CN104089947A - Method for detecting chemical components comprising nickel, chromium and manganese of stainless steel - Google Patents
Method for detecting chemical components comprising nickel, chromium and manganese of stainless steel Download PDFInfo
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- CN104089947A CN104089947A CN201410337750.8A CN201410337750A CN104089947A CN 104089947 A CN104089947 A CN 104089947A CN 201410337750 A CN201410337750 A CN 201410337750A CN 104089947 A CN104089947 A CN 104089947A
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- stainless steel
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- 239000010935 stainless steel Substances 0.000 title claims abstract description 51
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 51
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000011651 chromium Substances 0.000 title claims abstract description 32
- 239000011572 manganese Substances 0.000 title claims abstract description 30
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 24
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 22
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 22
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 18
- 239000000126 substance Substances 0.000 title abstract description 6
- 239000012086 standard solution Substances 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- -1 be settled to scale Substances 0.000 claims description 5
- 230000005477 standard model Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000006193 liquid solution Substances 0.000 claims description 3
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000012488 sample solution Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005034 decoration Methods 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for detecting chemical components comprising nickel, chromium and manganese of stainless steel. The method comprises the following steps: (1) preparing a standard stainless steel solution; (2) preparing a mixed standard solution; and (3) carrying out an ICP-OES (Inductively Coupled Plasma-Optical Emission Spectroscopy) detection method. By virtue of the method, series of standard stainless steel samples are used for establishing standard curves of the detected elements, and target elements are detected and determined by using the ICP-OES technology. The method focuses on the research of the detection of the contents of main elements Ni, Cr and Mn in the stainless steel. Compared with a current main detection method, the method according to the invention has the advantages that the standard stainless steel samples are used for establishing the standard curves of the detected elements, so that the matrix interference is fully removed, a detection result is relatively accurate, and the operation of preparing the standard sample solution is relatively simple and convent. The invention discloses a relatively accurate, simple and convenient method so as to provide detection basis for accurately detecting the chemical components of stainless steel products.
Description
Technical field
The invention belongs to stainless steel technical field, particularly a kind of stainless steel chemistry forms the detection method of nickel, chromium, manganese.
Background technology
Stainless steel material has the chemical etching dielectric corrosions such as the weak corrosive medium such as resistance to air, steam, water and acid, alkali, salt because of it, be difficult for producing the premium properties such as burn into spot corrosion, corrosion or wearing and tearing and be widely used in building decoration and fitment.The prosperity that is accompanied by decorations market, stainless steel material enjoys favor, thereby people extremely pay close attention to stainless quality.Impact is decorated by the factor of stainless-steel tube quality a lot, chief component chemical element (Cr for example wherein, Ni, Mn etc.) content is particularly important to stainless-steel tube quality influence, therefore decorations are detected by chemical composition in stainless steel material quality testing, be its important ingredient, stainless steel chemistry composition content detection mainly contains two kinds of methods at present, a kind of is inductively coupled plasma spectrometry method, these two kinds of methods all adopt standard substance to prepare step by step the series standard working curve of surveyed element, yet the interference that the method may exist sample complicated substrate is considered fully and use the content accuracy of this standard sample respective element to need further to be studied, and the method configuration series standard working curve process is relatively loaded down with trivial details, in a disguised form extended sense cycle.Another kind is spark discharge atomic emission spectrometry, this method is being brought into play vital role as the conventional method of stainless steel component assay aspect stainless steel product quality supervision, but the method is to use as a kind of detection method of routine in stainless steel chemistry composition measuring.
Summary of the invention
Goal of the invention: the problem and shortage existing for above-mentioned prior art, the object of this invention is to provide the detection method that a kind of stainless steel chemistry forms nickel, chromium, manganese.
Technical scheme: in order to solve the problems of the technologies described above, technical scheme provided by the invention is as follows: a kind of stainless steel chemistry forms the detection method of nickel, chromium, manganese, comprises the following steps:
1) stainless steel standard solution allocation: take the about 0.1g of stainless steel standard sample and be placed in beaker, be accurate to 0.1 mg, add 6 mL chloroazotic acid, low-temperature heat sample dissolution, it is cooling after sample fully dissolves, be transferred to 100 mL volumetric flasks, with Milli-Q pure water, be settled to scale, mix and obtain stainless steel standard solution;
2) mixed standard solution configuration: take high purity iron standard model 0.1g, be accurate to 0.1 mg and be placed in beaker, add 4 mL hydrochloric acid, low-temperature heat makes its dissolving, be cooled to room temperature, sample is transferred in 100 mL volumetric flasks, with Milli-Q pure water, be settled to scale, mix, measure a certain amount of Ni, Cr, Mn standard solution, stepwise dilution, be configured to the serial mixed standard solution of variable concentrations, pipette the iron-based liquid solution of same amount simultaneously, make the iron-based body that contains same concentrations in serial mixed standard solution, mix and obtain standardization solution;
3) ICP-OES detection method: using plasma observed pattern: carry out radial survey and obtain the content that stainless steel chemistry forms nickel, chromium, manganese.
