CN107192590A - Method for measuring oxygen, nitrogen and hydrogen content in titanium alloy - Google Patents
Method for measuring oxygen, nitrogen and hydrogen content in titanium alloy Download PDFInfo
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- CN107192590A CN107192590A CN201710485592.4A CN201710485592A CN107192590A CN 107192590 A CN107192590 A CN 107192590A CN 201710485592 A CN201710485592 A CN 201710485592A CN 107192590 A CN107192590 A CN 107192590A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 61
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000001257 hydrogen Substances 0.000 title claims abstract description 48
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 48
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000001301 oxygen Substances 0.000 title claims abstract description 32
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 116
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 57
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 19
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 238000007872 degassing Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002775 capsule Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000021110 pickles Nutrition 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229950005499 carbon tetrachloride Drugs 0.000 claims description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 10
- 238000002844 melting Methods 0.000 abstract description 8
- 230000008018 melting Effects 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 241001062009 Indigofera Species 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- -1 silk Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910001275 Niobium-titanium Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- HZUJFPFEXQTAEL-UHFFFAOYSA-N azanylidynenickel Chemical compound [N].[Ni] HZUJFPFEXQTAEL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for measuring oxygen, nitrogen and hydrogen contents in titanium alloy, which comprises the following steps: (1) cutting and polishing the high-purity electrolytic nickel plate to prepare a nickel granule fluxing agent; (2) putting the nickel particle fluxing agent into an inner high-purity graphite crucible of a lower electrode of an oxygen-nitrogen-hydrogen analyzer, and degassing under high power; (3) selecting a measuring condition, and measuring oxygen, nitrogen and hydrogen gas in the titanium alloy by adopting an oxygen, nitrogen and hydrogen analyzer; (4) and calculating the oxygen nitrogen hydrogen mass percentage content in the sample. According to the method, a self-made nickel particle fluxing agent with a high blank value can be used for replacing commercially available fluxing agents such as nickel baskets and nickel scraps, the oxygen, nitrogen and hydrogen content in the titanium alloy is determined by adopting a pulse melting method, the interference of the blank value can be remarkably reduced or eliminated by changing normal testing steps and analysis conditions, the same effect as that of the commercially available fluxing agent is achieved, the detection cost is greatly reduced, the method has the advantages of simplicity, high accuracy and the like, and the requirement of rapid detection is met.
Description
Technical field
It is more particularly to a kind of to determine Oxygen in Titanium Alloy nitrogen hydrogen content the present invention relates to a kind of titanium alloy material analysis field
Method.
Background technology
Titanium alloy has the advantages that lightweight, high specific strength, wear-resisting, flame resistant, anti-oxidant, and room temperature and high-temperature mechanics
Can be excellent, it has also become study one of most popular high-temperature structural material in the world, can be used as space shuttle engine and organism material
And the material such as automobile valve rocker, and there is good application prospect in fields such as biomedicine, auto industrys.Because of oxygen, nitrogen, hydrogen
Three kinds of elemental gas are larger in titanium alloy solubility, it has also become essential items for inspection.Write in Li great Cheng etc.《Titanium smelting process》One
In book, Oxygen in Titanium Alloy, nitrogen, carbon and the main nonmetallic inclusion performance of hydrogen are described in detail.Oxygen and nitrogen have significantly to titanium alloy
Strengthen effect, but decline its plasticity；Excessive hydrogen is dissolved in titanium alloy can produce hydride, and hydrogen content rises, also can shape
Into brittle layer, alloy is set to become fragile.As can be seen here, oxygen, nitrogen and hydrogen have significant impact to the performance of titanium alloy, accurate quick inspection
Survey Oxygen in Titanium Alloy, nitrogen and hydrogen are checked on all significant to quality of production control and product quality.
Titanium alloy is high due to its fusing point, when carrying out gas content analysis, gas therein is sufficiently released
Put, as material analysis personnel's Research Challenges.Existing GB/T 4698.7-2011 and GB/T the 4698.15-2011 sponges in the country
Titanium, titanium or titanium alloy chemical analysis method oxygen amount, nitrogen quantity, the measure of hydrogen amount；King is wide to wait inert gas fusion-infrared absorption determining titanium
Oxygen in molybdenum alloy；The inert gas fusions such as the new layer of stone-infrared thermal conductivity method determines oxygen and nitrogen, etc. analysis method in niobium titanium alloy simultaneously.
