CN104165856A - Method for testing content of nickel in industrial sulfuric acid by flame atomic absorption spectroscopy method - Google Patents
Method for testing content of nickel in industrial sulfuric acid by flame atomic absorption spectroscopy method Download PDFInfo
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- CN104165856A CN104165856A CN201410441085.7A CN201410441085A CN104165856A CN 104165856 A CN104165856 A CN 104165856A CN 201410441085 A CN201410441085 A CN 201410441085A CN 104165856 A CN104165856 A CN 104165856A
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- nickel
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Abstract
The invention relates to a method for testing the content of nickel in industrial sulfuric acid by a flame atomic absorption spectroscopy method. The method provided by the invention is mainly used for analyzing and detecting aiming at industrial sulfuric acid. A sample is not required to be subjected to digestion processing; the absorbance of a nickel element in a sample is determined by adopting an air-acetylene flame atomic absorption spectrometry, and the content of the nickel element is calculated by adopting a standard curve method. The method provided by the invention is accurate, rapid, and is good in trace amount and reproducibility, and is a method for rapidly analyzing and determining the content of the nickel element in the industrial sulfuric acid. In the preparation of industrial sulfuric acid, metal impurities of ferrum, copper, nickel and the like are inevitably brought into industrial sulfuric acid products for the reasons of mineral sources, pipelines, equipment and the like, the impurities not only affect the quality of the industrial sulfuric acid products, but also affect the use of the industrial sulfuric acid in the industries of electronics, reagents, pharmacy, textile and the like; in the quality standard of the domestic industrial sulfuric acid, the contents of ferrum, arsenic, lead and mercury are required correspondingly, but the content of metal nickel is not defined. According to the method provided by the invention, the metal nickel in the industrial sulfuric acid is detected by utilizing a flame atomic absorption spectrometer, an analytical method is established, and means and reference data are provided for completing relevant quality standard.
Description
Technical field
The method that the present invention relates to nickel content in a kind of flame atomic absorption spectrometry test industrial sulphuric acid, belongs to technical field of analysis and detection.
Background technology
Nickel is one of trace element of needed by human body, but excessive nickel can cause serious harm to human body.In the time that nickel content exceedes certain limit in body, can cause allergicly, bring out cancer, cause the nervous centralis of respiratory disorders and harm people.European Union member countries' regulation, in the product directly contacting for a long time with human body skin, the burst size of nickel must not exceed 0.5 μ g/mL weekly.
Industrial sulphuric acid is to produce the important auxiliary agent of preparing spinning bath in viscose rayon technological process, due to the reason of the aspects such as mineral resources, pipeline, equipment in its preparation process, the metallic impurity such as nickel are inevitably brought in industrial sulphuric acid product, the content of these impurity not only has influence on the quality of industrial sulphuric acid product, also has influence on the use of sulfuric acid in the industries such as electronics, reagent, pharmacy, weaving.In the quality standard of domestic industry sulfuric acid, only iron, arsenic, lead, mercury content are had to corresponding requirements, and the content of metallic nickel is limited.The present invention utilizes flame atomic absorption spectrophotometer to detect the metallic nickel in industrial sulphuric acid, and it is very necessary setting up a kind of quick, accurate, highly sensitive analyzing detecting method.
Summary of the invention
For assay industrial sulphuric acid product quality, the invention provides a kind of method of measuring metallic nickel content in industrial sulphuric acid of analyzing.The method is quick, accurate, highly sensitive.The method concrete steps are as follows:
The preparation of sample solution: pipette the industrial sulphuric acid of certain mass, with ultrapure water constant volume, be mixed with the sample solution with certain mass concentration.
The preparation of blank solution: with ultrapure water constant volume, analytical pure sulfuric acid is mixed with to the blank solution with sample solution with equal in quality concentration.
The preparation of standard solution: taking dilute sulfuric acid as solvent constant volume, the standard solution that the nickel titer of 1000 μ g/mL is mixed with to variable concentrations is for subsequent use.
Nickel content in Instrument measuring industrial sulphuric acid, affiliated instrument comprises: flame atomic absorption spectrophotometer, nickel hollow cathode lamp, oil-free gas compressor, design parameter arranges as follows:
Wavelength: 232.0 nm; Spectral band-width: 0.2 nm; Lamp current: 6.0 mA; Combustion head height: 7.0mm; Air pressure: 0.24 MPa; Acetylene gas pressure: 0.10 MPa; Acetylene gas flow: 1.4L/min.
With blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, drawing standard curve, calculate the content of metallic nickel.
Advantage of the present invention is:
(1) the present invention adopts the content of metallic nickel element in flame atomic absorption spectrometry analyzing and testing industrial sulphuric acid, has quick, sensitive, accurate, easy-operating advantage, at present domestic this type of report that there is no.
(2) this method sample is without clearing up processing, and required sample size is few, avoids the loss of metallic nickel in processing procedure.
Embodiment
In order to make those skilled in the art person understand better the present invention program, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with embodiment, the present invention is described in more detail.
A method for nickel content in Flame Atomic Absorption Spectrometry examination industrial sulphuric acid, comprises the following steps:
The preparation of sample solution: pipette certain mass industrial sulphuric acid sample solution, be settled in 100mL volumetric flask with ultrapure water, be mixed with mass concentration and be 10% sample solution.
The preparation of blank solution: analytical pure sulfuric acid is mixed with to the blank solution with sample solution with equal in quality concentration with ultrapure water dilution constant volume.
The preparation of standard solution: taking 10% dilute sulfuric acid as solvent constant volume, be the series standard solution of 0.00,0.10,0.20,1.00,2.00 μ g/mL by the nickel titer of 1000 μ g/mL (being provided by national ferrous materials test center Iron and Steel Research Geueral Inst) compound concentration.
