Device and method for rapidly analyzing content of hydrogen isotope in metal and metal hydride

Abstract

The invention discloses a device and a method for rapidly analyzing the content of hydrogen isotope in metal and metal hydride, and relates to the technical field of rapid detection of hydrogen isotope gas.The device comprises a sample cabin, a reactor, a first gas storage tank and a mass spectrograph which are sequentially connected through a pipeline, and a heating device for heating the interior of the reactor is arranged outside the reactor; a vacuum gas path is further connected to the sample cabin in parallel, a high-purity H2 gas tank, a high-purity D2 gas tank, a gas flow regulator, a pressure sensor and a second gas storage tank are sequentially mounted on the vacuum gas path, and the outlet end of the vacuum gas path is connected to the inlet end of the first gas storage tank in parallel; the vacuum air path and the first air storage tank are both connected with a vacuum pump, and a temperature sensor is installed on the second air storage tank. Accurate quantification can be achieved under the condition that a standard substance is not needed, the detection range is wide, the content of the hydrogen isotope in the full range of trace to large amount can be detected, metal and alloy thereof can be detected, metal hydride can also be detected, and the applicability is high.

Description

Technical Field

[0001] The present invention relates to the technical field of rapid detection of hydrogen isotope gases, and in particular, to a device and method for rapid analysis of hydrogen isotope content in metals and metal hydrides. Background Art

[0002] Hydrogen has three isotopes, namely protium (H), deuterium (D), and tritium (T). In fields such as deuterium-tritium fusion reactors, weapon manufacturing, aerospace, and hydrogen energy development, the hydrogen isotope content in metals and metal hydrides will greatly affect their structure and performance. The accurate analysis of the hydrogen isotope content is crucial for the safe operation of reactors and the performance of hydrogen storage materials.

[0003] Most methods for measuring the hydrogen content in metals, such as hydrogen determinators, thermal desorption spectroscopy, neutron imaging, β-ray induced X-ray spectrometry, laser-induced breakdown spectroscopy, gas chromatography, etc., all require certified reference materials for analysis. And because these methods are extremely susceptible to interference from the matrix, environment, and their own isotopes during measurement, the reference materials also need to be strictly matched with the samples in terms of matrix, composition, content, morphology, etc. However, it is difficult to obtain matrix-matched reference materials, especially for metal and metal tritide reference materials containing radioactive tritium. Currently, there are no metal reference materials containing tritium at home and abroad, which greatly limits the application of these methods.

[0004] In addition, the above technologies also have the following disadvantages: The hydrogen determinator can only measure the total hydrogen content, cannot measure the contents of hydrogen isotopes protium, deuterium, and tritium, and the detection range is very narrow, generally about 0.1 μg / g to 30 μg / g. Metals with higher hydrogen content such as metal hydrides cannot be measured. Before measurement, complex chemical and chromatographic systems are also required to separate and purify interfering gases such as CO2, N2, and H2 O etc.; The neutron imaging method can also only measure the total hydrogen content, cannot measure the hydrogen isotope content, and the detection limit of the method is high (about dozens of μg / g), a large amount of samples is required, the efficiency is low, a large neutron reactor is needed, and the operation and maintenance costs are extremely high, making it difficult to promote and apply; The β-ray induced X-ray spectrometry can only be used for the detection of tritium content, cannot detect the contents of hydrogen and deuterium isotopes, and a large amount of samples is required; The laser-induced breakdown spectroscopy can measure the hydrogen isotope content, but the accuracy is poor and the detection limit is high (about several hundred μg / g). For metals and alloys such as stainless steel, titanium, and zirconium used in the nuclear industry, their hydrogen isotope content is usually only a few μg / g or even lower, and this technology is difficult to accurately quantify; The gas chromatography has a long analysis cycle, requires a large amount of samples, poor stability, a high detection limit, and a complex method. To reduce the interference of impurity gases such as methane on the measurement of hydrogen isotopes, it is also necessary to separate and purify the sample gas by means of adsorption, cryogenic freezing, etc.

[0005] Therefore, in order to solve the problems existing in the existing methods for analyzing the hydrogen isotope content in metals, such as the need for reference materials for accurate quantification, the ability to only measure total hydrogen but not hydrogen isotopes, the ability to only measure metals and alloys but not metal hydrides, narrow detection range, high detection limit, large sample amount required, low efficiency, and complex methods, there is an urgent need for a device and method for rapid analysis of hydrogen isotope content in metals and metal hydrides. Summary of the Invention

[0006] In order to solve the problems existing in the existing methods for analyzing the hydrogen isotope content in metals, such as the need for reference materials for accurate quantification, the ability to only measure total hydrogen but not hydrogen isotopes, the ability to only measure metals and alloys but not metal hydrides, narrow detection range, high detection limit, large sample amount required, low efficiency, and complex methods, the present invention provides a device and method for rapid analysis of hydrogen isotope content in metals and metal hydrides, which can accurately quantify without the need for reference materials, has a wide detection range, can detect the content of hydrogen isotopes in the entire range from trace to large amounts, can not only detect metals and their alloys, but also detect metal hydrides, has strong applicability, is not limited by the type and form of samples. At the same time, the sample amount required during the detection process is small, the detection limit is low, and it can be directly detected without complex pretreatment steps such as separation, enrichment, and purification. The method is simple, rapid, accurate, and low-cost.

