CN105004710B - A kind of stainless steel chromium, nickel element analytic set method - Google Patents
A kind of stainless steel chromium, nickel element analytic set method Download PDFInfo
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Abstract
The invention discloses a kind of stainless steel chromium, nickel element analytic set method, the actual content scope of nickel, chromium composition in being produced according to stainless steel has carried out the exploitation of standard specimen fabricating technology:Voluntarily develop the standard sample that suitable stainless steel production sample is examined;Sum up stainless steel nickel, chromium standard curve analytic set technology:It is determined by experiment stainless steel standard curve element interference calibration mode;Using the accuracy measurement method compared with science:The degree of accuracy test of measuring method is carried out on curve according to high, medium and low three contents section, sample is controlled to substitute the method that low-carbon control sample purchased in market controls stainless steel crude steel water sample using high carbon stainless steel, obtained data compare with classical chemical method, as a result satisfactory.This method stainless steel nickel, chromium analysis precision are better than the ﹙ r ﹚ of GB11170 2008 precision.
Description
Technical field
The present invention relates to a kind of stainless steel chromium, nickel element analytic set method, and in particular to a kind of spark discharge atom hair
Spectrum analysis stainless steel chromium, the method for nickel element analytic set are penetrated, belongs to the detection field of metallurgical samples.
Background technology
Nickel and chromium are alloy auxiliary materials that is crucial, being also costliness in stainless steel production, and larger specific gravity is accounted in holistic cost.
Nickel, chromium recovery rate are relatively low to mean that part of nickel, chromium are lost in vain, directly influences stainless steel production cost and the market competitiveness.
Steel mill nickel recovery rate and recovery rate of iron are according to melting down crude molten steel composition and product composition in stainless steel-making production process
What data were calculated.The elementary analysis composition degrees of accuracy such as the melting down test sample nickel of stainless steel, chromium directly influence stainless melting down
Steel scrap clearing, the exceeded quality control of steel scrap harmful element, steelmaking process nickel, evanohm input, and refining period composition degree of accuracy shadow
Ring to the control of nickel lower limit composition.Current check analysis method is using the stainless steel calibration curve built in instrument, stainless steel-making life
In production the analysis deviation of melting down crude molten steel nickel, chromium spectrum and chemical analysis fluctuated in the range of 0.20%, product analysis it is inclined
Difference is fluctuated in the range of 0.13%, it is impossible to the need for meeting enterprise's stainless steel cost efficiency and lower limit composition STEELMAKING PRODUCTION.
The content of the invention
The present invention is intended to provide a kind of stainless steel chromium, nickel element analytic set method, nickel, chromium member in being produced according to stainless steel
The actual content scope of plain composition, has carried out the exploitation of standard specimen fabricating technology, has summed up stainless steel nickel, chromium analytic set
Technology, reduces third element interference correction;The need for meeting enterprise's stainless steel cost efficiency and lower limit composition STEELMAKING PRODUCTION.
