CN112557377A - Method for testing content of niobium in ferromolybdenum - Google Patents
Method for testing content of niobium in ferromolybdenum Download PDFInfo
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- 239000010955 niobium Substances 0.000 title claims abstract description 53
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 50
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000012360 testing method Methods 0.000 title claims abstract description 43
- 229910001309 Ferromolybdenum Inorganic materials 0.000 title claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 45
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012086 standard solution Substances 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 238000004090 dissolution Methods 0.000 claims abstract description 11
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 11
- 238000001228 spectrum Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 14
- 239000011975 tartaric acid Substances 0.000 claims description 14
- 235000002906 tartaric acid Nutrition 0.000 claims description 14
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 238000010998 test method Methods 0.000 claims description 10
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 7
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 7
- 229960001484 edetic acid Drugs 0.000 claims description 4
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000005070 sampling Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 26
- 238000004458 analytical method Methods 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- -1 molybdenum ions Chemical class 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
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- 238000001816 cooling Methods 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 238000005485 electric heating Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 239000000956 alloy Substances 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- VUGOTOYGNLHWPK-UHFFFAOYSA-N 2-hydroxybenzenesulfonyl chloride Chemical compound OC1=CC=CC=C1S(Cl)(=O)=O VUGOTOYGNLHWPK-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910001285 shape-memory alloy Inorganic materials 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000013582 standard series solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- 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
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- Chemical & Material Sciences (AREA)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a method for testing the content of niobium in ferromolybdenum, which comprises the following steps: (1) dissolving a ferromolybdenum sample by using mixed acid to obtain a dissolved solution, adding sulfuric acid into the dissolved solution, evaporating to dryness, and then adding an auxiliary agent to obtain a solution to be detected; (2) and (3) selecting standard solutions with 5-7 concentration gradients, drawing a standard curve by adopting a full-spectrum direct-reading inductively coupled plasma emission spectrometer, and testing the liquid to be tested obtained in the step (1). Through setting a sample dissolving process and a test standard in the test process, a proper acid and an auxiliary agent are selected, the high-efficiency dissolution of niobium in the ferromolybdenum is realized, meanwhile, through reasonable selection of a standard curve sampling point in the detection process, the high-efficiency and high-precision determination of the niobium content in the ferromolybdenum is realized, and the test process is simple and rapid.
Description
Technical Field
The invention relates to the field of elemental analysis, in particular to a method for testing niobium content in ferromolybdenum.
Background
8418 steel is high-performance hot-work die steel containing chromium, molybdenum and vanadium, and has good thermal fatigue crack resistance, thermal shock crack resistance, thermal abrasion resistance and plastic deformation resistance. In addition to controlling the main elements such as carbon, silicon, manganese, phosphorus, sulfur, chromium, molybdenum, vanadium, aluminum and the like, the production process needs to control the content of other residual elements and harmful elements, including niobium. A small amount of niobium has the advantages of improving the steel microstructure, refining steel grains, reducing the tempering brittleness of steel and the like, but the performance of the steel is influenced when the niobium exceeds a certain range. According to the judgment of the process for producing 8418 steel by research, niobium mainly exists in ferromolybdenum, and the content of niobium in the ferromolybdenum alloy serving as a production raw material needs to be detected.
One method for measuring the niobium content in the alloy by the traditional method is to obtain the niobium content by measuring the total amount of niobium, tantalum and titanium by a gravimetric method and then subtracting the amount of thallium and titanium, and the method is relatively suitable for measuring high-content niobium (50-80 percent); the other method is a chlorosulfonyl phenol S spectrophotometry, because niobium in ferromolybdenum is a high-molybdenum low-niobium liquid phase environment, molybdenum ions and niobium ions simultaneously react with chlorosulfonyl phenol S to generate a dark blue complex, a masking agent is required to be added to eliminate the interference of the molybdenum ions, the whole process is complicated, the analysis time is long, and more pollution links are easily introduced.
