CN104597000A CN104597000A CN201310534778.6A CN201310534778A CN104597000A CN 104597000 A CN104597000 A CN 104597000A CN 201310534778 A CN201310534778 A CN 201310534778A CN 104597000 A CN104597000 A CN 104597000A
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Abstract
The invention discloses a hydride generation-atomic florescence spectrometry method for determining a trace quantity of antimony in a galvanized steel sheet plating. The hydride generation-atomic florescence spectrometry method for determining a trace quantity of antimony in the galvanized steel sheet plating is established through researches on instrument measuring parameters, plated matrix zinc, acidity, the concentration of hexamethylene tetramine in a deplating solution, the use amount of hydrofluoric acid and other test conditions. The researches show that the matrix effect of zinc can be eliminated through a matrix matching technique, the acidity is controlled at 40% (V/V), and hexamethylene tetramine in the deplating solution and a small amount (not greater than 2mL) of hydrofluoric acid have no influences on the determination of antimony. The concentration of antimony in a range of 0.001-0.1[mu]g/mL has a good linear relationship with the fluorescence intensity; and the lower determination limit of the method is 0.2[mu]g/L. When the method is used to analyze antimony in the plating of each of two galvanized steel sheet samples, the relative standard deviations (RSD) are 1.0% and 1.2% respectively, the sample added recoveries are 96-101%, and determination results are consistent with a determination result obtained through an ICP-MS method.
Description
Technical field
The invention belongs to casting technology field, be specifically related to a kind of By Hydride Generation-atomic Fluorescence Spectrometry measuring Determination of Trace Amounts of Antimony in galvanized steel plain sheet coating.
Background technology
The zinc-plated process of surface of steel plate is the effective ways improving its weather-resistance, and imparts the ornamental of steel simultaneously.Galvanized steel plain sheet is mainly used in the fields such as auto manufacturing, building industry and light industry.The composition of zinc coat determines quality and the production cost of product, and research shows, in zinc coat, the content of alloying element antimony has extreme influence to structure of plating layer and corrosivity.The instrument compare that used detection method has is complicated, and some underactions, detect limit for height, has some difficulties when measuring.
Summary of the invention
In order to overcome the above-mentioned technical matters that prior art field exists, the object of the invention is to, provide a kind of By Hydride Generation-atomic Fluorescence Spectrometry measuring Determination of Trace Amounts of Antimony in galvanized steel plain sheet coating, instrument is simple, and flexibly, detection limit is low.
The By Hydride Generation-atomic Fluorescence Spectrometry of Determination of Trace Amounts of Antimony in mensuration galvanized steel plain sheet coating provided by the invention, comprises following content:
(1) instrument and measuring condition: AFS-830A type Double Channel-Atomic Fluorescence Spectrometry instrument (Beijing Ji Tian instrument company); Generation-Atomic Fluorescence Spectrometry hydride generator; The special hollow cathode lamp of antimony;
(2) reagent: hydrochloric acid, nitric acid, hydrofluorite: top grade is pure; Citric acid solution: 400g/L; Thiourea and ascorbic acid solution: take 10g thiocarbamide and 10g ascorbic acid respectively, is dissolved in 200mL water, mixing, matching while using; Reductive agent: take 5g potassium hydroxide, 20g potassium borohydride is dissolved in 1000mL water, matching while using; Current-carrying solution: 5% hydrochloric acid (V/V); Zinc coat cleaning fluid: absolute ethyl alcohol; Galvanized sheet takes off plating solution (being suitable for coating is zinc or kirsite): take 3.5g hexamethylenetetramine, be dissolved in 500mL hydrochloric acid, be diluted with water to 1000mL; Metallic zinc: high-purity; Antimony standard reserving solution (Iron and Steel Research Geueral Inst): 500 μ g/mL; Antimony standard solution: 1.0 μ g/mL and 0.10 μ g/mL, respectively by antimony standard reserving solution stepwise dilution formulated (except as otherwise noted, only use in testing confirm as the deionized water that analytically pure reagent and resistivity are 18M Ω cm);
(3) method of testing: certain model (D4) galvanized steel plain sheet producing 10 pieces of 40 ~ 60mm × 40 ~ 60mm, after clean with washes of absolute alcohol, weigh and (is designated as m
