CN116359466A - Method for measuring oxygen content in Fe-Si-Al magnetic alloy - Google Patents
Method for measuring oxygen content in Fe-Si-Al magnetic alloy Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000001301 oxygen Substances 0.000 title claims abstract description 122
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 64
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 55
- 229910002796 Si–Al Inorganic materials 0.000 title claims abstract description 45
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 claims abstract description 33
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 31
- 239000010959 steel Substances 0.000 claims abstract description 31
- 238000004164 analytical calibration Methods 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 17
- 230000010354 integration Effects 0.000 claims abstract description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 45
- 238000004458 analytical method Methods 0.000 claims description 24
- 238000012360 testing method Methods 0.000 claims description 23
- 239000002775 capsule Substances 0.000 claims description 19
- 238000005259 measurement Methods 0.000 claims description 17
- 229910000702 sendust Inorganic materials 0.000 claims description 15
- -1 iron-silicon-aluminum Chemical compound 0.000 claims description 11
- 230000004907 flux Effects 0.000 claims description 10
- 239000012086 standard solution Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 239000011261 inert gas Substances 0.000 abstract description 5
- 229910002651 NO3 Inorganic materials 0.000 abstract description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 4
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004566 IR spectroscopy Methods 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 17
- 229910052759 nickel Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 238000000691 measurement method Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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Abstract
The invention provides a method for measuring the oxygen content in Fe-Si-Al magnetic alloy, which comprises the following steps: performing instrument calibration by using a steel standard sample or a potassium hydrogen phthalate reference reagent; accurately weighing a sample of the Fe-Si-Al magnetic alloy to be measured in a fluxing agent; compacting and folding a fluxing agent containing a sample to be detected into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the particles, wherein the signal integration area of the particles is marked as A; according to the formula w= (A-A KB ) The oxygen content W in the sample was calculated by/(mXK), where A KB The integral area of the blank signal is the method blank signal containing fluxing agent, and K is the instrument calibration coefficient. The method for measuring the oxygen content in the Fe-Si-Al magnetic alloy can accurately detect the oxygen content in the Fe-Si-Al magnetic alloy sample; the standard reagent of nitrate or dichromate which is easy to explode is not needed, and the safety coefficient is high; fills the blank of measuring the oxygen content in the Fe-Si-Al magnetic alloy by the inert gas melting infrared spectrometry, and has good application effect.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for measuring oxygen content in Fe-Si-Al magnetic alloy.
Background
The Fe-Si-Al magnetic alloy is an alloy powder material with 82% -88% of iron, 7% -10% of silicon and 5% -7% of aluminum as basic components, has the granularity reaching-50 meshes (0.30 mm) to-500 meshes (0.025 mm), has the advantages of high DC bias magnetic resistance, high energy conversion efficiency, low hysteresis expansion coefficient, low temperature rise effect, low magnetic core loss and the like, and can be used for manufacturing soft magnetic powder cores, inversion reactors, high-frequency power filters, smooth chokes, wave absorbing materials and other products.
The impurity components of the Fe-Si-Al magnetic alloy mainly exist in the forms of oxides such as alumina, silicon oxide and the like, and directly influence the electromagnetic performance of the Fe-Si-Al magnetic alloy. If the oxygen content can be accurately and rapidly measured, the method is an effective section for indirectly characterizing the total impurity amount and performing quality inspection. However, the physical and chemical properties of the material form, the matrix composition, the melting point, the magnetism and the like are obviously different from those of steel, so that the analysis method related to the oxygen content in the steel is not applicable to the Fe-Si-Al magnetic alloy.
The method for measuring the oxygen content in the Fe-Si-Al magnetic alloy is not found in the standards of Fe-Si-Al alloy products such as YS/T1485-2021 (Fe-Si-Al-based composite wave absorbing material) and T/ZZB 2425-2021 (Fe-based electromagnetic wave absorbing composite material) and related journal or conference documents, and particularly the method for measuring the oxygen content in the Fe-Si-Al magnetic alloy by using an inert gas melting infrared spectrometry is not found.
In view of this, the present invention has been made.
Disclosure of Invention
The invention solves the technical problems that: the prior art is not suitable for the practical problems of incomplete oxygen content release, low measured value, use of nitrate or dichromate reference reagent which is easy to explode, and the like of the Fe-Si-Al magnetic alloy sample form and the oxygen content range.
