CN106226192A - A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy - Google Patents
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy Download PDFInfo
- Publication number
- CN106226192A CN106226192A CN201610738283.9A CN201610738283A CN106226192A CN 106226192 A CN106226192 A CN 106226192A CN 201610738283 A CN201610738283 A CN 201610738283A CN 106226192 A CN106226192 A CN 106226192A
- Authority
- CN
- China
- Prior art keywords
- niobium
- titanium
- acid
- solution
- precipitation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Engineering & Computer Science (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, and step is: preparation titanium-niobium alloy sample solution: weigh titanium-niobium alloy sample, dissolves；Niobium in tannic acid hydrating solution also precipitates: secondary precipitation；The mensuration of niobium.Present invention application HNO3, HF dissolution mechanism, effective；Using tannic acid to make niobium hydrolytic precipitation complete, and tannic acid calcination (decomposition) is complete, analysis result is stable；Spectroscopic test wave-length coverage is wider；Relative standard deviation is little.
Description
Technical field
The present invention relates to chemical analysis method, measure metal niobium in alloy more specifically to a kind of gravimetry and contain
The method of amount.
Background technology
Ti45Nb alloy is the U.S.'s a large amount of rivet bars used in Aerospace Products, and this alloy has in annealed condition
There are preferable tensile property, shear strength and high plasticity, are suitable for manufacturing the rivet joint of composite.With other
Aviation rivet bar is compared, and the specific strength of Ti45Nb alloy is the highest.In the titanium alloy material of rivet bar, titanium niobium rivet
It is easier riveting with pure titanium rivet to shape.The shear strength of titanium-niobium alloy, tensile strength are above pure titanium, and resistance of deformation
Less than pure titanium, so the U.S. has eliminated pure titanium rivet, Aerospace Products is all used the titanium of excellent cold-workability exhibiting instead
Niobium rivet.
China has also carried out the development of Ti45Nb alloy material in recent years, for obtaining high-quality rivet bar,
Ti45Nb alloy material must possess the important indicators such as preferable tensile property, shear strength and high plasticity, and these indexs are again
It is inseparable with its chemical composition.Therefore, the strict chemical composition controlling Ti45Nb silk material, finds a kind of stable, accurate
In the detection material that really property is high, the method for chemical composition is to ensure that an important step of quality of materials.
Especially for measuring in Ti45Nb alloy containing 40.0%～50.0% high-load niobium, all there is no one both at home and abroad at present
Plant disclosed, feasible method.That has found is broadly divided into a few class with niobium correlation analysis method: (1) spectrophotography (sulfur
Cyanate photometry, chlorosulfophenol S photometry etc.), this method is not suitable for the analysis of about 45% niobium, and analytical error is bigger；(2) inductance
Coupled plasma-atomic emission spectrometry, although have unit to use this method to carry out the analysis of niobium for many years, but this method exists one
Determine drawback: such as: a. needs standard substance or internal control sample, buys the most nowhere；The most too rely on standard solution,
Niobium standard solution seller have: Iron and Steel Research Geueral Inst, non-ferrous metal study total institute, China National Measuring Science Research Inst. etc., several standards
Between solution variant, bigger analytical error can be brought.(3) gravimetric method, point following several method: a. GB/T 223.38-1985
Ionic energy transfer-gravimetric detemination niobium amount, measurement range 1.00%-5.00%, analyze the upper limit low, uncomfortable high niobium measures, and
Separation has loss to bring error to analysis result；B. chromatographic separation gravimetric method, although existing analysis method GB 3654.1-83
Middle niobium analyst coverage is 50%-80%, and beyond Ti45Nb analyst coverage, but target material matrix is different: GB 3654.1-83 is
Ferro-niobium, also has a large amount of ferrum element to exist in addition to niobium element, is not suitable for the analysis of Ti45Nb in material；c. HB 5220.33-
2008 high temperature alloy chemical analysis method tetraphenylarsonium chloride hydrochloride gravimetric detemination content of niobium, measurement range > 1.00% but by
More expensive in tetraphenylarsonium chloride hydrochloride gravimetric method precipitant, and domestic do not produce, it is impossible to ensure normally carrying out of domestic test.Separately
Outward, needing to use " ammonium nitrate " chemical reagent in chromatographic separation gravimetric method, this reagent belongs to each big city disabling reagent；Above two
Plant the work of method the most unaccommodated niobium Element detection.
Owing to the limitation of current domestic prior art constrains promoting the use of memory alloy material, it can be seen that research
Detection method that go out a kind of unification, that precision is high, reproducible is come in Accurate Determining Ti45Nb memory alloy material containing 40.0%
～50.0% high-load niobium, the most beneficially development of new material more can guarantee that material utilization on product.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provides the mensuration Ti45Nb memory that a kind of precision is high, reproducible
The chemical analysis detection method of high-load niobium in alloy material.
For solving above-mentioned deficiency of the prior art, the present invention is achieved through the following technical solutions:
A kind of measuring the method for content of niobium in titanium-niobium alloy, step is:
S1 prepares titanium-niobium alloy sample solution: weigh titanium-niobium alloy sample, dissolves；
Niobium in S2 hydrating solution also precipitates:
S3 secondary precipitation；
The mensuration of S4 niobium.
The dissolving of described titanium-niobium alloy sample: weigh 0.15g～0.25g sample and be placed in 100 mL platinum wares, add 4 mL
～6 mL concentrated nitric acids (density is 1.42 g/mL), dropping about 3 mL～the dense Fluohydric acid. of 5 mL (density is 1.15 g/mL), low temperature
Heating for dissolving, the coldest, add 10 mL sulfuric acid solutions (being mixed by 1 part of pure water and 1 part of concentrated sulphuric acid), be heated to 2 min that smolder
～3 min, take off beaker and slightly cool down, then in beaker, blow water, be heated to emitting the 2nd sulphoxylic acid cigarette about 2 ~ 3min, cooling, in order to
Catch up with most F-Ion, cooling.Add 30mL ~ 40mL hydrochloric acid solution (being mixed by 1 part of pure water and 1 part of concentrated hydrochloric acid), heating for dissolving
Salt.
