CN104569128A - Method for determining content of solid-solution rear earth in steel - Google Patents
Method for determining content of solid-solution rear earth in steel Download PDFInfo
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Abstract
The invention discloses a method for determining the content of solid-solution rear earth in steel. The method comprises the following steps: taking a steel sample with the mass of m1 as an anode, taking stainless steel as a cathode, and taking an anhydrous methanol solution of anhydrous lithium chloride and acetylacetone as electrolyte for electrolysis, weighing the steel sample after electrolysis to obtain the mass m2; drying organic matters in the electrolyte after electrolysis by evaporation, and adding nitric acid to decompose residues and obtain a test solution to be measured; taking cesium as an internal standard element, determining the mass m of solid-solution rear earth in the test solution to be measured and the mass m0 of solid-solution rear earth in a blank solution by an inductively coupled plasma mass spectrometer; obtaining the content of solid-solution rear earth in steel by W%=10<-6>*(m-m0)/(m1-m2)*100. The method for determining the content of solid-solution rear earth in steel has high accuracy and precision.
Description
Technical field
The present invention relates to technical field of analytical chemistry, specifically, relate to the assay method of solid solution content of rare earth in a kind of steel.
Background technology
China is the rare earth big country of global rare earth resource and output first, is again the big steel country of output of steel first, but is not iron and steel power, and variety and quality also has sizable gap compared with Foreign Advanced Lerel, still has many steel to need import.Strengthen with this High-tech Material of rare earth and promote iron and steel conventional industries, trace rare-earth is added in low alloy steel, alloy steel, improve steel to enhance our international competitiveness, the resources advantage of rare earth is converted into species the advantage and the economic advantages of steel, there is very great meaning.
Rare earth in steel application has three to act on greatly: 1. cleaning molten steel.Rare earth has deoxidation, desulfidation, reduces and refinement steel inclusion.2. go bad and be mingled with.Rare earth adds in steel and generates spherical rare-earth sulfide or oxysulfide, replaces strip manganese sulfide inclusion, oxide morphology is controlled completely, improves the toughness plasticity particularly transverse impact toughness of steel, improves the anisotropy of steel.Rare earth makes the alumina inclusion of high rigidity be transformed into spherical oxysulfide and aluminic acid rare earth, improves the anti-fatigue performance of steel significantly.3. microalloying.Rare earth in steel has certain solid solution capacity, and it can suppress phosphorus sulphur and low-melting impurities lead, tin, arsenic, antimony in the segregation of crystal boundary, bismuth is in the segregation of crystal boundary or form the higher compound of fusing point with these impurity, eliminates the illeffects of low-melting impurities; Rare earth purification and strengthening crystal boundary, hinder formation and the expansion of intercrystalline crack, be conducive to improving plasticity especially high-temp plastic; Rare earth can suppress dynamic recrystallization, crystal grain thinning and precipitated phase size and promote Nb in ferrite (C, N), the precipitation of (Nb, Ti) (C, N) and V (C, N); The rare earth dissolved can change the Nomenclature Composition and Structure of Complexes of cementite and makes carbide spheroidization, refinement and be uniformly distributed.
At present, China's Cu-RE phosphorus weathering steel, Rare earth heat-resistant steel and containing niobium or vanadium RE Steel for Heavy Rail, containing niobium (niobium, titanium) rare earth pipe line steel, the commercial production all such as rare earth structural steel containing vanadium or manganese, rare earth significantly improves the performance such as mouldability, toughness plasticity, wearing quality, corrosion stability, endurance of steel, makes low alloy steel obtain more superior combination property.Therefore, development has the low alloy steel series of china natural resources advantage, should, as the research emphasis of rare earth micro alloyed steel, also be that resources advantage is converted to product advantage and economic advantages, the rare earth new steel grade of exploitation superior performance, a right way of meeting the need of market.Research shows, in steel, sulphur oxygen content is more than 0.002%, rare earth add still have purification and metamorphism, but in low-sulfur oxygen steel, note the Proper Match of the Microalloying Effect of rare earth and composition of steel, technique, play the advantageous effect of microalloying of rare earth, prevent adverse influence.Therefore, understand its different shape existed in steel and accurately provide the content of rare earth of different shape to play very important effect to exploitation high quality steel.
Although the research of the application of rare earth in steel, distribution etc. is a lot, due to the complicacy that rare earth in steel exists, the research report of chemical analysis method seldom, has metallurgical analysis information network recommend method at present---the mensuration of solid solution rare earth and snotter and steel middle rare earth solid solution capacity inductively coupled plasma spectrometry patent in steel.This recommend method adopts electrolytic separation-spectrphotometric method for measuring, and method is numerous and diverse, Monitoring lower-cut is high (0.001%), can not provide the content of single rare earth.In addition, prior art also has steel middle rare earth solid solution capacity inductively coupled plasma spectrometry method, its main points: electroextraction solid solution rare earth, by organic principle volatilization in system, adopt resin drip washing separation, acid adjustment degree, inductively coupled plasma spectrometry measures; The method operation is more numerous and diverse, and long flow path, in steel, the amount of solid solution rare earth is very low, is difficult to Accurate Determining.
Summary of the invention
Technical matters to be solved by this invention is to provide the assay method of solid solution content of rare earth in a kind of steel, can the content of solid solution rare earth in Accurate Determining steel.
Technical scheme of the present invention is as follows:
An assay method for solid solution content of rare earth in steel, comprising: be m by quality
1steel sample as anode, using stainless steel as negative electrode, using the absolute methanol solution of anhydrous Lithium chloride and diacetone as electrolytic solution electrolysis, the quality of the described steel sample after electrolysis of weighing is m
2; By the organism evaporate to dryness in the described electrolytic solution after electrolysis, add nitric acid residue decomposition and obtain test solution to be measured; Take caesium as internal standard element, adopt icp ms to measure the quality m of the solid solution rare earth in described test solution to be measured, and the quality m of solid solution rare earth in blank solution
0; Employing formula
obtain solid solution content of rare earth in steel.
Further: in described electrolytic solution, the mass percentage of anhydrous Lithium chloride is 0.9% ~ 1.1%, the percent by volume of diacetone is 5% ~ 7%.
Further: the volume of described electrolytic solution is 250mL.
Further: the electric current of described electrolysis is 0.3A ~ 0.6A, and temperature is less than-10 DEG C, and the time is 20min ~ 40min.
Further: the volume of nitric acid is 8 ~ 10mL, and density p is 1.42g/mL.
Further: described employing icp ms measures the quality m of the solid solution rare earth in described test solution to be measured, and the quality m of solid solution rare earth in blank solution
0process comprise: respectively to standard solution 0mL, 0.5mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL and 20.00mL of adding lanthanum, cerium, praseodymium, neodymium and samarium that concentration is 0.1 μ g/mL in 1.0g anhydrous Lithium chloride, add the nitric acid that 3mL density is 1.42g/mL, be diluted with water to 100mL, take caesium as internal standard element, described icp ms is adopted to measure, with the mass percentage of solid solution rare earth for horizontal ordinate, mass spectral intensities is ordinate, drawing curve; Described icp ms is adopted to measure the mass spectral intensities of the solid solution rare earth in described test solution to be measured, and the intensity of solid solution rare earth in blank solution; On described working curve, the quality m of the solid solution rare earth in corresponding test solution described to be measured is obtained according to the mass spectral intensities of the solid solution rare earth in the mass spectral intensities of the solid solution rare earth in described test solution to be measured, described blank solution, and the quality m of solid solution rare earth in described blank solution
0.
Further: the volume of the described test solution described to be measured for icp ms mensuration is 250mL.
Further: described be m by quality
1the process of steel sample as anode before, also comprise and described steel sample taken out after being soak 10 ~ 20min in the hydrochloric acid of 1.19g/mL in 25 ~ 30mL water, 25 ~ 30mL density, clean, alcohol flushing the step of drying.
Further: the shape of described steel sample is basal diameter is 8 ~ 10mm, and height is the column of 80 ~ 100mm.
Technique effect of the present invention is as follows:
Method of the present invention dissolves steel sample by nitration mixture, and under perchloric acid is fuming condition, the carbonide of niobium is decomposed completely, quantitatively retains the oxide of niobium, and then nitric acid, hydrofluorite decompose, can niobium oxide content in Accurate Determining steel by ICP-MS.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
In steel of the present invention, the concrete steps of the assay method of solid solution content of rare earth are as follows:
Step S1: steel sample to be made shape be basal diameter is 8 ~ 10mm, and height is the column of 80 ~ 100mm.
Step S2: by above-mentioned steel sample at 25 ~ 30mL water, is preferably 25mL water, 25 ~ 30mL hydrochloric acid, and being preferably 25mL density is take out after soaking 10 ~ 20min in the hydrochloric acid of 1.19g/mL, and clean, alcohol flushing also dries.
Step S3: using above-mentioned steel sample as anode, quality of weighing is m
1, using stainless steel as negative electrode, using the absolute methanol solution of anhydrous Lithium chloride and diacetone as electrolytic solution electrolysis, the quality of the steel sample after electrolysis of weighing is m
2.
Solid solution lanthanum, cerium, praseodymium, neodymium, samarium is extracted by this step.
Wherein, stainless steel can make tubular.The electric current of electrolysis is 0.3A ~ 0.6A, and temperature is less than-10 DEG C, and the time is 20min ~ 40min.In electrolytic solution, the mass percentage of anhydrous Lithium chloride is 0.9% ~ 1.1%, and the percent by volume of diacetone is 5% ~ 7%.The volume of electrolytic solution is 250mL.The process of this electrolysis is carried out in electrolytic cell, can hold electrolytic solution, then glass beaker is placed in electrolytic cell with glass beaker.
Step S4: by the organism evaporate to dryness in the electrolytic solution after electrolysis, adds nitric acid residue decomposition and obtains test solution to be measured.
Wherein, the volume of nitric acid is 8 ~ 10mL, and be preferably 8mL, density p is 1.42g/mL.This organism refers to diacetone, methyl alcohol etc.
Step S5: take caesium as internal standard element, adopts icp ms to measure the quality m of the solid solution rare earth in described test solution to be measured, and the quality m of solid solution rare earth in blank solution
0.
Wherein, the volume for the test solution to be measured of icp ms mensuration is 250mL.
Particularly, step S5 comprises following process:
Step S51: respectively to standard solution 0mL, 0.5mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL and 20.00mL of adding lanthanum, cerium, praseodymium, neodymium and samarium that concentration is 0.1 μ g/mL in 1.0g anhydrous Lithium chloride, add the nitric acid that 3mL density is 1.42g/mL, be diluted with water to 100mL, take caesium as internal standard element, employing icp ms measures, with the mass percentage of solid solution rare earth for horizontal ordinate, mass spectral intensities is ordinate, drawing curve;
Step S52: adopt icp ms to measure the mass spectral intensities of the solid solution rare earth in test solution to be measured, and the intensity of solid solution rare earth in blank solution;
Step S53: the quality m obtaining the solid solution rare earth in corresponding test solution to be measured according to the mass spectral intensities of the solid solution rare earth in the mass spectral intensities of the solid solution rare earth in test solution to be measured, blank solution on working curve, and the quality m of solid solution rare earth in blank solution
0.
Step S6: adopt formula
obtain solid solution content of rare earth in steel.
Below the parameter of method of the present invention is described further.
1, the selection of electrolytic solution
By Wuhan Iron and Steel Plant rare earth steel standard model and self-control rare earth steel sample, be 0.5A at Faradaic current, electrolyte temperature is less than-10 DEG C, adopts 1 of method of the present invention respectively
#electrolytic solution: the absolute methanol solution 250mL of 1% (mass percentage) anhydrous Lithium chloride and 6% (percent by volume) diacetone and 2 of recommend method of the prior art
#electrolytic solution: the ethanolic solution 250mL of 1% (mass percentage) lithium chloride, 5% (mass percentage) triethanolamine, 5% (percent by volume) ethylene glycol, electrolysis 20min Extraction of rare earth snotter total amount, take off, put into 250mL glass beaker supersonic oscillations power taking solution residue respectively, add the hydrochloric acid of 5mL ρ 1.19g/mL and the nitric acid of 5mL ρ 1.42g/mL respectively, heating for dissolving, adopts ICP-MS to measure, the results are shown in Table 1.
The steel Rare-Earth Content of table 1 different electrolytes electrolysis
| Electrolytic solution | Asserting value (%) | Measured value (%) |
| 1 # | 0.018 ~ 0.023 (steel Rare Earth Inclusions total amount) | 0.0221 |
| 2 # | 0.018 ~ 0.023 (steel Rare Earth Inclusions total amount) | 0.0194 |
| 1 # | 0.012 (steel middle rare earth total amount) | 0.0116 |
| 2 # | 0.012 (steel middle rare earth total amount) | 0.0098 |
As can be seen from Table 1,1 of the inventive method is adopted
#electrolytic solution extracts, ICP-MS measures re inclusion total amount value higher than recommend method 2
#electrolytic solution extracts, ICP-MS measures re inclusion total amount value, shows that the electrolytic solution of method of the present invention can solid solution rare earth in Quantitative Separation steel.Adopt 1
#in electrolytic solution electrolytic process, temperature-controllable is built in less than-10 DEG C, but 2
#in electrolytic solution electrolytic process, temperature raises gradually, and after about 20 minutes, temperature can reach more than 10 DEG C, can not meet the requirement of electrolysis temperature.
2, the interference of iron-based body
Be respectively in the standard solution of 5ng/mL, 20ng/mL in lanthanum, cerium, praseodymium, neodymium and samarium concentration, add the high purity iron mark liquid of 0g/mL, 0.2g/mL, 0.4mg/mL, 0.6mg/mL, 0.8mg/mL, 1mg/mL respectively, employing plasma mass spectrometry measures, the recovery of tested element in 95 ~ 105% scopes, namely in mensuration system below 1mg/mL iron-based body to mensuration element without remarkable interference.
3, the interference of coexistence elements
Under iron-based and electrolytical existence, the lanthanum of different content, cerium, praseodymium, neodymium, samarium mark liquid are carried out to the interference measurement of Mn, V, Ni, Mo, Cr, Ti, Cu, the results are shown in Table 2.The result of table 2 shows: Mn≤5.00%, and Cr, Ni, V≤2.00%, Ti, Mo≤2.00%, Cu≤0.5% is interference measurement not.
The test result of the interference of table 2 coexistence elements
| Element | La/％ | Ce/％ | Pr/％ | Nd/％ | Sm/％ |
| Mark liquid | 0.00005 | 0.00005 | 0.00005 | 0.00005 | 0.00005 |
| Measured value | 0.000048 | 0.000053 | 0.000051 | 0.000054 | 0.000047 |
| Mark liquid | 0.0005 | 0.0005 | 0.0005 | 0.0005 | 0.0005 |
| Measured value | 0.00052 | 0.00051 | 0.00047 | 0.00051 | 0.00052 |
| Mark liquid | 0.0020 | 0.0020 | 0.0020 | 0.0020 | 0.0020 |
| Measured value | 0.0019 | 0.0017 | 0.0023 | 0.0018 | 0.0017 |
| Mark liquid | 0.010 | 0.010 | 0.010 | 0.010 | 0.010 |
| Measured value | 0.012 | 0.018 | 0.018 | 0.012 | 0.013 |
With specific embodiment, technical scheme of the present invention is described further below.
In following embodiment, the inductively-coupled plasma spectrometer of the inductively-coupled plasma spectrometer of employing to be the model of PE company of the U.S. be ELAN DRC-e, the running parameter of this spectrometer is as shown in table 3.Measure isotope
139la,
140ce,
141pr,
143nd,
147sm.Conductor refrigeration power supply is that Tianjin refrigerator factory produces.
Table 3 Instrument working parameter
Note: measure isotope
139la,
140ce,
141pr,
146nd,
147sm.
Each embodiment agents useful for same: anhydrous Lithium chloride, analyzes pure; Diacetone, analyzes pure; Absolute ethyl alcohol, top grade is pure; Absolute methanol, analyzes pure; Iodine, top grade is pure; Nitric acid density is about 1.42g/mL, and top grade is pure; Hydrochloric acid density is 1.19g/mL, and top grade is pure; Hydrofluorite density is 1.13g/mL, and top grade is pure; Perchloric acid density is 1.68g/mL, and top grade is pure; Standard Stock solutions: lanthanum, cerium, praseodymium, neodymium, samarium are 1000 μ g/mL, State Standard Matter Research Centre; Caesium Standard Stock solutions: the concentration of caesium is 1000 μ g/mL, caesium inner mark solution: the concentration of caesium is 1.0 μ g/mL; Deionized water is self-control.
The acquisition methods of the working curve of the icp ms of each embodiment is as follows:
In 7 100mL volumetric flasks, accurately add 1.0g anhydrous Lithium chloride respectively; Pipette lanthanum that concentration is 0.1 μ g/mL, cerium, praseodymium, neodymium, samarium standard solution 0mL, 0.5mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL, 20.00mL respectively, be diluted with water to scale to shake up, take caesium as internal standard element, employing icp ms measures, the automatic drawing curve of instrument, its related coefficient is all more than 0.999.
Embodiment 1
The rare earth steel sample containing total amount of rare earth being 0.012% is made diameter 8mm, long 80mm column, digs apart from 4mm place, top the groove that a degree of depth is 2mm at it, observe and show atresia, flawless.
By sample fill 25mL water, 25mL ρ 1.19g/mL hydrochloric acid measuring cup in soak 10min take out, clean, alcohol flushing, dries.Accurately take steel sample weight m
1=92.6248g.The glass beaker of the electrolytic solution 250mL filling the absolute methanol solution of the diacetone of the anhydrous Lithium chloride comprising the mass percentage 1% and percent by volume 8% prepared is put into electrolytic cell, open conductor refrigeration power supply, temperature is adjusted to less than-20 DEG C, liquid temp to be electrolysed reaches less than-10 DEG C, using the steel sample of having weighed as anode, stainless steel cylinder is as negative electrode, electrolysis is carried out under Faradaic current 0.5A, electrolysis 30min, take off, steel sample is put into 150mL glass beaker and is wiped excellent power taking solution residue, the electrolysis residue on steel sample is rinsed with water, alcohol flushing dries, weigh m
2=92.3715g.
From electrolytic cell, take out glass beaker, take out stainless steel cylinder negative electrode, use alcohol flushing negative electrode.The glass beaker filling electrolytic solution is put into water-bath, by organism evaporates to dryness such as diacetones, add the nitric acid residue decomposition of 10mL ρ 1.42g/mL, constant volume obtains test solution to be measured in 250mL volumetric flask, in company with band reagent blank, take caesium as internal standard element, adopt icp ms to measure the quality m of the solid solution rare earth in test solution to be measured, and the quality m of solid solution rare earth in blank solution
0, m and m
0(or m-m
0) automatically provided by instrument.Following formula is adopted to obtain solid solution content of rare earth in steel.Measurement result is in table 4.
Embodiment 2
The Biobium rare-earth steel sample containing total amount of rare earth being 0.019% is made diameter 8.2mm, long 82mm column, digs apart from 3mm place, top the groove that a degree of depth is 2mm at it, observe and show atresia, flawless.
By sample fill 30mL water, 30mL ρ 1.19g/mL hydrochloric acid measuring cup in soak 15min take out, clean, alcohol flushing, dries.Accurately take steel sample weight m
1=94.0315g.The glass beaker of the electrolytic solution 250mL filling the absolute methanol solution of the diacetone of the anhydrous Lithium chloride comprising the mass percentage 0.9% and percent by volume 5% prepared is put into electrolytic cell, open conductor refrigeration power supply, temperature is adjusted to less than-20 DEG C, liquid temp to be electrolysed reaches less than-10 DEG C, using the steel sample of having weighed as anode, stainless steel cylinder is as negative electrode, electrolysis is carried out under Faradaic current 0.4A, electrolysis 35min, take off, steel sample is put into 150mL glass beaker and is wiped excellent power taking solution residue, the electrolysis residue on steel sample is rinsed with water, alcohol flushing dries, weigh m
2=93.7821g.
From electrolytic cell, take out glass beaker, take out stainless steel cylinder negative electrode, use alcohol flushing negative electrode.The glass beaker filling electrolytic solution is put into water-bath, by organism evaporates to dryness such as diacetones, add the nitric acid residue decomposition of 10mL ρ 1.42g/mL, constant volume obtains test solution to be measured in 250mL volumetric flask, in company with band reagent blank, take caesium as internal standard element, adopt icp ms to measure the quality m of the solid solution rare earth in test solution to be measured, and the quality m of solid solution rare earth in blank solution
0, m and m
0automatically provided by instrument.The computing formula of embodiment 1 is adopted to obtain solid solution content of rare earth in steel.Measurement result is in table 4.
Embodiment 3
The rare earth steel sample containing cerium being 0.0009% is made diameter 8.2mm, long 82mm column, digs apart from 4mm place, top the groove that a degree of depth is 2mm at it, observe and show atresia, flawless.
By sample fill 25mL water, 25mL ρ 1.19g/mL hydrochloric acid measuring cup in soak 20min take out, clean, alcohol flushing, dries.Accurately take steel sample weight m
1=94.3816g.The glass beaker of the electrolytic solution 250mL filling the absolute methanol solution of the diacetone of the anhydrous Lithium chloride comprising the mass percentage 1% and percent by volume 5% prepared is put into electrolytic cell, open conductor refrigeration power supply, temperature is adjusted to less than-20 DEG C, liquid temp to be electrolysed reaches less than-10 DEG C, using the steel sample of having weighed as anode, stainless steel cylinder is as negative electrode, electrolysis is carried out under Faradaic current 0.5A, electrolysis 30min, take off, steel sample is put into 150mL glass beaker and is wiped excellent power taking solution residue, the electrolysis residue on steel sample is rinsed with water, alcohol flushing dries, weigh m
2=94.1378g.
From electrolytic cell, take out glass beaker, take out stainless steel cylinder negative electrode, use alcohol flushing negative electrode.The glass beaker filling electrolytic solution is put into water-bath, by organism evaporates to dryness such as diacetones, add the nitric acid residue decomposition of 8mL ρ 1.42g/mL, constant volume obtains test solution to be measured in 250mL volumetric flask, in company with band reagent blank, take caesium as internal standard element, adopt icp ms to measure the quality m of the solid solution rare earth in test solution to be measured, and the quality m of solid solution rare earth in blank solution
0, m and m
0automatically provided by instrument.Following formula is adopted to obtain solid solution content of rare earth in steel.Measurement result is in table 4.
The each embodiment measurement result of table 4
| Embodiment | Sample | Total amount of rare earth measured value | Solid solution rare earth measured value |
| 1 | Rare earth steel sample | 0.012 | 0.00072 |
| 2 | Containing Biobium rare-earth steel sample | 0.019 | 0.0011 |
| 3 | Containing cerium steel sample | 0.00090(Ce) | 0.000068 |
As can be seen from Table 4, the results contrast adopting method of the present invention to test is accurate.
In sum, method of the present invention optimizes the composition of electrolytic solution of the prior art.The electrolytic solution internal resistance of method of the present invention is little, can ensure that in electrolytic process electrolysis temperature remains on less than-10 DEG C, the re inclusion of poor stability is avoided to decompose, and cause solid solution rare earth to increase, simultaneously, adopt ICP-MS to measure, give the amount of single solid solution rare earth, substantially increase accuracy and precision; For providing accurate data containing the research of the exploitation of rare earth steel grade and the mechanism of action of rare earth in steel, there is certain economic benefit and significant social benefit.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the assay method of solid solution content of rare earth in steel, is characterized in that, comprising:
Be m by quality
1steel sample as anode, using stainless steel as negative electrode, using the absolute methanol solution of anhydrous Lithium chloride and diacetone as electrolytic solution electrolysis, the quality of the described steel sample after electrolysis of weighing is m
2;
By the organism evaporate to dryness in the described electrolytic solution after electrolysis, add nitric acid residue decomposition and obtain test solution to be measured;
Take caesium as internal standard element, adopt icp ms to measure the quality m of the solid solution rare earth in described test solution to be measured, and the quality m of solid solution rare earth in blank solution
0;
Employing formula
Obtain solid solution content of rare earth in steel.
2. the assay method of solid solution content of rare earth in steel as claimed in claim 1, it is characterized in that: in described electrolytic solution, the mass percentage of anhydrous Lithium chloride is 0.9% ~ 1.1%, the percent by volume of diacetone is 5% ~ 7%.
3. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: the volume of described electrolytic solution is 250mL.
4. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: the electric current of described electrolysis is 0.3A ~ 0.6A, and temperature is less than-10 DEG C, and the time is 20min ~ 40min.
5. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: the volume of nitric acid is 8 ~ 10mL, and density p is 1.42g/mL.
6. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: described employing icp ms measures the quality m of the solid solution rare earth in described test solution to be measured, and the quality m of solid solution rare earth in blank solution
0process comprise:
Respectively to standard solution 0mL, 0.5mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL and 20.00mL of adding lanthanum, cerium, praseodymium, neodymium and samarium that concentration is 0.1 μ g/mL in 1.0g anhydrous Lithium chloride, add the nitric acid that 3mL density is 1.42g/mL, be diluted with water to 100mL, take caesium as internal standard element, described icp ms is adopted to measure, with the mass percentage of solid solution rare earth for horizontal ordinate, mass spectral intensities is ordinate, drawing curve;
Described icp ms is adopted to measure the mass spectral intensities of the solid solution rare earth in described test solution to be measured, and the intensity of solid solution rare earth in blank solution;
On described working curve, the quality m of the solid solution rare earth in corresponding test solution described to be measured is obtained according to the mass spectral intensities of the solid solution rare earth in the mass spectral intensities of the solid solution rare earth in described test solution to be measured, described blank solution, and the quality m of solid solution rare earth in described blank solution
0.
7. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: the volume of the described test solution described to be measured measured for icp ms is 250mL.
8. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: described be m by quality
1the process of steel sample as anode before, also comprise and described steel sample taken out after being soak 10 ~ 20min in the hydrochloric acid of 1.19g/mL in 20 ~ 30mL water, 20 ~ 30mL density, clean, alcohol flushing the step of drying.
9. the assay method of solid solution content of rare earth in steel as claimed in claim 1, is characterized in that: the shape of described steel sample is basal diameter is 8 ~ 10mm, and height is the column of 80 ~ 100mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954139A (en) * | 2016-05-04 | 2016-09-21 | 内蒙古工业大学 | Method for directly measuring solid solubility of rare earth in rare earth magnesium alloy |
| CN109374602A (en) * | 2018-11-13 | 2019-02-22 | 内蒙古科技大学 | Neodymium produces the measuring method of neodymium fluoride and fluorination lithium content in electrolyte |
| CN113109321A (en) * | 2021-04-07 | 2021-07-13 | 北京首钢吉泰安新材料有限公司 | Method for measuring content of solid solution yttrium in iron-chromium-aluminum alloy |
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| CN109374602A (en) * | 2018-11-13 | 2019-02-22 | 内蒙古科技大学 | Neodymium produces the measuring method of neodymium fluoride and fluorination lithium content in electrolyte |
| CN109374602B (en) * | 2018-11-13 | 2021-06-22 | 内蒙古科技大学 | Method for measuring content of neodymium fluoride and lithium fluoride in electrolyte produced by neodymium |
| CN113109321A (en) * | 2021-04-07 | 2021-07-13 | 北京首钢吉泰安新材料有限公司 | Method for measuring content of solid solution yttrium in iron-chromium-aluminum alloy |
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