A kind of stainless steel chromium that the present invention is provided, nickel element analytic set method, comprise the following steps:
(1)Carry out standard specimen preparation technology:Realize the batch production of stainless steel optical spectrum standard sample
1. low-carbon sample block of being cast on remaining stainless steel water is wrapped in continuous casting:
By engineer testing, the design of sample casting model, the control of casting process temperature, molten steel flow speed are determined, using continuous casting
Casting sample block completes the batch production of low carbon stainless steel spectral standard sample on the middle remaining molten steel of bag;
2. under electric furnace ladle stainless steel crude molten steel cast high-carbon sample block:
This technical study has made a kind of special original mold, and the mould is manufactured by fine copper, using copper steel welding method by mould
4 units with water tank cooling system are made, entirety are then combined into by moulding process, using producing stainless steel process crude molten steel
Realize and cast simultaneously, realize the batch production of high-carbon stainless steel optical spectrum standard sample;
Use with loading block preparation technology, developing each analytical element content in curve standard sample has appropriate gradient, grinds
System control sample and steelmaking process and the same type of finished product detection sample;
(2)Stainless steel nickel, chromium standard curve analytic set method:
1. Ni, Cr element actual analysis demand adjust constituent content, the composition of the Cr elements in being produced according to stainless steel
Analyst coverage is 14.00%-26.00%, and the composition of Ni elements sets scope to be 4.00%-9.50%;Between strict control standard sample
The change of matrix iron content is no more than 5.00%;
Stainless steel nickel, chromium analysis curve are made, the demand of production detection is met, constituent content analysis is controlled one
Determine scope;
2. add and approached with sample stainless steel host element nickel, chromium composition in curve, the identical self-control of smelting process
Control sample and participate in tracing analysis calibration,
3. curve interference element calibration experiments:
Standard specimen point is calibrated not in curve by experiment plus interference element;Having for nickel element is disturbed in stainless steel:
Cr, Mn, Mo element, disturb having for Cr elements:Ni, Mn element;Homemade control sample participates in tracing analysis calibration, calibration curve
Middle appearance standard sample purchased in market and self-control control sample result are variant, general to use deletion standard sample results purchased in market to retain
The new method of self-control control sample result;
4. the checking of standard curve and measuring method degree of accuracy test:
The checking of standard curve is used checks slope of curve coefficient a close to 1, curve intercept system after curves shift correction
Number b is close to zero, and control sample host element composition carries out the measuring method degree of accuracy according to high, medium and low three contents section on curve
Checking, confirms that measured value can meet GB/T 11170-2008 sample tolerances, the standard of being unsatisfactory for need to be entered to elemental standards curve
Step refining is recalibrated;
Control sample to be compared before in same instrument and other control samples, to its recommendation carry out confirm and
Correct, confirm it is errorless after reuse;
5. measuring method precision is tested:Choose good Cr, Ni stainless steel standard specimen of one piece of uniformity and carry out precision reality
Test, on the curve that this analysis method is drawn, 10 parallel analysis are carried out to the standard specimen, precision meets GB/T 11170-
2008;
6. sample size is analyzed, and sample parallel analysis is no less than twice, and parallel analysis result absolute deviation meets GB/ twice
T11170-2008 precision repeatability limit r, quote result and take the average value analyzed twice, parallel analysis result is definitely inclined twice
Difference >=r, carries out third time analysis;
6. sample size is analyzed, and sample parallel analysis is no less than twice, and the absolute Pian Cha≤r of parallel analysis result, is reported twice
Go out result and take the average value analyzed twice, twice parallel analysis result absolute deviation >=r, carry out third time analysis;
(3)Control sample correction
The stainless steel low-carbon control sample control melting down crude molten steel process high-carbon sample of stainless steel, carbon is to stainless steel host element
Chromium, nickel element influence it is larger, substitute low-carbon control sample control purchased in market not using high carbon stainless steel control sample is voluntarily developed
The method that the rust melting down crude molten steel of steel completely newly controls sample.
A kind of stainless steel chromium that the present invention is provided, nickel element analytic set method, comprise the following steps:
1st, analysis prepares:Make to carry out analysis spectrometer before working curve:Rub through mirror, spark chamber clearly
Slit Dings Wei ﹙ Miao Ji ﹚ and lantern test, it is ensured that under instrument is in shape;
2nd, selection standard sample:Standard specimen fabricating technology is developed according to the present invention, the standard sample developed is selected,
Sample each element content has the control sample participation element song of appropriate gradient, selection control steelmaking process and finished product detection sample
Line analysis is calibrated.Standard sample element content range is detected above and below specified in stainless steel product technical conditions according to covering
Limit, main component element detection range bound outwards can suitably extend 10%-30%, and this method selection standard sample is used with composition