The invention provides a method for measuring the oxygen content in an iron-silicon-aluminum magnetic alloy, which fully considers the influence of the sample amount of the iron-silicon-aluminum magnetic alloy on a measuring result, establishes an instrument calibration coefficient by adopting a steel standard sample or a potassium hydrogen phthalate reference reagent, accurately weighs 80-100mg of the iron-silicon-aluminum magnetic alloy sample to wrap in a tin capsule, uses a graphite crucible to measure under the analysis power of 5.0kW, and automatically obtains the oxygen content of the iron-silicon-aluminum magnetic alloy by the instrument after deducting the blank value of the tin capsule.
A method for measuring the oxygen content in Fe-Si-Al magnetic alloy includes: 1) Performing instrument calibration by using a steel standard sample or a potassium hydrogen phthalate reference reagent; 2) Accurately weighing a sample of the Fe-Si-Al magnetic alloy to be measured in a fluxing agent; 3) Compacting and folding a fluxing agent containing a sample to be detected into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the particles, wherein the signal integration area of the particles is marked as A; 4) According to the formula w= (A-A KB ) Calculating the oxygen content W in the Fe-Si-Al magnetic alloy sample, wherein m is the actual weighing mass of the sample, A KB The signal integration area is blank for the flux-containing method, and K is the instrument calibration coefficient.
Preferably, when the instrument calibration is performed using a steel standard sample, step 1) includes: s11, setting instrument parameters; s12, deducting system blank; s13, establishing a calibration coefficient; s14, blank deduction method.
Preferably, the analytical power of the instrument set in S11 is 4.5-5.5kW.
Preferably, when the instrument calibration is performed using a steel standard sample, S12 is specifically: setting the analysis power to 4.0-4.5kW, measuring the blank values of the graphite crucible and the instrument pipeline, selecting the blank test result of the system,and subtracted according to the signal integral area of oxygen, the blank signal integral area of the system is marked as A KB0 。
Preferably, when the instrument calibration is performed using a steel standard sample, S14 is specifically: setting the analysis power to 4.5-5.5kW, compacting and folding the fluxing agent into particles, then putting the particles into a gas analyzer to measure the oxygen content, selecting the blank test result of the method, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area is marked as A KB1 。
Preferably, when the instrument calibration is performed using a steel standard, S13 includes: s131, selecting and accurately weighing a steel standard sample with known oxygen content and the oxygen content ratio of 0.1-1 in the Fe-Si-Al magnetic alloy to be measured, wherein the mass of the steel standard sample is recorded as m B The method comprises the steps of carrying out a first treatment on the surface of the S132, putting the standard sample into a gas analyzer to measure the oxygen content, and recording the signal integral area as A B The method comprises the steps of carrying out a first treatment on the surface of the S133, selecting the measurement result of the standard sample, and inputting the oxygen content identification value W of the standard sample B According to the following formula K 1 ＝(A B -A KB0 )/(m B ×W B ) Establishing instrument calibration coefficients, wherein A KB0 The signal integration area for system blanking.
Preferably, when performing instrument calibration with a potassium hydrogen phthalate reference reagent, step 1) comprises: s11, setting instrument parameters; s12, deducting a method blank; s13, establishing a calibration coefficient.
Preferably, the analytical power of the instrument set in S11 is 4.5-5.5kW.
Preferably, when the instrument calibration is performed using a potassium hydrogen phthalate reference reagent, S12 is specifically: setting the analysis power to 4.5-5.5kW, compacting and folding the fluxing agent into particles, then putting the particles into a gas analyzer to measure the oxygen content, selecting the blank test result of the method, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area is marked as A KB2 。
Preferably, when the instrument calibration is performed using a potassium hydrogen phthalate reference reagent, S13 includes: s131, accurately weighing a certain amount of the mixture with the purity of (100+/-0.05)Potassium hydrogen phthalate reference reagent (C) 8 H 5 O 4 K) Preparing potassium hydrogen phthalate standard solution with pure water, wherein the mass concentration is marked as C P The method comprises the steps of carrying out a first treatment on the surface of the S132, quantitatively injecting V into the fluxing agent P The potassium hydrogen phthalate standard solution is dried at 100-120 ℃; s133, calculating the theoretical value W of the oxygen content of the potassium hydrogen phthalate P ＝C P ×V P ×10 -5 X 31.34%; s134, inputting sample mass m into the instrument P The flux containing potassium hydrogen phthalate is put into a gas analyzer to measure the oxygen content, and the signal integral area is marked as A P The method comprises the steps of carrying out a first treatment on the surface of the S135, selecting the above potassium hydrogen phthalate test result, and inputting the theoretical value of oxygen content (W P ) According to K 2 ＝(A P -A KB2 )/(m P ×W P ) Establishing instrument calibration coefficients, wherein A KB2 The signal integration area is blank for the flux-containing method.
