CN105675588A - Method for simultaneous detection of contents of Si, Mn, P, and Cr elements in GCr15 by using ICP plasma spectrometer - Google Patents
Method for simultaneous detection of contents of Si, Mn, P, and Cr elements in GCr15 by using ICP plasma spectrometer Download PDFInfo
- Publication number
- CN105675588A CN105675588A CN201610029913.5A CN201610029913A CN105675588A CN 105675588 A CN105675588 A CN 105675588A CN 201610029913 A CN201610029913 A CN 201610029913A CN 105675588 A CN105675588 A CN 105675588A
- Authority
- CN
- China
- Prior art keywords
- sample
- plasma
- gcr15
- speetrometer
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The invention belongs to the method of chemical analysis, and especially relates to a method for simultaneous detection of contents of Si, Mn, P, and Cr elements in GCr15 by using an ICP plasma spectrometer. The method is characterized in that the method comprises the following steps: weighing a sample, dissolving the sample, metering the volume, carrying out ICP determination, and drawing a working curve, etc. Dense perchloric acid and nitric acid are mixed into a sample dissolving acid, the acid is used for decomposing the sample at a low temperature, and the ICP plasma spectrometer is used for simultaneous detection of contents of Si, Mn, P, and Cr and other elements in GCr15 in the same mother liquor; the method has obvious superiority. The method has the advantages of simple operation, easy control, good linearity of each element, good reappearance of measuring results, high accuracy, and obviously improved operating efficiency.
Description
Technical field
The invention belongs to chemical analysis method, particularly relate to a kind of ICP of utilization plasma-speetrometer and detect the method for the constituent content such as Si, Mn, P, Cr in GCr15 simultaneously.
Background technology
Increasingly maturation along with ICP plasma light spectral technology, the chemical composition analysis of metal material also adopts ICP multielement simultaneous determination more, such as GB/T20125-2006 " the mensuration ICP-AES of low-alloy steel multielement content ", but the chemical composition analysis of the product so similar to GCr15 or material is difficult to carry out all elements at same mother solution to be measured, because the C content of this material is about 1%, Cr content is about 1.5%, sample exists the chromium carbide of densification, common nitric acid or hydrochloric acid, nitric acid mixed acid can not destroy the chromium carbide of densification completely, cause testing result on the low side, therefore can only be undertaken in two steps in the chemical composition analyzing this series products of GCr15 or material:
First, the mensuration of the constituent contents such as Si, Mn, P is carried out by GB/T20125-2006 " the mensuration ICP-AES of low-alloy steel multielement content ".
Second, again through by sample salt, nitre mixed-acid dissolution and emit perchloric acid cigarette, constant volume, separatory, carry out the mensuration of Cr constituent content.
Namely two steps are walked: the 1. mensuration of Si, Mn, P: namely a1. claims the molten sample of sample → a2. → a3. constant volume → a4. filtration → a5.ICP to measure; 2. the mensuration of Cr: namely b1. claims the molten sample → b3. of sample → b2. to emit chloric acid cigarette → b3. constant volume → b4. filtration → b5.ICP mensuration.
Must making two set standard solution as GCr15 carries out chemical composition analysis under the two-step, because measuring the acid used by element such as Si, Mn, P is hydrochloric acid and nitric acid medium, and measuring the acid used by Cr element is perchloric acid, and operating process is complicated.
Summary of the invention
In order to solve above technical problem, the purpose of the present invention is exactly when ensureing testing result accuracy, improves work efficiency, it is achieved operation operating process is simple, it is easy to operation, reproducible high with accuracy rate.
The method solving a kind of ICP of the utilization plasma-speetrometer in the present invention of upper technical problem detected simultaneously the constituent contents such as Si, Mn, P, Cr in GCr15, specifically comprises the following steps that
(1) molten sample acid: perchloric acid and nitric acid being mixed, the volume ratio of perchloric acid and nitric acid is 3.5-4.5:1;
(2) preparation of solution: include 5 some for the standard sample solution of instrument calibration, 1 the standard sample solution for measuring process control and sample solution, its operating process is to weigh sample 100mg in the dual-purpose bottle of 100mL iron and steel, add molten sample acid 5mL, on electric furnace, low-temperature heat adds water 10mL after dissolving, it is cooled to room temperature, it is diluted to scale with water, shakes up to be measured;
(3) measure:
The first, determine the relevant parameter of instrument: RF high frequency generator power 1.2KW, cooling gas flow 14.0L/min, plasma gas flow rate 1.20L/min, carrier gas flux 0.70L/L, solvent clean time 50s, the time of integration 3s;
The second, the calibration of instrument: detect 5 emitted luminescence intensities for the standard sample solution S i of instrument calibration, Mn, P, Cr by plasma-speetrometer, by element emitted luminescence intensity and content drawing curve;
3rd, the detection of process control standard sample: detect the content of Si, Mn, P, Cr in process control standard sample by plasma-speetrometer;
4th, the detection of sample: detect the content of sample Si, Mn, P, Cr by plasma-speetrometer;
Linear coefficient R >=0.999 of each element and have at least 5 points on line during instrument calibration described in testing result, for having detected.