Make the niobium in the titanium-niobium alloy sample after dissolving hydrolyze, obtain impure niobium pentaoxide precipitation: test solution is proceeded to 500
In mL beaker, add 20 mL boric acid saturated solutions, be diluted with water to 250 mL, be heated to 70 DEG C～80 DEG C, add 100 mL～
150 mL tannic acid solutions (20 g/L) and a small amount of paper pulp, heated and boiled 10 min, static 1 hour.With filter paper at a slow speed and paper pulp
Filtering, niobium pentaoxide precipitation tannic acid-hydrochloric acid cleaning mixture (5g/L) is washed 7-8 time.First time filtrate is stored in 500 mL
In volumetric flask, it is diluted to scale, shakes up.
Secondary precipitation, obtains pure niobium pentaoxide precipitation: together with filter paper, niobium pentaoxide precipitation is placed in constant weight (quality
It is designated as m2) platinum crucible in, dry, ashing completely, in 1000 DEG C of calcination 0.5 h, is taken out, the coldest, is placed in exsiccator, cold
But to room temperature, weigh, and repeatedly calcination to constant weight.Add 4 g potassium pyrosulfates (solid), in 700 DEG C of Muffle furnaces, add heat fusing
Dissolve completely to oxide, cooling, it is placed in 250 mL beakers, (dense by 1 part of pure water and 1 part with 30mL ~ 40mL hydrochloric acid solution
Mixed in hydrochloric acid forms) leach frit, wash out crucible, be diluted with water to 250 mL, be placed in the water-bath of 70 DEG C～80 DEG C
0.5 h, takes out, and is subsequently adding 100 mL～150 mL tannic acid solutions (20 g/L) and a small amount of paper pulp, boils 10 min, static
1 h is with import filter paper (diameter 12.5 cm, aperture 8 μm) and paper pulp filtering, heavy with tannic acid-hydrochloric acid lotion (5g/L) washing
Form sediment 7～8 times.
Niobium, tantalum, the correction of titanium and measurement: pure niobium pentaoxide precipitation is placed in same platinum earthenware used together with filter paper
In crucible, it is dried, ashing, takes out in 1000 DEG C of calcination 0.5 h, the coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and instead
To constant weight, (quality is designated as m in multiple calcination1)。
With 4 mL～6 mL concentrated nitric acids (density is 1.42 g/mL), and 3 mL～the dense Fluohydric acid. of 5 mL (density is 1.15
G/mL) the pure niobium pentaoxide precipitation obtained before dissolving, uses ICP-AES afterwards
Measure a small amount of tantalum and the quality of titanium in oxide；Carry out the filtrate of first time isolated point taking simultaneously, use inductance coupling
Close plasma atomic emission spectrometry and measure the niobium element quality wherein run off.
Finally by platinum crucible and quality m of precipitation1Deduct clean quality m of platinum crucible2Deduct five oxidations a small amount of in oxide
Two tantalums and the quality of titanium dioxide, add a small amount of niobium element quality run off in filtrate, finally obtains in sample niobium accurately
The content of element.
Compared with prior art, it is an advantage of the current invention that:
Method the most of the present invention, because having taken into full account that content is up to the impact of about 50% titanium, uses " nitric acid-hydrogen fluorine
Acid-sulphuric acid " dissolution method, can be with rapid solution titanium-niobium alloy material, sample solution is clarified and stable, and prior art should be all
Low to material titaniums such as iron and steel, the alloy more containing impurity such as chromium, tungsten, molybdenum, zirconium, tantalums dissolves, and is mostly to use hydrochloric acid-nitric acid molten
Solve, or add hydrogen peroxide oxidation, with arsenobenzene Acid precipitation niobium and tantalum；Or dissolve with hydrochloric acid-nitric acid, use perchloric acid oxygen
Changing, danger is bigger；Or in Muffle furnace high-temperature fusion, but these methods are not because accounting for titanium elements, be used for dissolve
Ti45Nb material, sample or dissolving are incomplete, or dissolution time is long, or become turbid, it is impossible to carry out follow-up analysis.
Method the most of the present invention has taken into full account in niobium pentaoxide precipitation containing a small amount of impurity titanium, the correction of tantalum.
In precipitation containing the reason of titanium be because titanium () it is most stable of state, also it is the modal oxidation state of titanium.Titanium () at water
Being stable in solution, it can be likely to be formed in denseer hydrochloric acid solution in different ionic conditions in different solution
Coordinate anion；Titanium () easily hydrolyze and form multinuclear ion, it is in weakly acidic solution, or standing time is longer, titanium (
) easily hydrolyze to form white metatitanic acid precipitation or colloid, even if once occurring that this situation improves that acidity is the most extremely difficult is re-dissolved in acid
, unless emitted sulphuric acid cigarette again or added and emit sulphuric acid cigarette such as Fluohydric acid. again.Method of the present invention uses the examination of nitric acid, hydrofluoric acid dissolution
Sample is smoldered through sulphuric acid again, and when adding tannic acid, solution acidity is less, has the titanium of " not fixed amount " to form white while niobium precipitation
Metatitanic acid precipitation or colloid so that all contain " Ti " in the precipitation of niobium after separating, want in the precipitation obtained the last time every time
" Ti " is corrected.Due to niobium and tantalum atom radius very close to, thus the character of niobium and tantalum is closely similar, and always symbiosis
's.Niobates easily hydrolyzes, and generates the niobic acid (Nb of white gum2O5·5H2O) precipitation, tantalates the most easily hydrolyzes, and generates white
Tantalic acid (the Ta of coloring agent shape2O5·5H2O) precipitation so that all contain " Ta " in the precipitation of niobium after every time separating, the last time
To precipitation in " Ta " is corrected.
The key technology of the present invention is the titanium unit having taken into full account compared to existing technology and having contained high-load in sample Ti45Nb
Element, therefore uses and precipitation is carried out secondary separation.Because finding that each precipitate and separate calcination thing is impure by research likely to contain
There is titanium dioxide precipitation, need to separate next time, after last separation, titanium, tantalum are corrected, thus obtain accurately
Analysis result.And compare prior art JIS G1237-86 " niobium pentaoxide gravimetric method " although have also contemplated that in precipitation and containing
There is Ti, but because prior art is the mensuration for iron and steel, in iron and steel, Ti content is the lowest, uses the light splitting light wasted time and energy
The tantalum contained in degree method mensuration precipitation and titanium, and the method for the secondary separation that the present invention is selected by research and the electricity consumption of employing
Sense coupled plasma-atomic emission spectrographic determination tantalum and titanium are more convenient, accurate, reasonable.