Preferably, the weight of the iron-silicon-aluminum magnetic alloy sample is 80-120mg.
Preferably, the fluxing agent is tin capsules.
Compared with the prior art, the method for measuring the oxygen content in the Fe-Si-Al magnetic alloy has the following beneficial effects: 1) The detection limit of the measuring method is 0.003%, the quantitative limit is 0.010%, the relative standard deviation of the actual measuring result is less than 7%, the standard recovery rate is 90% -109%, and the oxygen content of the powdery Fe-Si-Al magnetic alloy sample can be accurately detected; 2) Nitrate or dichromate is not needed, so that the safety coefficient is high; 3) Fills the blank of measuring the oxygen content in the Fe-Si-Al magnetic alloy by the inert gas melting infrared spectrometry, and has good application effect.
Drawings
FIG. 1 shows the effect of the sample size on the oxygen content measurement result in the Fe-Si-Al magnetic alloy.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. It should be noted that the features of the various embodiments of the invention may be combined with each other without conflict.
Because the physical and chemical properties of the iron-silicon-aluminum magnetic alloy, such as material morphology, matrix composition, melting point, magnetism and the like are obviously different from those of steel, the existing analysis method for the oxygen content in the steel cannot be suitable for measuring the oxygen content in the iron-silicon-aluminum magnetic alloy; for example, the GB/T11261-2006 pulse heating inert gas melting-infrared absorption method for determining the oxygen content of iron and steel requires that a round bar sample be prepared (see GB/T11261-2006, 6.1), and the sample amount be limited to 0.5-1.0g (see GB/T11261-2006, 8.1), and the detection requirement of the form of the Fe-Si-Al magnetic alloy powdery sample cannot be met. YB/T4305-2012 (determination of oxygen content of iron and Steel and alloy) the inert gas melting-infrared absorption method prescribes a determination range of 0.00075% -0.010%, and the actual range of the oxygen content in the Fe-Si-Al magnetic alloy is not less than 0.020% in general; and clause 7.2 of YB/T4305-2012 defines a sample amount of about 1.0g, the base composition of the sample used in appendix a differs significantly from that of the sendust, and is not suitable for oxygen determination in sendust powder in the form of high melting point alumina and silica impurities, resulting in incomplete oxygen release and low measured values. In addition, YB/T4305-2012 uses a potassium nitrate calibration instrument, and the reagent is a strong oxidant, has combustion supporting and explosion hazard and is strictly regulated by being listed in a list of easy explosion hazard chemicals. For this, the applicant proposes the following technical solutions:
for convenience of explanation, the following description will be first made on related materials used in the present specification: tin capsule A (Φ5mm×11mm, mass 0.15-0.20 g), tin capsule B (Φ6mm×16mm, mass 0.25-0.30 g), tin capsule C (Φ6mm×11mm, mass 0.08+ -0.01 g), steel standard sample A (oxygen content of 0.0241%), steel standard sample B (oxygen content of 0.0112%), steel standard sample C (oxygen content of 0.014%), and steel standard sample D (oxygen content of 0.0197%).
Example 1
A method for measuring the oxygen content in Fe-Si-Al magnetic alloy includes:
1) The method adopts a steel standard sample to calibrate the instrument, and specifically comprises the following steps:
s11, setting instrument parameters: setting the degassing power of the instrument to be 5.5kW, the analysis time to be 40s, the comparison level to be 20mV or the comparator level to be 3%, the minimum integration time to be 30s and the maximum integration time to be 60s;
s12, deducting system blank, specifically comprising: s121, setting analysis power to be 4.0kW; s122, inputting 500mg of sample mass into an instrument; s123, measuring blank values of the graphite crucible and an instrument pipeline, and independently measuring at least 2 times in parallel; s124, selecting the blank test result of the system, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area of the system is marked as A KB0 ；
S13, establishing a calibration coefficient, specifically:
s131, selecting a steel standard sample with known oxygen content and the oxygen content ratio of 0.1-1 in the Fe-Si-Al magnetic alloy to be detected; s132, accurately weighing 0.5g of the steel standard sample, and inputting the actual weighing mass (marked as m) into an instrument B ) The method comprises the steps of carrying out a first treatment on the surface of the S133, the standard sample is put into a gas analyzer to measure the oxygen content, and is independently measured for at least 2 times in parallel, and the signal integral area is recorded as A B The method comprises the steps of carrying out a first treatment on the surface of the S134, selecting the measurement result of the standard sample, and inputting the oxygen content identification value (denoted as W B ) According to the following formula K 1 ＝(A B -A KB0 )/(m B ×W B ) And establishing an instrument calibration coefficient.
