CN103454175B - Method for determining niobium content in aeronautical material Ti45Nb titanium alloy - Google Patents
Method for determining niobium content in aeronautical material Ti45Nb titanium alloy Download PDFInfo
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Abstract
The invention discloses a method for determining niobium content in aeronautical material Ti45Nb titanium alloy. The method comprises the following steps: dissolving an insoluble specimen with mixed acid of hydrochloric acid, nitric acid and hydrofluoric acid; generating stable clathrate from titanium and aluminium ions by the hydrofluoric acid in a hydrofluoric acid medium; completely generating sediments from niobium and tetraphenylarsonium chloride hydrochloride; generating soluble sediments from trace magnesium ions; preventing a hydrated oxide sediment from being separated out by high-priced metal ions by using tartaric acid; washing and dissolving magnesium sediments after filtering; finally baking, ashing and burning the sediments into niobium pentoxide; weighing and calculating the niobium content in the alloy. By adopting the method disclosed by the invention, the alloy material of which the mass fraction of niobium is 40.0-50.0% can be determined; the method has the advantages of being simple and convenient to operate, high in accuracy, small in error, good in stability and the like.
Description
Technical field
The invention belongs to chemical analysis field, be specifically related to a kind of method of tetraphenylarsonium chloride hydrochloride gravimetric determination aeronautical material Ti45Nb Nb in Ti Alloys content.
Background technology
In existing mensuration alloy, content of niobium adopts standard GB/T 223.5 " steel and alloy chemical analysis method: ionic energy transfer-gravimetric determination content of niobium method, be by containing the hydrofluorite-hydrochloric acid sample solution of niobium by strong alkalinity anion exchange column time, other metallic elements such as niobium and iron, nickel etc. are separated, add after boric acid shelters fluorine in niobium leacheate, at hydrochloric acid medium with cupferron quantitative deposition niobium, become niobium pentaoxide through calcination, weigh, calculate the massfraction of niobium.But there is following point in the method: 1, the method is only suitable for the mensuration of niobium amount in alloy steel, high temperature alloy, Precise Alloy; 2, ion-exchange step is loaded down with trivial details, and practicality is not very strong; 3, be difficult to shelter separation to high-load titanium.
Separately have GB GB/T4698.22 " titanium sponge, titanium or titanium alloy chemical analysis method 5-Br-PADAP spectrophotometry niobium amount " in addition, but the method measures the scope of the massfraction of niobium only 0.20% ~ 3.00%, cannot to the mensuration of high-load niobium.
Summary of the invention
The technical problem to be solved in the present invention is that to measure the measurement range that content of niobium in alloy exists in prior art narrow, the problems such as complex operation, the invention provides a kind of method of tetraphenylarsonium chloride hydrochloride gravimetric determination aeronautical material Ti45m Nb in Ti Alloys content, having the massfraction that can measure niobium amount is the alloy material of 40.0% ~ 50.0%, easy and simple to handle, accuracy is high, error is little and the stable advantage such as good.
The technical solution used in the present invention: the method measuring aeronautical material Ti45Nb Nb in Ti Alloys content, comprises the following steps:
(1) take sample 0.1000g, put into the polytetrafluoroethylplastic plastic cup of 200mL, add hydrochloric acid that 30mL density is 1.19g/mL and 5mL density is the nitric acid of 1.42g/mL, low temp. electric hot plate heats 10min;
(2) hydrofluorite that 15mL ~ 20mL density is 1.15g/mL is added; after dissolving; add the hydrofluorite of 40mL ~ 45mL equal densities and the tartaric acid solution of 15mL200g/L again; 20min is incubated in boiling water bath; rare to 120mL with water; under constantly stirring, add 25mL20g/L tetraphenylarsonium chloride hydrochloride solution, be placed in hot bath at 70 DEG C ~ 80 DEG C insulation 30min;
(3) add a little paper pulp with quantitative filter paper to filter on plastic funnel; 18 ~ 20 times are fully washed with cleansing solution; wherein cleansing solution is add 10mL20g/L tetraphenylarsonium chloride hydrochloride solution in 1000mL dilute hydrofluoric acid solution (1+4) ~ (1+3), mixing;
(4) filter paper and sediment are placed in platinum crucible, on electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper moves in the porcelain crucible of constant weight, after ashing, at 900 DEG C of calcination 30min in high temperature furnace after sallow, take out cooling, put into exsiccator and be cooled to room temperature, weigh, calculate the massfraction of niobium.