Method the most of the present invention considers to be measured the niobium element in filtrate, finally substitutes into end product
In calculating.This is to find that in primary filtrate, niobium is in the form of an ion or complex form enters in process of the test through research
In filtrate, there is no hydrolytic precipitation, if not considering to measure this part content of niobium, last Lower result can be made.And prior art is all
Do not account for measuring the niobium element content in filtrate so that measurement result is inaccurate.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
1. test apparatus: inductively coupled plasma atomic emission spectrometer.
2. test reagent
Except as otherwise noted, should use in analysis and confirm as the water of the pure reagent of top grade and redistilled water or suitable purity.
Standard solution required in test is in addition to the compound method preparation specified by this standard, it is possible to use national standard material (standard
Solution).
2.1 hydrochloric acid, ρ about 1.19 g/mL.
2.2 nitric acid, ρ about 1.42 g/mL.
2.3 Fluohydric acid .s, ρ about 1.15 g/mL.
2.4 sulphuric acid, ρ about 1.84 g/mL.
2.5 hydrochloric acid, are mixed by 1 part of pure water and 1 part of concentrated hydrochloric acid.
2.6 sulphuric acid, are mixed by 1 part of pure water and 1 part of concentrated sulphuric acid.
2.7 boric acid saturated solutions.
2.8 potassium pyrosulfates, solid.
2.9 ammonium sulfate, solid.
2.10 tannic acid solutions, 20 g/L.
2.11 tannic acid-hydrochloric acid lotion, 5 g/L.
2.12 tartaric acid solutions, 300 g/L.
2.13 import filter paper: diameter 12.5 cm, aperture 8 μm.
2.14 niobium standard solution A, 0.50 mg/mL.
Weigh 0.3578 g and be pre-dried to high-purity niobium pentaoxide of constant, be placed in 50 mL porcelain crucibles, add 12 g
Potassium pyrosulfate (2.8), puts into high temperature furnace, melts to transparent in 650 DEG C, takes out cooling.It is placed in 400 mL beakers, uses 70 mL
Tartaric acid solution (2.12) leaching frit, boils to solution transparent, the coldest, adds 200 mL sulphuric acid (2.6), is cooled to room temperature,
Move in 500 mL volumetric flasks, be diluted with water to scale, shake up.
2.15 niobium standard solution B, 0.10 mg/mL.
Pipette 20.00 mL niobium standard solution A (2.14), be placed in 100 mL volumetric flasks, add 20 mL sulphuric acid (2.6),
It is diluted with water to scale, shakes up.
2.16 titanium standard solution A, 1.00 mg/mL.
Weigh titanium dioxide (spectroscopic pure) 0.8340 g in 950 DEG C of calcinations to constant weight, be placed in 400 mL beakers, add
Entering 10 g ammonium sulfate (2.9), 50 mL sulphuric acid (2.6), cap upper surface ware, high-temperature heating is to emitting sulphuric acid cigarette, until it is molten to obtain clarification
Till liquid.It is cooled to room temperature, moves in the 500 mL beakers filling water, the coldest, move into 500 mL volumetric flasks, be cooled to room temperature
After, it is diluted with water to scale, shakes up.
2.17 titanium standard solution B, 0.10 mg/mL.
Pipette 20.00 mL titanium standard solution A (2.16) in 200 mL volumetric flasks, add 40 mL sulphuric acid (2.6), use water
It is diluted to scale, shakes up.
2.18 tantalum standard solution A, 1.00 mg/mL.
Weigh the 0.6106 high-purity tantalum pentoxide of g to be placed in platinum crucible, add 10 mL Fluohydric acid .s (2.3), 2 mL nitric acid
(2.2), slight fever is dissolved, until adding 10 mL Fluohydric acid .s (2.3) after solution is transparent, cooling, dilute with water constant volume are in 500
In mL plastics volumetric flask, shake up.
2.19 tantalum standard solution B, 0.10 mg/mL.
Pipette 20.00 mL tantalum standard solution A (2.18) in 200 mL volumetric flasks, add 20 mL sulphuric acid (2.6), use water
It is diluted to scale, shakes up.
Liquid at the bottom of 2.20 titaniums, 1.00mg/mL.
Weigh 0.2500 g metallic titanium powder (mass fraction of titanium is not less than 99.95 %), be placed in 300 mL beakers, add
50 mL sulphuric acid (2.6), low-temperature heat is dissolved, and drips nitric acid (2.2) and be wholly absent to purple after dissolving completely, and cooling is blown water and added
Heat of solution salt, the coldest, move in 250 mL volumetric flasks, be diluted with water to scale, shake up.
Embodiment 1
3 sample test portions
Weigh 0.1781 g Ti45Nb sample test portion, be accurate to 0.0001 g.
Prepared by 4 test solutions
Test portion (3) is placed in 100 mL platinum wares by 4.1, adds 4 mL concentrated nitric acids (density is 1.42 g/mL), drips about 3 mL
Dense Fluohydric acid. (density is 1.15 g/mL), at 60 DEG C～80 DEG C, heating for dissolving is complete, the coldest, adds 10 mL sulphuric acid
(2.6), it is heated to 2 min～3 min that smolder, takes off beaker and slightly cool down, then in beaker, blow water, be heated to emitting the 2nd sulphoxylic acid
Cigarette about 2 min ~ 3min, cooling, in order to catch up with most F-Ion, cooling, add 30 mL hydrochloric acid (2.5), heating for dissolving salt.