In these methods, due to pulse stove power limited, for high-melting-point titanium alloy sample, direct PULSE HEATING, it is impossible to fully molten
Solution, gas can not discharge completely, and analysis result is relatively low or without result.Therefore all selection adds the nickel basket of certain mass, nickel bits, nickel
The fluxing agents such as silk, nickel capsule and sample are mixed together melting, to reduce high temperature compound boiling point, so that gas is fully released in sample
Put, and then Accurate Determining.In the market has the special fluxing agent sale of the nickel such as nickel indigo plant, nickel bits, nickel capsule, its oxygen, nitrogen, hydrogen component content one
As require be less than 0.0010%, its smelt and manufacturing procedure it is cumbersome, cost is higher, causes procurement price also very high.High-purity electrolysis
Nickel plate has obvious price advantage relative to the fluxing agent such as nickel on the market indigo plant, nickel bits, nickel capsule.High-purity sheet nickel table
Face is coarse, there is oxide layer, through processing after, be prepared into Nickel particle.But oxygen, nitrogen, hydrogen composition contain in high-purity sheet nickel
Amount is higher than commercially available nickel fluxing agent, that is, the blank value tested is higher.If instrument test step routinely：First by interior graphite earthenware
Crucible first deaerates, and nickel fluxing agent and sample are then thrown into sample simultaneously, then is analyzed with PULSE HEATING melting, then measurement result is nickel
The summation of fluxing agent and gas content in sample.It must deduct the blank value of nickel fluxing agent using the test mode, complex steps,
And can have large effect to the test of low content elemental gas sample.
The content of the invention
It is an object of the invention to propose a kind of method for determining Oxygen in Titanium Alloy nitrogen hydrogen content, contained by using homemade
The Nickel particle fluxing agent having compared with Higher blank value fruit replaces the fluxing agents such as blue, the nickel bits of commercially available nickel, and titanium alloy is determined using impulse melting method
Middle oxygen nitrogen hydrogen content, by changing proper testing step and analysis condition, significantly reduces or eliminates the interference of blank value, reduction inspection
Survey cost.
For achieving the above object, present invention employs following technical scheme：
A kind of method for determining Oxygen in Titanium Alloy nitrogen hydrogen content, comprises the following steps：
(1) Nickel particle is made by oneself：Take high-purity sheet nickel to carry out surface polishing, cut into quality shape between 0.20~2.00g
The Nickel particle of shape rule；
(2) it is surface-treated：Surface oxide layer is removed using pickle pickling, is cleaned in organic solvent；After drying, storage
It is standby in air-tight bottle；
(3) deaerate：Self-control Nickel particle fluxing agent is manually added in oxygen nitrogen hydrogen combined measuring instrument high purity graphite crucible, in power 5500
PULSE HEATING under~6000W, removing fluxing agent and the hollow white spirit of graphite crucible are disturbed, degassing time 10s~60s；
(4) oxygen nitrogen hydrogen content is determined：Analysis power 5000W~5800W, analysis time 30s~75s, and sample with
Fluxing agent mass ratio is 1：4~1：Under conditions of 20, Oxygen in Titanium Alloy nitrogen hydrogen content is determined using oxygen nitrogen hydrogen combined measuring instrument.
Further, in the step of method of described measure Oxygen in Titanium Alloy nitrogen hydrogen content (1), oxygen in high-purity sheet nickel
Nitrogen hydrogen content is both less than 0.01%.
Further, in the step of method of described measure Oxygen in Titanium Alloy nitrogen hydrogen content (2), pickle by glacial acetic acid,
It is one or more kinds of in nitric acid, hydrochloric acid, hydrofluoric acid, hydrogen peroxide, phosphoric acid, sulfuric acid to prepare；Organic solvent be methanol, ethanol,
It is more than one or both of acetone, ether, chloroform, tetrachloromethane.
Further, in the step of method of described measure Oxygen in Titanium Alloy nitrogen hydrogen content (4), when sample is graininess
When, the automatic sample loading mode of throwing of selection is measured；When sample is bits shape, first bits shape sample is fitted into tin capsule, after compacting, then selected
Automatic sample loading mode of throwing is selected to be measured.