Above-mentioned blank solution is measured according to above-mentioned set parameter with the U.S. S2D2AA of THEROM company type Atomic Absorption Spectrometer, proofread and correct spectrometer zero point, sequentially determining series standard solution again, instrument automatic data processing, and display standard curve, equation of linear regression is: A=0.0237c+0.0003(R
2=0.9996), wherein, the concentration (μ g/mL) that c is element to be measured, A is the absorbance recording.The range of linearity is: 0～2.00 μ g/mL.
Under arranging, above-mentioned same parameters carries out the mensuration of sample solution, prepare 5 parts of parallel sample solutions, measure respectively the wherein absorbance of nickel element, according to the content of nickel element in regression equation calculation 5 duplicate samples, average, show that in industrial sulphuric acid, nickel element content is 0.2211 μ g/g.
Above embodiment is only unrestricted for technical scheme of the present invention is described, those of ordinary skill in the art will be appreciated that, can suitably revise or be equal to replacement detection method of the present invention, and not departing from aim of the present invention and scope, it all should be encompassed in claim scope of the present invention.
Claims (9)
1. a method for nickel content in Flame Atomic Absorption Spectrometry examination industrial sulphuric acid, is characterized in that: comprise the following steps: the preparation of sample solution: pipette certain mass industrial sulphuric acid sample solution, and with ultrapure water constant volume, the sample solution of preparation certain mass concentration.
2. the preparation of blank solution: with ultrapure water dilution constant volume, analytical pure sulfuric acid is mixed with to the blank solution with sample solution with equal in quality concentration.
3. the preparation of standard solution: the nickel standard solution of preparation variable concentrations is for subsequent use taking dilute sulfuric acid as solvent.
4. the nickel content in Instrument measuring industrial sulphuric acid, affiliated instrument comprises: flame atomic absorption spectrophotometer, nickel hollow cathode lamp, oil-free gas compressor, design parameter arranges as follows:
Wavelength: 232.0 nm; Spectral band-width: 0.2 nm; Lamp current: 6.0 mA; Combustion head height: 7.0mm; Air pressure: 0.24 MPa; Acetylene gas pressure: 0.10 MPa; Acetylene gas flow: 1.4L/min.
5. with blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, drawing standard curve, calculates the content of metallic nickel.
6. the method for nickel content in Flame Atomic Absorption Spectrometry examination industrial sulphuric acid according to claim 1, is characterized in that: industrial sulphuric acid sample is without clearing up processing.
7. the method for nickel content in Flame Atomic Absorption Spectrometry examination industrial sulphuric acid according to claim 1, is characterized in that: it is pure that sulfuric acid used is analysis, and institute's water is ultrapure water.
8. the method for nickel content in Flame Atomic Absorption Spectrometry examination industrial sulphuric acid according to claim 3, is characterized in that: in described method, series standard solution is to prepare with commercially available nickel standard solution.
9. the method for nickel content in Flame Atomic Absorption Spectrometry examination industrial sulphuric acid according to claim 5, is characterized in that: the measured matter in described method is industrial sulphuric acid.
Priority Applications (1)
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| CN201410441085.7A CN104165856A (en) | 2014-09-02 | 2014-09-02 | Method for testing content of nickel in industrial sulfuric acid by flame atomic absorption spectroscopy method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104914061A (en) * | 2015-06-19 | 2015-09-16 | 贵州出入境检验检疫局检验检疫综合技术中心 | Method for determining thallium content of agricultural product by flame atomic absorption spectrometry |
| CN105319208A (en) * | 2015-02-05 | 2016-02-10 | 温州医科大学 | On-site rapid detection method for nickel ions in water capable of eliminating reagent blank influences |
| CN107917885A (en) * | 2017-11-17 | 2018-04-17 | 重庆万里新能源股份有限公司 | The detection method of nickel, manganese, cadmium in sulfuric acid |
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| UA43581U (en) * | 2009-03-16 | 2009-08-25 | Донецкий Национальный Университет | Method for determination of cobalt, nickel, cadmium, zink in atmospheric air |
| CN101968436A (en) * | 2010-09-03 | 2011-02-09 | 沈阳工业大学 | Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS) |
| CN103558173A (en) * | 2013-09-26 | 2014-02-05 | 苏州国环环境检测有限公司 | Method for determining nickel content in soil by microwave digestion-flame atomic absorption spectrometry |
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| UA43581U (en) * | 2009-03-16 | 2009-08-25 | Донецкий Национальный Университет | Method for determination of cobalt, nickel, cadmium, zink in atmospheric air |
| CN101968436A (en) * | 2010-09-03 | 2011-02-09 | 沈阳工业大学 | Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS) |
| CN103558173A (en) * | 2013-09-26 | 2014-02-05 | 苏州国环环境检测有限公司 | Method for determining nickel content in soil by microwave digestion-flame atomic absorption spectrometry |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319208A (en) * | 2015-02-05 | 2016-02-10 | 温州医科大学 | On-site rapid detection method for nickel ions in water capable of eliminating reagent blank influences |
| CN105319208B (en) * | 2015-02-05 | 2018-06-05 | 温州医科大学 | Nickel ion field fast detection method in a kind of water for eliminating reagent blank influence |
| CN104914061A (en) * | 2015-06-19 | 2015-09-16 | 贵州出入境检验检疫局检验检疫综合技术中心 | Method for determining thallium content of agricultural product by flame atomic absorption spectrometry |
| CN107917885A (en) * | 2017-11-17 | 2018-04-17 | 重庆万里新能源股份有限公司 | The detection method of nickel, manganese, cadmium in sulfuric acid |
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