[0007] To achieve the object of the present invention, the technical solution adopted is: a device for rapid analysis of hydrogen isotope content in metals and metal hydrides, comprising a sample chamber, a reactor and a first gas storage tank connected in sequence by a metal pipeline; specifically, a first valve is installed at the feed inlet of the sample chamber, and the first valve is used to control the sampling of the sample to be analyzed, and a second valve is installed at the outlet end of the sample chamber; a heating device for heating the inside thereof is arranged outside the reactor, and the heating device can heat the inside of the reactor to decompose the sample in the reactor into a sample gas to be measured containing hydrogen isotopes; the first gas storage tank is used to store the sample gas and the mixed gas to be measured; a mass spectrometer is installed on the first gas storage tank, and the mass spectrometer is used to measure the hydrogen isotope abundance, and a fourth automatic valve is installed at the inlet end of the mass spectrometer; a vacuum pipeline is also connected in parallel to the sample chamber, and a high-purity H2 gas tank, a high-purity D2 gas tank, a gas flow regulator, a third vacuum gauge and a second gas storage tank are installed in sequence on the vacuum pipeline, wherein the high-purity H2 gas tank is used to load high-purity H2 gas with a purity and abundance of not less than 99.9%, the high-purity D2 gas tank is used to load high-purity D2 gas with a purity and abundance of not less than 99.9%, the second gas storage tank is used to store a certain amount of high-purity H2 or high-purity D2 for filling, a second vacuum valve is installed at the inlet end of the vacuum pipeline, and the high-purity H2 gas tank, the high-purity D2 gas tank and the third vacuum gauge are all connected in parallel to the vacuum pipeline, a fifth automatic valve is installed at the outlet end of the high-purity H2 gas tank, a sixth automatic valve is installed at the outlet end of the high-purity D2 gas tank, a tenth automatic valve is installed at the inlet end of the second gas storage tank, and the outlet end of the vacuum pipeline is connected in parallel to the inlet end of the first gas storage tank, and a third automatic valve and a first pressure sensor are also installed at the inlet end of the first gas storage tank; vacuum pumps are connected in parallel to the inlet end of the vacuum pipeline and the outlet end of the first gas storage tank, and a temperature sensor is installed on the second gas storage tank, and the temperature sensor is used to monitor the temperature of the high-purity H2 or high-purity D2 injected into the second gas storage tank.

[0008] Further, the heating device is an electric resistance furnace or an induction furnace, the heating range of the heating device is from room temperature to 1300 °C, its temperature control accuracy is ±1 °C, and the temperature to be heated can be set according to actual needs when the heating device is in use; at the same time, when the reactor is installed, the reactor can be directly inserted vertically into the heating device so that the heater wraps around the outside of the reactor to improve the heating effect.

[0009] Further, the material of the reactor is ceramic, quartz or Hastelloy, and the specific selection of the reactor material can be determined according to the actual situation.

[0010] Furthermore, a first vacuum gauge is installed at the outlet end of the reactor. The outlet end of the reactor is connected to a first gas path and a second gas path arranged in parallel. The outlet ends of the first gas path and the second gas path are both connected in parallel to the inlet end of the first gas storage tank. A gas transfer pump is installed on the first gas path. A third valve is installed at the inlet end of the gas transfer pump, and a first automatic valve is installed at the outlet end of the gas transfer pump. A second automatic valve is installed on the second gas path.

[0011] Furthermore, the gas transfer pump is a molecular pump with a pumping speed for H2 of not less than 40 L / S, which is used to transfer the gas to be measured decomposed from the sample in the reactor to the first gas storage tank.

[0012] Furthermore, there are three pressure sensors on the vacuum gas path. The three pressure sensors are the third pressure sensor, the fourth pressure sensor, and the fifth pressure sensor respectively. A seventh automatic valve is installed at the inlet end of the third pressure sensor, an eighth automatic valve is installed at the inlet end of the fourth pressure sensor, and a ninth automatic valve is installed at the inlet end of the fifth pressure sensor. Through the cooperation of the third pressure sensor, the fourth pressure sensor, and the fifth pressure sensor, it is used to monitor the sample gas pressure or the pressure of high-purity H2 or high-purity D2 gas injected into the first gas storage tank. A first vacuum valve is also installed on the vacuum gas path, and the first vacuum valve is located between the second vacuum valve and the fifth automatic valve.

[0013] Furthermore, the vacuum pumps on the vacuum gas path and the first gas storage tank are both two vacuum pumps connected in series once. Specifically, the two vacuum pumps installed on the vacuum gas path are the first vacuum pump and the second vacuum pump. The first vacuum pump is located between the second vacuum pump and the vacuum gas path, and a third vacuum valve is installed at the outlet end of the first vacuum pump. A fourth vacuum gauge is installed between the third vacuum valve and the first vacuum valve. The two vacuum pumps installed on the first gas storage tank are the third vacuum pump and the fourth vacuum pump respectively. The third vacuum pump is located between the first gas storage tank and the fourth vacuum pump. The first vacuum pump and the third vacuum pump are molecular pumps with an ultimate vacuum better than 5×10 -9 mbar, and the second vacuum pump and the fourth vacuum pump are dry pumps with an ultimate vacuum better than 5 Pa and a pumping speed of not less than 5 L / s. The first vacuum pump, the second vacuum pump, the third vacuum pump, and the fourth vacuum pump are all used to evacuate the device.

[0014] Furthermore, the high-purity H2 gas tank and the high-purity D2 gas tank are both stainless steel gas storage tanks with a volume of 1 - 2 L and a pressure resistance of not less than 10 MPa; the first gas storage tank is a stainless steel tank with a volume of 50 - 1000 mL and a pressure resistance of not less than 1 MPa; the second gas storage tank is a stainless steel tank with a volume of 50 - 100 mL and a pressure resistance of not less than 1 MPa.

[0015] Further, the gas flow regulator is a gas leakage valve, a fine tuning valve or a micro mass flow regulator. The gas flow regulator can automatically adjust the flow rate of the outlet gas according to the feedback signal output by the first pressure sensor or the second pressure sensor, and the minimum adjustable gas flow rate is less than 2×10 -11 Pa·m 3 ·s -1 or 2 sccm.

[0016] Further, a second vacuum gauge is also connected to the first gas storage tank, and the mass spectrometer is a quadrupole mass spectrometer or a time-of-flight mass spectrometer with a mass resolution better than 1 amu and a hydrogen isotope abundance measurement accuracy better than 1%, and has a variety of communication interfaces for system control and data transmission.

