CN102207464A - Analytical method of trace elements of Ni, Cr and Cu in low and medium alloy steels - Google Patents
Analytical method of trace elements of Ni, Cr and Cu in low and medium alloy steels Download PDFInfo
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- CN102207464A CN102207464A CN 201110073108 CN201110073108A CN102207464A CN 102207464 A CN102207464 A CN 102207464A CN 201110073108 CN201110073108 CN 201110073108 CN 201110073108 A CN201110073108 A CN 201110073108A CN 102207464 A CN102207464 A CN 102207464A
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Abstract
The invention relates to an analytical method of trace elements of Ni, Cr and Cu in low and medium alloy steels. The technical scheme of the invention comprises the following processing steps of firstly, adding 1+3 nitric acid into a standard sample, heating the mixture to be dissolved, cooling the heated mixture to room temperature, carrying out a constant volume process on the cooled mixture, filtering and carrying out a determination by an inductively coupled plasma atomic emission spectroscopy, drawing a standard sample working curve graph, and secondly, adding 1+3 nitric acid into a sample needing to be tested, heating the mixture to be dissolved, cooling the heated mixture to room temperature, carrying out a constant volume process on the cooled mixture, filtering and carrying out a determination of trace elements of Ni, Cr and Cu in a low and medium alloy steel by an inductively coupled plasma atomic emission spectroscopy. The analytical method utilizes 1+3 nitric acid to dissolve a sample and is easy to be operated. The positive effects of the invention comprise that the analytical method is scientific, advanced and applicative, and has the characteristics of simplicity and convenience of sample dissolving, short analysis time, high accuracy, low reagent consumption, and less pollution on environment.
Description
Technical field
The present invention relates to TRACE ELEMENTS ANALYSIS method in a kind of middle-low alloy steel, the analytical approach of particularly micro-Ni, Cr, Cu belongs to metallurgical chemistry analytical test technical field.
Background technology
In iron and steel enterprise, the content of micro-Ni, Cr, Cu height directly influences the physical property of middle-low alloy steel in the middle-low alloy steel.The accuracy of analysis of so micro-Ni, Cr, Cu and analysis speed just seem particularly important, and therefore, the analysis of micro-Ni, Cr, Cu has very strong realistic meaning.Traditional chemical analysis method, complex operation, analysis speed is slow, and it is many to consume reagent, and environmental pollution is comparatively serious, and precision is poor, is difficult to satisfy the needs of producing reality.
Summary of the invention
The analytical approach that the purpose of this invention is to provide micro-Ni, Cr, Cu in a kind of middle-low alloy steel, molten sample is simple, weak point consuming time, reagent dosage is few, and environmental pollution is little, and accuracy meets the demands.Solve the problems referred to above that background technology exists.
Technical scheme of the present invention is:
The analytical approach of micro-Ni, Cr, Cu in the middle-low alloy steel, comprise following processing step: heat after at first in standard sample, adding 1+3 nitric acid, until dissolving, be cooled to room temperature, constant volume, filter, re-using inductively coupled plasma atomic emission spectrometer measures, drawing standard sample working curve diagram heats behind the adding 1+3 nitric acid in sample, then until dissolving, be cooled to room temperature, constant volume filters, and can measure micro-Ni, Cr, Cu in the middle-low alloy steel with ICP-AES.
Said 1+3 nitric acid is: the volume ratio of water and nitric acid is 1:3.
The standard model that the present invention selects for use is six of the standard substances that content has certain gradient, and nitric acid uses the pure nitric acid of top grade.
The present invention adopts 1+3 nitric acid dissolve sample, and ICP-AES is measured micro-Ni, Cr, Cu in the middle-low alloy steel.Use is made curve and the consistent analysis condition of control with the standard model workmanship that the analytic sample matrix is close, and has overcome the influence of Physical Interference and matrix effect.By confirming that this method has science, advance, applicability, molten sample is simple, analysis time is short, accuracy is high, reagent dosage is few, and environmental pollution is little, accuracy characteristics such as meet the demands.
Good effect of the present invention is: this method has science, advance, applicability, molten sample is simple, analysis time is short, accuracy is high, and reagent dosage is few, and environmental pollution is little, accuracy characteristics such as meet the demands.