Compared with prior art, the present invention at least has the advantages that：
1. the present invention uses the homemade nickel containing higher oxygen nitrogen hydrogen content under conditions of normal testing procedure is changed
Grain fluxing agent replaces the fluxing agents such as commercially available nickel basket, nickel bits, determines Oxygen in Titanium Alloy nitrogen hydrogen content using impulse melting method, has
The advantages of method is simple, the degree of accuracy is high, fully meets the requirement of quick detection.
2. the throwing sample loading mode of the invention by changing instrument, Nickel particle fluxing agent and graphite crucible are added at high power together
Oxygen nitrogen hydrogen in heat, removing fluxing agent and graphite crucible.Which directly eliminates blank interference, it is not necessary to by test result
Deduct blank value；Moreover, quickly being melted during testing sample to be put into the nickel liquid of melting, which ratio is fluxing by solid nickel
Agent and sample throw simultaneously sample reheat the mode fusing speed of melting faster, it is more efficient.
3. the cheap sheet nickel of present invention selection, through processing such as polishing, cuttings, is cleaned with organic solvent, is prepared into nickel
Grain fluxing agent, can substantially save analysis cost.
Embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
(1) the high-purity sheet nickel for taking oxygen nitrogen hydrogen content to be respectively less than 0.01% carries out surface polishing derusting, cuts into wide about
0.5~2.5mm strip, cuts into quality rectangular Nickel particle fluxing agent regular between 1.50 ± 0.10g；
(2) 40~50s of pickling in the pickle of 75mL glacial acetic acid+25mL nitric acid+2mL hydrochloric acid, Nickel particle surface is failed
The sand grains pickling that surface is bumped into when the micro amount of oxygen compound or grinder buffing of polishing completely clean is removed, and uses supersonic cleaning machine and third
Ketone organic reagent Rapid Cleaning is decontaminated, after drying, standby in storage sealed plastic bottle.
(3) after under electrode drop, Nickel particle fluxing agent is put into oxygen nitrogen hydrogen combined measuring instrument high purity graphite crucible manually, lower electricity is risen
Pole, PULSE HEATING deaerates under 5800W power, and degassing time 20s, Nickel particle fluxing agent and graphite crucible are de-gassed place together
Reason, reduces or eliminates blank.
(4) when sample is graininess, the automatic sample loading mode of throwing of selection is measured；When sample is bits shape, shape will be first considered to be worth doing
Sample is fitted into tin capsule, after compacting, and reselection is thrown sample loading mode and is measured automatically.Pass through the automatic throwing sample prescription of oxygen nitrogen hydrogen analyzer
Formula puts into about 0.10g sample in the nickel liquid of melting in graphite crucible, and sample is 1 with fluxing agent mass ratio：15, in analysis
Power 5300W, analysis time 45s, instrument automatically begin to stabilization, and afterpulse stove to be stablized begins to warm up until analysis result, used
Titanium alloy standard substance calibrates oxygen nitrogen hydrogen analyzer, and Oxygen in Titanium Alloy nitrogen hydrogen content is provided automatically.
(5) analysis margin of Nickel particle fluxing agent, as shown in table 1.
As can be seen from Table 1：Make in Nickel particle fluxing agent nitrogen and hydrogen content and basically identical in nickel basket, and stability by oneself
Also it is preferable, but oxygen content has bigger difference；The laggard line blank analysis of analysis process is improved, because nickel fluxing agent is first taken off
Gas, then puts into sample and is analyzed, the oxygen nitrogen hydrogen of Nickel particle is removed in advance, and blank value is almost null value again.
Table 1 improves the analysis margin before and after analysis process
(6) accuracy test：
Under these experimental conditions, the gas content in llowing group of materials is analyzed respectively as fluxing agent using self-control Nickel particle,
And using conventional method acquired results to be compared as fluxing agent with nickel indigo plant, measurement result is as shown in table 2.
(7) Oxygen in Titanium Alloy nitrogen hydrogen content test result, as shown in table 2.
The accuracy test result of table 2
This method carries out data result in accuracy validation, table 2 with sample and shows that deviation is smaller, measured value and recommendation
Meet preferably.
From 1~table of table 2, method of the invention has the advantages that blank value is low and the degree of accuracy is high, beneficial to popularization and application.
Embodiment described above only expresses the embodiment of the present invention, but can not be therefore understands that for the present invention
The limitation of the scope of the claims.Those skilled in the art exists under the enlightenment of present inventive concept to any variation that the present invention is done
In protection scope of the present invention.
Claims (4)
1. a kind of method for determining Oxygen in Titanium Alloy nitrogen hydrogen content, it is characterised in that comprise the following steps：
(1) Nickel particle is made by oneself：Take high-purity sheet nickel to carry out surface polishing, cut into quality shape between 0.20~2.00g and advise
Nickel particle then；
(2) it is surface-treated：Surface oxide layer is removed using pickle pickling, is cleaned in organic solvent；After drying, it is stored in and fills
It is standby in air-tight bottle；
(3) deaerate：Will self-control Nickel particle fluxing agent be manually added in oxygen nitrogen hydrogen combined measuring instrument high purity graphite crucible, power 5500~
PULSE HEATING under 6000W, removing fluxing agent and the hollow white spirit of graphite crucible are disturbed, degassing time 10s~60s；
(4) oxygen nitrogen hydrogen content is determined：Analysis power 5000W~5800W, analysis time 30s~75s, and sample with it is fluxing
Agent mass ratio is 1：4~1：Under conditions of 20, Oxygen in Titanium Alloy nitrogen hydrogen content is determined using oxygen nitrogen hydrogen combined measuring instrument.
2. the method according to claim 1 for determining Oxygen in Titanium Alloy nitrogen hydrogen content, it is characterised in that the step (1)
In, oxygen nitrogen hydrogen content is both less than 0.01% in high-purity sheet nickel.
3. the method according to claim 1 for determining Oxygen in Titanium Alloy nitrogen hydrogen content, it is characterised in that the step (2)
In, pickle is one or more kinds of in glacial acetic acid, nitric acid, hydrochloric acid, hydrofluoric acid, hydrogen peroxide, phosphoric acid, sulfuric acid to be prepared；Have
Machine solvent is more than one or both of methanol, ethanol, acetone, ether, chloroform, tetrachloromethane.
4. the method according to claim 1 for determining Oxygen in Titanium Alloy nitrogen hydrogen content, it is characterised in that the step (4)
In, when sample is graininess, the automatic sample loading mode of throwing of selection is measured；When sample is bits shape, first bits shape sample is loaded
In tin capsule, after compacting, reselection is thrown sample loading mode and is measured automatically.
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| CN201710485592.4A CN107192590A (en) | 2017-06-23 | 2017-06-23 | Method for measuring oxygen, nitrogen and hydrogen content in titanium alloy |
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Cited By (9)
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|---|---|---|---|---|
| CN107941738A (en) * | 2017-12-19 | 2018-04-20 | 武汉钢铁有限公司 | The method of inspection of nitrogen content in a kind of variety steel magnesium oxide coating |
| CN108508176A (en) * | 2018-02-06 | 2018-09-07 | 太原重工股份有限公司 | The analysis determining method of nitrogen content in alloy |
| CN109342351A (en) * | 2018-11-28 | 2019-02-15 | 北京科技大学 | A method of measuring oxygen content in high hydrogen Titanium |
| CN110865168A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Method for rapidly analyzing main amount, trace amount and trace elements in alloy slag |
| CN112415049A (en) * | 2020-11-09 | 2021-02-26 | 辽宁红银金属有限公司 | Method for measuring oxygen content in metal rhenium |
| CN113588584A (en) * | 2020-04-30 | 2021-11-02 | 中国科学院金属研究所 | Method for measuring oxygen content in lanthanum, cerium metal or lanthanum-cerium alloy |
| CN113740142A (en) * | 2020-05-27 | 2021-12-03 | 宝山钢铁股份有限公司 | Method for obtaining hydrogen content of galvanized sheet matrix |
| CN113820289A (en) * | 2021-10-12 | 2021-12-21 | 天津市医疗器械质量监督检验中心 | Method for simultaneously measuring oxygen and nitrogen contents in titanium material |
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