[0017] Further, the sample chamber is equipped with a stainless steel vacuum transmission device. The stainless steel vacuum transmission device can support 10 samples for continuous injection at a time, and can automatically send the samples into the reactor according to the signal values fed back by the first vacuum gauge and the fourth vacuum gauge.

[0018] Further, the sample chamber, the reactor jacket, the joints and pipelines connecting each component in the device are all made of stainless steel with electrolytically polished inner walls, and their materials are 316 stainless steel, 316L stainless steel, 304 stainless steel or 304L stainless steel, with a pressure resistance of not less than 1 MPa, and the sealing materials therein all adopt stainless steel or pure copper, or directly adopt argon arc, electron beam, laser or direct welding for sealing.

[0019] Further, the first valve, the second valve and the third valve are all high-vacuum automatic valves or manual valves. For example, electromagnetic switches, pneumatic switches, gate valves or baffle valves, etc.; the nominal diameters of the first valve, the second valve and the third valve are not less than 40 mm, the pressure resistance is not less than 10 MPa, and the leakage rate is better than 1×10 -9 Pa·m 3 ·s -1 .

[0020] Further, the first automatic valve, the second automatic valve, the third automatic valve, the fourth automatic valve, the fifth automatic valve, the sixth automatic valve, the seventh automatic valve, the eighth automatic valve, the ninth automatic valve, the tenth automatic valve, the eleventh automatic valve, the first vacuum valve and the second vacuum valve and the third vacuum valve are all electromagnetic switches, pneumatic switches, diaphragm valves, bellows or needle valves, and the pressure resistance is not less than 10 MPa, and the leakage rate is better than 1×10 -9 m 3 ·Pa·s -1 .

[0021] Further, the accuracies of the first pressure sensor, the second pressure sensor, the third pressure sensor, the fourth pressure sensor, and the fifth pressure sensor are all better than 0.2%, and they have feedback signal outputs; the pressure measurement ranges of the first pressure sensor and the third pressure sensor are both 0 to 1000 Torr, the pressure measurement ranges of the second pressure sensor and the fourth pressure sensor are 0 - 1 Torr, and the pressure measurement range of the fifth pressure sensor is 0 to 10 Torr.

[0022] A method for rapid analysis of hydrogen isotope content in metals and metal hydrides, comprising the following steps:

[0023] Step 1: Evacuate the pipeline in the device to a vacuum better than 5×10 -3 Pa, and send the feed port of the metal or metal hydride sample chamber with a mass of 1 - 500 mg and accurately weighed m into the reactor for heating, and heat it at 700 - 1200 °C for 5 - 15 min. The gas containing hydrogen isotopes released by heating is sent into the first gas storage tank, and the abundance A H of protium, the abundance A D of deuterium, and the abundance A T of tritium in the sample are measured by a mass spectrometer;

[0024] Step 2: According to the measurement results of the abundances of protium, deuterium, and tritium in the sample, and according to the signal feedback from the pressure sensor on the vacuum pipeline, charge high-purity H2 with a known volume V in the high-purity H2 gas tank or high-purity D2 with a known volume V in the high-purity D2 gas tank into the second gas storage tank, monitor its pressure P through the pressure sensor, monitor its temperature T through the temperature sensor, and then mix the high-purity H2 or high-purity D 2送入 in the second gas storage tank with the sample gas in the first gas storage tank, and measure the hydrogen isotope abundances A 混H of the mixed gas again by a mass spectrometer;

[0025] Step 3: The hydrogen isotope content in the metal and metal hydride sample can be calculated by using the following formula:

[0026]

[0027] where C H is the protium content, C D is the deuterium content, C T is the tritium content; when the sample A H / A D > 1, the protium content C H is calculated using formula (1); when the sample A H / A D ≤ 1, the protium content C H is calculated using formula (2).

[0028] Further, the metal in Step 1 is tungsten, zirconium, uranium, plutonium, palladium, titanium, aluminum, lithium, nickel, stainless steel and their alloys, and the metal hydrides are lithium deuteride, uranium deuteride, and titanium tritide.

[0029] The beneficial effects of the present invention are as follows:

[0030] 1. The present invention can accurately quantify hydrogen isotopes in metals and metal hydrides without the need for reference materials. It can not only analyze total hydrogen, but also simultaneously analyze the contents of hydrogen isotopes protium (H), deuterium (D), and tritium (T), and is a high-precision absolute quantification method.

[0031] 2. The present invention has a wide detectable range, which is more than 4 orders of magnitude higher than conventional methods. It can detect trace and ultra-trace hydrogen isotopes in metals and their alloys, and can also detect up to several tens of percent of the constant hydrogen isotopes in metal hydrides, achieving full coverage of the detectable range of hydrogen isotope content.

[0032] 3. The present invention requires an extremely small sample amount, and the minimum sampling amount can be as low as 1 mg; the detection limit of the present invention is low. The detection limit of protium (H) content in metals and hydrides is as low as 0.1 μg / g, the detection limit of deuterium (D) content is as low as 0.01 μg / g, and the detection limit of tritium (T) content is as low as 0.01 μg / g; the present invention is not restricted by the sample form, type, and composition, and is applicable to the accurate analysis of hydrogen isotope content in various forms (such as bulk, rod-shaped, chip-shaped, powder-shaped, etc.), various types of metals (such as tungsten, zirconium, uranium, plutonium, palladium, titanium, aluminum, lithium, nickel, stainless steel, etc.) and their alloys, as well as metal hydrides (such as lithium hydride (deuteride), uranium hydride (deuteride), deuterium (tritium) titanium, etc.) in the fields of fusion reactors, weapon manufacturing, and aerospace, with strong applicability.

[0033] 4. The present invention does not require complex devices and steps such as adsorbents and cryogenic freezing to enrich, separate, and purify hydrogen isotopes in samples. It can achieve continuous injection and detection operations of multiple samples without replacing the reactor or removing the analyzed samples in the system. The entire process can be completed in about ten minutes, and the method is fast, simple, and accurate.

[0034] 5. The structure of this device is compact, with low cost and maintenance-free. Moreover, the entire device and analysis method can achieve full automation and unattended operation, effectively solving the safety protection problem of radioactive samples from reactors and weapon systems, and greatly reducing the radiation risk to staff. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The drawings illustrate exemplary embodiments of the present invention and, together with the description thereof, are used to explain the principles of the present invention. These drawings are included to provide a further understanding of the present invention and are included in this specification and form a part of this specification.

[0036] Figure 1 It is a system diagram of a device for rapid analysis of the hydrogen isotope content in metals and metal hydrides.

[0037] Marks in the attached drawings and corresponding component names:

[0038] 11. First valve; 2. Sample chamber; 3. Second valve; 4. Reactor jacket; 5. Reactor; 6. Heating device; 7. First vacuum gauge; 8. Third valve; 9. Gas transfer pump; 10. First automatic valve; 11. Second automatic valve; 12. Third automatic valve; 13. First pressure sensor; 14. First gas storage tank; 15. Second pressure sensor; 16. Second vacuum gauge; 17. Fourth automatic valve; 18. Mass spectrometer; 19. High-purity H2 gas tank; 20. Fifth automatic valve; 21. High-purity D2 gas tank; 22. Sixth automatic valve; 23. Gas flow regulator; 24. Third pressure sensor; 25. Seventh automatic valve; 26. Fourth pressure sensor; 27. Eighth automatic valve; 28. Fifth pressure sensor; 29. Ninth automatic valve; 30. Tenth automatic valve; 31. Third vacuum gauge; 32. Second gas storage tank; 33. Temperature sensor; 34. Eleventh automatic valve; 35. First vacuum valve; 36. Second vacuum valve; 37. Fourth vacuum gauge; 38. Third vacuum valve; 39. First vacuum pump; 40. Second vacuum pump; 41. Fourth vacuum valve; 42. Third vacuum pump; 43. Fourth vacuum pump. Specific embodiments

[0039] The present invention will be further described in detail below in conjunction with the attached drawings and embodiments. It can be understood that the specific embodiments described herein are only used to explain the relevant content and do not limit the present invention. Additionally, it should be noted that for the sake of description, only parts related to the present invention are shown in the attached drawings.

[0040] It should be noted that, without conflict, the embodiments in the present invention and the features in the embodiments can be combined with each other. The present invention will be described in detail below with reference to the attached drawings and embodiments.

[0041] As Figure 1As shown in the figure, a device for rapid analysis of hydrogen isotope content in metals and metal hydrides provided by the present invention includes a first valve 1, a sample chamber 2, a second valve 3, and a reactor jacket 4 connected in sequence through a metal pipeline. Among them, the inlet end of the metal pipeline serves as the sample inlet, and the opening and closing of the inlet end of the metal pipeline are controlled by opening and closing the first valve 1, thereby controlling the sampling of the sample to be analyzed; a reactor 5 is installed on the reactor jacket 4, the reactor 5 is vertically inserted into a heating device 6, and a first vacuum gauge 7 is installed at the outlet end of the reactor 5. The outlet end of the reactor 5 is also respectively connected in parallel with a first gas path and a second gas path. The first gas path is sequentially installed with a third valve 8, a gas transfer pump 9, and a first automatic valve 10. A second automatic valve 11 is installed on the second gas path. The first gas path and the second gas path can be automatically selected according to the signal value fed back by the first vacuum gauge 7. When the reading of the first vacuum gauge 7 is greater than 50 Pa, the first gas path is opened. When the reading of the first vacuum gauge 7 is less than or equal to 50 Pa, the second gas path is opened; the outlet ends of the first gas path and the second gas path are jointly installed with a third automatic valve 12, and the outlet end of the third automatic valve 12 is connected to a first gas storage tank 14.

[0042] A vacuum pipeline is also connected to the sample chamber 2. The vacuum pipeline is sequentially installed with a second vacuum valve 36, a first vacuum valve 35, a gas flow regulator 23, a tenth automatic valve 30, and a second gas storage tank 32; a first vacuum pump 39 and a fourth vacuum gauge 37 are also connected in parallel on the vacuum pipeline. The first vacuum pump 39 and the fourth vacuum gauge 37 are located between the second vacuum valve 36 and the first vacuum valve 35, and a third vacuum valve 37 is installed at the inlet end of the first vacuum pump 39. A second vacuum pump 40 is also connected in series on the first vacuum pump 39; a high-purity H2 gas tank 19 and a high-purity D2 gas tank 21 are also connected in parallel on the vacuum pipeline. The high-purity H2 gas tank 19 and the high-purity D2 gas tank 21 are located between the first vacuum valve 35 and the gas flow regulator 23, and a fifth automatic valve 20 is installed at the outlet end of the high-purity H2 gas tank 19, and a sixth automatic valve 22 is installed at the outlet end of the high-purity D2 gas tank 21; a third pressure sensor 24, a fourth pressure sensor 26, and a fifth pressure sensor 28 are also connected in parallel on the vacuum pipeline. The third pressure sensor 24, the fourth pressure sensor 26, and the fifth pressure sensor 28 are all located between the gas flow regulator 2 and the tenth automatic valve 30. A seventh pneumatic valve 25 is installed at the inlet end of the third pressure sensor 24, an eighth automatic valve 27 is installed at the inlet end of the fourth pressure sensor 26, and a ninth automatic valve 29 is installed at the inlet end of the fifth pressure sensor 28; a third vacuum gauge 31 is also connected in parallel on the vacuum pipeline. The third vacuum gauge 31 is located between the tenth automatic valve 30 and the second gas storage tank 32, and a temperature sensor 33 is also installed on the second gas storage tank 32. An eleventh automatic valve 34 is installed at the outlet end of the second gas storage tank 32; the outlet end of the vacuum pipeline is connected in parallel to the inlet end of the third automatic valve 12, and a first pressure sensor 13 is connected in parallel between the third automatic valve 12 and the first gas storage tank 14.