For example, CN107315001A discloses a method for determining the niobium content in a titanium-niobium alloy, which comprises the following steps: preparing a Ti45Nb sample solution; taking a Ti45Nb sample solution, and developing with a PAR solution; measuring the absorbance of the developed solution at a wavelength of 520nm-530nm on a spectrophotometer; preparing a niobium standard solution; preparing a titanium base solution; a series of standard solutions were prepared with niobium concentrations ranging from 0.00% to 0.25X 10 for establishing the curve-3%, corresponding to a niobium concentration in the alloy sample of from 0% to 50%; establishing a working curve: developing the series of standard solutions of S6, measuring absorbance values, and establishing a working curve with the concentration as an abscissa and the absorbance values as an ordinate; and (3) reflecting a corresponding concentration value on the established working curve according to the absorbance value measured after the Ti45Nb sample is dissolved and developed, so as to obtain the niobium content in the Ti45Nb memory alloy material. The method has the advantages of stable color development, satisfactory working curve and good data repeatability.
CN111089771A discloses a detection method for determining the content of niobium and tantalum in niobium-tantalum ore, which comprises the following steps: (1) placing a niobium-tantalum ore sample in a polytetrafluoroethylene beaker, and adding deionized water for wetting; (2) sequentially adding nitric acid, perchloric acid and hydrofluoric acid into a polytetrafluoroethylene beaker, slightly shaking up, washing the wall of the beaker by deionized water, and putting the polytetrafluoroethylene beaker on an electric hot plate at 180-220 ℃ for heating and decomposing; (3) heating until the perchloric acid smoke is exhausted, adding 8-10mL of aqua regia solution, keeping the temperature until the sample is dissolved, washing the cup wall with deionized water when 3-4mL of aqua regia solution is left, and keeping the temperature for 10 minutes after washing; (4) cooling to room temperature, transferring to a 50mL colorimetric tube, and fixing the volume; (5) preparing a mixed standard series solution: (6) taking the solution in the step (4) to perform determination on an inductively coupled plasma emission spectrometer; (7) and drawing a working curve. The method can realize safe and smooth detection process and simple operation process.
However, the above test scheme still has the problems of complex test process, low test precision and the like.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for testing the content of niobium in ferromolybdenum, which realizes high-efficiency and high-precision measurement of the content of niobium in the ferromolybdenum by setting a sample dissolving process and a test standard in a testing process, and the testing process is simple and rapid.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for testing the content of niobium in ferromolybdenum, which comprises the following steps:
(1) dissolving a ferromolybdenum sample by using mixed acid to obtain a dissolved solution, adding sulfuric acid into the dissolved solution, evaporating to dryness, and then adding an auxiliary agent to obtain a solution to be detected;
(2) and (3) selecting standard solutions with 5-7 concentration gradients, drawing a standard curve by adopting a full-spectrum direct-reading inductively coupled plasma emission spectrometer, and testing the liquid to be tested obtained in the step (1). Through setting a sample dissolving process and a test standard in the test process, a proper acid and an auxiliary agent are selected, the high-efficiency dissolution of niobium in the ferromolybdenum is realized, meanwhile, through reasonable selection of a standard curve sampling point in the detection process, the high-efficiency and high-precision determination of the niobium content in the ferromolybdenum is realized, and the test process is simple and rapid.
In the invention, the liquid to be tested needs to be diluted during the test, so that the liquid phase meets the sample testing requirement of the full-spectrum direct-reading inductively coupled plasma emission spectrometer.
As a preferable technical scheme of the invention, the mixed acid in the step (1) comprises hydrofluoric acid, nitric acid and hydrochloric acid.
