CN109752366A - Method that is a kind of while measuring multielement content in potassium steel - Google Patents
Method that is a kind of while measuring multielement content in potassium steel Download PDFInfo
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- CN109752366A CN109752366A CN201910154461.7A CN201910154461A CN109752366A CN 109752366 A CN109752366 A CN 109752366A CN 201910154461 A CN201910154461 A CN 201910154461A CN 109752366 A CN109752366 A CN 109752366A
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Abstract
The present invention provides method that is a kind of while measuring multielement content in potassium steel, pass through the preparation and processing to sample, excitation measurement is carried out to it after spectrum trace, drift correction using glow discharge emission spectrometer, including following content: 1) the glow discharge emission spectrometer excitation voltage is 1250V, excitation current is 45mA, prespark period is 60s, time of integration 10s；2) potassium steel samples: it is required that sample composition is uniform, representative, and being free of and is mingled in sample, crackle, stomata, greasy dirt, dust, oxide；3) potassium steel sample preparation: it is required that sample is two-sided smooth, sample analysis face will carefully polish；4) ensure the purity and flow of analysis argon gas.The method of the invention has many advantages, such as that precision is high, detection limit is low, matrix effect is small, detectable concentration wide dynamic range, can detect that multiple elements, analysis time is short, sample pre-treatment is simple, no pollution to the environment simultaneously.
Description
Technical field
The present invention relates to chemical composition analysis technical fields, and in particular to a kind of to measure multielement content in potassium steel simultaneously
Method.
Background technique
Potassium steel has good work hardening ability, safe and reliable, wear-resisting, long-lived under HI high impact load.For a long time
Since, on the basis of being still trapped in chemical analysis test to the detection means of each element in potassium steel, existing traditional chemical wet process,
The content of single element in potassium steel can only be measured, and analytical cycle is long, cumbersome, agents useful for same has environment certain
Pollution；Technical staff also analyzes the constituent content in potassium steel using some instruments, such as glimmering using direct reading spectrometry or X-ray
Manganese in light spectrographic determination potassium steel；Or it is measured in potassium steel simultaneously using inductively coupled plasma emission spectrography
Several elements of silicon, manganese, phosphorus, chromium；But the method for measuring multielement content in potassium steel simultaneously in the prior art is very rare, together
When due in potassium steel manganese content it is higher, manganese and iron form complicated substrate, and the interference of matrix or coexistence elements keeps spectroscopic assay difficult
It is even more to be difficult to analyze to trace element therein to carry out.
Summary of the invention
Technical assignment of the invention is to be directed to the above the deficiencies in the prior art, and provide a kind of while measuring more in potassium steel
The method of constituent content.
The technical solution adopted by the present invention to solve the technical problems is: a kind of while measuring multielement content in potassium steel
Method, it is right after spectrum trace, drift correction using glow discharge emission spectrometer by the preparation and processing to sample
It carries out excitation measurement, including following content:
1) the glow discharge emission spectrometer excitation voltage be 1250V, excitation current 45mA, prespark period 60s,
Time of integration 10s；
2) potassium steel samples: it is required that sample composition is uniform, representative, and in sample without be mingled with, crackle, stomata,
Greasy dirt, dust, oxide；
3) potassium steel sample preparation: it is required that sample is two-sided smooth, sample analysis face will carefully polish, after polishing immediately with alcohol or
Acetone cleaning, hot blast drying, it is ensured that smooth clean is pollution-free, and analyzes and finish in four hours；
4) ensure 99.999% or more analysis purity of argon, argon flow ensures that point meter pressure is 280KPa.
Further, sample diameter is between 20~80mm in the step 3), and thickness is between 5~65mm.
Further, the element of measurement includes certain several element or the institute in C, Si, Mn, P, S, Cr, Ni, Mo, Cu, V, Ti
There is element.