Test solution in 4.1 is proceeded in 500 mL beakers by 4.2, adds 20 mL boric acid saturated solution (2.7), is diluted with water to
250 mL, are placed into 0.5 h in the water-bath of 70 DEG C～80 DEG C, take out, are subsequently adding 100 mL tannic acid solutions (2.10)
Heated and boiled 10 min, static 1 h.With import filter paper (2.13) and paper pulp filtering, tannic acid-hydrochloric acid lotion (2.11) washing is heavy
Form sediment 7～8 times.Filtrate is stored in 500 mL volumetric flasks, is diluted to scale, shakes up.
5 precipitate and separate
Together with filter paper, the precipitation in 4.2 is placed in constant weight, and (quality is designated as m2=28.5733g) platinum crucible in, dry, be ashed
Entirely, in 1000 DEG C of calcination 0.5 h, take out, the coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and calcination is the most permanent repeatedly
Weight.Adding 4 g potassium pyrosulfates (2.8), in 700 DEG C of Muffle furnaces, heating melts to oxide dissolving completely, and cooling is placed into
In 250 mL beakers, leach frit with 30mL hydrochloric acid solution (2.5), wash out crucible, be diluted with water to 250 mL, be placed into 70
DEG C～the water-bath of 80 DEG C in 0.5 h, take out, be subsequently adding 100 mL tannic acid solution (2.10) and 0.9g～1.2g paper pulp,
Boil 10 min, static 1 h, with import filter paper (2.13) and paper pulp filtering, heavy with tannic acid-hydrochloric acid lotion (2.11) washing
Form sediment 7～8 times.
6 measure
Precipitation (5) is placed in same platinum crucible used together with filter paper, is dried, ashing, take out in 1000 DEG C of calcination 0.5 h,
The coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and then calcination to constant weight weighs that (quality is designated as m repeatedly1=
28.7094g)。
7 niobiums, tantalum, the correction of titanium
The correction of 7.1 niobiums
7.1.1 the preparation of test solution
Pipette 25.00 mL filtrates (4.2) in 50 mL plastics volumetric flasks, add 10 Fluohydric acid .s (2.3), 5 mL hydrochloric acid
(2.1), it is diluted with water to scale, shakes up.
7.1.2 the preparation of standard curve serial solution
7.1.2.1 high standard solution
Pipette the blank assay solution of 25.00 mL and filtrate (4.2) synchronization gain in 50 mL plastics volumetric flasks, according to filtrate
Middle titanium, the content range of niobium, be separately added into liquid (2.20) at the bottom of appropriate titanium, niobium standard solution (2.14 or 2.15) in volumetric flask,
It is used as the niobium national standard solution of respective concentration, makes the content of niobium in high standard solution be slightly above the content of niobium in filtrate, add
Enter 10 Fluohydric acid .s (2.3), 5 mL hydrochloric acid (2.1), be diluted with water to scale, shake up.
7.1.2.2 low mark solution
Pipette the blank reagent solution of 25.00 mL and filtrate (4.2) synchronization gain in 50 mL plastics volumetric flasks, add 10
Fluohydric acid. (2.3), 5 mL hydrochloric acid (2.1), it is diluted with water to scale, shakes up.
7.2 tantalums, the correction of titanium
7.2.1 the preparation of test solution
By in 6 equipped with the platinum crucible of oxide precipitation adds 4 mL concentrated nitric acids (density is 1.42 g/mL), and 3 mL dense hydrogen fluorine
Acid (density is 1.15 g/mL), heats at 60 DEG C～80 DEG C, and after about 20 min, oxide starts to dissolve, after dissolving completely,
Move in 100 mL plastics volumetric flasks, be diluted with water to scale, shake up.
Many parts of Timing Belt blank reagent solution, during for preparation standard curve serial solution.
7.2.2 the preparation of standard curve serial solution
7.2.2.1 high standard solution
Move in 100 mL plastics volumetric flasks by 7.2.1 synchronizes blank reagent solution, according to tantalum in oxide precipitation, the containing of titanium
Weight range, is separately added into appropriate tantalum standard solution (2.18 or 2.19), titanium standard solution (2.16 or 2.17), also in volumetric flask
The tantalum of respective concentration, titanium national standard solution can be used, make tantalum in high standard solution, the content of titanium be slightly above in oxide precipitation
Tantalum, the content of titanium, be diluted with water to scale, shake up.
7.3.4.2.2.2 low mark solution
Move into 7.2.1 synchronizes blank reagent solution in 100 mL plastics volumetric flasks, be diluted with water to scale, shake up.
7.3 measure
Instrument optimization is made, after instrument stabilizer, selected by inductively coupled plasma atomic emission spectrometer description
Under instrument working condition and analysis of line wavelength, use the standard curve serial solution (7.1.2 and 7.2.2) of preparation that instrument is carried out
Standardization, in sequentially determining test solution (7.1.1 and 7.2.1), in niobium, tantalum, the quality of titanium or percentage composition, respectively filtrate, niobium contains
Amount w1It is 0.448%；In precipitation niobium pentaoxide, tantalum content is 0.00012g, and Ti content is 0.00445g.
The calculating of 8 analysis results
In the precipitation niobium pentaoxides that 8.1 will record in 7.3, tantalum, Ti content are converted into the matter of tantalum pentoxide, titanium dioxide
Amount, is designated as m respectively3、m4, m3=G, 0.8189 is Ta2O5Conversion coefficient, m4=G, 0.5995 is TiO2Conversion coefficient.
8.2 calculate the mass fraction of niobium by formula (1)w, numerical value represents with %:
... ... ... ... (1)
In formula:
Platinum crucible and the quality of precipitation, unit is gram (g)；
The quality of platinum crucible, unit is gram (g)；
The quality of tantalum pentoxide in precipitation, unit is gram (g)；
The quality of titanium dioxide in precipitation, unit is gram (g)；
The quality of test portion, unit is gram (g)；
The mass fraction of niobium element in filtrate for the first time.
50.93%
Embodiment 2
3 sample test portions
Weigh 0.1997 g Ti45Nb sample test portion, be accurate to 0.0001 g.