Preferably, the volume ratio of hydrofluoric acid to nitric acid to hydrochloric acid in the mixed acid is 1: (0.4-1), for example, the above-mentioned range may include, but is not limited to, 1:1:0.4, 1:1:0.42, 1:1:0.44, 1:1:0.46, 1:1:0.48, 1:1:0.5, 1:1:0.52, 1:1:0.54, 1:1:0.56, 1:1:0.58, 1:1:0.6, 1:1:0.62, 1:1:0.64, 1:1:0.66, 1:1:0.68, 1:1:0.7, 1:1:0.72, 1:1:0.74, 1:1:0.76, 1:1:0.78, 1:1:0.8, 1:1:0.82, 1:1:0.84, 1:1:0.86, 1:1:0.88, 1:1: 1:0.9, 1:1:0.92, 1:0.94, 1:0.96, 1: 1.98, 1:0.98, and the range may include other values.
As a preferred embodiment of the present invention, the temperature for the dissolution in the step (1) is 200 ℃ to 300 ℃, and may be, for example, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃ or 300 ℃, but is not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the dissolving time in step (1) is 50-70min, such as 50min, 52min, 54min, 56min, 58min, 60min, 62min, 64min, 66min, 68min or 70min, but not limited to the recited values, and other values not recited in the range are also applicable.
In a preferred embodiment of the present invention, the mass concentration of the sulfuric acid in the step (1) is 40 to 60%, and may be, for example, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, or 60%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the amount of the sulfuric acid added in step (1) is 10-20% by volume of the dissolution solution, for example, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20% or the like, but not limited to the recited values.
As a preferable technical scheme of the invention, the auxiliary agent in the step (1) comprises tartaric acid solution and ethylene diamine tetraacetic acid solution.
As a preferred embodiment of the present invention, the tartaric acid has a mass concentration of 200-400g/L, such as 200g/L, 250g/L, 300g/L, 310g/L, 320g/L, 330g/L, 340g/L, 350g/L, 360g/L, 370g/L, 380g/L, 390g/L or 400g/L, but not limited to the values listed, and other values not listed within this range are also applicable.
Preferably, the mass concentration of the disodium ethylene diamine tetraacetate is 20-40g/L, for example, 20g/L, 22g/L, 24g/L, 26g/L, 28g/L, 30g/L, 32g/L, 34g/L, 36g/L, 38g/L or 40g/L, etc., but is not limited to the enumerated values, and other unrecited values in the range are also applicable.
In a preferred embodiment of the present invention, the tartaric acid solution in the adjuvant in step (1) is added in an amount of 1 to 1.2 times, for example, 1 time, 1.02 time, 1.04 time, 1.06 time, 1.08 time, 1.1 time, 1.12 time, 1.14 time, 1.16 time, 1.18 time or 1.2 time the volume of the dissolution solution, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the amount of disodium edetate added to the adjuvant in step (1) is 0.5 to 0.75 times the volume of the dissolution solution, for example, 0.5, 0.55, 0.6, 0.65, 0.7 or 0.75 times, but not limited to the recited values, and other values not recited in this range are also applicable.
In a preferred embodiment of the present invention, the correlation coefficient of the standard curve in step (2) is not less than 0.9999, and may be, for example, 0.9999, 0.99991, 0.99992, 0.99993, 0.99994, 0.99995, 0.99996, 0.99997, 0.99998, 0.99999, 0.999991, or 0.999992, but is not limited to the above-mentioned values, and other values not listed in this range are also applicable.
As a preferred embodiment of the present invention, the relative standard deviation of the test in step (2) is 5% or less, and may be, for example, 5%, 4.5%, 4%, 3.5%, 3%, 2.5%, 2%, 1.5%, 1%, or 0.5%, etc., but is not limited to the values listed, and other values not listed in this range are also applicable.
As a preferred technical scheme of the invention, the test method comprises the following steps:
(1) dissolving a ferromolybdenum sample by using mixed acid to obtain a dissolved solution, adding sulfuric acid into the dissolved solution, evaporating to dryness, and then adding an auxiliary agent to obtain a solution to be detected;
(2) selecting standard solutions with 5-7 concentration gradients, drawing a standard curve by adopting a full-spectrum direct-reading inductively coupled plasma emission spectrometer, and testing the liquid to be tested obtained in the step (1);
the volume ratio of hydrofluoric acid, nitric acid and hydrochloric acid in the mixed acid in the step (1) is 1:1 (0.4-1), and the dissolving time is 50-70 min;
the auxiliary agent in the step (1) comprises tartaric acid solution and ethylene diamine tetraacetic acid solution, wherein the mass concentration of the tartaric acid solution is 200-400 g/L; the mass concentration of the ethylene diamine tetraacetic acid disodium solution is 20-40 g/L.