Description of drawings:
The working curve diagram of Cr in Fig. 1 standard sample;
The working curve diagram of Cu in Fig. 2 standard sample;
The working curve diagram of Ni in Fig. 3 standard sample.
Embodiment
The present invention will be further described below by embodiment.
Heat after at first in standard sample, adding 1+3 nitric acid,, be cooled to room temperature until dissolving, constant volume, filter, re-use inductively coupled plasma atomic emission spectrometer and measure, drawing standard sample working curve diagram, heat after in sample, adding 1+3 nitric acid then, until dissolving, be cooled to room temperature, constant volume, filter, can measure micro-Ni, Cr, Cu in the middle-low alloy steel with ICP-AES.
Embodiment more specifically:
One, process conditions
1, ICP-7510 type inductively coupled plasma atomic emission spectrometer (day island proper Tianjin).High frequency power: 1.2 kW; Observed altitude: Hi; Observed ray: radially; Cooling gas flow: 14.0 L/min; Plasma gas flow rate: 1.20 L/min; Carrier gas flux: 0.70 L/min; Integral time: 3s; Argon gas: argon volume fraction〉99.99%; Analytical line: Cr 267.796 nm; Ni 231.604nm; Cu 327.396nm scan pattern: sequential scanning.
2, main agents
Nitric acid (1.42 g/mL) preparation 1+3 nitric acid
Water is secondary deionized water, and it is pure that reagent is top grade
Two, operational sequence
1, the drafting of working curve
Take by weighing 0.25g(and be accurate to 0.000 1 g) middle-low alloy steel standard model (as table 1) that Ni, Cr, Cu content have certain gradient, in the 300mL conical flask, add 15mL1+3 nitric acid, in water-bath, heat, dissolve to standard model.Be cooled to room temperature, move in the 100mL volumetric flask, constant volume filters, and is standby.Do blank solution simultaneously with same method, standby.
Table 1 standard model
Under above-mentioned condition of work blank and series standard solution are measured, Automatic Program is drawn out working curve.With reference to accompanying drawing 1,2,3, the linearly dependent coefficient of Cr=0.99976.The linearly dependent coefficient of Cu=0.99994.The linearly dependent coefficient of Ni=0.99997.
2, the processing of sample and mensuration
Take by weighing 0.25g(and be accurate to 0.000 1 g) sample in the 300mL beaker, add 1+3 nitric acid 15mL, in water-bath, heat, dissolve to standard model.Be cooled to room temperature, move in the 100mL volumetric flask, constant volume filters, and is standby.Carry out strength detection after instrument transferred to optimum condition.
Technical parameter:
1, the selection of analysis spectral line
Select wherein highly sensitively by observing spectrogram, Physical Interference is less, and lower one of background intensity is as analytical line, and the analysis of line wavelength of experimental selection is Cr 267.796 nm; Ni 231.604nm; Cu 327.396nm.
2, the selection of background deduction point
This experiment profile spectrogram left-right symmetric can directly adopt get its minimum point background correction at 2.
3, the elimination of Physical Interference and matrix effect
In this experiment, selected to disturb little, highly sensitive analytical line, and made the analysis condition unanimity as far as possible, can eliminate Physical Interference basically.In addition, select the standard model series workmanship who is close with the analytic sample matrix to make curve in this experiment, eliminate the influence of matrix effect basically.
4, sampler-dissolving method is selected
The acid of dissolved samples is selected to go molten interference to play an important role to reducing atomizing.Because the introducing of mineral acid all makes suction speed and line strength of solution reduce, and according to above-listed HNO
3, HCl, HClO
4, H
2SO
4, H
3PO
4Aggravate in proper order.In sample analysis, also notice guaranteeing under the prerequisite that sample fully dissolves, introduce the kind of acid as far as possible less and control the low acidity of trying one's best, overcoming atomizing to greatest extent and going molten interference.Therefore, in the sample pretreatment, eliminate nitric acid as far as possible, selected viscosity little, surface tension is little, the nebulization efficiency height, and the HNO of strong complexing and oxidation is arranged
3Come dissolved samples.