Prepared by 4 test solutions
Test portion (3) is placed in 100 mL platinum wares by 4.1, adds 5mL concentrated nitric acid (density is 1.42 g/mL), and about 4 mL are dense in dropping
Fluohydric acid. (density is 1.15 g/mL), at 60 DEG C～80 DEG C, heating for dissolving is complete, the coldest, adds 10 mL sulphuric acid (2.6),
It is heated to 2 min～3 min that smolder, takes off beaker and slightly cool down, then in beaker, blow water, be heated to emitting the 2nd sulphoxylic acid cigarette about 2
Min ~ 3min, cooling, in order to catch up with most F-Ion, cooling, add 35 mL hydrochloric acid (2.5), heating for dissolving salt.
Test solution in 4.1 is proceeded in 500 mL beakers by 4.2, adds 20 mL boric acid saturated solution (2.7), is diluted with water to
250 mL, are placed into 0.5 h in the water-bath of 70 DEG C～80 DEG C, take out, are subsequently adding 120 mL tannic acid solutions (2.10)
Heated and boiled 10 min, static 1 h.With import filter paper (2.13) and paper pulp filtering, tannic acid-hydrochloric acid lotion (2.11) washing is heavy
Form sediment 7～8 times.Filtrate is stored in 500 mL volumetric flasks, is diluted to scale, shakes up.
5 precipitate and separate
Together with filter paper, the precipitation in 4.2 is placed in constant weight, and (quality is designated as m2=29.5042g) platinum crucible in, dry, be ashed
Entirely, in 1000 DEG C of calcination 0.5 h, take out, the coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and calcination is the most permanent repeatedly
Weight.Adding 4 g potassium pyrosulfates (2.8), in 700 DEG C of Muffle furnaces, heating melts to oxide dissolving completely, and cooling is placed into
In 250 mL beakers, leach frit with 35mL hydrochloric acid solution (2.5), wash out crucible, be diluted with water to 250 mL, be placed into 70
DEG C～the water-bath of 80 DEG C in 0.5 h, take out, be subsequently adding 120 mL tannic acid solution (2.10) and 0.9g～1.2g paper pulp,
Boil 10 min, static 1 h, with import filter paper (2.13) and paper pulp filtering, heavy with tannic acid-hydrochloric acid lotion (2.11) washing
Form sediment 7～8 times.
6 measure
Precipitation (5) is placed in same platinum crucible used together with filter paper, is dried, ashing, take out in 1000 DEG C of calcination 0.5 h,
The coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and then calcination to constant weight weighs that (quality is designated as m repeatedly1=
29.6436g)。
7 niobiums, tantalum, the correction of titanium
The correction of 7.1 niobiums
7.1.1 the preparation of test solution
Pipette 25.00 mL filtrates (4.2) in 50 mL plastics volumetric flasks, add 10 Fluohydric acid .s (2.3), 5 mL hydrochloric acid
(2.1), it is diluted with water to scale, shakes up.
7.1.2 the preparation of standard curve serial solution
7.1.2.1 high standard solution
Pipette the blank assay solution of 25.00 mL and filtrate (4.2) synchronization gain in 50 mL plastics volumetric flasks, according to filtrate
Middle titanium, the content range of niobium, be separately added into liquid (2.20) at the bottom of appropriate titanium, niobium standard solution (2.14 or 2.15) in volumetric flask,
It is used as the niobium national standard solution of respective concentration, makes the content of niobium in high standard solution be slightly above the content of niobium in filtrate, add
Enter 10 Fluohydric acid .s (2.3), 5 mL hydrochloric acid (2.1), be diluted with water to scale, shake up.
7.1.2.2 low mark solution
Pipette the blank reagent solution of 25.00 mL and filtrate (4.2) synchronization gain in 50 mL plastics volumetric flasks, add 10
Fluohydric acid. (2.3), 5 mL hydrochloric acid (2.1), it is diluted with water to scale, shakes up.
7.2 tantalums, the correction of titanium
7.2.1 the preparation of test solution
By in 6 equipped with the platinum crucible of oxide precipitation adds 5 mL concentrated nitric acids (density is 1.42 g/mL), and 4 mL dense hydrogen fluorine
Acid (density is 1.15 g/mL), heats at 60 DEG C～80 DEG C, and after about 20 min, oxide starts to dissolve, after dissolving completely,
Move in 100 mL plastics volumetric flasks, be diluted with water to scale, shake up.
Many parts of Timing Belt blank reagent solution, during for preparation standard curve serial solution.
7.2.2 the preparation of standard curve serial solution
7.2.2.1 high standard solution
Move in 100 mL plastics volumetric flasks by 7.2.1 synchronizes blank reagent solution, according to tantalum in oxide precipitation, the containing of titanium
Weight range, is separately added into appropriate tantalum standard solution (2.18 or 2.19), titanium standard solution (2.16 or 2.17), also in volumetric flask
The tantalum of respective concentration, titanium national standard solution can be used, make tantalum in high standard solution, the content of titanium be slightly above in oxide precipitation
Tantalum, the content of titanium, be diluted with water to scale, shake up.
7.3.4.2.2.2 low mark solution
Move into 7.2.1 synchronizes blank reagent solution in 100 mL plastics volumetric flasks, be diluted with water to scale, shake up.
7.3 measure
Instrument optimization is made, after instrument stabilizer, selected by inductively coupled plasma atomic emission spectrometer description
Under instrument working condition and analysis of line wavelength, use the standard curve serial solution (7.1.2 and 7.2.2) of preparation that instrument is carried out
Standardization, in sequentially determining test solution (7.1.1 and 7.2.1), in niobium, tantalum, the quality of titanium or percentage composition, respectively filtrate, niobium contains
Amount w1It is 0.355%；In precipitation niobium pentaoxide, tantalum content is 0.00010g, and Ti content is 0.00376g.
The calculating of 8 analysis results
In the precipitation niobium pentaoxides that 8.1 will record in 7.3, tantalum, Ti content are converted into the matter of tantalum pentoxide, titanium dioxide
Amount, is designated as m respectively3、m4, m3=G, 0.8189 is Ta2O5Conversion coefficient, m4=G, 0.5995 is TiO2Conversion coefficient.
8.2 calculate the mass fraction of niobium by formula (1)w, numerical value represents with %:
... ... ... ... (1)
In formula:
Platinum crucible and the quality of precipitation, unit is gram (g)；
The quality of platinum crucible, unit is gram (g)；
The quality of tantalum pentoxide in precipitation, unit is gram (g)；
The quality of titanium dioxide in precipitation, unit is gram (g)；
The quality of test portion, unit is gram (g)；
The mass fraction of niobium element in filtrate for the first time.