[0043] A fourth automatic valve 17 and a mass spectrometer 18 are successively connected to the first gas storage tank 14. A second pressure sensor 15, a second vacuum gauge 16, and a first vacuum valve 35 are connected in parallel between the first gas storage tank 14 and the fourth automatic valve 17. A fourth vacuum valve 41 is installed at the inlet end of the first vacuum valve 35, and a fourth vacuum pump 43 is connected in series with the first vacuum valve 35.

[0044] In this embodiment, the heating range of the heating device 6 is from room temperature to 1300 °C. The heating device 6 selects a resistance furnace reactor 5 with a temperature control accuracy better than 1 °C, and the material of the resistance furnace reactor 5 is quartz.

[0045] The gas transfer pump 6 is a turbomolecular pump with a pumping speed for H2 of 60 L / S; the first vacuum pump 39 and the third vacuum pump 42 are turbomolecular pumps with an ultimate vacuum of 1×10 -9 mbar; the second vacuum pump 40 and the fourth vacuum pump 43 are scroll dry pumps with an ultimate vacuum of 5 Pa and a pumping speed of 5 L / s.

[0046] The high-purity H2 gas cylinder 19 and the high-purity D2 gas cylinder 21 are stainless steel gas storage cylinders with a volume of 1 L and a pressure resistance greater than 10 MPa. The high-purity H2 gas cylinder 19 is used to store high-purity H2 gas with a purity of 99.999% and an abundance of 99.98%. The high-purity D2 gas cylinder 21 is used to store high-purity D2 gas with a purity of 99.999% and an abundance of 99.82%. The first gas storage tank 14 is a stainless steel tank with a volume of 150 mL and a pressure resistance greater than 1 MPa; the second gas storage tank 32 is a stainless steel tank with a calibrated volume of 0.0000512 m 3 and a pressure resistance greater than 1 MPa.

[0047] The gas flow regulator 23 is a gas leakage valve with a minimum adjustable gas flow of 1.5×10 -11 Pa·m 3 ·s -1 The gas flow regulator 23 can automatically adjust the flow rate of the gas at its outlet according to the feedback signal output by the first pressure sensor 13 or the second pressure sensor 15.

[0048] The accuracies of the first pressure sensor 13, the second pressure sensor 15, the third pressure sensor 24, the fourth pressure sensor 26, and the fifth pressure sensor 28 are all 0.15% (FS), and they have feedback signal outputs. The pressure measurement ranges of the first pressure sensor 13 and the third pressure sensor 24 are both 0 - 1000 Torr. The pressure measurement ranges of the second pressure sensor 15 and the fourth pressure sensor are 0 - 1 Torr. The pressure measurement range of the fifth pressure sensor 28 is 0 - 10 Torr. The first pressure sensor 13 and the second pressure sensor 15 are used to monitor the pressure of the sample gas. The third pressure sensor 24, the fourth pressure sensor 26, and the fifth pressure sensor 28 are used to monitor the pressure of high-purity H2 or high-purity D2.

[0049] The first valve 1, the second valve 3, and the third valve 8 are all high-vacuum pneumatic gate valves with a nominal diameter of 40 mm, a pressure resistance of not less than 10 MPa, and a leak rate better than 5×10 -10 Pa·m 3 ·s -1 ; The first automatic valve, the second automatic valve, the third automatic valve, the fourth automatic valve, the fifth automatic valve, the sixth automatic valve, the seventh automatic valve, the eighth automatic valve, the ninth automatic valve, the tenth automatic valve, the eleventh automatic valve, the first vacuum valve, the second vacuum valve, and the third vacuum valve are all pneumatic valves with a leak rate better than 1×10 -9 m 3 ·Pa·s -1 such as diaphragm valves, bellows, or needle valves, etc.

[0050] The fifth automatic valve 20 and the sixth automatic valve 22 can be selectively opened according to the measurement results (A H , A D ) of the sample protium and deuterium abundances by the mass spectrometer 18: when A H / A D > 1, open the sixth automatic valve 22; when A H / A D ≤1, open the fifth automatic valve 20. The seventh automatic valve 25, the eighth automatic valve 27, and the ninth automatic valve 29 can be selectively opened according to the magnitude of the pressure signal fed back by the first pressure sensor 13 or the second pressure sensor 15; after the tenth automatic valve 30 is opened, when the pressure values fed back by the third pressure sensor 24, the fourth pressure sensor 26, or the fifth pressure sensor 28 are consistent with the pressure signal fed back by the first pressure sensor 13 or the second pressure sensor 15, it will automatically close.

[0051] The temperature measurement accuracy of the temperature sensor 33 is better than 0.2% (FS), and the measurable range is from room temperature to 50 °C. It is used to monitor the pressure of high-purity H2 or high-purity D2 in the second gas storage tank 32. The mass spectrometer 18 is a quadrupole mass spectrometer with a mass resolution better than 1 amu and a hydrogen isotope abundance measurement accuracy better than 1%. It is used to measure the hydrogen isotope abundance in the sample gas and the mixed gas.

[0052] The sample chamber 2, the reactor jacket 4, and the joints and gas pipelines connecting each component are all made of 316L stainless steel with electrolytically polished inner walls, with a pressure resistance of not less than 1 MPa, and the sealing material is stainless steel.

[0053] Before the device provided by the present invention performs analysis, first, turn on the resistance furnace to heat to a certain temperature and maintain a constant temperature; second, open the first valve 1 to allow the metal or metal hydride sample to be analyzed to enter the sample chamber 2 through the feed port, and open the gas transfer pump 9, the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, the fourth vacuum pump 43, the third valve 8, the first automatic valve 10, the second automatic valve 11, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the gas flow regulator 23, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, and the fourth vacuum valve 41. The entire analysis device is evacuated by the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, and the fourth vacuum pump 43. The steps are as follows:

[0054] The first vacuum gauge 7, the second vacuum gauge 16, the third vacuum gauge 31, and the fourth vacuum gauge 37 are used to monitor the vacuum degree at the corresponding parts of the device, and a vacuum evacuation operation of the entire device is required for each analysis operation.

[0055] When the readings of the first vacuum gauge 7, the second vacuum gauge 16, the third vacuum gauge 31, and the fourth vacuum gauge 37 are all less than 5×10 - 3When the pressure is Pa, the first automatic valve 10, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, and the fourth vacuum valve 4 are automatically closed, and the second valve 3 is opened. The sample enters the reactor 5 in sequence through the stainless-steel vacuum transmission device in the sample chamber 2 and is heated for a certain period of time. During this process, when the reading of the first vacuum gauge 7 is greater than 50 Pa, the third valve 8, the transfer air pump 9, the first automatic valve 10, and the third automatic valve 12 are opened. The measured gas containing hydrogen isotopes decomposed from the sample in the reactor 5 enters the first gas storage tank 14 through the first transfer gas path; when the reading of the first vacuum gauge 7 is less than or equal to 50 Pa, the second automatic valve 11 and the third automatic valve 12 are opened. The measured gas containing hydrogen isotopes decomposed from the sample in the reactor 5 enters the first gas storage tank 14 through the second transfer gas path; the fourth automatic valve 17 is opened, and the mass spectrometer 18 performs a mass spectrometry measurement operation on the hydrogen isotope abundance of the sample gas in the first gas storage tank 14.

[0056] Subsequently, according to the measurement results of the abundances of protium, deuterium, and tritium in the sample, when A H / A D ≤1, the fifth automatic valve 20 is opened, or when A H / A D >1, the sixth automatic valve 22 is opened; according to the magnitude of the pressure signal fed back by the first pressure sensor 13 or the second pressure sensor 15, the gas flow regulator 23, the tenth automatic valve 30, and the seventh automatic valve 25, the eighth automatic valve 27, or the ninth automatic valve 29 are opened, and the tenth automatic valve 30 is opened. Thus, high-purity H2 with a known volume V in the high-purity H2 gas cylinder or high-purity D2 with a known volume V in the high-purity D2 gas cylinder is injected into the second gas storage tank 32, and the gas pressure injected into the second gas storage tank 32 is monitored by the third pressure sensor 24, the fourth pressure sensor 26, or the fifth pressure sensor 28. When the fed-back pressure signal is consistent with the value of the first pressure sensor 13 or the second pressure sensor 15, the tenth automatic valve 30 is automatically closed, and the tenth automatic valve 34 is opened. The high-purity hydrogen isotope gas enters the first gas storage tank 14 to be mixed with the sample gas, and the mass spectrometer 18 is used again to measure the hydrogen isotope abundance of the mixed gas.

[0057] Finally, the hydrogen isotope content in the metal and metal hydride sample can be calculated using the following formula:

[0058]

[0059] Among them, C H is the protium content, C D is the deuterium content, C T is the tritium content; when the sample A H / AD When it is greater than 1, the protium content C is calculated using formula (1). H ; When the sample A H / A D ≤1, the protium content C is calculated using formula (2). H content.

[0060] Demonstration Example 1

[0061] Analysis of Trace Hydrogen Content in Zirconium Alloy Reference Material

[0062] Before analysis, heat the resistance furnace to 1100 ± 1 °C and keep it at a constant temperature. Secondly, open the first valve 1 to allow the metal or metal hydride sample to be analyzed to enter the sample chamber 2 through the feed port. Open the transfer gas pump 9, the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, the fourth vacuum pump 43, the third valve 8, the first automatic valve 10, the second automatic valve 11, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the gas flow regulator 23, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, the fourth vacuum valve 41, and evacuate the entire analysis device through the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, and the fourth vacuum pump 43; then place 3 accurately weighed zirconium alloy standard samples AR630 (ALPHA, USA, nominal H content: w(H) = (10 ± 2) μg / g, numbered 1, 2, 3, with masses m1 = 0.33734 g, m2 = 0.35002 g, m3 = 0.34076 g respectively) into the sample chamber. When the readings of the first vacuum gauge 7, the second vacuum gauge 16, the third vacuum gauge 31, and the fourth vacuum gauge 37 are all less than 5×10 -3 Pa, automatically close the first automatic valve 10, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, the fourth vacuum valve 4, open the second valve 3, and the sample enters the reactor 5 in sequence through the stainless steel vacuum transmission device in the sample chamber 2 and is heated for 10 min. During this process, when the reading of the first vacuum gauge 7 is less than 50 Pa, open the third valve 8, the transfer gas pump 9, the first automatic valve 10, the third automatic valve 12, and the hydrogen isotope-containing gas to be measured decomposed from the sample in the reactor 5 enters the first gas storage tank 14 through the first transfer gas path for storage. Open the fourth automatic valve 17, and the mass spectrometer 18 measures the mass spectrum of the hydrogen isotope abundance of the sample gas in the first gas storage tank 14. The measurement results are respectively: A 1H = 99.97%, A 1D = 0.03%, A2H = 99.98%, A 2D = 0.02%, A 3H = 99.99%, A 3D = 0.01%.

[0063] Subsequently, according to the pressure value feedback by the second pressure sensor 15 and the mass spectrometry measurement results of the sample hydrogen isotope abundance, the sixth automatic valve 22, the gas flow regulator 23, and the seventh automatic valve 25, the eighth automatic valve 27 or the ninth automatic valve 29 are opened, and the tenth automatic valve 30 is opened to charge the second gas storage tank 32 with a calibrated volume V of 0.0000512 m 3 with high-purity D2 gas with pressures of P1 = 76.21 Pa, P2 = 80.93 Pa, P3 = 80.54 Pa respectively, which are consistent with the pressure value feedback by the second pressure sensor 15, and temperatures of T1 = 17 °C, T2 = 16.9 °C, T3 = 16.9 °C respectively, and mix them evenly.

[0064] Finally, the protium abundance in the mixed gas is measured again by the mass spectrometer 18, and the measurement results are A 1混H = 50.80%, A 2混H = 50.14%, A 3混H = 50.15%). Since the hydrogen isotope abundance test results A in the samples, the hydrogen (H) content in sample 1 is 9.90 μg / g, the hydrogen (H) content in sample 2 is 9.84 μg / g, and the hydrogen (H) content in sample 3 is 10.10 μg / g calculated by formulas (1) and (2) in the implementation manner. It can be seen that the analysis results of this device and method are consistent with the nominal values of the reference materials within the uncertainty range.

[0065] Demonstration Example 2

[0066] Analysis of deuterium content in lithium deuteride metal compound

[0067] Before analysis, heat the resistance furnace to 700 ± 1 °C and keep it at a constant temperature. Secondly, open the first valve 1 to allow the metal or metal hydride sample to be analyzed to enter the sample chamber 2 through the feed port. Open the transfer gas pump 9, the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, the fourth vacuum pump 43, the third valve 8, the first automatic valve 10, the second automatic valve 11, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the gas flow regulator 23, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, and the fourth vacuum valve 41. Evacuate the entire analysis device with the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, and the fourth vacuum pump 43. Then place a lithium deuteride powder sample with a precisely weighed mass m of 0.00358 g (Maclean, factory value: D abundance = 98.025%, purity > 99.95%, D content 22.210%) into the sample chamber. When the readings of the first vacuum gauge 7, the second vacuum gauge 16, the third vacuum gauge 31, and the fourth vacuum gauge 37 are all less than 5 × 10 -3 Pa, automatically close the first automatic valve 10, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, and the fourth vacuum valve 4. Open the second valve 3, and the sample enters the reactor 5 in sequence through the stainless steel vacuum transmission device in the sample chamber 2 and is heated for 10 min. During this process, when the reading of the first vacuum gauge 7 > 50 Pa, open the second automatic valve 11 and the third automatic valve 12. The hydrogen isotope-containing gas to be measured decomposed from the sample in the reactor 5 enters the first gas storage tank 14 through the first transfer gas path for storage. Open the fourth automatic valve 17, and the mass spectrometer 18 measures the mass spectrum of the hydrogen isotope abundance of the sample gas in the first gas storage tank 14. The measurement results are respectively: A H = 1.97%, A D = 98.03%.

[0068] Subsequently, according to the pressure value feedback by the second pressure sensor 15 and the mass spectrum measurement results of the sample hydrogen isotope abundance, open the fifth automatic valve 20, the gas flow regulator 23, and the seventh automatic valve 25, the eighth automatic valve 27, or the ninth automatic valve 29, and open the tenth automatic valve 30. Charge the second gas storage tank 32 with a calibrated volume V of 0.0000512 m 3 with high-purity H2 gas with a pressure P = 8962.20 Pa and a temperature T = 17.0 °C that is consistent with the pressure value feedback by the second pressure sensor 15 and mix it evenly.

[0069] Finally, the mass spectrometer 18 is used again to measure the hydrogen isotope abundances in the gas mixture, and the measurement result is A 混H = 50.58%. Since the hydrogen isotope abundance test result A in the sample is used to calculate the deuterium content in the sample as 22.209% according to the formulas (2) and (3) in the embodiment. It can be seen that the analysis results of the present device and method are consistent with their factory values within the uncertainty range.

[0070] Demonstration Example 3

[0071] Analysis of the contents of hydrogen isotopes protium (H), deuterium (D), and tritium (T) in tungsten

[0072] Before analysis, the resistance furnace is heated to 1100 ± 1 °C and kept at a constant temperature. Secondly, the first valve 1 is opened to allow the metal or metal hydride sample to be analyzed to enter the sample chamber 2 through the feed port. Then, the transfer gas pump 9, the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, the fourth vacuum pump 43, the third valve 8, the first automatic valve 10, the second automatic valve 11, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the gas flow regulator 23, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, and the fourth vacuum valve 41 are opened, and the entire analysis device is evacuated by the first vacuum pump 39, the second vacuum pump 40, the third vacuum pump 42, and the fourth vacuum pump 43; then, a certain gas-phase thermal charging deuterium-tritium experimental sample of tungsten, the first wall material of the fusion reactor, with a precisely weighed mass m of 0.30895 g is placed into the sample chamber. When the readings of the first vacuum gauge 7, the second vacuum gauge 16, the third vacuum gauge 31, and the fourth vacuum gauge 37 are all less than 5 × 10 -3 Pa, the first automatic valve 10, the third automatic valve 12, the fifth automatic valve 20, the sixth automatic valve 22, the seventh automatic valve 25, the eighth automatic valve 27, the ninth automatic valve 29, the tenth automatic valve 30, the eleventh automatic valve 34, the first vacuum valve 35, the second vacuum valve 36, the third vacuum valve 38, and the fourth vacuum valve 4 are automatically closed, and the second valve 3 is opened. The sample enters the reactor 5 in sequence through the stainless-steel vacuum transmission device in the sample chamber 2 and is heated for 5 minutes. During this process, the reading of the first vacuum gauge 7 is less than 50 Pa, and the third valve 8, the transfer gas pump 9, the first automatic valve 10, and the third automatic valve 12 are opened. The gas to be measured containing hydrogen isotopes decomposed from the sample in the reactor 5 enters the first gas storage tank 14 through the first transfer gas path for storage. The fourth automatic valve 17 is opened, and the mass spectrometer 18 measures the mass spectrum of the hydrogen isotope abundances in the sample gas in the first gas storage tank 14. The measurement results are respectively: A H = 0.12%, A D = 80.56%, A T = 19.32%.

[0073] Subsequently, according to the pressure value feedback by the second pressure sensor 15 and the mass spectrometry measurement result of the hydrogen isotope abundance of the sample, the fifth automatic valve 20, the gas flow regulator 23, and the seventh automatic valve 25, the eighth automatic valve 27 or the ninth automatic valve 29 are opened, and the tenth automatic valve 30 is opened to fill the second gas storage tank 32 with a calibrated volume V of 0.0000512 m 3 with high-purity H2 gas with a pressure of 80.29 Pa and a temperature of T = 17.0 °C that is consistent with the pressure value feedback by the second pressure sensor 15 and mix them evenly.