Beneficial effect: compared with prior art, the present invention adopts the typical curve of the series stainless steel standard specimen configuration element of surveying, and uses inductively coupled plasma atomic emission technology object element is detected and determine.In application primary study the mensuration of essential element Ni, Cr, Mn content in stainless steel, compare with current main detection method, the method has adopted the stainless steel standard specimen configuration element typical curve of surveying, fully getting rid of matrix disturbs, testing result is more accurate, and standard specimen solution preparation operation is simultaneously easier.The present invention explored a kind of more accurately and short-cut method, the detection foundation providing for stainless steel product chemical composition Accurate Measurement.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.
Embodiment 1:
Stainless steel standard specimen and Ni, Cr, tri-kinds of constituent content: GSB03-1546-2003 of Mn (Ni:4.04%, Cr:15.66%, Mn:0.615%), YSBC 41320c-2006 (Ni:9.86%, Cr:18.56%, Mn:0.803%), YSB C11311-93 (Ni:11.18%, Cr:19.32%, Mn:6.52%), YSB C37362-10 (Ni:8.49, Cr:18.56, Mn:1.44), GBW (E) 010215 (Ni:4.05, Cr:12.48, Mn:9.45), chooses the typical curve (BXG that these 5 kinds of stainless steel standard specimens configure the elements of surveying
-BQ).Ni standard solution (GSB 04-1740-2004), Cr(GSBG62017-90), Mn(GSB G 62019-90), Fe metallic pure material standard specimen (YSB C 11001-99) is for preparing the serial mixed standard solution (HH of variable concentrations
-BQ).Stainless steel 201 standard model HLB S 11025-2010 ZG1Cr17Mn6Ni5N(Ni:4.06, Cr:16.69, Mn:6.48), stainless steel 304 standard model QDG 05-70 0Cr18Ni9(Ni:8.16, Cr:18.74, Mn:1.24), three kinds of stainless steel standard samples of YSB C11343-2007 (Ni:5.24, Cr:20.94, Mn:0.63) are used for verifying two kinds of working curves and detection method accuracy.The chemical reagent such as nitric acid, hydrochloric acid be analyze pure, the water using in experimentation for Milli-Q level pure.
Inductively coupled plasma atomic emission (ICP-AES), PerkinElmer, Optima 8000.
stainless steel standard solution allocation (BXG
-BQ
)
Take the about 0.1g of stainless steel standard sample and be placed in beaker, be accurate to 0.1 mg, add 6 mL chloroazotic acid (according to hydrochloric acid and nitric acid volume ratio 3:1 preparation), low-temperature heat sample dissolution.Cooling after sample fully dissolves, be transferred to 100 mL volumetric flasks, with Milli-Q pure water, be settled to scale, mix, be ready to use in the typical curve (BXG-BQ) of configuration element to be measured.
mixed standard solution configuration (HH
-BQ
)
Take high purity iron standard model 0.1g, be accurate to 0.1 mg and be placed in beaker, add 4 mL hydrochloric acid, low-temperature heat is dissolved it, is cooled to room temperature.Sample, just like in 100 mL volumetric flasks, is settled to scale with Milli-Q pure water, mixes.Measure a certain amount of Ni, Cr, Mn standard solution, stepwise dilution, is configured to the serial mixed standard solution of variable concentrations, pipette the iron-based liquid solution of same amount simultaneously, make the iron-based body that contains same concentrations in serial mixed standard solution, mix, be ready to use in preparation mixed sample typical curve (HH
-BQ).
detection method
Plasma observed pattern: carried out respectively axial observation (Ax) and radial survey (Ra), and contrasted two kinds of observation detection accuracy.
data instance:by above-mentioned three prescription cases, three kinds of stainless steel standard specimen Ni, Cr, Mn content have been tested respectively
1) adopt stainless steel standard curve and mixed sample typical curve, Ni, Cr, Mn content in the stainless steel that ICP-OES radial survey method is measured.