46.91%
Embodiment 3
3 sample test portions
Weigh 0.2411 g Ti45Nb sample test portion, be accurate to 0.0001 g.
Prepared by 4 test solutions
Test portion (3) is placed in 100 mL platinum wares by 4.1, adds 6mL concentrated nitric acid (density is 1.42 g/mL), and about 5 mL are dense in dropping
Fluohydric acid. (density is 1.15 g/mL), at 60 DEG C～80 DEG C, heating for dissolving is complete, the coldest, adds 10 mL sulphuric acid (2.6),
It is heated to 2 min～3 min that smolder, takes off beaker and slightly cool down, then in beaker, blow water, be heated to emitting the 2nd sulphoxylic acid cigarette about 2
Min ~ 3min, cooling, in order to catch up with most F-Ion, cooling, add 40 mL hydrochloric acid (2.5), heating for dissolving salt.
Test solution in 4.1 is proceeded in 500 mL beakers by 4.2, adds 20 mL boric acid saturated solution (2.7), is diluted with water to
250 mL, are placed into 0.5 h in the water-bath of 70 DEG C～80 DEG C, take out, are subsequently adding 150 mL tannic acid solutions (2.10)
Heated and boiled 10 min, static 1 h.With import filter paper (2.13) and paper pulp filtering, tannic acid-hydrochloric acid lotion (2.11) washing is heavy
Form sediment 7～8 times.Filtrate is stored in 500 mL volumetric flasks, is diluted to scale, shakes up.
5 precipitate and separate
Together with filter paper, the precipitation in 4.2 is placed in constant weight, and (quality is designated as m2=31.0540g) platinum crucible in, dry, be ashed
Entirely, in 1000 DEG C of calcination 0.5 h, take out, the coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and calcination is the most permanent repeatedly
Weight.Adding 4 g potassium pyrosulfates (2.8), in 700 DEG C of Muffle furnaces, heating melts to oxide dissolving completely, and cooling is placed into
In 250 mL beakers, leach frit with 40mL hydrochloric acid solution (2.5), wash out crucible, be diluted with water to 250 mL, be placed into 70
DEG C～the water-bath of 80 DEG C in 0.5 h, take out, be subsequently adding 150 mL tannic acid solution (2.10) and 0.9g～1.2g paper pulp,
Boil 10 min, static 1 h, with import filter paper (2.13) and paper pulp filtering, heavy with tannic acid-hydrochloric acid lotion (2.11) washing
Form sediment 7～8 times.
6 measure
Precipitation (5) is placed in same platinum crucible used together with filter paper, is dried, ashing, take out in 1000 DEG C of calcination 0.5 h,
The coldest, it is placed in exsiccator, is cooled to room temperature, weigh, and then calcination to constant weight weighs that (quality is designated as m repeatedly1=
31.1908g)。
7 niobiums, tantalum, the correction of titanium
The correction of 7.1 niobiums
7.1.1 the preparation of test solution
Pipette 25.00 mL filtrates (4.2) in 50 mL plastics volumetric flasks, add 10 Fluohydric acid .s (2.3), 5 mL hydrochloric acid
(2.1), it is diluted with water to scale, shakes up.
7.1.2 the preparation of standard curve serial solution
7.1.2.1 high standard solution
Pipette the blank assay solution of 25.00 mL and filtrate (4.2) synchronization gain in 50 mL plastics volumetric flasks, according to filtrate
Middle titanium, the content range of niobium, be separately added into liquid (2.20) at the bottom of appropriate titanium, niobium standard solution (2.14 or 2.15) in volumetric flask,
It is used as the niobium national standard solution of respective concentration, makes the content of niobium in high standard solution be slightly above the content of niobium in filtrate, add
Enter 10 Fluohydric acid .s (2.3), 5 mL hydrochloric acid (2.1), be diluted with water to scale, shake up.
7.1.2.2 low mark solution
Pipette the blank reagent solution of 25.00 mL and filtrate (4.2) synchronization gain in 50 mL plastics volumetric flasks, add 10
Fluohydric acid. (2.3), 5 mL hydrochloric acid (2.1), it is diluted with water to scale, shakes up.
7.2 tantalums, the correction of titanium
7.2.1 the preparation of test solution
By in 6 equipped with the platinum crucible of oxide precipitation adds 6 mL concentrated nitric acids (density is 1.42 g/mL), and 5 mL dense hydrogen fluorine
Acid (density is 1.15 g/mL), heats at 60 DEG C～80 DEG C, and after about 20 min, oxide starts to dissolve, after dissolving completely,
Move in 100 mL plastics volumetric flasks, be diluted with water to scale, shake up.
Many parts of Timing Belt blank reagent solution, during for preparation standard curve serial solution.
7.2.2 the preparation of standard curve serial solution
7.2.2.1 high standard solution
Move in 100 mL plastics volumetric flasks by 7.2.1 synchronizes blank reagent solution, according to tantalum in oxide precipitation, the containing of titanium
Weight range, is separately added into appropriate tantalum standard solution (2.18 or 2.19), titanium standard solution (2.16 or 2.17), also in volumetric flask
The tantalum of respective concentration, titanium national standard solution can be used, make tantalum in high standard solution, the content of titanium be slightly above in oxide precipitation
Tantalum, the content of titanium, be diluted with water to scale, shake up.
7.3.4.2.2.2 low mark solution
Move into 7.2.1 synchronizes blank reagent solution in 100 mL plastics volumetric flasks, be diluted with water to scale, shake up.
7.3 measure
Instrument optimization is made, after instrument stabilizer, selected by inductively coupled plasma atomic emission spectrometer description
Under instrument working condition and analysis of line wavelength, use the standard curve serial solution (7.1.2 and 7.2.2) of preparation that instrument is carried out
Standardization, in sequentially determining test solution (7.1.1 and 7.2.1), in niobium, tantalum, the quality of titanium or percentage composition, respectively filtrate, niobium contains
Amount w1It is 0.524%；In precipitation niobium pentaoxide, tantalum content is 0.00012g, and Ti content is 0.00410g.