S14, blank deduction method, specifically: s141, setting analysis power to be 5.0kW; s142, inputting 100mg of sample mass into an instrument; s143, compacting and folding the tin bag into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the tin bag, wherein the oxygen content is independently measured for at least 2 times in parallel; s144, selecting the blank test result of the method, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area is marked as A KB1 。
2) A sample assay comprising:
s21, accurately weighing 80-100mg of the Fe-Si-Al magnetic alloy sample to be measured in a tin bag, and inputting the actual weighing mass (recorded as m) into an instrument;
s22, compacting and folding a tin bag containing a sample to be tested into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the tin bag, wherein the signal integral area is recorded as A;
s23, according to the sample mass (m) and the signal integration area (A) of oxygen, combining the calibration coefficient instrument established in the step one according to the ratio of W= (A-A) KB1 )/(m×K 1 ) And calculating the oxygen content of the sample.
Example 2
A method for measuring the oxygen content in Fe-Si-Al magnetic alloy includes:
1) The instrument calibration is carried out by adopting a potassium hydrogen phthalate reference reagent, and specifically comprises the following steps:
s11, setting instrument parameters: setting the degassing power of the instrument to be 5.5kW, the analysis power to be 5.0kW, the analysis time to be 40s, the comparison level to be 20mV or the comparator level to be 3%, the minimum integration time to be 30s and the maximum integration time to be 60s;
s12, deducting a blank of a method, specifically comprising the following steps: s121, inputting 100mg of sample mass into an instrument; s122, folding the tin bag into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the tin bag, wherein the oxygen content is independently measured for at least 2 times in parallel; s123, selecting the blank test result of the method, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area is marked as A KB2 。
S13, establishing a calibration coefficient, which specifically comprises the following steps:
s131, accurately weighing a certain amount of potassium hydrogen phthalate reference reagent (C) with the purity of (100+/-0.05) 8 H 5 O 4 K) Preparing a potassium hydrogen phthalate standard solution with the mass concentration of about 10mg/mL by adopting high-purity water with the resistivity of not less than 18MΩ & cm, wherein the accurate actual mass concentration is recorded as C P ；
S132, quantitatively injecting the potassium hydrogen phthalate standard solution into the tin capsule by adopting a 10-50 mu L micropipette, wherein the injection volume is recorded as V P And drying at 110 ℃;
s133, calculating the theoretical value W of the oxygen content of the potassium hydrogen phthalate P ＝C P ×V P ×10 -5 ×31.34％；
S134, the mass of the input sample in the instrument is 100mg (denoted as m P ) The tin capsule containing potassium hydrogen phthalate is put into a gas analyzer to measure the oxygen content, and the oxygen content is measured at least 2 times independently in parallel, and the signal integral area is recorded as A P ；
S135, selecting the above potassium hydrogen phthalate test result, and inputting the theoretical value of oxygen content (W P ) According to K 2 ＝(A P -A KB2 )/(m P ×W P ) And establishing an instrument calibration coefficient.
2) A sample assay comprising:
s21, accurately weighing 80-100mg of the Fe-Si-Al magnetic alloy sample to be measured in a tin bag, and inputting the actual weighing mass (recorded as m) into an instrument;
s22, compacting and folding a tin bag containing a sample to be tested into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the tin bag, wherein the signal integral area is recorded as A;
s23, according to the sample mass (m) and the signal integration area (A) of oxygen, combining the calibration coefficient instrument established in the step one according to the ratio of W= (A-A) KB2 )/(m×K 2 ) And calculating the oxygen content of the sample.
The method blank test was continuously performed 10 times in the same manner as in example 1 or 2 and the standard deviation of the method blank value was calculated, and the detection limit and the quantitative limit of the method were obtained at 3 times and 10 times the standard deviation, and the results are shown in Table 1.