Uniformly, definite value accurately voluntarily develops standard sample, high carbon stainless steel and controls based on sample, to increase a part of standard sample purchased in market
Product;
3rd, the drafting of calibration curve
Control sample is commonly used in inspection will participate in the new method of calibration curve as far as possible, and calibration curve is frequently with primary line
Or secondary line, when conic section is negative parabola, curve high point easily causes result distortion, cautiously to use secondary negative parabola,
Typically without cubic curve;
4th, curve interference element calibration experiments, standard specimen point can carry out school not in curve by experiment plus interference element
Just:If standard sample purchased in market and the self-control quasi- ﹚ sample results of Kong ﹙ or Biao are variant, it is proposed that make Kong ﹙ or mark by oneself using retaining
Quasi- ﹚ sample results, typically delete standard sample results purchased in market.As disturbed having for nickel element in stainless steel:Cr, Mn, Mo, etc. member
Element, disturbs having for Cr elements:The elements such as Ni, Mn, plus interference element are prudent, and curve linear is good sometimes, but accuracy of analysis is not
It is high, it is contemplated that to be not added with interference element;
5th, the measuring method degree of accuracy is tested:In sample analysis the control sample close with analysis sample size should be used to carry out
Correction, it is prudent using control sample, use preceding control that will be close with similar steel grade, element component content on same instrument
Sample is compared, its recommendation is confirmed and corrected, confirm it is errorless after reuse.Sample host element composition according to it is high,
In, low three contents section on curve carry out degree of accuracy test;
6th, measuring method precision is tested:Choose good Cr, Ni stainless steel standard specimen of one piece of uniformity and carry out precision reality
Test, on the curve that this analysis method is drawn, 10 parallel analysis are carried out to the standard specimen, precision meets GB/T 11170-
2008;
7th, sample size is analyzed, and sample parallel analysis is no less than twice, and the absolute Pian Cha≤r of parallel analysis result, is reported twice
Go out result and take the average value analyzed twice, twice parallel analysis result absolute deviation >=r, carry out third time analysis.
Beneficial effects of the present invention:
Nickel, the actual content scope of chromium composition during the present invention is produced according to stainless steel, have carried out standard specimen preparation technology
Technological development, develops the control sample for meeting the required curve standard sample of stainless steel analysis and controlling sample survey, always
Stainless steel nickel, chromium analytic set technology are born, third element interference correction is reduced, is replaced using high carbon stainless steel control sample
The method that sample controls stainless steel crude steel water sample is controlled for low-carbon purchased in market, obtained data compare with classical chemical method,
As a result it is satisfactory.This method stainless steel nickel, chromium analysis precision are better than GB11170-2008 ﹙ r ﹚ precision, meet enterprise
The need for stainless steel cost efficiency and lower limit composition STEELMAKING PRODUCTION.
Brief description of the drawings
Fig. 1 does not add the nickel calibration curve of interference.
Fig. 2 adds the nickel calibration curve that chromium is disturbed.
Nickel element calibration curve built in Fig. 3.
Embodiment
With reference to implementing to make 304 series stainless steel element alignment curves, illustrate stainless steel chromium of the present invention, nickel element point
The embodiment of calibration method is analysed, but the embodiment of the present invention is not limited to following embodiments.
304 series stainless steel element alignment curves are made, for 304 series stainless steel production processes and product chemical composition
Analysis, wherein main element analysis scope:Chromium 14.00%-26%, nickel 4.00%-9.5%, its step is as follows:
1st, analysis prepares:Make before working curve to analytical equipment used:Carry out it is clear rub through mirror, spark chamber, slit and Ding Wei ﹙ retouch
Ji ﹚ and lantern test, it is ensured that under instrument is in shape, the analytical equipment of this method experiment are ARL-340 points of Switzerland
Analyse spectrometer;
2nd, selection standard sample
According to the melting down crude molten steel of 304 series stainless steels and product composition Cr, Ni elemental composition control range, curve is chosen
Standard sample includes:Voluntarily develop high carbon stainless steel control sample table 2, voluntarily develop standard sample table 3, increase a part of purchased in market
Standard sample(Table 1)
The standard sample purchased in market of table 1
The self-control control sample of table 2
Table 3 makes standard sample by oneself
3rd, the making of calibration curve:With each element relative intensity value average value to be measured to the element in standard sample with it is interior
The concentration ratio for marking element draws calibration curve, is illustrated below by taking the foundation of nickel element calibration curve as an example, spectrometer record storage
Deposit the raw intensity values of 23 standard sample nickel elements, corrected using conic section, standard sample 72-1,301,350,988,
The intensity level deflection curve of 182 nickel elements is deleted, and is not involved in nickel element calibration curve, and control sample participates in calibration curve, this
The change of method Plays sample matrices constituent content does not carry out matrix correction not less than 5%, Ni elemental profiles, and element Ni does not add dry
Disturb calibration curve and see Fig. 1.Fig. 1 represents concentration-strength relationship of nickel element.
4th, interference element correction test
Nickel element adds interference element correction test:Nickel adds Cr interference curves linear graph 2 to be better than not plus disturb using secondary line
Fig. 1, curve linear is good, but accuracy of analysis is not high, refers to Fig. 2.Fig. 2 represents corrected concentrations-strength relationship of nickel element.
5th, the measuring method degree of accuracy is tested:
(1)Using high carbon stainless steel control sample 2#, 137 replacement 3# purchased in market, 106 low-carbons control sample is voluntarily developed, control
The method of melting down crude molten steel 1#, 101-3 sample of stainless steel processed, reduction carbon is improved stainless to chromium, the influence of nickel element analysis
Steel nickel, such as the chromium spectrum analysis degree of accuracy, table 4:
Influence of the carbon of table 4 to chromium nickel element
(2)It is prudent using control sample, to be compared before on same instrument with other control samples, to it
Recommendation confirmed and corrected, confirm it is errorless after reuse;
(3)The calibration curve degree of accuracy is tested
1. degree of accuracy survey is carried out according to high, medium and low three contents section on Ni, Cr element alignment curve that this method is drawn
Examination, Ni elements are not added with interference element correction, Cr elements using conic section and use secondary analysis curve plus interference element Ni, Mn schools
Timing, the result of Cr, Ni elementary analysis is shown in Table 5 closer to standard value, as a result satisfactory test data:
The interference test data summarization of table 5
2. this method draws the stainless steel calibration curve curve degree of accuracy survey built in Ni, Cr element alignment curve and instrument
Although examination, the stainless steel calibration curve analysis result built in Fig. 3 instruments meets GB/T11170-2008 analysis requirement, but due to
The nickel element analyst coverage 0.001% of curve --- 35% is wider, exist nickel content section it is larger in 6.00%-8.50% analytical errors,
Two methods test 137,111,144,301 standard sample results and are shown in Table 6.
Table 6
Knot is analyzed from the two methods test No. of table 6 for 137,111,144,301 standard sample comparison result this method
The degree of accuracy of fruit is better than producer
6th, Precision Experiment
Choose 304 good stainless steel standard specimens of one piece of uniformity and carry out Precision Experiment.Under the analysis condition that experiment is determined
On the working curve drawn, 10 parallel analysis are carried out to the standard specimen, measurement result is shown in Table 7.
The Precision Experiment data of table 7
In table 7, the result extreme difference of 10 tests is far smaller than the precision requirement of national standard, and RSD is relatively low, illustrates institute
The program of foundation has good analysis precision.
7th, sample size is analyzed, and sample parallel analysis is no less than twice, twice parallel analysis result:
Absolute Pian Cha≤r, quotes result and takes the average value analyzed twice, twice parallel analysis;
As a result absolute deviation >=r, carries out third time analysis.
8th, conclusion
According to GB/T11170-2008 standards, the present invention using homemade curve standard sample draw refinement stainless steel nickel,
Chromium analytic set curve, standard sample nickel, chromium composition and sample composition are close, are rationally disturbed using setting
Correcting mode, science calibration curve accuracy measurement method, using voluntarily developing, high carbon stainless steel control sample replacement is purchased in market low
The method that the carbon control sample control melting down crude molten steel of stainless steel completely newly controls correcting sample, improves stainless steel nickel, chromium spectrum
Accuracy of analysis, is controlled within ± 0.06% using the deviation of nickel element spectrum and chemical analysis results in this method stainless steel.
Chromium deviation is controlled within ± 0.08%.
A kind of stainless steel chromium of the present invention, nickel element calibration curve and spark discharge Atomic Emission Spectral Analysis method, are also fitted
The other elemental profiles calibrations of stainless steel and spectrum analysis are closed, this method is adapted to all kinds spark discharge Atomic Emission Spectrometer AES,
It can also be used for other analysis spectrometer elemental profiles calibrations and analyze, there is higher practical value.
Claims (4)
1. a kind of stainless steel chromium, nickel element analytic set method, it is characterised in that:Comprise the following steps:
(1)Carry out standard specimen preparation technology:Realize the batch production of stainless steel optical spectrum standard sample
1. low-carbon sample block of being cast on remaining stainless steel water is wrapped in continuous casting:
By engineer testing, the design of sample casting model, the control of casting process temperature, molten steel flow speed are determined, is wrapped using in continuous casting
Casting sample block completes the batch production of low carbon stainless steel spectral standard sample on remaining molten steel;
2. under electric furnace ladle stainless steel crude molten steel cast high-carbon sample block:
Research has made a kind of special original mold, and original mold is manufactured by fine copper, mould is made using copper steel welding method cold with water tank
But 4 units of system, are then combined into entirety by moulding process, are realized and poured simultaneously using producing stainless steel process crude molten steel
Casting, realizes the batch production of high-carbon stainless steel optical spectrum standard sample;
Develop standard sample and analysis sample smelting process, to constitute structure identical, according to the melting down crude molten steel of stainless steel and product into
Part Cr, Ni elemental composition control range, develops corresponding standard sample;
(2)Stainless steel nickel, chromium standard curve analytic set method
1. Ni, Cr element actual analysis demand determine Ni, Cr elementary analysis scope in being produced according to stainless steel, strictly control standard
The change of sample room matrix iron content is no more than 5.00%;
Stainless steel nickel, chromium standard curve are made, the demand of production detection is met;
2. add and approached with sample stainless steel host element nickel, chromium composition in curve, the identical homemade control of smelting process
Sample preparation product simultaneously participate in tracing analysis calibration;
3. interference element calibration experiments:
Standard specimen point is calibrated not in curve by experiment plus interference element;Having for nickel element is disturbed in stainless steel:Cr、Mn、
Mo elements, disturb having for Cr elements:Ni, Mn element;
4. the checking of standard curve and measuring method degree of accuracy test:
The checking of standard curve is used checks slope of curve coefficient a close to 1 after curves shift correction, and curve intercept coefficient b connects
Nearly zero, control sample host element composition carries out measuring method accuracy validation according to high, medium and low three contents section on curve,
Confirm that measured value can meet GB/T 11170-2008 sample tolerances, the standard of being unsatisfactory for need to be further thin to elemental standards curve
Change and recalibrate;
5. measuring method precision is tested:Choose good Cr, Ni stainless steel standard specimen of one piece of uniformity and carry out Precision Experiment,
On the curve that this analysis method is drawn, 10 parallel analysis are carried out to the standard specimen, precision meets GB/T 11170-2008;
6. sample size is analyzed, and sample parallel analysis is no less than twice, and parallel analysis result absolute deviation meets GB/ twice
T11170-2008 precision repeatability limit r, quote result and take the average value analyzed twice, parallel analysis result is definitely inclined twice
Difference >=r, carries out third time analysis;
(3)Control sample correction
The low-carbon control sample control melting down crude steel water sample of stainless steel purchased in market is substituted using high carbon stainless steel control sample is voluntarily developed
The method of product.
2. stainless steel chromium, nickel element analytic set method according to described in claim 1, it is characterised in that:The chromium, nickel element
Standard curve analyst coverage:Cr is 14.00%-26.00%, and Ni is 4.00%-9.50%;Above and below chromium, nickel element standard curve range
Limit outwards can suitably extend 10%-30%.
3. stainless steel chromium, nickel element analytic set method according to described in claim 1, it is characterised in that:The step(2)The
2. in walking, occur standard sample purchased in market in calibration curve and self-control control sample result is variant, using deletion standard sample purchased in market
Product result, the method for retaining self-control control sample result.
4. stainless steel chromium, nickel element analytic set method according to described in claim 1, it is characterised in that:The step(2)The
3. in walking, by disturbing the degree of accuracy to test, Ni elements do not add interference calibration to use secondary analysis curve, and Cr elements add Ni, Mn member
Element, interference correction uses secondary analysis curve.
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