The calculating of 8 analysis results
In the precipitation niobium pentaoxides that 8.1 will record in 7.3, tantalum, Ti content are converted into the matter of tantalum pentoxide, titanium dioxide
Amount, is designated as m respectively3、m4, m3=G, 0.8189 is Ta2O5Conversion coefficient, m4=
G, 0.5995 is TiO2Conversion coefficient.
8.2 calculate the mass fraction of niobium by formula (1)w, numerical value represents with %:
... ... ... ... (1)
In formula:
Platinum crucible and the quality of precipitation, unit is gram (g)；
The quality of platinum crucible, unit is gram (g)；
The quality of tantalum pentoxide in precipitation, unit is gram (g)；
The quality of titanium dioxide in precipitation, unit is gram (g)；
The quality of test portion, unit is gram (g)；
The mass fraction of niobium element in filtrate for the first time.
38.19%。
Claims (7)
1. a method for content of niobium in gravimetric detemination titanium-niobium alloy, step is:
S1 prepares titanium-niobium alloy sample solution: weigh titanium-niobium alloy sample, dissolves；
Niobium in S2 hydrating solution also precipitates:
S3 secondary precipitation；
The mensuration of S4 niobium.
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, it is characterised in that described step
The dissolving method of rapid S1 titanium-niobium alloy sample is:
Weighing 0.15g～0.25g sample to be placed in 100 mL platinum wares, (density is 1.42 g/ to add 4 mL～6 mL concentrated nitric acids
ML), dropping about 3 mL～the dense Fluohydric acid. of 5 mL (density is 1.15 g/mL), 60 80 DEG C of heating for dissolving, the coldest, add 10 mL
Sulfuric acid solution (is mixed by 1 part of pure water and 1 part of concentrated sulphuric acid), is heated to 2 min～3 min that smolder, takes off beaker and slightly cool down,
Blowing water again in beaker, be heated to emitting the 2nd sulphoxylic acid cigarette about 2 ~ 3min, cooling, in order to catch up with most F-Ion, cooling；Add 30mL
The solution that ~ 40mL is mixed by 1 part of pure water and 1 part of concentrated hydrochloric acid, heating for dissolving salt.
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, it is characterised in that described step
Niobium in rapid S2 hydrating solution the method precipitated be:
Test solution is proceeded in 500 mL beakers, add 20 mL boric acid saturated solutions, be diluted with water to 250 mL, be heated to 70 DEG C
～80 DEG C, add 100 mL～150 mL tannic acid solutions (20 g/L) and 0.9g～1.2g paper pulp, heated and boiled 10 min, quiet
Only 1 hour；With filter paper at a slow speed and paper pulp filtering, niobium pentaoxide precipitation tannic acid-hydrochloric acid cleaning mixture (5g/L) is washed 7-8 time.
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, it is characterised in that described step
The method of rapid S3 secondary precipitation is:
Together with filter paper, niobium pentaoxide precipitation is placed in constant weight, and (quality is designated as m2) platinum crucible in, dry, ashing completely, in
1000 DEG C of calcination 0.5 h, take out, the coldest, be placed in exsiccator, be cooled to room temperature, weigh, and repeatedly calcination to constant weight；Add
4 g potassium pyrosulfates (solid), in 700 DEG C of Muffle furnaces, heating melts to oxide dissolving completely, and cooling is placed into 250 mL
In beaker, leach frit with 30mL ~ 40mL hydrochloric acid solution (being mixed by 1 part of pure water and 1 part of concentrated hydrochloric acid), wash out crucible, use
Water is diluted to 250 mL, is placed into 0.5 h in the water-bath of 70 DEG C～80 DEG C, takes out, is subsequently adding 100 mL～150 mL
Tannic acid solution (20 g/L) and a small amount of paper pulp, boil 10 min, static 1 h, with filter paper (diameter 12.5 cm, aperture 8 μm)
And paper pulp filtering, precipitate 7～8 times with tannic acid-hydrochloric acid lotion (5g/L) washing.
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, it is characterised in that described step
The assay method of rapid S4 niobium is:
Pure niobium pentaoxide precipitation being placed in same platinum crucible used together with filter paper, be dried, ashing, in 1000 DEG C
Calcination 0.5 h takes out, the coldest, is placed in exsiccator, is cooled to room temperature, weighs, and calcination is designated as m to constant weight, quality repeatedly1；
With 4 mL～6 mL concentrated nitric acids (density is 1.42 g/mL), and 3 mL～the dense Fluohydric acid. of 5 mL (density is 1.15 g/mL)
The pure niobium pentaoxide precipitation obtained before dissolving, rear employing ICP-AES measures oxygen
Tantalum a small amount of in compound and the quality of titanium；
By platinum crucible and quality m of precipitation1Deduct clean quality m of platinum crucible2, then deduct tantalum pentoxide a small amount of in oxide
With the quality of titanium dioxide, obtain the content of niobium element in sample.
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, it is characterised in that described
The content of step S4 niobium element also should be plus the niobium element quality run off in filtrate, and the niobium element quality run off in filtrate is will
In step S2, for the first time the filtrate of isolated carries out point taking, the niobium unit quality that employing aes determination wherein runs off
Amount.