In described step (1), the volume ratio of perchloric acid and nitric acid is 4:1.
500ml perchloric acid and 125ml nitric acid are mixed by described step (1).
Described perchloric acid ρ=1.42g/ml, nitric acid ρ=1.19g/ml.
Low temperature described in step (2) is≤120 DEG C, and optimizing temperature can be 40-90 DEG C.
Heating for dissolving is that furnace temperature can not be too high, it is to avoid solution bubble is most, affects sample dissolution velocity and solute effect, can add a thermal insulation board or of short duration closedown hot plate if desired in the middle of the dual-purpose bottle of electric furnace and iron and steel.
The detection range of each element is Si:0.020～2.02%, Mn:0.010～2.36%, P:0.003～0.092%, Cr:0.008～2.88% respectively.
Should again detecting or calibrating when the measured value controlling standard specimen occurs overproof with the nominal value of standard specimen occur in the detection of described process control standard sample.
Detection method in the present invention improves work efficiency, it is not necessary to preparation two set standard substance and sample solution, and the dissolution velocity of sample is fast, it is not required that through operations such as filtration, constant volume, separatory; Secondly, the present invention need not separately inject capital into and carry out test transformation, and merely with ready-made chemical reagent, required reagent dosage reduces, and reduces testing cost; 3rd, the measurement result of the present invention is compared with GB/T20125-2006 " the mensuration ICP-AES of low-alloy steel multielement content ", reproducible, accuracy is high. Use the technical program detection GCr15 and the chemical composition of similar products or material, reducing testing cost, improve testing result accuracy and especially improve work efficiency etc. in can obtain particularly apparent effect.
Accompanying drawing explanation
Fig. 1 is the calibration curve of Si in the present invention
Fig. 2 is the calibration curve of Mn in the present invention
Fig. 3 is the calibration curve of P in the present invention
Fig. 4 is the calibration curve of Cr in the present invention
Detailed description of the invention
Embodiment 1
(1) molten sample acid: 500ml perchloric acid and 125ml nitric acid are mixed; Perchloric acid ρ=1.42g/ml, nitric acid ρ=1.19g/ml.
(2) preparation of solution: include 5 some for the standard sample solution of instrument calibration, 1 (being not used in the standard sample of the instrument calibration) solution of the standard sample for measuring process control and sample solution, its operating process is to weigh sample 100.0mg in the dual-purpose bottle of 100mL iron and steel, add molten sample acid 5mL, on electric furnace, low-temperature heat is dissolved, boil to bottle tobacco drive to the greatest extent, container bottom limpid after, take off the dual-purpose bottle of iron and steel, add water 10mL, it is cooled to room temperature, it is diluted to scale with water, shakes up to be measured;
Low temperature is≤120 DEG C, and low-temperature heat refers to that furnace temperature can not be too high, it is to avoid solution bubble is most, affects sample dissolution velocity and solute effect, can add a thermal insulation board or of short duration closedown hot plate if desired in the middle of the dual-purpose bottle of electric furnace and iron and steel.
(3) measure:
The first, the relevant parameter of instrument is determined. RF merit frequency generator 1.2KW; Cooling gas 14.0L/min; Plasma (orifice) gas 1.20L/min; Carrier gas 0.70L/L; Solvent clean time 50s; The time of integration 3s;
The second, the calibration of instrument: detect 5 emitted luminescence intensities for the standard sample solution S i of instrument calibration, Mn, P, Cr by plasma-speetrometer, by element emitted luminescence intensity and content drawing curve;
3rd, the detection of process control standard sample: utilize the content of Si, Mn, P, Cr in plasma-speetrometer detection process control standard sample; Linear coefficient R >=0.999 of each element and have at least 5 points on line during described drafting calibration curve;
4th, the detection of sample: utilize the content of plasma-speetrometer detection sample Si, Mn, P, Cr; In described assay method, the detection range of each element is Si:0.015～2.02%, Mn:0.010～2.36%, P:0.002～0.092%, Cr:0.008～2.88% respectively.