2), then immerse 80 ~ 120mL galvanized steel plain sheet and take off in plating solution, immediately parent plate is taken out after vigorous reaction, clean up with pure water, dry up immediately, weigh and (be designated as m
2).After cleaning, solution is incorporated to and takes off in plating solution, is then quantitatively transferred in volumetric flask, is diluted with water to scale, as the sample solution analyzing antimony in galvanized steel plain sheet coating; In experiment, high for silicone content, need the sample adding hydrofluorite, involved vessel all use beaker or the volumetric flask of teflon, and the addition of hydrofluorite is no more than 2mL; Now, the mass concentration ρ coating=(m of coating in sample solution
2-m
2)/200, content of hydrochloric acid is 25%(V/V); Divide and get 10mL plating solution in 50mL volumetric flask, then add 17.5mL hydrochloric acid, make controlling pH at 40%(V/V), add 5 ~ 15mL thiourea and ascorbic acid solution, be settled to scale; Place half an hour, measure its fluorescence intensity;
(4) calibration curve: take 0.1000g metallic zinc in a series of 50mL beaker, add 20mL hydrochloric acid dissolution in low temperature, cooling, be transferred in 50mL volumetric flask, add 0.10 μ g/mL antimony standard solution 0.5,1.0mL successively, 1.0 μ g/mL antimony standard solution 0.2,0.5 and 1.0mL, then add 10mL thiourea and ascorbic acid solution, be diluted with water to scale, mixing; Now, in solution, antimony concentration is respectively 0,0.001,0.002,0.004,0.010,0.020 and 0.100 μ g/mL; After placing half an hour, atomic fluorescence spectrometer measures the atomic fluorescence intensity of antimony in test solution, with antimony concentration (μ g/mL) for horizontal ordinate, with antimony atoms fluorescence intensity for ordinate draws calibration curve from low to high.
The By Hydride Generation-atomic Fluorescence Spectrometry of Determination of Trace Amounts of Antimony in mensuration galvanized steel plain sheet coating provided by the invention, its beneficial effect is, overcome prior art processing flange bolt hole, operation is more, the problem that workload is large, improves production efficiency; Avoid because of the defective mass defect caused of bolt hole processing, utilization rate of raw materials is high, reduces production cost; The flange bolt hole aperture of the finished product cast out and pitch-row size accurately, without the need to machining, effectively ensure that casting quality.
Embodiment
Below in conjunction with an embodiment, the By Hydride Generation-atomic Fluorescence Spectrometry of Determination of Trace Amounts of Antimony in mensuration galvanized steel plain sheet coating provided by the invention is described in detail.
Embodiment
The By Hydride Generation-atomic Fluorescence Spectrometry of Determination of Trace Amounts of Antimony in the mensuration galvanized steel plain sheet coating of the present embodiment, comprises the following steps:
(1) instrument and measuring condition: AFS-830A type Double Channel-Atomic Fluorescence Spectrometry instrument (Beijing Ji Tian instrument company); Generation-Atomic Fluorescence Spectrometry hydride generator; The special hollow cathode lamp of antimony;
(2) reagent: hydrochloric acid, nitric acid, hydrofluorite: top grade is pure; Citric acid solution: 400g/L; Thiourea and ascorbic acid solution: take 10g thiocarbamide and 10g ascorbic acid respectively, is dissolved in 200mL water, mixing, matching while using; Reductive agent: take 5g potassium hydroxide, 20g potassium borohydride is dissolved in 1000mL water, matching while using; Current-carrying solution: 5% hydrochloric acid (V/V); Zinc coat cleaning fluid: absolute ethyl alcohol; Galvanized sheet takes off plating solution (being suitable for coating is zinc or kirsite): take 3.5g hexamethylenetetramine, be dissolved in 500mL hydrochloric acid, be diluted with water to 1000mL; Metallic zinc: high-purity; Antimony standard reserving solution (Iron and Steel Research Geueral Inst): 500 μ g/mL; Antimony standard solution: 1.0 μ g/mL and 0.10 μ g/mL, respectively by antimony standard reserving solution stepwise dilution formulated (except as otherwise noted, only use in testing confirm as the deionized water that analytically pure reagent and resistivity are 18M Ω cm);
(3) method of testing: certain model (D4) galvanized steel plain sheet producing 10 pieces of 50mm × 50mm, after clean with washes of absolute alcohol, weigh and (is designated as m