[0074] Finally, the system measures the hydrogen isotope abundance in the mixed gas again using the mass spectrometer 18, and the measurement result is A 混H = 50.04%. According to the formulas (2), (3), and (4) in the implementation manner of the hydrogen isotope abundance test result A of the sample, the content of protium H in the sample is 0.02 ug / g, the content of deuterium D is 24.02 ug / g, and the content of tritium T is 8.64 ug / g.

[0075] Those skilled in the art should understand that the above implementation manners are only for clearly explaining the present invention and not for limiting the scope of the present invention. For those skilled in the art, other changes or modifications can be made based on the above disclosure, and these changes or modifications are still within the scope of the present invention.

Claims

1. A device for rapid analysis of the hydrogen isotope content in metals and metal hydrides, characterized in that, It includes a sample chamber, a reactor, a first gas storage tank, and a mass spectrometer connected in sequence through a pipeline. There is a heating device outside the reactor for heating its interior, and a vacuum pipeline is also connected in parallel to the sample chamber. A high-purity H2 gas tank, a high-purity D2 gas tank, a gas flow regulator, a pressure sensor, and a second gas storage tank are installed in sequence on the vacuum pipeline. The outlet end of the vacuum pipeline is connected in parallel to the inlet end of the first gas storage tank; both the vacuum pipeline and the first gas storage tank are connected to a vacuum pump, and a temperature sensor is installed on the second gas storage tank.

2. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, characterized in that, The heating device is a resistance furnace or an induction furnace, and the reactor is inserted into the heating device; the reactor is made of ceramic, quartz, or Hastelloy.

3. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, wherein A first vacuum gauge is installed at the outlet end of the reactor. The outlet end of the reactor is connected to a first gas pipeline and a second gas pipeline arranged in parallel. The outlet ends of the first gas pipeline and the second gas pipeline are both connected in parallel to the inlet end of the first gas storage tank, and a gas transfer pump is installed on the first gas pipeline, and automatic valves are installed on both the first gas pipeline and the second gas pipeline.

4. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 3, wherein The gas transfer pump is a molecular pump with a pumping speed for H2 of not less than 40 L / S.

5. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, characterized in that, There are three pressure sensors on the vacuum pipeline. The three pressure sensors are the third pressure sensor, the fourth pressure sensor, and the fifth pressure sensor respectively. The pressure measurement range of the third pressure sensor is 0 - 1000 Torr, the pressure measurement range of the fourth pressure sensor is 0 - 1 Torr, and the pressure measurement range of the fifth pressure sensor is 0 - 10 Torr.

6. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1 or 5, characterized in that, There are two vacuum pumps on both the vacuum pipeline and the first gas storage tank, and the two vacuum pumps on the vacuum pipeline and the two vacuum pumps connected to the first gas storage tank are connected in series.

7. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 6, wherein Both of the two vacuum pumps on the vacuum pipeline and the two vacuum pumps connected to the first gas storage tank are molecular pumps with a performance better than 5×10 - 9 mbar and dry pumps with an ultimate vacuum better than 5 Pa.

8. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, wherein, The high-purity H2 gas tank and the high-purity D2 gas tank are both stainless steel gas storage tanks with a volume of 1 - 2 L and a pressure resistance of not less than 10 MPa; the first gas storage tank is a stainless steel tank with a volume of 50 - 1000 mL and a pressure resistance of not less than 1 MPa; the second gas storage tank is a stainless steel tank with a volume of 50 - 100 mL and a pressure resistance of not less than 1 MPa.

9. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, characterized in that, The gas flow regulator is a gas leak valve, a fine adjustment valve, or a micro mass flow regulator.

10. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, characterized in that, A second vacuum gauge is also connected to the first gas storage tank, and the mass spectrometer is a quadrupole mass spectrometer or a time-of-flight mass spectrometer with a mass resolution better than 1 amu and a hydrogen isotope abundance measurement accuracy better than 1%.

11. The device for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 1, characterized in that, There is a stainless steel vacuum drive device in the sample chamber.

12. A method for rapid analysis of hydrogen isotope content in metals and metal hydrides, characterized in that, It includes the following steps: Step 1: Evacuate the pipeline in the device to a vacuum state, and send the precisely weighed metal or metal hydride with a mass of m into the reactor for heating. The gas containing hydrogen isotopes released by heating is sent into the first gas storage tank, and the abundance A of protium in the sample is measured by a mass spectrometer. H , the abundance A of deuterium D , the abundance A of tritium T ; Step 2: According to the measurement results of the abundances of protium, deuterium, and tritium in the sample, and based on the signals fed back by the pressure sensors on the vacuum pipeline, fill high-purity H2 with a known volume V in the high-purity H2 gas cylinder or high-purity D2 with a known volume V in the high-purity D2 gas cylinder into the second gas storage tank, monitor its pressure P through the pressure sensor, and monitor its temperature T through the temperature sensor. Subsequently, mix the high-purity H2 or high-purity D in the second gas storage tank with the sample gas, and measure the hydrogen isotope abundance A of the mixed gas again through the mass spectrometer 2送入 in the first gas storage tank, and then measure the hydrogen isotope abundance A of the mixed gas again through the mass spectrometer 混H ; Step 3, the hydrogen isotope content in the metal and metal hydride samples can be calculated using the following formula: Among them, C H is the protium content, C D is the deuterium content, C T is the tritium content; when the sample A H / A D > 1, the protium content C H is calculated using formula (1); when the sample A H / A D ≤ 1, the protium content C H .

13. The method for rapid analysis of hydrogen isotope content in metals and metal hydrides according to claim 12, characterized in that, The metal in Step 1 is tungsten, zirconium, uranium, plutonium, palladium, titanium, aluminum, lithium, nickel, stainless steel, and their alloys, and the metal hydrides are lithium deuteride, uranium deuteride, and titanium tritide.

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