A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy, it is characterised in that described former
Sub-emission spectrometry is ICP-AES.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610738283.9A CN106226192A (en) | 2016-08-29 | 2016-08-29 | A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610738283.9A CN106226192A (en) | 2016-08-29 | 2016-08-29 | A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106226192A true CN106226192A (en) | 2016-12-14 |
Family
ID=57555672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610738283.9A Pending CN106226192A (en) | 2016-08-29 | 2016-08-29 | A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106226192A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108169216A (en) * | 2017-12-29 | 2018-06-15 | 清远先导材料有限公司 | The assay method of platinum family element in metallurgical material |
| CN109387450A (en) * | 2017-08-08 | 2019-02-26 | 上海老凤祥首饰研究所有限公司 | Platinum content measuring method in a kind of platinum-nickel alloys ornaments |
| CN111307783A (en) * | 2018-12-11 | 2020-06-19 | 中核北方核燃料元件有限公司 | Method for determining content of impurity elements in uranium nitride solid sample |
| CN111879845A (en) * | 2020-07-24 | 2020-11-03 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving chromium-tantalum-titanium alloy and preparation method and application thereof |
| CN113916875A (en) * | 2021-09-30 | 2022-01-11 | 中国航发北京航空材料研究院 | Method for determining element niobium in high-temperature alloy |
| CN114199857A (en) * | 2021-12-09 | 2022-03-18 | 中国第一汽车股份有限公司 | Method for detecting zirconium content in chromium-free passivation solution |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6078335A (en) * | 1983-10-06 | 1985-05-04 | Meidensha Electric Mfg Co Ltd | Analyzing method of niobium in barium titanate |
| CN102998303A (en) * | 2012-11-22 | 2013-03-27 | 攀钢集团江油长城特殊钢有限公司 | Detection method for determining contents of niobium and tantalum in steel by applying microwave digestion-ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN103115916A (en) * | 2013-01-25 | 2013-05-22 | 内蒙古包钢钢联股份有限公司 | Method for testing niobium content in niobium-iron alloy |
| CN103454175A (en) * | 2013-08-15 | 2013-12-18 | 贵州航天精工制造有限公司 | Method for determining niobium content in aeronautical material Ti45Nb titanium alloy |
| CN104020157A (en) * | 2014-06-12 | 2014-09-03 | 航天精工股份有限公司 | Method for measuring elemental niobium content of titanium-niobium alloy |
-
2016
- 2016-08-29 CN CN201610738283.9A patent/CN106226192A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6078335A (en) * | 1983-10-06 | 1985-05-04 | Meidensha Electric Mfg Co Ltd | Analyzing method of niobium in barium titanate |
| CN102998303A (en) * | 2012-11-22 | 2013-03-27 | 攀钢集团江油长城特殊钢有限公司 | Detection method for determining contents of niobium and tantalum in steel by applying microwave digestion-ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN103115916A (en) * | 2013-01-25 | 2013-05-22 | 内蒙古包钢钢联股份有限公司 | Method for testing niobium content in niobium-iron alloy |
| CN103454175A (en) * | 2013-08-15 | 2013-12-18 | 贵州航天精工制造有限公司 | Method for determining niobium content in aeronautical material Ti45Nb titanium alloy |
| CN104020157A (en) * | 2014-06-12 | 2014-09-03 | 航天精工股份有限公司 | Method for measuring elemental niobium content of titanium-niobium alloy |
Non-Patent Citations (2)
| Title |
|---|
| 司徒杰生主编: "《化工产品手册 无机化工产品》", 31 January 2004, 北京：化学工业出版社 * |
| 曹宏燕主编: "《冶金材料分析技术与应用》", 30 September 2008, 北京：冶金工业出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109387450A (en) * | 2017-08-08 | 2019-02-26 | 上海老凤祥首饰研究所有限公司 | Platinum content measuring method in a kind of platinum-nickel alloys ornaments |
| CN109387450B (en) * | 2017-08-08 | 2021-02-19 | 上海老凤祥首饰研究所有限公司 | Method for measuring platinum content in platinum-palladium alloy ornament |
| CN108169216A (en) * | 2017-12-29 | 2018-06-15 | 清远先导材料有限公司 | The assay method of platinum family element in metallurgical material |
| CN111307783A (en) * | 2018-12-11 | 2020-06-19 | 中核北方核燃料元件有限公司 | Method for determining content of impurity elements in uranium nitride solid sample |
| CN111879845A (en) * | 2020-07-24 | 2020-11-03 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving chromium-tantalum-titanium alloy and preparation method and application thereof |
| CN113916875A (en) * | 2021-09-30 | 2022-01-11 | 中国航发北京航空材料研究院 | Method for determining element niobium in high-temperature alloy |
| CN114199857A (en) * | 2021-12-09 | 2022-03-18 | 中国第一汽车股份有限公司 | Method for detecting zirconium content in chromium-free passivation solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106226192A (en) | A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy | |
| CN102253030B (en) | Method for determining impurity content in high-titanium slag | |
| CN102207475B (en) | Metal alloy XRF spectrometry utilizing new sample preparation technology | |
| CN102928364B (en) | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid | |
| CN101762576B (en) | Method for measuring niobium content in tungsten carbide added with niobium or simultaneously added with tantalum and niobium | |
| CN106596518A (en) | Method for determining zirconium and impurity contents in uranium-zirconium alloy | |
| CN103604800A (en) | Analysis method for determining titanium, vanadium, tungsten, manganese and silicon in K25 chromium-base high temperature alloy | |
| CN108872203A (en) | The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag | |
| CN102393371B (en) | Sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN103954610B (en) | A kind of measure the method for arsenic in high-chromium-nickel steel | |
| CN103698317A (en) | Method for measuring contents of silicon, magnesium and aluminum in coal combustion-supporting agent | |
| CN111257097A (en) | Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof | |
| CN111307797A (en) | Combined determination method for tungsten and silicon content in ferrotungsten | |
| CN107315001B (en) | A kind of method of content of niobium in measurement titanium-niobium alloy | |
| CN101526497B (en) | Method for preparing sample solution for detecting titanium tetrachloride | |
| CN109632769A (en) | Rutile type TiO in titanium ore2Method (2) | |
| CN104215541A (en) | Method for high efficiently and precisely measuring contents of high purity alumina and impurities | |
| CN114136953A (en) | Analysis method for detecting chloride content in sodium sulfate by ICP-AES (inductively coupled plasma-atomic emission Spectrometry) | |
| CN103091155B (en) | Method for dissolving high purity zirconia | |
| CN112710650A (en) | Method for rapidly and accurately measuring main chemical component content of cement | |
| CN105259302B (en) | Directly measure the method for trivalent vanadium content in vanadium slag | |
| CN109596407A (en) | A method of aluminium content in measurement molten iron slag gathering agent | |
| CN105973749A (en) | Method for detecting silicon dioxide in carbide slag | |
| CN106124688A (en) | The mensuration of sulfur content and control method in calcium superphosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161214 |