Three, measurement result
Use the method micro-Ni, Cr, Cu in the standard model to be measured its analysis result such as following table 2.
The analysis result of table 2 standard model trace element Ni, Cr, Cu
It is as follows to get data to same sample analysis:
Above data show that this analytical approach has higher accuracy and precision, and Repeatability and Reproducibility is good.
Claims (3)
1. micro-Ni in the middle-low alloy steel, Cr, the analytical approach of Cu, it is characterized in that comprising following processing step: heat after at first in standard sample, adding 1+3 nitric acid, until dissolving, be cooled to room temperature, constant volume, filter, re-using inductively coupled plasma atomic emission spectrometer measures, drawing standard sample working curve diagram heats behind the adding 1+3 nitric acid in sample, then until dissolving, be cooled to room temperature, constant volume filters, and can measure micro-Ni in the middle-low alloy steel with ICP-AES, Cr, Cu.
According to claim 1 described among the analytical approach of micro-Ni, Cr, Cu in the low alloy steel, it is characterized in that standard sample is six of the standard substances that content has certain gradient.
According to claim 1 described among the analytical approach of micro-Ni, Cr, Cu in the low alloy steel, it is characterized in that water is secondary deionized water in the 1+3 nitric acid, nitric acid uses the pure nitric acid of top grade.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103335999A (en) * | 2013-06-27 | 2013-10-02 | 武汉科技大学 | Method for testing element distribution in alloy board |
| RU2518292C1 (en) * | 2013-01-24 | 2014-06-10 | Нина Валерьевна Молчан | Control over steel structure |
| CN105806826A (en) * | 2015-11-18 | 2016-07-27 | 华东理工大学 | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method |
| CN107703119A (en) * | 2017-08-14 | 2018-02-16 | 广西德邦科技有限公司 | The method of nickel content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN108956589A (en) * | 2018-04-25 | 2018-12-07 | 山西建龙实业有限公司 | The measuring method of chromium content in ferrochrome |
| CN109211880A (en) * | 2018-11-08 | 2019-01-15 | 北京星航机电装备有限公司 | A method of with copper coin cellulose content in ICP-OES measurement brass |
-
2011
- 2011-03-25 CN CN 201110073108 patent/CN102207464A/en active Pending
Non-Patent Citations (5)
| Title |
|---|
| 《2008年中国机械工程学会年会暨甘肃省学术年会论文集》 20081231 刘金祥等 ICP-AES法同时测定低合金钢中常量及痕量元素 120-123 1-3 , * |
| 《冶金分析》 20081231 崔宏利 电感耦合等离子体原子发射光谱法测定中低合金钢中微量铅 13-15 1-3 第28卷, 第4期 * |
| 《冶金分析》 20081231 徐建平 电感耦合等离子体原子发射光谱法测定钢中硫时试样溶解的影响 31 1-3 第28卷, 第12期 * |
| 《物理测试》 19971231 宋兆华等 ICP-AES法测定钢铁中的磷 38-42 1-3 , 第4期 * |
| 《理化检验－化学分册》 20081231 王艳萍等 电感耦合等离子体质谱法测定中低合金钢中痕量铝 116 1-3 第44卷, * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2518292C1 (en) * | 2013-01-24 | 2014-06-10 | Нина Валерьевна Молчан | Control over steel structure |
| CN103335999A (en) * | 2013-06-27 | 2013-10-02 | 武汉科技大学 | Method for testing element distribution in alloy board |
| CN103335999B (en) * | 2013-06-27 | 2015-04-15 | 武汉科技大学 | Method for testing element distribution in alloy board |
| CN105806826A (en) * | 2015-11-18 | 2016-07-27 | 华东理工大学 | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method |
| CN107703119A (en) * | 2017-08-14 | 2018-02-16 | 广西德邦科技有限公司 | The method of nickel content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN108956589A (en) * | 2018-04-25 | 2018-12-07 | 山西建龙实业有限公司 | The measuring method of chromium content in ferrochrome |
| CN109211880A (en) * | 2018-11-08 | 2019-01-15 | 北京星航机电装备有限公司 | A method of with copper coin cellulose content in ICP-OES measurement brass |
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Application publication date: 20111005 |