CN106290314A - The assay method of content of niobium in rare earth alloy - Google Patents
The assay method of content of niobium in rare earth alloy Download PDFInfo
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- CN106290314A CN106290314A CN201610627243.7A CN201610627243A CN106290314A CN 106290314 A CN106290314 A CN 106290314A CN 201610627243 A CN201610627243 A CN 201610627243A CN 106290314 A CN106290314 A CN 106290314A
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Abstract
The invention discloses the assay method of content of niobium in a kind of rare earth alloy, including: rare earth alloy sample nitric acid, Fluohydric acid. low-temperature heat are dissolved, and add perchloric acid smoked, add nitric acid, Fluohydric acid. heating for dissolving, obtain test solution with water constant volume after cooling after taking off cooling；With content of niobium in inductance coupled plasma optical emission spectrophotometer test solution.The present invention utilizes inductively-coupled plasma spectrometer directly to measure niobium amount in rare earth alloy, and inspection range is wider, analyzes method simple and fast, and agents useful for same is less, analyzes speed fast, and precision is good.
Description
Technical field
The present invention relates to a kind of metallurgical analysis technology, specifically, relate to the assay method of content of niobium in a kind of rare earth alloy.
Background technology
In prior art, with the content of niobium in xylenol orange spectrphotometric method for measuring steel alloy.The method is be applicable to steel alloy
The mensuration of the content of niobium of mass fraction 0.01%～1.60%.Sample mixed-acid dissolution is also evaporated to dryness with perchloric acid smoked,
Prevent with Fluohydric acid. the hydrolysis of niobium, the fluorion of excess from eliminating the effects of the act with aluminum sulfate complexation in hydrochloric acid medium, add Vitamin C
Acid reduction ferric iron is to eliminate interference.In the hydrochloric acid medium of 0.17～0.19mol/L, niobium generates salmon pink network with xylenol orange
Compound, measures absorbance at wavelength 520nm, calculates the mass fraction of niobium.
But, in rare earth alloy, the analysis detection of content of niobium there are no national standard method, rower and enterprise's mark method.
Summary of the invention
Technical problem solved by the invention is to provide the assay method of content of niobium in a kind of rare earth alloy, utilizes inductance coupling
Closing plasma spectrometer and directly measure niobium amount in rare earth alloy, inspection range is wider, analyzes method simple and fast, agents useful for same
Less, analyze speed fast, precision is good.
Technical scheme is as follows:
The assay method of content of niobium in a kind of rare earth alloy, including:
Rare earth alloy sample nitric acid, Fluohydric acid. low-temperature heat are dissolved, and add perchloric acid smoked, add nitre after taking off cooling
Acid, Fluohydric acid. heating for dissolving, obtain test solution with water constant volume after cooling；
With content of niobium in inductance coupled plasma optical emission spectrophotometer test solution.
Further: to claim 0.2～0.5g rare earth alloy sample, be accurate to 0.0001g, in polytetrafluoroethylene beaker, add
10～15mL, ρ 1.42 nitric acid and 5mL, ρ 1.13 Fluohydric acid., low-temperature heat is dissolved, and adds 5mL, ρ 1.68 perchloric acid smoked, after cooling
Add 5mL nitric acid, 2mL Fluohydric acid. heating for dissolving, after cooling after be transferred in 100mL plastics volumetric flask, with pure water be diluted to carve
Degree, obtains test solution after shaking up.
Further: on inductively-coupled plasma spectrometer, selected Instrument working parameter, with the atomization of hydrofluoric acid resistant
Device and quarter bend system, select the optimized analysis spectral line 269.706nm of niobium, measure niobium working curve standard solution and test solution simultaneously
The spectral intensity of niobium, draws content of niobium.
Further: to obtain according to the niobium working curve that content and the corresponding light spectral intensity of the niobium of niobium working curve standard solution are done
Go out the content of niobium in tested test solution.
Further: to measure working curve standard solution 5 point of niobium, obtain 5 corresponding spectral intensities of known content of niobium, and
Make niobium working curve；Measure the corresponding light spectral intensity obtaining niobium in test solution again, then draw rare earth further according to niobium working curve
The content of niobium in alloy sample.