Sample catabolic process adopts the acid of specific molten sample, improves damage capability to sample, meanwhile, adopt dissolution in low temperature, it is ensured that the silicon in sample does not precipitate out, thus utilize in ICP spectrophotometer GCr15 the constituent contents such as Si, Mn, P, Cr at same mother solution.
Described assay method includes measuring process control (SPC) step, should again detect when the measured value of process control standard specimen occurs overproof with the nominal value of standard specimen or calibrate.
Embodiment 2
Other content such as embodiment 1, molten sample acid: perchloric acid (ρ=1.42g/ml)+nitric acid (ρ=1.19g/ml)=4.5+1
, low temperature 100 DEG C heating.
Embodiment 3
Other content such as embodiment 1, molten sample acid: perchloric acid (ρ=1.42g/ml)+nitric acid (ρ=1.19g/ml)=3.5+1
, low temperature 60 DEG C heating.
Embodiment 4
(1) reagent:
Molten sample acid: perchloric acid (ρ=1.42g/ml)+nitric acid (ρ=1.19g/ml)=4+1
(2) measuring process:
(2.1) weigh the steel standard specimen 5 (see table 1) of same or similar trade mark 0.1000g, be respectively placed in the dual-purpose bottle of 100ml iron and steel.
(2.2) solubilization sample acid 5ml, 80 DEG C of heating for dissolving of low temperature to tobacco in bottle drives to the greatest extent, limpid at the bottom of bottle, takes off, and add water 10mL, shakes up, and is cooled to room temperature;
(2.3) it is diluted to scale with water, shakes up to be measured.
(2.4) on ICP spectrogrph, each constituent content is detected.
(3) drafting of standard curve. (standard curve is shown in Fig. 1, Fig. 2, Fig. 3 and Fig. 4)
The table 1 steel standard specimen material for calibrating
(4) measuring process control (SPC)
Choose the standard substance 1 being not used in calibration, see table 2 below, prepare solution by measuring process (2). Immediately the standard substance of this SPC should be measured after instrument calibration.
Table 2 controls standard sample (spc)
Should again detect when the measured value of process control standard specimen occurs overproof with the nominal value of standard specimen or calibrate.
Test example
The present invention is respectively through carrying out detecting to standard substance and actual sample and analyzing, as follows:
Standard substance
Standard sample (the numbering: YSBC11217-94) being used as sample, detect by summary of the invention, testing result is in Table 3, table 4 that Iron and Steel Research Geueral Inst is produced by the present invention.
Table 3 method repeatability data
Table 4 method accuracy data
Testing result shows, in the present invention, assay method is reproducible, and accuracy is high.
Sample test
CSR Ziyang Locomotive Co., Ltd. matinal electromechanics submitted sample (numbering 20120230201, material GCr15) was detected by the present invention on February 16th, 2012, and detection data are in Table 5.
Table 5 sample detection data
Testing result shows, this sample meets technology requirement, meets expection.
The present invention is simple to operate, it is not necessary to preparation two set standard substance and sample solution, the dissolution velocity of sample is fast, it is not required that through operations such as filtration, separatory, work efficiency significantly improves. The present invention is prone to grasp simultaneously, it is simple to promote.
In the present invention, the calibration curve of each element adopts 5 different standard substances (see table 1), and the operation described in summary of the invention is measured and draws calibration curve, shown in below figure 1-4.
Can be seen that from above figure, the calibration curve dependency of each element of the present invention is good, Corr. in linearly dependent coefficient R(and Fig. 1～4 of each element alignment curve) it is all higher than 0.999, fully meet the requirement of standard GB/T20125-2006 " the mensuration ICP-AES of low-alloy steel multielement content ".
The present invention is by mixing the acid of molten sample through low-temperature decomposition sample with dense perchloric acid and nitric acid, and in same mother solution, the daughter spectrogrph such as employing ICP measures in GCr15 the constituent contents such as Si, Mn, P, Cr simultaneously, and method has obvious superiority. Simple to operate, it is easy to operation, in method, each element is linearly good, measurement result favorable reproducibility, and accuracy is high, and work efficiency significantly improves.