In table, result shows that typical curve test Ni, the Cr of the configuration of stainless steel standard specimen, the content of Mn more approach actual value than the content of mixed sample typical curve, show that the accuracy of the typical curve that stainless steel standard specimen configures is higher.
2) identical typical curve, Ni, Cr, Mn content in the stainless steel that different ICP-OES observed rays is measured.
Use stainless steel standard specimen standard solution to do typical curve, carry out respectively ICP-OES radial survey and axial observation test stainless steel material Ni, Cr, Mn content
Use mixed standard solution to do typical curve, carry out respectively ICP-OES radial survey and axial observation test stainless steel material Ni, Cr, Mn content
Above-mentioned two show results shows, no matter be the typical curve of stainless steel standard sample configuration or the typical curve of mixed sample configuration, Ni, Cr, Mn content that ICP-OES radial survey is measured all approach its actual value more than its axial observation measured value.
Claims (1)
1. stainless steel chemistry forms a detection method for nickel, chromium, manganese, it is characterized in that, comprises the following steps:
1) stainless steel standard solution allocation: take the about 0.1g of stainless steel standard sample and be placed in beaker, be accurate to 0.1 mg, add 6 mL chloroazotic acid, low-temperature heat sample dissolution, it is cooling after sample fully dissolves, be transferred to 100 mL volumetric flasks, with Milli-Q pure water, be settled to scale, mix and obtain stainless steel standard solution;
2) mixed standard solution configuration: take high purity iron standard model 0.1g, be accurate to 0.1 mg and be placed in beaker, add 4 mL hydrochloric acid, low-temperature heat makes its dissolving, be cooled to room temperature, sample is transferred in 100 mL volumetric flasks, with Milli-Q pure water, be settled to scale, mix, measure a certain amount of Ni, Cr, Mn standard solution, stepwise dilution, be configured to the serial mixed standard solution of variable concentrations, pipette the iron-based liquid solution of same amount simultaneously, make the iron-based body that contains same concentrations in serial mixed standard solution, mix and obtain standardization solution;
3) ICP-OES detection method: using plasma observed pattern: carry out radial survey and obtain the content that stainless steel chemistry forms nickel, chromium, manganese.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004710A (en) * | 2015-07-27 | 2015-10-28 | 山西太钢不锈钢股份有限公司 | Analysis and calibration method for stainless steel chromium and nickel elements |
| CN106596520A (en) * | 2016-12-30 | 2017-04-26 | 攀钢集团江油长城特殊钢有限公司 | Method for detecting elements through ICP-AES and application of method |
| CN109060777A (en) * | 2018-10-09 | 2018-12-21 | 山西太钢不锈钢股份有限公司 | The measuring method of nickel content in siderochrome nickel corrosion resisting alloy |
| CN111323410A (en) * | 2020-04-24 | 2020-06-23 | 钢研纳克成都检测认证有限公司 | Method for detecting content of multiple elements in stainless steel |
| CN115598110A (en) * | 2022-10-31 | 2023-01-13 | 华夏生生药业（北京）有限公司（Cn） | Method for detecting nickel element in mannitol bulk drug |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004710A (en) * | 2015-07-27 | 2015-10-28 | 山西太钢不锈钢股份有限公司 | Analysis and calibration method for stainless steel chromium and nickel elements |
| CN105004710B (en) * | 2015-07-27 | 2017-09-01 | 山西太钢不锈钢股份有限公司 | A kind of stainless steel chromium, nickel element analytic set method |
| CN106596520A (en) * | 2016-12-30 | 2017-04-26 | 攀钢集团江油长城特殊钢有限公司 | Method for detecting elements through ICP-AES and application of method |
| CN109060777A (en) * | 2018-10-09 | 2018-12-21 | 山西太钢不锈钢股份有限公司 | The measuring method of nickel content in siderochrome nickel corrosion resisting alloy |
| CN111323410A (en) * | 2020-04-24 | 2020-06-23 | 钢研纳克成都检测认证有限公司 | Method for detecting content of multiple elements in stainless steel |
| CN115598110A (en) * | 2022-10-31 | 2023-01-13 | 华夏生生药业（北京）有限公司（Cn） | Method for detecting nickel element in mannitol bulk drug |
| CN115598110B (en) * | 2022-10-31 | 2023-11-07 | 华夏生生药业(北京)有限公司 | Method for detecting nickel element in mannitol bulk drug |
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