Further, the concentrations range of each element is, based on mass fraction, C:0.002~2.50%；Si:0.002
~2.00%；Mn:0.005~25.00%；P:0.001~0.20%；S:0.001~0.15%；Cr:0.002~4.00%；
Ni:0.002~3.50；Mo:0.003~2.00%；Cu:0.002~1.20%；V:0.003~0.55%；Ti:0.001~
0.35%.
Further, as follows, C:165.701nm, 710V is arranged in each element wavelength, Photomultiplier tube voltage；Si:
288.158nm,900V；Mn:403.449nm, 680V；P:177.497nm, 900V；S:180.731nm, 900V；Cr:
267.716nm,900V；Ni:341.477nm, 825V；Mo:386.411nm, 900V；Cu:327.396nm, 900V；V:
411.179nm,900V；Ti:337.279nm, 900V；Internal standard element Fe:371.994nm, 600V.
Further, the glow discharge Atomic Emission Spectrometer AES is daily before carrying out any standardization or before measurement analysis
A trace must be run, trace uses iron-based sample, to adjust the exit slit position of glow spectrometer, it is ensured that maximum intensity
Light pass through.
Further, trace process is carried out using Fe371.994nm as internal standard line.
Further, the glow discharge Atomic Emission Spectrometer AES need to be floated using the standard substance of determining concentration daily
Shift correction, regular calibration working curve is to compensate long-term instrumental shift, in the continuous mode after drift correction, runs one or more
A standard substance determines the accuracy of the glow discharge Atomic Emission Spectrometer AES.
Further, in drift correction process accepted standard substance be SUS RH12-21, SUS RN13-78, SUS
RN14-56, SUS tetra- pieces of RN19-70 determining concentration standard substance.
The side of the present invention for measuring multielement content in potassium steel simultaneously using glow discharge Atomic Emission Spectrometer AES
Method, have precision is high, detection limit is low, matrix effect is small, detectable concentration wide dynamic range, can detect simultaneously multiple elements, point
The advantages that time is short, sample pre-treatment is simple, no pollution to the environment is analysed, carrying out to each element in potassium steel for efficiently and accurately is capable of
Measurement.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The fixed present invention.
Embodiment
The present embodiment instrument is GDS850A glow spectrometer (LECO company, the U.S.): 0.75m focal length；Paschen-
Runge bracket multiple tracks vacuum spectrometer；Grating line number is 2400/mm；Resolution ratio is 0.025nm；Wavelength be 119~
600nm；58 channels；Anode diameter is 4mm direct current (DC) glow discharge source and is equipped with 4mm radio frequency (RF) glow discharge source；Very
Empty set system；Entrance slit is 0.015nm；Exit slit is 0.040nm；Detector: photomultiplier tube (PMT).
Method that is a kind of while measuring multielement content in potassium steel, by the preparation and processing to sample, using aura
Electric discharge emission spectrometer carries out excitation measurement to it after spectrum trace, drift calibration, including following content:
1) instrument operating condition: experiment room temperature is 18~26 DEG C；Humidity is 20%~80%RH；Anode diameter is
4mm；Analysis working method is constant voltage-current system；Starting voltage is 1000V；The starting time is 3s；Excitation voltage is
1250V；Excitation current is 45mA；Prespark period is 60s；The time of integration is 10s；Integral number of times is 3 times；
2) potassium steel samples: it is required that sample composition is uniform, representative, and in sample without be mingled with, crackle, stomata,
Greasy dirt, dust, oxide, if in sample such as containing be mingled with, crackle, stomata, greasy dirt, dust, oxide, this kind of sample is close
Feng Shihui gas leakage makes the light intensity ejected variation cause measurement result inaccurate, even can not Discharge analysis when serious.Tool
Body sampling method is according to GB/T20066-2006 " sampling of steel and iron chemical composition sample and method for making sample " Lai Jinhang；
3) potassium steel sample preparation: it is required that sample diameter, between 20~80mm, thickness is between 5~65mm；It is required that sample is double
Face is smooth, and sample analysis face will carefully polish, and is cleaned immediately with alcohol or acetone after polishing, hot blast drying, it is ensured that smooth clean
It is pollution-free, and analyze and finish in four hours.When sample surfaces are not smooth enough, although sample can excite, excitation point
It is bad with the O-ring sealing of instrument, atrament can be left after the place excitation of contact, the light intensity ejected, which can decay, to die down
Cause measurement result inaccurate；According to GB/T4336-2016, " carbon steel and middle-low alloy steel multielement contain specific method for making sample
Spark discharge atomic emission spectrometry (conventional method) is determined in measurement " and the GB/T22368-2008 " survey of low-alloy steel multielement content
Determine glow discharge atomic emission spectrometry (conventional method) " sample preparation specification carry out；
4) ensure 99.999% or more analysis purity of argon, purification for argon device can be added to purify when necessary, avoid low-purity
Argon gas enters aura instrument, and argon flow ensures that point meter pressure is 280KPa；
Further, the element of measurement includes certain several element or the institute in C, Si, Mn, P, S, Cr, Ni, Mo, Cu, V, Ti
There is element.