Claims (7)
1. detect the method for Si, Mn, P, Cr constituent content in GCr15 by plasma-speetrometer simultaneously, it is characterised in that: specifically comprise the following steps that
(1) molten sample acid: perchloric acid and nitric acid being mixed, the volume ratio of perchloric acid and nitric acid is 3.5-4.5:1;
(2) preparation of solution: include 5 some for the standard sample solution of instrument calibration, 1 the standard sample solution for measuring process control and sample solution, its operating process is to weigh sample 100mg in the dual-purpose bottle of 100mL iron and steel, add molten sample acid 5mL, on electric furnace, low-temperature heat adds water 10mL after dissolving, it is cooled to room temperature, it is diluted to scale with water, shakes up to be measured;
(3) measure:
The first, determine the relevant parameter of instrument: RF high frequency generator power 1.2KW, cooling gas flow 14.0L/min, plasma gas flow rate 1.20L/min, carrier gas flux 0.70L/L, solvent clean time 50s, the time of integration 3s;
The second, the calibration of instrument: detect 5 emitted luminescence intensities for the standard sample solution S i of instrument calibration, Mn, P, Cr by plasma-speetrometer, by element emitted luminescence intensity and content drawing curve;
3rd, the detection of process control standard sample: detect the content of Si, Mn, P, Cr in process control standard sample by plasma-speetrometer;
4th, the detection of sample: detect the content of sample Si, Mn, P, Cr by plasma-speetrometer;
Linear coefficient R >=0.999 of each element and have at least 5 points on line during instrument calibration described in testing result, for having detected.
2. plasma-speetrometer according to claim 1 detects the method for Si, Mn, P, Cr constituent content in GCr15 simultaneously, it is characterised in that: in described step (1), the volume ratio of perchloric acid and nitric acid is 4:1.
3. plasma-speetrometer according to claim 2 detects the method for Si, Mn, P, Cr constituent content in GCr15 simultaneously, it is characterised in that: 500ml perchloric acid and 125ml nitric acid are mixed by described step (1).
4. according to any one of claim 1-3, detect the method for Si, Mn, P, Cr constituent content in GCr15 by plasma-speetrometer simultaneously, it is characterised in that: described perchloric acid ρ=1.42g/ml, nitric acid ρ=1.19g/ml.
5. plasma-speetrometer according to claim 1 detects the method for Si, Mn, P, Cr constituent content in GCr15 simultaneously, it is characterised in that: low temperature described in step (2) is≤120 DEG C.
6. plasma-speetrometer according to claim 1 detects the method for Si, Mn, P, Cr constituent content in GCr15 simultaneously, it is characterised in that: the detection range of each element is Si:0.020～2.02%, Mn:0.010～2.36%, P:0.003～0.092%, Cr:0.008～2.88% respectively.
7. plasma-speetrometer according to claim 1 detects the method for Si, Mn, P, Cr constituent content in GCr15 simultaneously, it is characterised in that: should again detecting or calibrating when the measured value controlling standard specimen occurs overproof with the nominal value of standard specimen occur in the detection of described process control standard sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610029913.5A CN105675588B (en) | 2016-01-18 | 2016-01-18 | The method for detecting Si, Mn, P, Cr constituent content in GCr15 simultaneously with plasma spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610029913.5A CN105675588B (en) | 2016-01-18 | 2016-01-18 | The method for detecting Si, Mn, P, Cr constituent content in GCr15 simultaneously with plasma spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105675588A true CN105675588A (en) | 2016-06-15 |
| CN105675588B CN105675588B (en) | 2018-10-09 |
Family
ID=56301237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610029913.5A Active CN105675588B (en) | 2016-01-18 | 2016-01-18 | The method for detecting Si, Mn, P, Cr constituent content in GCr15 simultaneously with plasma spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105675588B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546574A (en) * | 2016-10-28 | 2017-03-29 | 山西太钢不锈钢股份有限公司 | The spectrum analyses and bearing calibration of trace nitrogen in a kind of steel |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101042349A (en) * | 2007-04-28 | 2007-09-26 | 云南出入境检验检疫局检验检疫技术中心 | Measuring method for harmful elements including lead, copper, chromium and cadmium in lotus root |
| CN101685081A (en) * | 2009-08-24 | 2010-03-31 | 云南出入境检验检疫局检验检疫技术中心 | Method for measuring various elements in food additive citric acid through ICP-MS |
| US20100229999A1 (en) * | 2009-03-10 | 2010-09-16 | Brennan Ryan G | System and Method For Automated Sample Introduction |