TABLE 1 method blank, detection limit and quantification limit (mass fraction,%)
| Carrying container (flux) | Calibration method | Blank value ±Standard deviation (n=10) | Detection limit | Quantitative limit |
| Tin bag A | Example 1 | 0.0119±0.0011 | 0.0033 | 0.011 |
| Tin bag B | Example 1 | 0.0094±0.0010 | 0.0031 | 0.010 |
| Tin bag C | Example 1 | 0.0080±0.0012 | 0.0036 | 0.012 |
| Tin bag A | Example 2 | 0.0115±0.0011 | 0.0031 | 0.011 |
| Tin bag B | Example 2 | 0.0090±0.0010 | 0.0030 | 0.010 |
| Tin bag C | Example 2 | 0.0077±0.0012 | 0.0035 | 0.012 |
As is clear from Table 1, the detection limit of the measurement method of the present invention was 0.003%, and the quantitative limit was 0.010%.
The measurement was repeated 6 times by taking different sendust samples according to the method of example 1 or 2 and the Relative Standard Deviation (RSD) of the calculated results was used as precision, and the results are shown in table 2.
TABLE 2 determination of oxygen content in actual samples of Fe-Si-Al magnetic alloys
As is clear from Table 2, the relative standard deviation of the results obtained by the corresponding measurement methods of examples 1 and 2 of the present invention was less than 7%, and the precision was good.
To the tin capsule, 10. Mu.L of potassium hydrogen phthalate standard solution (10.105 mg/mL) was quantitatively injected, and the mixture was dried at 110℃for 1 hour, with a theoretical addition amount of oxygen of 31.7. Mu.g. 80-100mg of H# sample is accurately weighed into the tin bag containing the trace potassium hydrogen phthalate, the actual weighing mass of the H# sample is input, the background quantity of oxygen is obtained according to the data in the table 2, the oxygen content of the trace potassium hydrogen phthalate and the H# sample is measured by the method, the measured total quantity, the recovery quantity and the recovery rate of the oxygen are calculated, and the result is shown in the table 3.
TABLE 3 labeling recovery test results of actual samples of Fe-Si-Al magnetic alloys
As shown in Table 3, the standard recovery rate of the measurement methods of examples 1 and 2 of the present invention is between 90% and 109%, and the measurement methods have good accuracy.
The calibration coefficient of the instrument was determined as in example 1 or 2, the analysis power was adjusted to 4.0kW, and steel standard samples of different materials, components, and oxygen contents were measured at the calibration coefficient and analysis power to verify the accuracy of the calibration coefficient, and the results are shown in table 4.
TABLE 4 determination of oxygen content in Steel Standard samples
As can be seen from Table 4, the measurement results of the steel standard samples are all within the uncertainty range of the measurement of the identification value, which shows that the calibration coefficient obtained by the instrument calibration method provided by the invention is accurate and reliable.
The determination method in the above embodiment 1 or 2 can accurately detect the oxygen content of the sendust, especially the oxygen content with the mass fraction of 0.02% to 0.2%, solve the practical problems that the prior art is not suitable for the form and the oxygen content range of sendust samples, the oxygen content release is incomplete and the measured value is low, and nitrate or dichromate is used to easily make explosion dangerous chemicals, and the like, and provide a rapid, accurate and safe method for determining the oxygen content and indirectly checking impurities in sendust.
Experimental example 1 influence of sample amount on measurement result
Taking 64# and H # iron-silicon-aluminum magnetic alloy actual samples as examples, experiments were carried out according to the measurement method of example 1, and the influence of different sample amounts on the measurement result of the oxygen content in the iron-silicon-aluminum magnetic alloy is shown in FIG. 1, wherein 4.5kW of analysis power is used for 64# and 5.0kW of analysis power is used for H #.
From this, it can be seen that: (1) At an analytical power of 4.5kW, the sample size significantly influences the oxygen measurement. The sample weighing is within the range of 50-120mg, the sample and the fluxing agent are completely melted, the melt is sintered into a sphere or a hemisphere, and the measurement result is stabilized at a higher level; with increasing sample weight, part of the sample was not completely melted, slag was found as powdery residue, and high-melting point oxides such as silica and alumina were not sufficiently melted and completely decomposed in a short time, and the oxygen release peak shape was widened, the profile was deteriorated, and the release rate and the measured value were lowered to 80% or less of normal value. (2) At an analytical power of 5.0kW, a larger sample size still leads to a broadening of the oxygen release peak shape and a deterioration of the profile. In order to ensure that the sample is fully melted and oxygen is fully released and improve the precision of the method, the sample size of the Fe-Si-Al magnetic alloy must be controlled between 50 and 120mg, and the optimal sample size range is 80 to 100mg.