2), then immerse 100mL galvanized steel plain sheet and take off in plating solution, immediately parent plate is taken out after vigorous reaction, clean up with pure water, dry up immediately, weigh and (be designated as m
2).After cleaning, solution is incorporated to and takes off in plating solution, is then quantitatively transferred in 200mL volumetric flask, is diluted with water to scale, as the sample solution analyzing antimony in galvanized steel plain sheet coating; In experiment, high for silicone content, need the sample adding hydrofluorite, involved vessel all use beaker or the volumetric flask of teflon, add hydrofluorite 2mL; Now, the mass concentration ρ coating=(m of coating in sample solution
2-m
2)/200, content of hydrochloric acid is 25%(V/V); Divide and get 10mL plating solution in 50mL volumetric flask, then add 17.5mL hydrochloric acid, make controlling pH at 40%(V/V), add 10mL thiourea and ascorbic acid solution, be settled to scale; Place half an hour, measure its fluorescence intensity;
(4) calibration curve: take 0.1000g metallic zinc in a series of 50mL beaker, add 20mL hydrochloric acid dissolution in low temperature, cooling, be transferred in 50mL volumetric flask, add 0.10 μ g/mL antimony standard solution 0.5,1.0mL successively, 1.0 μ g/mL antimony standard solution 0.2,0.5 and 1.0mL, then add 10mL thiourea and ascorbic acid solution, be diluted with water to scale, mixing; Now, in solution, antimony concentration is respectively 0,0.001,0.002,0.004,0.010,0.020 and 0.100 μ g/mL; After placing half an hour, atomic fluorescence spectrometer measures the atomic fluorescence intensity of antimony in test solution, with antimony concentration (μ g/mL) for horizontal ordinate, with antimony atoms fluorescence intensity for ordinate draws calibration curve from low to high.
Claims (1)
1. measure a By Hydride Generation-atomic Fluorescence Spectrometry for Determination of Trace Amounts of Antimony in galvanized steel plain sheet coating, it is characterized in that:
Get 10 pieces of galvanized steel plain sheets, after clean with washes of absolute alcohol, weigh, then immerse 80 ~ 120mL galvanized steel plain sheet and take off in plating solution, immediately parent plate is taken out after vigorous reaction, clean up with pure water, dry up immediately, weigh; After cleaning, solution is incorporated to and takes off in plating solution, is then quantitatively transferred in volumetric flask, is diluted with water to scale, as the sample solution analyzing antimony in galvanized steel plain sheet coating; The mass concentration ρ coating=(m of coating in sample solution
2-m
2)/200, content of hydrochloric acid is 25%(V/V); Divide and get 10mL plating solution in 50mL volumetric flask, then add 17.5mL hydrochloric acid, make controlling pH at 40%(V/V), add 5 ~ 15mL thiourea and ascorbic acid solution, be settled to scale; Place half an hour, measure its fluorescence intensity.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106814126A (en) * | 2017-03-27 | 2017-06-09 | 山东钢铁集团日照有限公司 | A kind of method of testing of galvanizing layer weight and wherein trace element distribution |
| CN106896168A (en) * | 2017-02-14 | 2017-06-27 | 中国环境科学研究院 | Sb in a kind of soil or deposit（Ⅲ）Detection method |
| CN108254363A (en) * | 2016-12-29 | 2018-07-06 | 富士康(昆山)电脑接插件有限公司 | The chemical method of rhodium ruthenium content in a kind of efficient detection coating |
| CN111948159A (en) * | 2020-08-17 | 2020-11-17 | 沈阳飞机工业（集团）有限公司 | Method for testing nickel content of zinc-nickel alloy coating |
| CN113740142A (en) * | 2020-05-27 | 2021-12-03 | 宝山钢铁股份有限公司 | Method for obtaining hydrogen content of galvanized sheet matrix |
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2013
- 2013-11-04 CN CN201310534778.6A patent/CN104597000A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108254363A (en) * | 2016-12-29 | 2018-07-06 | 富士康(昆山)电脑接插件有限公司 | The chemical method of rhodium ruthenium content in a kind of efficient detection coating |
| CN106896168A (en) * | 2017-02-14 | 2017-06-27 | 中国环境科学研究院 | Sb in a kind of soil or deposit（Ⅲ）Detection method |
| CN106814126A (en) * | 2017-03-27 | 2017-06-09 | 山东钢铁集团日照有限公司 | A kind of method of testing of galvanizing layer weight and wherein trace element distribution |
| CN113740142A (en) * | 2020-05-27 | 2021-12-03 | 宝山钢铁股份有限公司 | Method for obtaining hydrogen content of galvanized sheet matrix |
| CN111948159A (en) * | 2020-08-17 | 2020-11-17 | 沈阳飞机工业（集团）有限公司 | Method for testing nickel content of zinc-nickel alloy coating |
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