In the invention, all reagents are superior pure, acid in the mixed acid can be added step by step or can be added at one time, the auxiliary agent is the same, the adding amount of the mixed acid is determined according to the amount of the sample, and the sample can be dissolved.
The volume of the dissolution solution in the present invention can be directly converted from the volume of the acid added during the dissolution process, or can be obtained by measurement.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) through setting a sample dissolving process and a test standard in the test process, a proper acid and an auxiliary agent are selected, the high-efficiency dissolution of niobium in the ferromolybdenum is realized, meanwhile, through reasonable selection of a standard curve sampling point in the detection process, the high-efficiency and high-precision determination of the niobium content in the ferromolybdenum is realized, and the test process is simple and rapid.
(2) The method for determining the content of niobium in the ferro-molybdenum alloy provided by the invention has the advantages that interference factors are few in the determination process, multiple test results show that relative standard deviations are less than or equal to 5%, the repeatability is good, the results are stable, absolute values of detected deviations are less than or equal to 0.01%, the absolute values of detected deviations are less than or equal to allowable deviations, the detection recovery rate is between 98% and 102%, the accuracy is high, and scientific control data can be provided for production.
Drawings
FIG. 1 is a standard curve of niobium in example 1 of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a method for testing the content of niobium in ferromolybdenum, which comprises the following steps:
(1) weighing 0.2g of sample, accurately measuring to +/-0.0001 g, placing the sample in a polytetrafluoroethylene beaker, adding 5mL of super-pure hydrofluoric acid, slowly dropwise adding 5mL of nitric acid on a low-temperature electric heating plate, heating to micro-boiling, adding 5mL of super-pure hydrochloric acid, continuously dissolving for 10min, adding 1mL of dilute sulfuric acid (1+1), namely mixing 1 volume part of water and 1 volume part of concentrated sulfuric acid, adjusting the electric heating plate to the medium temperature, continuously heating to near dryness, taking down and cooling.
(2) Adding 20mL of newly prepared superior pure tartaric acid (300g/L) for dissolving salt, cooling to 40 ℃, adding 5mL of disodium ethylene diamine tetraacetate (20g/L), immediately using first-grade ultrapure water for containing in a 100mL volumetric flask, and shaking uniformly to be tested;
(3) preparing 7 standard solutions with certain gradient Nb content without hitting a matrix. In the experiment, 1000 mu g/mL of niobium standard solution is used for stepwise dilution to prepare standard solution with the content of 0.0%, 0.1%, 0.3%, 0.5%, 0.7%, 0.9% and 1.2%; 10mL of hydrochloric acid (1+1), namely 1 part by volume of water and 1 part by volume of concentrated hydrochloric acid are added and mixed, the volume is fixed to 100mL scale by first-grade water, and the mixture is shaken up and kept stand.
(4) Selecting an analysis spectral line, optimizing related parameters and analysis conditions of the inductively coupled plasma emission spectrometer, and analyzing the niobium standard solution in sequence to draw a niobium standard curve, as shown in fig. 1. For the analysis of niobium in the experiment, nb309.418 was chosen.
Example 2
The embodiment provides a method for testing the content of niobium in ferromolybdenum, which comprises the following steps:
(1) weighing 0.2g of sample, accurately obtaining +/-0.0001 g of sample, placing the sample in a polytetrafluoroethylene beaker, adding 5mL of super-grade pure hydrofluoric acid, slowly dropwise adding 5mL of nitric acid on a low-temperature electric heating plate, heating to slight boiling, adding 2mL of super-grade pure hydrochloric acid, continuously dissolving for 10min, adding 2mL of dilute sulfuric acid (1+1), namely mixing 1 volume part of water and 1 volume part of concentrated sulfuric acid, adjusting the electric heating plate to the medium temperature, continuously heating to near dryness, taking down and cooling.