Experimental example 2 analysis of Power Effect on measurement results
Taking H# practical samples as an example, tests were carried out according to the measurement methods of examples 1 or 2, and the influence of different analysis powers on the measurement results of the oxygen content in the Fe-Si-Al magnetic alloy is given, and the results are shown in tables 5 and 6. Table 5 results of comparative tests of oxygen content in FeSiAl magnetic alloys at different analytical powers (example 1)
Table 6 results of comparative tests for oxygen content in FeSiAl magnetic alloys at different analytical powers (example 2)
As can be seen from tables 5 and 6, the analysis power is required to be 4.5-5.5kW, and the result of the measuring method is more accurate and reliable. Preferably, the analytical power is 5.0kW.
Experimental example 3 Effect of fluxing agent on measurement results
Taking an H# Fe-Si-Al magnetic alloy actual sample as an example, testing according to the testing method of the embodiment 1 or 2, and the corresponding testing results of different bearing containers (fluxing agents) are shown in tables 7 and 8; wherein the test results have been determined and subtracted from the blank values of the different carrying containers (fluxing agents) respectively.
TABLE 7 comparative test results of oxygen content in Fe-Si-Al magnetic alloy for different carrying vessels (fluxing agent) (example 1)
| Sample of | Carrying container (flux) | Measurement/% | Average/% | RSD/％ |
| H# | Tin bag A | 0.125,0.129,0.123 | 0.126 | 2.1 |
| H# | Tin bag B | 0.126.0.129,0.132,0.125 | 0.128 | 2.5 |
| H# | Tin bag C | 0.120,0.135,0.127,0.126 | 0.127 | 4.6 |
| H# | Tin bag C + tin sheet (bath) | 0.120,0.132,0.122,0.126 | 0.125 | 3.9 |
| H# | Tin bag C+nickel bag (bath) | 0.077,0.069 | 0.073 | 7.5 |
| H# | Tin bag C+nickel basket (bath) | 0.058,0.073 | 0.065 | 16.5 |
| H# | Tin bag C+nickel basket (wrapping) | 0.050 | 0.050 | — |
| H# | Nickel bag | 0.054,0.0680.070 | 0.064 | 14.2 |
| H# | Nickel foil cone | 0.070,0.048,0.056 | 0.058 | 19.1 |
TABLE 8 comparative test results of oxygen content in Fe-Si-Al magnetic alloy for different carrying vessels (fluxing agent) (example 2)
As can be seen from tables 7 and 8 in combination with the actual experimental phenomena, the oxygen measurement value is significantly reduced under the fluxing conditions of nickel cone, nickel capsule, tin capsule and nickel basket, and the nickel is unfavorable for releasing oxygen in the Fe-Si-Al alloy powder. The oxygen measurement values corresponding to tin fluxing agents (baths) with different specifications and dosages such as tin capsule A, tin capsule B, tin capsule C, tin capsule and tin sheet are highly matched, and the precision is not significantly different, so the invention requires the tin capsule to be used as a bearing container (fluxing agent).
The determination method of the invention adopts a steel standard sample or a potassium hydrogen phthalate reference reagent to establish an instrument calibration coefficient, accurately weighs 80-100mg of the Fe-Si-Al magnetic alloy sample to wrap in a tin capsule, uses a graphite crucible to determine under the analysis power of 5.0kW, and calculates the oxygen content of the Fe-Si-Al magnetic alloy after deducting the blank value of the tin capsule.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention, and the scope of the invention should be assessed accordingly to that of the appended claims.
Claims (10)
1. The method for measuring the oxygen content in the Fe-Si-Al magnetic alloy is characterized by comprising the following steps of:
1) Performing instrument calibration by using a steel standard sample or a potassium hydrogen phthalate reference reagent, determining an instrument calibration coefficient, and deducting a method blank containing a fluxing agent according to the signal integral area of oxygen;
2) Accurately weighing a sample of the Fe-Si-Al magnetic alloy to be measured in a fluxing agent;
3) Compacting and folding a fluxing agent containing a sample to be detected into particles, and then putting the particles into a gas analyzer to measure the oxygen content of the particles, wherein the signal integration area of the particles is marked as A;
4) According to the formula w= (A-A KB ) Calculating the oxygen content W in the Fe-Si-Al magnetic alloy sample, wherein m is the actual weighing mass of the sample, A KB The signal integration area is blank for the flux-containing method, and K is the instrument calibration coefficient.