Further: the preparation of niobium working curve standard solution includes, when content of niobium≤0.005% in rare earth alloy sample
Time, claim the 0.5000g 5 parts of the same kind rare earth alloy sample without niobium, shift respectively after sample dissolution cooling and mould in 5 100mL
0%, 0.0020% for bottoming in material volumetric flask, it is separately added into 10.0 μ g/mL niobium standard solution and is configured to content of niobium and be:,
0.004%, the niobium working curve standard solution of 0.0080%, 0.010%5 point, the addition of niobium amount be respectively as follows: 0mL,
1.00mL、2.00mL、4.00mL、5.00mL；As content of niobium ＞ 0.005%, the 0.2000g same kind rare earth without niobium is claimed to close
5 parts of sample of gold, shifting respectively after the cooling of rare earth alloy sample dissolution in 5 100mL plastics volumetric flasks is bottoming, is separately added into
20.0 μ g/mL niobium standard solution are configured to content of niobium and are: 0%, 0.010%, 0.100%, 0.500%, and 0.500% this point is used
100.0 μ g/mL niobium standard solution preparation, be configured to the niobium working curve standard solution of 5 points, the addition of niobium amount be respectively 0mL,
1.00mL、5.00mL、10.00mL、10.00mL。
Further: also to include the step that preci-sion and accuracy is tested.
Compared with prior art, the technology of the present invention effect includes: after the present invention uses acid dissolved samples, utilize inductive
Plasma spectrometer directly measures niobium amount in rare earth alloy, inspection range wider (0.001～0.500%), analyzes method letter
Single quick, agents useful for same is less, analyzes speed fast, and precision is good, and accuracy is high, meets the demand of research and production.
(1) used by, chemical reagent is less, cost efficiency.
Rare earth alloy sample nitric acid, Fluohydric acid. low-temperature heat are dissolved, and add perchloric acid smoked and do near, take off the coldest, add
Enter nitric acid, Fluohydric acid. heating for dissolving, with water constant volume after cooling.
(2) easy and simple to handle quickly.
Launching on (ICP-AES) spectrogrph at inductively coupled plasma, machine of can directly going up after sample dissolution constant volume measures.
(3) inspection range more a width of 0.0010～0.500%, analyzes method simple and fast, and agents useful for same is less, precision
Good, accuracy is high, meets the demand of research and production, great application value.
Detailed description of the invention
Below with reference to preferred embodiment, technical solution of the present invention is elaborated.
1, analyrical reagent, standard solution, instrument are prepared.
Nitric acid (ρ 1.42, top grade is pure)；Fluohydric acid. (ρ 1.13, top grade is pure)；Perchloric acid (ρ 1.68, top grade is pure).
Niobium standard solution: with the niobium standard solution of 1000 μ g/mL (ferrous materials test center of country Iron and Steel Research Geueral Inst),
Dilution is configured to 100.0 μ g/mL, 20.0 μ g/mL, the niobium standard solution of 10.0 μ g/mL.
Experimental water is two grades of pure water.
Key instrument and test condition:
PE company of the U.S. produces, Optima5300DV inductively-coupled plasma spectrometer.
Instrument parameter: see running parameter table 1
Table 1 running parameter
| Parameter | Higher frequency | Power | Plasma gas flow rate | Secondary air amount | Carrier gas flux | Solution elevating amount |
| Numerical value | 40.68MHZ | 1300W | 15L/min | 0.2L/min | 0.8L/min | 1.5mL/min |
| Parameter | Washing time | Prespark period | The time of integration | Reading time delay | Observed altitude | Observed pattern |
| Numerical value | 8s | 45s | 2～10s is automatic | 30s | 15mm | Axially |
The analysis of line wavelength of niobium element uses 269.706nm.
2, the assay method of content of niobium in rare earth alloy.
The assay method of content of niobium in rare earth alloy, comprises the following steps:
Step 1: rare earth alloy sample nitric acid, Fluohydric acid. low-temperature heat are dissolved, adds perchloric acid smoked and does near, take off slightly
Cold, add nitric acid, Fluohydric acid. heating for dissolving, after cooling, obtain test solution with water constant volume.
Claim 0.2～0.5g rare earth alloy sample, be accurate to 0.0001g, in polytetrafluoroethylene beaker, add 10～
15mL, ρ 1.42 nitric acid, 5mL, ρ 1.13 Fluohydric acid., low-temperature heat dissolves, add 5mL, ρ 1.68 perchloric acid smoked near dry, take off
The coldest, add 5mL nitric acid, 2mL Fluohydric acid. heating for dissolving, take off the coldest after be transferred in 100mL plastics volumetric flask, dilute with pure water
Release to scale, shake up and (do blank assay in company with sample.
In the case of blank assay is not added with sample exactly, the examination being analyzed by analysis operating condition and the step of sample
Testing, acquired results is blank value.Its effect is exactly to eliminate the niobium amount introduced due to factors such as reagent, pure water and vessel.Sample
The measured value of solution deducts the actual value that blank value is sample.
Step 2: with content of niobium in inductance coupled plasma optical emission (ICP-AES) spectrophotometer test solution.
On inductively-coupled plasma spectrometer, under selected Instrument working parameter (being shown in Table 1), with the mist of hydrofluoric acid resistant
Change device and quarter bend system, select the optimized analysis spectral line 269.706nm of niobium, to niobium working curve standard solution and test solution (test solution
Being exactly sample solution, test solution with the relation of niobium working curve standard solution is: according to the niobium of niobium working curve standard solution
The working curve that does of content and corresponding light spectral intensity can calculate the content of niobium in tested test solution) measure the spectrum of niobium simultaneously
Intensity, computer automatic returning calculates analysis result.
Upper machine measures working curve standard solution 5 point of niobium, can obtain 5 corresponding spectral intensities of known content of niobium,
And make niobium working curve.Measure test solution the most again, the corresponding spectrum of niobium in sample (rare earth alloy sample) can be obtained
Intensity, then the working curve further according to niobium just can calculate the content of niobium in sample.
Performance characteristics according to different inductively-coupled plasma spectrometers, it is also possible to select other glitch-free niobiums to divide
Analysis line is analyzed.
The preparation of niobium working curve standard solution: when content of niobium≤0.005% in rare earth alloy sample, claims 0.5000g
Without 5 parts of the same kind rare earth alloy sample of niobium, shift respectively after carrying out sample dissolution cooling by step 1 in 5 100mL plastics
0%, 0.0020% for bottoming in volumetric flask, it is separately added into 10.0 μ g/mL niobium standard solution and is configured to content of niobium and be:,
0.004%, the niobium working curve standard solution of 0.0080%, 0.010%5 point, the addition of niobium amount be respectively as follows: 0mL,
1.00mL、2.00mL、4.00mL、5.00mL；As content of niobium ＞ 0.005%, the 0.2000g same kind rare earth without niobium is claimed to close
5 parts of sample of gold, by step 1, shifting respectively after the cooling of rare earth alloy sample dissolution in 5 100mL plastics volumetric flasks is bottoming,
It is separately added into 20.0 μ g/mL niobium standard solution and is configured to content of niobium and be: 0%, 0.010%, 0.100%, 0.500%, 0.500%
This point, with 100.0 μ g/mL niobium standard solution preparations, is configured to the niobium working curve standard solution of 5 points, and the addition of niobium amount divides
Wei 0mL, 1.00mL, 5.00mL, 10.00mL, 10.00mL.
Step 3: preci-sion and accuracy is tested.
To rare earth alloy sample, empirically method carries out the test of precision, accuracy.Analysis result is shown in Table 2.
Table 2 precision, accuracy test
| Title and numbering | Measure average (11 times)/% | Add niobium mark liquid value/% | RSD/% (n=11) | The response rate/% |
| Rare earth alloy 1# | 0.235 | 0.05 | 2.46 | 98.9 |
| Rare earth alloy 2# | 0.036 | 0.01 | 1.91 | 100.3 |
| Rare earth alloy 2# | 0.036 | 0.40 | 3.72 | 101.2 |
As can be seen from Table 2, the inventive method has higher precision and preferable accuracy, can meet production and scientific research
Needs, great application value.
Claims (7)
1. an assay method for content of niobium in rare earth alloy, including:
Rare earth alloy sample nitric acid, Fluohydric acid. low-temperature heat are dissolved, and add perchloric acid smoked, add nitric acid, hydrogen after taking off cooling
Fluoric acid heating for dissolving, obtains test solution with water constant volume after cooling；
With content of niobium in inductance coupled plasma optical emission spectrophotometer test solution.
2. the assay method of content of niobium in rare earth alloy as claimed in claim 1, it is characterised in that: claim 0.2～0.5g rare earth to close
Gold sample, is accurate to 0.0001g, in polytetrafluoroethylene beaker, adds 10～15mL, ρ 1.42 nitric acid and 5mL, ρ 1.13 hydrogen fluorine
Acid, low-temperature heat is dissolved, and adds 5mL, ρ 1.68 perchloric acid smoked, adds 5mL nitric acid, 2mL Fluohydric acid. heating for dissolving after cooling, cold
But it is transferred in 100mL plastics volumetric flask after after, is diluted to scale with pure water, after shaking up, obtains test solution.
3. the assay method of content of niobium in rare earth alloy as claimed in claim 1, it is characterised in that: at inductively coupled plasma
On spectrogrph, selected Instrument working parameter, by nebulizer and the quarter bend system of hydrofluoric acid resistant, select the optimized analysis spectral line of niobium
269.706nm, measures the spectral intensity of niobium simultaneously, draws content of niobium niobium working curve standard solution and test solution.
4. the assay method of content of niobium in rare earth alloy as claimed in claim 3, it is characterised in that: according to niobium working curve standard
The niobium working curve that the content of the niobium of solution and corresponding light spectral intensity are done draws the content of niobium in tested test solution.
5. the assay method of content of niobium in rare earth alloy as claimed in claim 3, it is characterised in that: measure the working curve mark of niobium
Quasi-solution 5 point, obtains 5 corresponding spectral intensities of known content of niobium, and makes niobium working curve；Measure again and obtain niobium in test solution
Corresponding light spectral intensity, then draw the content of niobium in rare earth alloy sample further according to niobium working curve.
6. the assay method of content of niobium in rare earth alloy as described in any one of claim 3 to 5, it is characterised in that: niobium work song
The preparation of line standard solution includes, when content of niobium≤0.005% in rare earth alloy sample, claims the 0.5000g same product without niobium
Planting 5 parts of rare earth alloy sample, shifting respectively after sample dissolution cooling in 5 100mL plastics volumetric flasks is bottoming, is separately added into
10.0 μ g/mL niobium standard solution are configured to content of niobium and are: 0%, 0.0020%, 0.004%, 0.0080%, 0.010%5 point
Niobium working curve standard solution, the addition of niobium amount is respectively as follows: 0mL, 1.00mL, 2.00mL, 4.00mL, 5.00mL；When niobium contains
During amount ＞ 0.005%, claim the 0.2000g 5 parts of the same kind rare earth alloy sample without niobium, divide after the cooling of rare earth alloy sample dissolution
Do not shift in 5 100mL plastics volumetric flasks as bottoming, be separately added into 20.0 μ g/mL niobium standard solution and be configured to content of niobium and be:
0%, 0.010%, 0.100%, 0.500%, 0.500% this point, with 100.0 μ g/mL niobium standard solution preparations, is configured to 5
The niobium working curve standard solution of point, the addition of niobium amount is respectively 0mL, 1.00mL, 5.00mL, 10.00mL, 10.00mL.
7. the assay method of content of niobium in rare earth alloy as described in any one of Claims 1-4, it is characterised in that: also include essence
Density and the step of accuracy experiment.
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Cited By (4)
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| CN108760722A (en) * | 2018-03-26 | 2018-11-06 | 包头钢铁（集团）有限责任公司 | The method for measuring the content of La, Ce, Pr, Nd and Sm |
| CN113029730A (en) * | 2021-02-26 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Mixed acid solution for dissolving copper-phosphorus alloy sample and preparation method and application thereof |
| CN115078057A (en) * | 2022-06-16 | 2022-09-20 | 中航金属材料理化检测科技有限公司 | Determination of Ti based on ICP-AES method 2 Method for content of niobium and copper in AlNb |
| CN117030635A (en) * | 2023-10-09 | 2023-11-10 | 自贡市凤祥化工有限公司 | Quality analysis method of aluminum sulfate based on multi-index measurement |
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| CN115078057A (en) * | 2022-06-16 | 2022-09-20 | 中航金属材料理化检测科技有限公司 | Determination of Ti based on ICP-AES method 2 Method for content of niobium and copper in AlNb |
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| CN117030635A (en) * | 2023-10-09 | 2023-11-10 | 自贡市凤祥化工有限公司 | Quality analysis method of aluminum sulfate based on multi-index measurement |
| CN117030635B (en) * | 2023-10-09 | 2023-12-15 | 自贡市凤祥化工有限公司 | Quality analysis method of aluminum sulfate based on multi-index measurement |
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Application publication date: 20170104 |