(2) Adding 20mL of newly prepared superior pure tartaric acid (400g/L) for dissolving salt, cooling to 50 ℃, adding 10mL of disodium ethylene diamine tetraacetate (30g/L), immediately using first-grade ultrapure water for being dissolved in a 100mL volumetric flask, and shaking uniformly to be tested;
(3) preparing 7 standard solutions with certain gradient Nb content without hitting a matrix. In the experiment, 1000 mu g/mL of niobium standard solution is used for stepwise dilution to prepare standard solution with the content of 0.0%, 0.1%, 0.3%, 0.5%, 0.7%, 0.9% and 1.2%; 4mL of hydrochloric acid (1+1), namely 1 part by volume of water and 1 part by volume of concentrated hydrochloric acid are added and mixed, the volume is adjusted to 100mL scale by using first-grade water, and the mixture is shaken up and kept stand.
(4) And selecting an analysis spectral line, optimizing related parameters and analysis conditions of the inductively coupled plasma emission spectrometer, and analyzing the niobium standard solution in sequence to draw a niobium standard curve. For the analysis of niobium in the experiment, nb309.418 was chosen.
Example 3
The embodiment provides a method for testing the content of niobium in ferromolybdenum, which comprises the following steps:
(1) weighing 0.2g of sample, accurately obtaining +/-0.0001 g of sample, placing the sample in a polytetrafluoroethylene beaker, adding 5mL of superior pure hydrofluoric acid, slowly dropwise adding 5mL of nitric acid on a low-temperature electric heating plate, heating to slight boiling, adding 3mL of superior pure hydrochloric acid, continuously dissolving for 10min, adding 1.5mL of dilute sulfuric acid (1+1), namely mixing 1 volume part of water and 1 volume part of concentrated sulfuric acid, adjusting the electric heating plate to the medium temperature, continuously heating to near dryness, taking down and cooling.
(2) Adding 10mL of newly prepared superior pure tartaric acid (300g/L) for dissolving salt, cooling to 70 ℃, adding 5mL of disodium ethylene diamine tetraacetate (40g/L), immediately using first-grade ultrapure water for containing in a 100mL volumetric flask, and shaking uniformly to be tested;
(3) preparing 7 standard solutions with certain gradient Nb content without hitting a matrix. In the experiment, 1000 mu g/mL of niobium standard solution is used for stepwise dilution to prepare standard solution with the content of 0.0%, 0.1%, 0.3%, 0.5%, 0.7%, 0.9% and 1.2%; 6mL of hydrochloric acid (1+1), namely 1 part by volume of water and 1 part by volume of concentrated hydrochloric acid are added and mixed, the volume is adjusted to 100mL mark by using first-grade water, and the mixture is shaken up and kept stand.
(4) And selecting an analysis spectral line, optimizing related parameters and analysis conditions of the inductively coupled plasma emission spectrometer, and analyzing the niobium standard solution in sequence to draw a niobium standard curve. For the analysis of niobium in the experiment, nb316.340 was chosen.
Comparative example 1
The only difference from example 1 is that the sulfuric acid of step (1) is replaced by perchloric acid of equal mass.
Comparative example 2
The only difference from example 1 is that the tartaric acid of step (2) was replaced with an equal concentration of citric acid.
The instruments and analysis conditions used in the above examples and comparative examples were as follows: an experimental instrument: full spectrum direct reading inductively coupled plasma emission spectrometer, instrument model: iCAP 6300Radial, assay conditions: analysis of pump speed 50rpm, RF power 1150W, auxiliary gas flow 0.5L/min, atomizer gas flow 0.65L/min vertical viewing height: 12 mm. And 99.999 percent of high-purity argon.
Test and results
1. Recovery test
And (4) verifying the data accuracy by adopting a labeling recovery method when the ferromolybdenum does not find a standard sample containing the niobium element. The recovery test was conducted on the unknown sample # 1, and the detection methods provided in examples and comparative examples were evaluated. The results of the recovery rate tests of examples and comparative examples are shown in table 1.
TABLE 1
2. Precision test
The detection methods provided in examples and comparative examples were evaluated by precision tests, and the test was repeated 5 times for each of the unknown sample # 1 and the unknown sample # 2.
The results of the examples and comparative examples measured for unknown sample # 1 and unknown sample # 2 are shown in table 3.
TABLE 2
According to the results of the embodiment and the comparative example, the content of niobium in the ferromolybdenum is measured efficiently and accurately, and the test process is simple and rapid. The method provided by the invention has the advantages that the high precision recovery rate is 98-102%, and the data accuracy meets the requirement.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The method for testing the content of niobium in ferromolybdenum is characterized by comprising the following steps of:
(1) dissolving a ferromolybdenum sample by using mixed acid to obtain a dissolved solution, adding sulfuric acid into the dissolved solution, evaporating to dryness, and then adding an auxiliary agent to obtain a solution to be detected;
(2) and (3) selecting standard solutions with 5-7 concentration gradients, drawing a standard curve by adopting a full-spectrum direct-reading inductively coupled plasma emission spectrometer, and testing the liquid to be tested obtained in the step (1).
2. The test method of claim 1, wherein the mixed acid of step (1) comprises hydrofluoric acid, nitric acid, and hydrochloric acid;
preferably, the volume ratio of the hydrofluoric acid to the nitric acid to the hydrochloric acid in the mixed acid is 1:1 (0.4-1).
3. The test method as claimed in claim 1 or 2, wherein the temperature of the dissolution in step (1) is 200-300 ℃;
preferably, the dissolving time of the step (1) is 50-70 min.
4. The test method according to any one of claims 1 to 3, wherein the mass concentration of the sulfuric acid in the step (1) is 40 to 60%;
preferably, the adding amount of the sulfuric acid in the step (1) is 10-20% of the volume of the dissolving solution.
5. The test method as claimed in any one of claims 1 to 4, wherein the auxiliary agent in step (1) comprises a tartaric acid solution and a disodium ethylenediaminetetraacetate solution.
6. The test method as claimed in claim 5, wherein the tartaric acid solution has a mass concentration of 200-400 g/L;
preferably, the mass concentration of the disodium ethylene diamine tetraacetate is 20-40 g/L.
7. The test method according to any one of claims 1 to 6, wherein the tartaric acid solution in the auxiliary of step (1) is added in an amount of 1 to 1.2 times the volume of the dissolution solution;
preferably, the addition amount of the disodium ethylene diamine tetraacetate in the auxiliary agent in the step (1) is 0.5-0.75 time of the volume of the dissolving solution.
8. The test method according to any one of claims 1 to 7, wherein the correlation coefficient of the standard curve in the step (2) is not less than 0.9999.
9. The test method defined in any one of claims 1-8, wherein the relative standard deviation of the test of step (2) is ≦ 5%.
10. The test method according to any one of claims 1 to 9, characterized in that it comprises the steps of:
(1) dissolving a ferromolybdenum sample by using mixed acid to obtain a dissolved solution, adding sulfuric acid into the dissolved solution, evaporating to dryness, and then adding an auxiliary agent to obtain a solution to be detected;
(2) selecting standard solutions with 5-7 concentration gradients, drawing a standard curve by adopting a full-spectrum direct-reading inductively coupled plasma emission spectrometer, and testing the liquid to be tested obtained in the step (1);
the volume ratio of hydrofluoric acid, nitric acid and hydrochloric acid in the mixed acid in the step (1) is 1:1 (0.4-1), and the dissolving time is 50-70 min;
the auxiliary agent in the step (1) comprises tartaric acid solution and ethylene diamine tetraacetic acid solution, wherein the mass concentration of the tartaric acid solution is 200-400 g/L; the mass concentration of the ethylene diamine tetraacetic acid solution is 20-40 g/L.
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