2. The method for measuring the oxygen content in the sendust according to claim 1, wherein when the instrument calibration is performed using a standard steel sample, step 1) includes: s11, setting instrument parameters; s12, deducting system blank; s13, establishing a calibration coefficient; s14, blank deduction method.
3. The method for measuring the oxygen content in the sendust according to claim 2, wherein when the instrument calibration is performed by using a steel standard sample, S12 is specifically: setting the analysis power to 4.0-4.5kW, measuring the blank values of the graphite crucible and the instrument pipeline, selecting the blank test result of the system, and deducting according to the signal integral area of oxygen, wherein the system blank signal integral area is marked as A KB0 . S14 specifically comprises the following steps: setting the analysis power to 4.5-5.5kW, compacting and folding the fluxing agent into particles, then putting the particles into a gas analyzer to measure the oxygen content, selecting the blank test result of the method, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area is marked as A KB1 。
4. The method for measuring the oxygen content in the sendust according to claim 2, wherein when the instrument calibration is performed using a steel standard, S13 comprises:
s131, selecting and accurately weighing the oxygen with known oxygen contentThe mass of the steel standard sample with the oxygen content ratio of 0.1-1 in the iron-silicon-aluminum magnetic alloy to be detected is recorded as m B ；
S132, putting the standard sample into a gas analyzer to measure the oxygen content, and recording the signal integral area as A B ；
S133, selecting the measurement result of the standard sample, and inputting the oxygen content identification value W of the standard sample B According to the following formula K 1 ＝(A B -A KB0 )/(m B ×W B ) Establishing instrument calibration coefficients, wherein A KB0 The signal integration area for system blanking.
5. The method for measuring the oxygen content in the sendust according to claim 1, wherein when the instrument calibration is performed using a potassium hydrogen phthalate reference reagent, the step 1) includes: s11, setting instrument parameters; s12, deducting a method blank; s13, establishing a calibration coefficient.
6. The method for measuring oxygen content in an iron-silicon-aluminum magnetic alloy according to claim 5, wherein when the instrument calibration is performed by using a potassium hydrogen phthalate reference reagent, S12 is specifically: setting the analysis power to 4.5-5.5kW, compacting and folding the fluxing agent into particles, then putting the particles into a gas analyzer to measure the oxygen content, selecting the blank test result of the method, and deducting according to the signal integral area of oxygen, wherein the blank signal integral area is marked as A KB2 。
7. The method for measuring the oxygen content in the sendust according to claim 5, wherein when the instrument calibration is performed using a potassium hydrogen phthalate reference reagent, S13 comprises:
s131, accurately weighing a certain amount of potassium hydrogen phthalate reference reagent (C) with the purity of (100+/-0.05) 8 H 5 O 4 K) Preparing potassium hydrogen phthalate standard solution with pure water, wherein the mass concentration is marked as C P ；
S132, direction assistanceThe quantitative injection volume in the flux is V P The potassium hydrogen phthalate standard solution is dried at 100-120 ℃;
s133, calculating the theoretical value W of the oxygen content of the potassium hydrogen phthalate P ＝C P ×V P ×10 -5 ×31.34％；
S134, inputting sample mass m into the instrument P The flux containing potassium hydrogen phthalate is put into a gas analyzer to measure the oxygen content, and the signal integral area is marked as A P ；
S135, selecting the above potassium hydrogen phthalate test result, and inputting the theoretical value of oxygen content (W P ) According to K 2 ＝(A P -A KB2 )/(m P ×W P ) Establishing instrument calibration coefficients, wherein A KB2 The signal integration area is blank for the flux-containing method.
8. The method for measuring the oxygen content in the sendust according to claim 1, wherein the sample weight of the sendust is 80-120mg.
9. The method for measuring the oxygen content in the sendust according to claims 1-8, wherein the flux is a tin capsule.
10. The method for measuring the oxygen content in the sendust according to claim 2 or 5, wherein the analysis power of the instrument set in S11 is 4.5 to 5.5kW.
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