| CN102854180A (en) * | 2011-06-30 | 2013-01-02 | 中国石油天然气股份有限公司 | Method for detecting chromium content in chromium diethyl hexanoate by plasma emission spectrometry |
| CN103411960A (en) * | 2013-08-26 | 2013-11-27 | 核工业理化工程研究院 | Method for determining content of plurality of elements in high-silicon low-alloy steel by virtue of ICP (Inductively Coupled Plasma) spectrograph |
-
2016
- 2016-01-18 CN CN201610029913.5A patent/CN105675588B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101042349A (en) * | 2007-04-28 | 2007-09-26 | 云南出入境检验检疫局检验检疫技术中心 | Measuring method for harmful elements including lead, copper, chromium and cadmium in lotus root |
| US20100229999A1 (en) * | 2009-03-10 | 2010-09-16 | Brennan Ryan G | System and Method For Automated Sample Introduction |
| CN101685081A (en) * | 2009-08-24 | 2010-03-31 | 云南出入境检验检疫局检验检疫技术中心 | Method for measuring various elements in food additive citric acid through ICP-MS |
| CN102854180A (en) * | 2011-06-30 | 2013-01-02 | 中国石油天然气股份有限公司 | Method for detecting chromium content in chromium diethyl hexanoate by plasma emission spectrometry |
| CN103411960A (en) * | 2013-08-26 | 2013-11-27 | 核工业理化工程研究院 | Method for determining content of plurality of elements in high-silicon low-alloy steel by virtue of ICP (Inductively Coupled Plasma) spectrograph |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106546574A (en) * | 2016-10-28 | 2017-03-29 | 山西太钢不锈钢股份有限公司 | The spectrum analyses and bearing calibration of trace nitrogen in a kind of steel |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105675588B (en) | 2018-10-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102253030B (en) | Method for determining impurity content in high-titanium slag | |
| CN103175824B (en) | Inductively coupled plasma spectrometry transmitter measures the method for Silicon in Ferromanganese phosphorus content | |
| CN103926236B (en) | The method of impurity element and matrix element content of niobium in simultaneous determination ferrocolumbium | |
| CN104597037A (en) | Method for determining zirconium content in silicon-zirconium alloy | |
| CN103267754B (en) | The method of macroelement and arsenic, tin, antimony trace element in quantitative measurement carbon steel or low alloy steel | |
| CN102854179B (en) | Method for analyzing and detecting cadmium impurity element in tungsten or tungsten compound | |
| CN107290333A (en) | A kind of method that ICP AES methods determine impurity element in the special low titanium ferrophosphorus of high grade silicon steel | |
| CN108896536A (en) | Aluminium in a kind of high niobium aluminum titanium alloy, niobium, tungsten, chromium content measuring method | |
| CN106290318A (en) | ICP AES method measures the method for phosphorus magnesium-ferrum-aluminum silico-calcium titanium manganese content of strontium in phosphorus ore simultaneously | |
| CN104807813A (en) | Rapid analysis method for content of manganese in ferromanganese iron | |
| CN107271430A (en) | A kind of method of inductively coupled plasma atomic emission spectrometry to aluminium, silicon, phosphorus simultaneous determination in ferro-boron | |
| CN104237208A (en) | Method for measuring niobium content in iron ore | |
| CN108020541A (en) | The method of sulfur content in inductively coupled plasma emission spectrography measure ferrosilicon | |
| CN104777153A (en) | Rapid determination method for molybdenum content and tungsten content in tungsten-containing high-molybdenum product | |
| CN108872201A (en) | A kind of method of chromium, manganese content in measurement ferronickel | |
| CN108169214A (en) | A kind of method of lanthanum element in measure cobalt base superalloy | |
| CN105675588A (en) | Method for simultaneous detection of contents of Si, Mn, P, and Cr elements in GCr15 by using ICP plasma spectrometer | |
| CN105911051A (en) | Continuous determination method for calcium oxide and magnesium oxide in rare earth ore concentrate | |
| CN107192708A (en) | A kind of method of potassium and sodium in measure sefstromite concentrate | |
| CN103808791A (en) | Method for determining iron content in silicon nitride material | |
| CN105806826A (en) | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method | |
| CN106290438A (en) | A kind of X-ray fluorescence spectra fusion method measures the method for Calcium Fluoride Content in fluorite | |
| Mariet et al. | Relevance of NH4F in acid digestion before ICP-MS analysis | |
| CN110320201A (en) | The detection method of cobalt content in a kind of monel | |
| CN109030465A (en) | The detection method of the content of strontium, iron, barium, magnesium, calcium in a kind of zinc strontium alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |