CN100425978C - Device for determining halium in metal using pulse heat conduction method and its application - Google Patents
Device for determining halium in metal using pulse heat conduction method and its application Download PDFInfo
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- CN100425978C CN100425978C CNB2004100505695A CN200410050569A CN100425978C CN 100425978 C CN100425978 C CN 100425978C CN B2004100505695 A CNB2004100505695 A CN B2004100505695A CN 200410050569 A CN200410050569 A CN 200410050569A CN 100425978 C CN100425978 C CN 100425978C
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- cupric oxide
- thermal conductivity
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Abstract
The present invention relates to a device for measuring helium in metal in a pulse thermal conductance method, which is used for converting a pulse thermal conductance hydrogen measuring instrument into a helium measuring instrument, and an application thereof. The device comprises a quick interface and a cupric oxide stove, wherein the cupric oxide stove comprises a quartz stove tube, glass wool, filamentary cupric oxide, heating wires, a heating power supply and a thermostat. Both ends of the quick interface are connected with the quartz stove tube through pipelines, and the glass wool and the filamentary cupric oxide are arranged in the quartz stove tube. Both ends of the quartz stove tube use the glass wool, the middle uses the filamentary cupric oxide, and the heating wires are arranged at the outer side of the quartz stove tube. A Schutze reagent tube of the pulse thermal conductance hydrogen measuring instrument is taken out, and the quick interface of the device substitutes for the Schutze reagent tube. The quick interface is respectively communicated with an argon outlet and an argon inlet, and the helium measurement is carried out. The present invention slightly changes the pulse thermal conductance hydrogen measuring instrument so as to measure helium in metal. The method which uses a built-in air mark system of the instrument to be combined with the quick interface so as to measure helium in the metal is simple and effective. A pulse heating and an inert gas melting thermal conduction methods can accurately measure helium in solid specimens.
Description
Technical field
The present invention relates to pulse thermal conductance hydrogen determinator is converted to the technology of helium determinator, be specially a kind of pulse thermal conductivity method and measure helium device and application thereof in the metal.
Background technology
Helium content is low in the metal, does not measure the demand of helium in the metal decades.In recent years, along with the development and the development of storage helium alloy, the mensuration of helium is essential to the development of this type of new material in the metal.External use helium in inert gas fusion mass spectrum or the gas chromatography determination metal, domesticly do not see precedent.For cooperating Metal Inst., Chinese Academy of Sciences's storage helium alloy development problem, carry out the work that helium is measured in the metal.
Summary of the invention
The object of the present invention is to provide a kind of pulse thermal conductivity method that pulse thermal conductance hydrogen determinator can be converted to helium determinator to measure helium device and application thereof in the metal, use built-in gas mark chamber helium and demarcate solid nitrogen steel mark checking computation process.
Technical scheme of the present invention is:
The pulse thermal conductivity method is measured helium device in the metal, comprise fast interface, cupric oxide stove, the cupric oxide stove comprises Quartz stove tube, glass wool, wire cupric oxide, electric furnace heating wire, heating power supply, temperature controller, the fast interface two ends link to each other with Quartz stove tube by pipeline, glaze cotton, wire cupric oxide in the Quartz stove tube, glass wool is adopted at two, the middle wire cupric oxide that adopts, the Quartz stove tube outside is provided with electric furnace heating wire and temperature thermocouple, temperature thermocouple links to each other with temperature controller, the heating power supply of electric furnace heating wire links to each other with temperature controller, by temperature controller control heating.
The described electric furnace heating wire outside is provided with heat-insulation layer, and heat-insulation layer is made by materials such as asbestos or zeyssatite.
Described pulse thermal conductivity method is measured helium device and application thereof in the metal, Soviet Union's thatch reagent pipe of RH-404 hydrogen determinator is taken off, measure the fast interface of helium device in the metal with the pulse thermal conductivity method and replace Soviet Union's thatch reagent pipe, fast interface communicates respectively with the argon gas gateway, carry out deciding helium, the hydrogen that argon gas carries, carbon dioxide, carbon monoxide, helium, nitrogen are completely oxidized to CO by the wire cupric oxide with CO earlier through the copper dioxide stove
2, H
2Be oxidized to H
2O; Again by the alkali asbestos of purification pipe and water absorbing agent with CO
2And H
2O absorbs removal; He and N
2After being written into chromatographic column and separating, helium goes out the peak earlier, is provided with to stop automatically after thermal conductivity detector (TCD) detects the helium peak integral time, to remove the influence at nitrogen peak; Computing machine is still pressed the thermal conductivity coefficient integral and calculating helium peak of hydrogen, shows and prints with the form of [H] ppm; Final calibrated and calculate the result of helium content.
Described cupric oxide stove at 580-600 ℃, is beneficial to remove hydrogen by temperature controller control temperature.
The invention has the beneficial effects as follows:
1, the present invention transforms hydrogen determinator the helium content that just can measure in the metal a little.
2, the present invention is simple and effective in conjunction with the method for helium in the fast interface conversion mensuration metal with the built-in gas mark system of instrument.
3, the present invention adopts PULSE HEATING, inert gas fusion-thermal conductivity can accurately measure helium in the solid-state sample.
Description of drawings
Fig. 1 is a RH-404 type pulse thermal conductance hydrogen determinator structural representation.
Fig. 2 is a structural representation of the present invention.
Fig. 3 is a helium gas target linearity curve.
Embodiment
RH-404 pulse thermal conductance hydrogen determinator as shown in Figure 1, comprise that analytic unit 1 and heating carry gas unit 2, analytic unit 1 comprises gas circuit unit 11, computing machine 12 and detecting device 13, gas circuit unit 11 is provided with and purifies stove 111, flowmeter 112, purification pipe 113, Soviet Union's thatch reagent pipe 114, tensimeter 115, absorption tube 116 etc., heating carry gas unit 2 be provided with can lifting pulsed electrode stove 21, suction cleaner 22 etc.Pulsed electrode stove 21 is with in the metal melting process; feeding argon gas protects; argon gas is through purifying stove 111; tensimeter 115; purification pipe 113 is to pulsed electrode stove 21; produce hydrogen in pulsed electrode stove 21 courses of work; carbon dioxide; carbon monoxide; helium; nitrogen etc.; with the argon gas is carrier gas; with hydrogen; carbon dioxide; carbon monoxide; helium; nitrogen carries; through Soviet Union's thatch reagent pipe 114; absorption tube 116 is to detecting device 13; the effect that purifies stove 111 is the impurity of removing in the argon gas; dress alkali asbestos and water absorbing agent in purification pipe 113 and the absorption tube 116; the alkali asbestos are on the upper strata; water absorbing agent is in lower floor; can absorbing carbon dioxide and water etc., dress iodic anhydrides in Soviet Union's thatch reagent pipe 114 can be converted into carbon dioxide with carbon monoxide.
Pulse thermal conductivity method of the present invention is as shown in Figure 2 measured helium apparatus structure synoptic diagram in the metal, comprise fast interface 3, cupric oxide stove 4, cupric oxide stove 4 comprises Quartz stove tube 41, glass wool 42, wire cupric oxide 43, electric furnace heating wire 44, heating power supply 45, temperature controller 46, metal joint 47, heat-insulation layer 48 (materials such as asbestos or zeyssatite are made), temperature thermocouple 49 etc., fast interface 3 replaces Soviet Union's thatch reagent pipe 114, be installed on the argon gas loop, fast interface 3 two ends link to each other with Quartz stove tube 41 through metal joint 47 by pipeline, glaze cotton 42 in the Quartz stove tube 41, wire cupric oxide 43, glass wool 42 is adopted at two, the middle wire cupric oxide 43 that adopts, Quartz stove tube 41 outsides are provided with electric furnace heating wire 44, between Quartz stove tube 41 and electric furnace heating wire 44, be provided with temperature thermocouple 49 in the outside, Quartz stove tube 41 middle parts, temperature thermocouple 49 links to each other with temperature controller 46, the heating power supply 45 of electric furnace heating wire 44 links to each other with temperature controller 46, by temperature controller 46 control heating.Arrow A is the gas inlet among the figure, and arrow B is the gas outlet, and arrow C is the gas circuit loop.
Development process of the present invention is as follows:
1 experimental section
1.1 instrument
Use U.S. Leco Corporation and produce the RH-404 hydrogen determinator, adopt the heating of pulsed electrode stove, Inert Gas Fusion Method to carry gas; Thermal conductivity method detects.
1.2 principle
The pulsed electrode stove heats sample, and maximum temperature can reach 3000 ℃.Sample fusion under the noble gas protection, gas discharges, and the argon carrier gas is brought the gas that discharges into analytic unit, through the cupric oxide stove CO is oxidized to CO
2, H
2Be oxidized to H
2O, and then the impurity aspiration is received through absorption tube detects tested gas by the thermal conductivity detector (TCD) in the analytic unit, will record signal again and send into computing machine, goes out net result by the coefficient calculations of hydrogen and shows and print, through obtaining the measured value of helium after calculating.Thermal conductivity coefficient is the important parameter that thermal conductivity method detects and calculates, H
2, He, N
2, four kinds of gases of Ar molecular weight and thermal conductivity coefficient see Table 1.When instrument dispatched from the factory, producer had provided with the helium instead of hydrogen and has done gas target calibration value, and analytic unit can detect the helium of the 1.0 μ g/g orders of magnitude.
The molar weight and the thermal conductivity coefficient of four kinds of gases of table 1
[1] Sun Chuanjing, gas chromatographic analysis philosophy and technique, 1981
1.3 the transformation of instrument
Self-control fast interface cupric oxide stove is replaced the Soviet Union's thatch reagent pipe on the RH-404 hydrogen determinator.Cupric oxide is removed by water absorbing agent after hydrogen-oxygen can being changed into water; Alternative again Soviet Union thatch reagent is oxidized to carbon dioxide with carbon monoxide simultaneously.Do not change former hydrogen determinator function on the whole, again hydrogen is removed fully.
1.4 decide the helium flow journey
Sample drops into the application of sample mouth, behind heat de-airing, falls into scorching hot graphite crucible automatically.The pulsed electrode stove is heated to 2000-2200 ℃ with crucible, and under this temperature, helium, hydrogen and nitrogen discharge from the sample of fusion with simple substance form in the metal.Oxygen in the sample is CO and a spot of CO by graphite reduction
2The argon carrier gas is brought the gas that discharges into analytic unit, earlier through (change and add) cupric oxide stove, CO is completely oxidized to CO
2H
2Be oxidized to H
2O, again by alkali asbestos and water absorbing agent with CO
2And H
2O absorbs removal.He and N
2After being written into chromatographic column and separating, helium goes out the peak earlier, is provided with to stop automatically after thermal conductivity detector (TCD) detects the helium peak integral time, to remove the influence at nitrogen peak.Owing to do not change computer software programs, computing machine still press the thermal conductivity coefficient integral and calculating helium peak of hydrogen, with the form demonstration of [H] ppm with print.Final calibrated and calculate the result of helium content.
2 results and discussion
2.1 helium gas mark is demarcated
When this RH-404 hydrogen determinator dispatched from the factory, the gas scale value that the automatic injecting systems of quantity tube injects a pin hydrogen was 16.12 μ g/g, and the gas mark displayed value that injects a pin helium is 9.82 μ g/g.Two kinds of gas are marked on identical pressure, under the identical temperature, inject the gas of equal volume.According to The Ideal-Gas Equation PV=nRT, the identical n of the molal quantity of then every pin injecting gas
Helium=n
Hydrogen, establishing the mass percent that M is a gas, μ is that molecular weight then has: M
Helium/ μ
Helium=M
Hydrogen/ μ
Hydrogen
M
Helium=(μ
Helium/ μ
Hydrogen) M
Hydrogen=(4.0026/2.0159) 16.12=32.01 μ g/g
Calculating the actual gas scale value that injects a pin helium thus is 32.01 μ g/g, and being different from displayed value 9.82 μ g/g is to cause because of the calculation of parameter such as thermal conductivity coefficient of computing machine by hydrogen.
Helium content: displayed value=32.01: 9.82
Displayed value=3.26 displayed values of helium content=(32.01/9.82)
2.2 helium gas target linearity
Helium gas target linearity as shown in Figure 3, when the volume that injects helium with the integer increases added-time, gas mark detected value also increases with identical integral multiple.
2.3 nitrogen steel target is demarcated
Owing to also do not have the solid-state standard specimen of helium at present, demarcate with the nitrogen steel, with the consistance of checking gaseous state standard specimen and solid-state standard specimen.Because producer does not provide the nitrogen calibration value of this instrument, earlier with high purity nitrogen self-calibration, recording nitrogen mark displayed value is 1.42 μ g/g, and according to The Ideal-Gas Equation, the molal quantity that injects a pin gas is identical, calculates by aforementioned formula:
M
Nitrogen=(μ
Nitrogen/ μ
Hydrogen) M
Hydrogen=(28.0134/2.0159) 16.12=224.01 μ g/g
Displayed value=157.75 displayed values of nitrogen content=(224.01/1.42)
Use nitrogen steel mark [N]=440 ± 10 μ g/g and demarcate, the actual displayed value that records is 2.84 μ g/g, calculates [N]=157.75 * 2.84=448 μ g/g, drops in the standard specimen tolerance.Use LECO nitrogen steel mark 502-195[N]=564 ± 13 μ g/g demarcation, displayed value is 3.55 μ g/g, measured value [N]=157.75 * 3.55=560 μ g/g drops in the standard specimen tolerance fully.
2.4 the measurement result of helium in the metal
2.4.1 test condition
Analysis condition: adopt tin capsule parcel alloy powder sample, the 5300W degassing, 5000W analyzes.
Blank value: the helium blank value of graphite crucible and tin capsule is 0.00 μ g/g.
2.4.2 measured result
Measured the helium content of several alloys, Zr-Co alloy 1A1
#Sample [He]=5.3 μ g/g; Zr-Co alloy 5C3
#[He]=2.4 μ g/g; La-Ni alloy 7R2
#[He]=5.9 μ g/g; La-Ni alloy 8E5
#[He]=9.8 μ g/g.
2.5 discuss
2.5.1 the absolute value problem in gas mark chamber
Tradition gas mark injects with μ l level micro syringe, the stainless steel quantity tube machinery injection of this instrument, and the gas mark absolute value that injects a pin hydrogen is 16.12 μ g or n=7.996 * 10
-6Mol (sample is heavily pressed 1.0000g and calculated).The absolute value of gas mark chamber V can obtain by two kinds of approach: (1) is by The Ideal-Gas Equation PV=nRT; P=40psi=2.71atm; R=0.08206atmL/molK; T=298K calculates V ≈ 72 μ L or 72mm
3Yet 2.7 atmospheric gases, and non-ideal gas, the V that calculates only are approximate value.(2) gas marked lumen pull down after, measure V with the method for physics.Tear gas mark lumen open and will destroy Primordial Qi gas road, cause the loss that to retrieve.Measuring the quantity tube outer diameter is that Φ 1.5mm length is 40-60mm, and the volume that estimates quantity tube thus is 62-92mm
3, this shows that this instrument injects the about 72 μ L of volume of a pin mark gas under the demarcation state, value is about 8.0 * 10
-6Mol.This paper is all basis mutually with the molar weight of injecting a pin mark gas, and the absolute value problem in gas mark chamber does not have influence on the degree of accuracy of calculating.
2.5.2 the solid target reliability of nitrogen
The correction factor that the RH-404 hydrogen determinator is measured helium is 3.26, can accept basically.And the correction factor of nitrogen is up to 157.75, and the degree of accuracy of revising the nitrogen content that obtains thus reduces greatly than hydrogen and helium.The basic detection principle of thermal conductivity detector (TCD) is poor based on carrier gas and tested gas conductance coefficient, and two kinds of gas conductance coefficient difference are big more, and under the same terms, gage beam and reference arm difference large-signal more are strong more.Thermal conductivity coefficient difference by the visible hydrogen of table 1, helium and argon is big, is respectively 37.6 and 30.8; The thermal conductivity coefficient difference of nitrogen and argon is little, only is 1.8.Argon is made the carrier gas thermal conductivity method and is detected nitrogen, and the weak sensitivity of signal is low, does not almost see the pulse thermal conductance azotometer of doing carrier gas with argon.Demarcate with nitrogen steel mark herein, do not relate to the problem of hydrogen and high nitrogen translocation sensitivity, only for verifying the correctness of account form, gas mark and solid target consistance.
3 conclusions
3.1RH-404 just transforming a little, hydrogen determinator can measure helium in the metal.
3.2 it is simple and effective in conjunction with the method for helium in the fast interface conversion mensuration metal with the built-in gas mark system of instrument.
3.3 PULSE HEATING, inert gas fusion-thermal conductivity can accurately be measured helium in the solid-state sample.
Claims (4)
1, the pulse thermal conductivity method is measured helium device in the metal, it is characterized in that: comprise fast interface (3), cupric oxide stove (4), the cupric oxide stove comprises Quartz stove tube (41), glass wool (42), wire cupric oxide (43), electric furnace heating wire (44), heating power supply (45), temperature controller (46), fast interface (3) two ends link to each other with Quartz stove tube (41) by pipeline, the interior glaze cotton of Quartz stove tube (41) (42), wire cupric oxide (43), two is glass wool (42), the centre is wire cupric oxide (43), Quartz stove tube (41) outside is provided with electric furnace heating wire (44) and temperature thermocouple (49), temperature thermocouple (49) links to each other with temperature controller (46), the heating power supply (45) of electric furnace heating wire (44) links to each other with temperature controller (46), by temperature controller (46) control heating.
2, measure helium device in the metal according to the described pulse thermal conductivity method of claim 1, it is characterized in that: the described electric furnace heating wire outside is provided with heat-insulation layer, and heat-insulation layer is made by asbestos or diatomite material.
3, measure the application of helium device in the metal according to the described pulse thermal conductivity method of claim 1, it is characterized in that: Soviet Union's thatch reagent pipe of RH-404 hydrogen determinator is taken off, measure the fast interface of helium device in the metal with described pulse thermal conductivity method and replace Soviet Union's thatch reagent pipe, fast interface communicates respectively with the argon gas gateway, carry out deciding helium, the hydrogen that argon gas carries, carbon dioxide, carbon monoxide, helium, nitrogen are completely oxidized to CO earlier through the copper dioxide stove with CO
2, H
2Be oxidized to H
2O; Again by the alkali asbestos of purification pipe and water absorbing agent with CO
2And H
2O absorbs removal; He and N
2After being written into chromatographic column and separating, helium goes out the peak earlier, is provided with to stop automatically after thermal conductivity detector (TCD) detects the helium peak integral time, to remove the influence at nitrogen peak; Computing machine is still pressed the thermal conductivity coefficient integral and calculating helium peak of hydrogen, shows and prints with the form of [H] ppm; Final calibrated and calculate the result of helium content.
4, measure the application of helium device in the metal according to the described pulse thermal conductivity method of claim 3, it is characterized in that: described cupric oxide stove is controlled temperature at 580-600 ℃ by temperature controller.
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|---|---|---|---|
| CNB2004100505695A CN100425978C (en) | 2004-10-10 | 2004-10-10 | Device for determining halium in metal using pulse heat conduction method and its application |
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| CN100425978C true CN100425978C (en) | 2008-10-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101144794B (en) * | 2007-10-29 | 2010-11-24 | 钢铁研究总院 | Impulse melting mass spectrometry analysis method for element |
| CN101144795B (en) * | 2007-10-29 | 2010-06-02 | 钢铁研究总院 | Impulse melting-flying time mass spectrometry for element |
| CN101975711B (en) * | 2010-10-08 | 2011-11-30 | 中国航空工业集团公司北京航空材料研究院 | Method for measuring hydrogen content in powder high-temperature alloy |
| CN102507894B (en) * | 2011-10-17 | 2014-08-20 | 攀钢集团江油长城特殊钢有限公司 | Method for determining hydrogen content in titanium and titanium alloy |
| CN103048289B (en) * | 2012-12-17 | 2015-02-18 | 中国科学院金属研究所 | Argon-oxygen or nitrogen-oxygen combined determinator and use method thereof |
| CN105223152A (en) * | 2015-09-18 | 2016-01-06 | 苏州萨伯工业设计有限公司 | A kind of oxygen nitrogen analysis detection method |
| CN105136661A (en) * | 2015-09-18 | 2015-12-09 | 苏州萨伯工业设计有限公司 | Oxygen and nitrogen analyzer |
| CN110632233A (en) * | 2019-10-24 | 2019-12-31 | 上海裕达实业有限公司 | Constant temperature chromatographic device |
| CN112858376B (en) * | 2021-01-04 | 2023-12-29 | 广西防城港核电有限公司 | Method for measuring content of dissolved hydrogen in primary loop of reactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4305906A (en) * | 1979-08-15 | 1981-12-15 | Horiba, Ltd. | Apparatus for analyzing oxygen, nitrogen and hydrogen contained in metals |
| JPS61161442A (en) * | 1985-01-09 | 1986-07-22 | Kobe Steel Ltd | Method for measuring hydrogen and oxygen concentration in molten copper or copper alloy |
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| DE10003676A1 (en) * | 2000-01-28 | 2001-08-02 | Grunewald Axel Ulrich | Determining concentration of mixed hydrogen and helium from thermal conductivity, comprises determination and calibration at two or more temperatures |
| CN1467493A (en) * | 2002-07-11 | 2004-01-14 | 郭跃辉 | Control method and equipment for electronic control system of intelligent type helium mass spectrometer leak detector |
-
2004
- 2004-10-10 CN CNB2004100505695A patent/CN100425978C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4305906A (en) * | 1979-08-15 | 1981-12-15 | Horiba, Ltd. | Apparatus for analyzing oxygen, nitrogen and hydrogen contained in metals |
| JPS61161442A (en) * | 1985-01-09 | 1986-07-22 | Kobe Steel Ltd | Method for measuring hydrogen and oxygen concentration in molten copper or copper alloy |
| JP2001033437A (en) * | 1999-07-26 | 2001-02-09 | Mitsubishi Heavy Ind Ltd | Method for measuring trace quantity of helium in metal |
| DE10003676A1 (en) * | 2000-01-28 | 2001-08-02 | Grunewald Axel Ulrich | Determining concentration of mixed hydrogen and helium from thermal conductivity, comprises determination and calibration at two or more temperatures |
| CN1467493A (en) * | 2002-07-11 | 2004-01-14 | 郭跃辉 | Control method and equipment for electronic control system of intelligent type helium mass spectrometer leak detector |
Non-Patent Citations (1)
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