Wherein, the massfraction of aeronautical material Ti45Nb Nb in Ti Alloys amount is 40.0% ~ 50.0%.
Calculate the massfraction formula of niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m, wherein m
1the quality of-precipitation and porcelain crucible, m
2-crucible quality, m-samples quality, and 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
The beneficial effect that the present invention reaches: the method for the present invention's tetraphenylarsonium chloride hydrochloride gravimetric determination Ti45Nb Nb in Ti Alloys amount, its principle is: indissoluble test portion hydrochloric acid, nitric acid, hydrofluorite mixed-acid dissolution, in the hydrofluoric medium of 9mol/L ~ 12mol/L, titanium, aluminium ion are generated stable complex compound by hydrofluorite, niobium and tetraphenylarsonium chloride hydrochloride generate precipitation completely, and trace magnesium ion generates solubility precipitation.Prevent high volence metal ion from separating out hydrous oxid precipitation with tartrate, after filtration, magnesium precipitate is washed dissolving.Precipitation oven dry, ashing, calcination become niobium pentaoxide, weighs, calculate.Overcome in standard " titanium sponge, titanium or titanium alloy chemical analysis method (GB/T4698.22) " defect Ti45Nb titanium alloy test portion can not dissolved and high-load niobium can not be measured, for production control, scientific research provide the compositional data of chemical element accurately, the direction that directs study, guarantee aeronautical product quality.The present invention can measure the content of niobium of 40.00% ~ 50.00% (m/m) in Ti45Nb titanium alloy, and metrical error is ± 0.15%.
Embodiment
Embodiment 1
Take sample 0.1095g (m=0.1095g), put into the polytetrafluoroethylplastic plastic cup of 200mL, add 30mL hydrochloric acid (ρ is 1.19g/mL) and 5mL nitric acid (ρ is 1.42g/mL), after low temp. electric hot plate heats 10min, after adding 15mL hydrofluorite (ρ is 1.15g/mL) continuation dissolving, add 45mL hydrofluorite (ρ is 1.15g/mL) and 15mL tartaric acid solution (200g/L), 20min is incubated in boiling water bath, rare to about 120mL with water, under constantly stirring, add 25mL tetraphenylarsonium chloride hydrochloride solution (20g/L), be placed in hot bath at 70 DEG C ~ 80 DEG C scope insulation 30min.Add a little paper pulp with quantitative filter paper (middling speed) to filter on plastic funnel, [in 1000mL dilute hydrofluoric acid solution (1+4), add 10mL tetraphenylarsonium chloride hydrochloride solution (20g/L), mixing with cleansing solution.], fully washing 18 times.Filter paper and sediment are placed in platinum crucible, on the electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper and move to (porcelain crucible m in the porcelain crucible of constant weight after sallow
2=23.5054), after ashing, at 900 DEG C of calcination 30min in high temperature furnace.Take out cooling, put into exsiccator and be cooled to room temperature, weigh, m
1=23.5768.And repeatedly calcination to constant weight.Massfraction by following formulae discovery niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m.[in formula: m
1the quality (g) of-precipitation and porcelain crucible; m
2-porcelain crucible quality (g); M-samples quality (g); 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
ω(Nb)%=[(23.5768-23.5054)×0.6990]×100/0.1095
ω(Nb)%=45.58%。
Embodiment 2
Take sample 0.1051g (m=O.1051g), put into the polytetrafluoroethylplastic plastic cup of 200mL, add 30mL hydrochloric acid (ρ is 1.1gg/mL) and 5mL nitric acid (ρ is 1.42g/mL), after low temp. electric hot plate heats 10min, after adding 20mL hydrofluorite (ρ is 1.15g/mL) continuation dissolving, add 40mL hydrofluorite (ρ is 1.15g/mL) and 15mL tartaric acid solution (200g/L), 20min is incubated in boiling water bath, rare to about 120mL with water, under constantly stirring, add 25mL tetraphenylarsonium chloride hydrochloride solution (20g/L), be placed in hot bath at 70 DEG C ~ 80 DEG C scope insulation 30min.Add a little paper pulp with quantitative filter paper (middling speed) to filter on plastic funnel, [in 1000mL dilute hydrofluoric acid solution (1+3), add 10mL tetraphenylarsonium chloride hydrochloride solution (20g/L), mixing with cleansing solution.], fully washing 20 times.Filter paper and sediment are placed in platinum crucible, on the electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper and move to (porcelain crucible m in the porcelain crucible of constant weight after sallow
2=23.6915), after ashing, at 900 DEG C of calcination 30min in high temperature furnace.Take out cooling, put into exsiccator and be cooled to room temperature, weigh, m
1=237545.And repeatedly calcination to constant weight.Massfraction by following formulae discovery niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m.[in formula: m
1the quality (g) of-precipitation and porcelain crucible; m
2-porcelain crucible quality (g); M-samples quality (g); 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
ω(Nb)%=[(23.7545-23.6915)×0.6990]×100/0.1051
ω(Nb)%=41.90%。
Embodiment 3
Take sample 0.1092g (m=0.1092g), put into the polytetrafluoroethylplastic plastic cup of 200mL, add 30mL hydrochloric acid (ρ is 1.19g/mL) and 5mL nitric acid (ρ is 1.42g/mL), after low temp. electric hot plate heats 10min, after adding 15mL hydrofluorite (ρ is 1.15g/mL) continuation dissolving, add 45mL hydrofluorite (ρ is 1.15g/mL) and 15mL tartaric acid solution (200g/L), 20min is incubated in boiling water bath, rare to about 120mL with water, under constantly stirring, add 25mL tetraphenylarsonium chloride hydrochloride solution (20g/L), be placed in hot bath at 70 DEG C ~ 80 DEG C scope insulation 30min.Add a little paper pulp with quantitative filter paper (middling speed) to filter on plastic funnel, [in 1000mL dilute hydrofluoric acid solution (1+4), add 10mL tetraphenylarsonium chloride hydrochloride solution (20g/L), mixing with cleansing solution.], fully washing 18 times.Filter paper and sediment are placed in platinum crucible, on the electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper and move to (porcelain crucible m in the porcelain crucible of constant weight after sallow
2=23.3537), after ashing, at 900 DEG C of calcination 30min in high temperature furnace.Take out cooling, put into exsiccator and be cooled to room temperature, weigh, m
1=23.4202.And repeatedly calcination to constant weight.Massfraction by following formulae discovery niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m.[in formula: m
1the quality (g) of-precipitation and porcelain crucible; m
2-porcelain crucible quality (g); M-samples quality (g); 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
ω(Nb)%=[(23.4202-23.3537)×0.6990]×100/0.1092
ω(Nb)%=42.57%。
Embodiment 4
Take sample 0.10499 (m=0.1049g), put into the polytetrafluoroethylplastic plastic cup of 200mL, add 3OmL hydrochloric acid (ρ is 1.19g/mL) and 5mL nitric acid (ρ is 1.42g/mL), after low temp. electric hot plate heats 10min, after adding 20mL hydrofluorite (ρ is 1.15g/mL) continuation dissolving, add 40mL hydrofluorite (ρ is 1.15g/mL) and 15mL tartaric acid solution (200g/L), 20min is incubated in boiling water bath, rare to about 120mL with water, under constantly stirring, add 25mL tetraphenylarsonium chloride hydrochloride solution (20g/L), be placed in hot bath at 70 DEG C ~ 80 DEG C scope insulation 30min.Add a little paper pulp with quantitative filter paper (middling speed) to filter on plastic funnel, [in 1000mL dilute hydrofluoric acid solution (1+3), add 10mL tetraphenylarsonium chloride hydrochloride solution (20g/L), mixing with cleansing solution.], fully washing 20 times.Filter paper and sediment are placed in platinum crucible, on the electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper and move to (porcelain crucible m in the porcelain crucible of constant weight after sallow
2=24.0120), after ashing, at 900 DEG C of calcination 30min in high temperature furnace.Take out cooling, put into exsiccator and be cooled to room temperature, weigh, m
1=24.0780.And repeatedly calcination to constant weight.Massfraction by following formulae discovery niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m.[in formula: m
1the quality (g) of-precipitation and porcelain crucible; m
2-porcelain crucible quality (g); M-samples quality (g); 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
ω(Nb)%=[(24.0780-24.0120)×0.6990]×100/0.1049
ω(Nb)%=43.98%。
Embodiment 5
Take sample 0.1018g (m=0.1018g), put into the polytetrafluoroethylplastic plastic cup of 200mL, add 30mL hydrochloric acid (ρ is 1.19g/mL) and 5mL nitric acid (ρ is 1.42g/mL), after low temp. electric hot plate heats 10min, after adding 15mL hydrofluorite (ρ is 1.15g/mL) continuation dissolving, add 45mL hydrofluorite (ρ is 1.15g/mL) and 15mL tartaric acid solution (200g/L), 20min is incubated in boiling water bath, rare to about 120mL with water, under constantly stirring, add 25mL tetraphenylarsonium chloride hydrochloride solution (20g/L), be placed in hot bath at 70 DEG C ~ 80 DEG C scope insulation 30min.Add a little paper pulp with quantitative filter paper (middling speed) to filter on plastic funnel, [in 1000mL dilute hydrofluoric acid solution (1+4), add 10mL tetraphenylarsonium chloride hydrochloride solution (20g/L), mixing with cleansing solution.], fully washing 18 times.Filter paper and sediment are placed in platinum crucible, on the electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper and move to (porcelain crucible m in the porcelain crucible of constant weight after sallow
2=23.8557), after ashing, at 900 DEG C of calcination 30min in high temperature furnace.Take out cooling, put into exsiccator and be cooled to room temperature, weigh, m
1=30.5478.And repeatedly calcination to constant weight.Massfraction by following formulae discovery niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m.[in formula: m
1the quality (g) of-precipitation and porcelain crucible; m
2-porcelain crucible quality (g); M-samples quality (g); 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
ω(Nb)%=[(23.9286-23.8557)×0.6990]×100/0.1018
ω(Nb)%=50.06%。Test findings and definite value error are 0.15% to the maximum.
Claims (3)
1. measure a method for aeronautical material Ti45Nb Nb in Ti Alloys content, it is characterized in that: comprise the following steps:
(1) take sample 0.1000g, put into the polytetrafluoroethylplastic plastic cup of 200mL, add hydrochloric acid that 30mL density is 1.19g/mL and 5mL density is the nitric acid of 1.42g/mL, low temp. electric hot plate heats 10min;
(2) hydrofluorite that 15mL ~ 20mL density is 1.15g/mL is added, after dissolving, add the hydrofluorite of 40mL ~ 45mL equal densities and the tartaric acid solution of 15mL 200g/L again, 20min is incubated in boiling water bath, rare to 120mL with water, under constantly stirring, add 25mL 20g/L tetraphenylarsonium chloride hydrochloride solution, be placed in hot bath at 70 DEG C ~ 80 DEG C insulation 30min;
(3) add a little paper pulp with quantitative filter paper to filter on plastic funnel, 18 ~ 20 times are fully washed with cleansing solution, wherein cleansing solution is the dilutability of 1000mL is add 10mL 20g/L tetraphenylarsonium chloride hydrochloride solution in the dilute hydrofluoric acid solution of 1+4 to 1+3, mixing;
(4) filter paper and sediment are placed in platinum crucible, on electric furnace in vent cabinet after low-temperature bake, folded filter paper, continue to dry filter paper moves in the porcelain crucible of constant weight, after ashing, at 900 DEG C of calcination 30min in high temperature furnace after sallow, take out cooling, put into exsiccator and be cooled to room temperature, weigh, calculate the massfraction of content of niobium.
2. a kind of method measuring aeronautical material Ti45Nb Nb in Ti Alloys content according to claim 1, is characterized in that: the massfraction of aeronautical material Ti45Nb Nb in Ti Alloys amount is 40.0% ~ 50.0%.
3. a kind of method measuring aeronautical material Ti45Nb Nb in Ti Alloys content according to claim 1, is characterized in that: the massfraction formula calculating niobium: ω (Nb) %=[(m
1-m
2) × 0.6990] × 100/m, wherein m
1the quality of-precipitation and porcelain crucible, m
2-crucible quality, m-sample quality, 0.6990-niobium pentaoxide is converted into the coefficient of niobium.
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| CN104020157B (en) * | 2014-06-12 | 2017-01-11 | 航天精工股份有限公司 | Method for measuring elemental niobium content of titanium-niobium alloy |
| CN105467061A (en) * | 2014-09-12 | 2016-04-06 | 贵州航天精工制造有限公司 | Method for determining niobium content in Ti45Nb titanium alloy by using tetraphenylarsonium chloride hydrochloride weight method |
| CN106226192A (en) * | 2016-08-29 | 2016-12-14 | 成都飞机工业（集团）有限责任公司 | A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy |
| CN110231247A (en) * | 2019-07-16 | 2019-09-13 | 内蒙古路易精普检测科技有限公司 | The measuring method of total sulfate in water and waste water |
| CN113063743A (en) * | 2021-03-03 | 2021-07-02 | 中航金属材料理化检测科技有限公司 | Method for measuring trace magnesium content in tungsten-containing high-temperature alloy material |
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