Each element, wavelength, Photomultiplier tube voltage setting are as shown in table 1；
Each element working curve essential information (relative concentration of the Cx- analytical element in table, Ix- analysis elements as shown in table 2
The spectral intensity of element).To guarantee consistent spectra1 interfer- between more matrixes in the present invention, the analyst coverage of each element is expanded, is worked
Standard substance used in curve has low-alloy steel, stainless steel, potassium steel series, specific as follows: SS491-2, SS494-2, SS495-3
(BAS Ltd-UK, BAS company, Britain)；BS11B,BS12B,BS13B,BS14B,BS17A,BS18A,BS19A(Brammer
Standard Co.Inc.-USA, BS company, the U.S.)；NIST\1761,NIST\1762,NIST\1763,NIST\1764,
NIST\1765、NIST\1766、NIST\1767(National Institute of Standards and Technology-
USA, NIST company, the U.S.).
Further, one must be run before the glow discharge Atomic Emission Spectrometer AES standardizes daily or before measurement analysis
Secondary trace sample adjusts the exit slit position of glow spectrometer, it is ensured that the light of maximum intensity passes through, to improve analysis result
Accuracy carries out trace using Fe371.994nm as internal standard line in the present invention.
Further, the glow discharge Atomic Emission Spectrometer AES need to be floated using the standard substance of determining concentration daily
Shift correction, regular calibration working curve is to compensate long-term instrumental shift, in the continuous mode after drift correction, runs one or more
A standard substance determines the accuracy of the glow discharge Atomic Emission Spectrometer AES, the present invention using SUS RH12-21, SUS
RN13-78, SUS RN14-56, SUS the standard substance of tetra- pieces of RN19-70 determining concentration carry out drift correction.
It is needed after measurement to glow discharge Atomic Emission Spectrometer AES electrode alcohol swab cleaning, it is ensured that analysis work
It is continuous feasible.
In the embodiment of the present invention choose 3 pieces of different quality containings potassium steel standard substance GBW01642, GBW01643,
GBW01644 (analysis testing research institute, Iron and Steel Research Geueral Institute and Beijing NaKe Analytical Instrument Co., Ltd develop), according to the method
(after spectrum trace, drift correction) is measured in parallel 11 times, and measurement result and its relative standard deviation are shown in Table 3；It can by table 3
Know: measurement result is consistent with asserting value, and error is within the scope of the tolerance of standard substance certificate；11 times repetitive test is opposite
Standard deviation is 0.81%~9.7%, meets wanting for 2016 spark discharge Atomic Emission Spectral Analysis method general rule of GB/T14203-
It asks.
Table 1 measures element, wavelength, Photomultiplier tube voltage setting
2 each element working curve essential information of table
3 potassium steel standard sample measurement result of table and its relative standard deviation (n=11)
The operation principle of the present invention is that: in glow discharge emission spectrometer, sample itself is placed on anode as cathode
Front makes sample surfaces generate uniform sputtering by the argon ion that electromagnetic field accelerates.The atom sputtered out is in anode region and argon
Ion collision and be excited, generate sample composition element characteristic spectrum.The light of different wave length is divided and detects each monochromatic light
Light intensity obtains the intensity of each element by computer disposal.Pass through the working curve of each element that has built up (concentration and strong
The relationship of degree), computer calculates the concentration of each element automatically.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (9)
1. a kind of method for measuring multielement content in potassium steel simultaneously, it is characterised in that: by the preparation and processing to sample,
Excitation measurement is carried out to it after spectrum trace, drift correction using glow discharge emission spectrometer, in following
Hold:
1) the glow discharge emission spectrometer excitation voltage is 1250V, excitation current 45mA, prespark period 60s, integral
Time 10s；
2) potassium steel samples: it is required that sample composition is uniform, representative, and in sample without be mingled with, crackle, stomata, greasy dirt,
Dust, oxide；
3) potassium steel sample preparation: it is required that sample is two-sided smooth, sample analysis face will carefully polish, and use alcohol or acetone after polishing immediately
Cleaning, hot blast drying, it is ensured that smooth clean is pollution-free, and analyzes and finish in four hours；
4) ensure that 99.999% or more analysis purity of argon, flow ensure that argon gas divides meter pressure to be 280KPa.
2. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 1, it is characterised in that: described
Sample diameter is between 20~80mm in step 3), and thickness is between 5~65mm.
3. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 1, it is characterised in that: measurement
Element include certain several element or all elements in C, Si, Mn, P, S, Cr, Ni, Mo, Cu, V, Ti.
4. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 3, it is characterised in that: each member
Element concentrations range be, based on mass fraction, C:0.002~2.50%；Si:0.002~2.00%；Mn:0.005~
25.00%；P:0.001~0.20%；S:0.001~0.15%；Cr:0.002~4.00%；Ni:0.002~3.50；Mo:
0.003~2.00%；Cu:0.002~1.20%；V:0.003~0.55%；Ti:0.001~0.35%.
5. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 3, it is characterised in that: each member
Element, wavelength, Photomultiplier tube voltage setting are as follows, and each element wavelength, Photomultiplier tube voltage setting are as follows, C:165.701nm,
710V；Si:288.158nm, 900V；Mn:403.449nm, 680V；P:177.497nm, 900V；S:180.731nm, 900V；
Cr:267.716nm, 900V；Ni:341.477nm, 825V；Mo:386.411nm, 900V；Cu:327.396nm, 900V；V:
411.179nm,900V；Ti:337.279nm, 900V；Internal standard element Fe:371.994nm, 600V.
6. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 1, it is characterised in that: described
Glow discharge Atomic Emission Spectrometer AES must run a trace sample before carrying out any standardization or before measurement analysis daily,
Adjust the exit slit position of glow spectrometer, it is ensured that the light of maximum intensity passes through.
7. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 1, it is characterised in that: trace
Process carries out Fe371.994nm as internal standard line using iron-based sample.
8. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 1, it is characterised in that: described
Glow discharge Atomic Emission Spectrometer AES need to be daily using the standard substance progress drift correction for determining concentration, and regular calibration work is bent
Line is to compensate long-term instrumental shift, and in the continuous mode after drift correction, it is described to determine to run one or more standard substances
The accuracy of glow discharge Atomic Emission Spectrometer AES.
9. a kind of method for measuring multielement content in potassium steel simultaneously according to claim 8, it is characterised in that: drift
In correction course accepted standard substance be SUS RH12-21, SUS RN13-78, SUS RN14-56, SUS tetra- pieces of RN19-70
Determine the standard substance of concentration.
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| CN114113291A (en) * | 2020-08-25 | 2022-03-01 | 江苏隆达超合金航材有限公司 | Method for determining content of main element in multi-element alloy by using proportional coefficient correction glow mass spectrometry |
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