CN110426423B - Device for detecting content of single constant impurity gas in neon - Google Patents

Device for detecting content of single constant impurity gas in neon Download PDF

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CN110426423B
CN110426423B CN201910731335.3A CN201910731335A CN110426423B CN 110426423 B CN110426423 B CN 110426423B CN 201910731335 A CN201910731335 A CN 201910731335A CN 110426423 B CN110426423 B CN 110426423B
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neon
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李琦
孙云
陆峻峰
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/045Circuits
    • G01N27/046Circuits provided with temperature compensation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/14Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
    • G01N27/18Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature caused by changes in the thermal conductivity of a surrounding material to be tested
    • G01N27/185Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature caused by changes in the thermal conductivity of a surrounding material to be tested using a catharometer

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Abstract

The embodiment of the invention discloses a device for detecting the content of a single constant impurity gas in neon, which comprises a detection unit and a calculation unit, wherein based on the principle of gas thermal conductivity, the thermal conductivity of a mixed gas to be detected is changed relative to pure neon due to the existence of the single impurity gas in neon, the resistance value change of a thermistor caused by the change of the thermal conductivity is detected through a Wheatstone bridge, and the thermal conductivity of the mixed gas to be detected is calculated, so that the content of the impurity gas in neon is obtained, the online detection of the content of the single constant impurity gas in neon can be realized, compared with a chromatographic separation detection mode, the cost is greatly saved, the real-time detection purpose is achieved, and the problem of difficulty in flow control is solved.

Description

Device for detecting content of single constant impurity gas in neon
Technical Field
The embodiment of the invention relates to the technical field of chemical detection, in particular to a device for detecting the content of single constant impurity gas in neon.
Background
When purifying neon mixed with a small amount of impurity gases (such as nitrogen, helium, hydrogen or oxygen) or measuring the content of the impurity gases in the neon, the prior art generally adopts the principle of chromatographic separation to separate the impurity gases in the neon and leads the measured gases to a corresponding detector to detect the content of the impurity gases, however, the cost of using a chromatographic analyzer is very high, and because each component needs to be separated by a chromatographic column, the process needs about five minutes to obtain the result, so that the real-time control of the operation flow cannot be realized, and the control difficulty exists.
Disclosure of Invention
Therefore, the embodiment of the invention provides a device for detecting the content of a single-term constant impurity gas in neon to solve the problems of high cost and long test time when a small amount of impurity gas in neon is separated or measured by adopting a chromatographic separation method in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions: the device for detecting the content of the single constant impurity gas in the neon comprises a detection unit and a calculation unit;
the detection unit comprises four groups of constant temperature thermal conductivity cells, wherein thermistors are arranged in the constant temperature thermal conductivity cells, two groups of constant temperature thermal conductivity cells are used as reference cells, the other two groups of constant temperature thermal conductivity cells are used as measurement cells, reference gas is packaged in the reference cells, gas to be measured flows in the measurement cells, the gas to be measured is neon containing single constant impurity gas, the four groups of thermistors form a Wheatstone bridge, the thermistors of the two groups of reference cells or the thermistors of the two groups of measurement cells are arranged oppositely, and constant current is conducted in the Wheatstone bridge;
the calculating unit is used for calculating the resistance value of the thermistor in the measuring cell according to the unbalanced potential output by the Wheatstone bridge, calculating the heat conductivity of the gas to be measured according to the resistance value, and calculating the content of the impurity gas in the gas to be measured according to the heat conductivity.
Further, the thermistors of the two groups of reference cells are respectively R1 and R2, the thermistors of the two groups of measuring cells are respectively R3 and R4, and the series branch of the thermistor R1 and the thermistor R3 is connected with the series branch of the thermistor R2 and the thermistor R4 in parallel to form a Wheatstone bridge.
Further, a node between the thermistor R1 and the thermistor R3 is a first output terminal, a node between the thermistor R2 and the thermistor R4 is a second output terminal, and the unbalanced potential output by the wheatstone bridge is a potential difference between the first output terminal and the second output terminal.
Furthermore, the two ends of the measuring pool are respectively provided with an air inlet and an air outlet, and the gas to be measured flows in through the air inlet and flows out through the air outlet.
Furthermore, the constant temperature thermal conductivity cell is arranged in the constant temperature device.
Further, the reference gas is pure neon, and the gas to be detected is neon containing single-term constant impurity gas.
Further, the reference gas is neon containing single-term constant impurity gas with known content, and the gas to be detected is neon containing single-term constant impurity gas of the same kind as the reference gas.
Further, the single-term constant impurity gas is any one of nitrogen, helium, oxygen or hydrogen.
Further, the content of the single-term constant impurity gas contained in the neon gas of the reference gas is changed so as to change the measuring range and the precision of detection of the corresponding single-term impurity gas.
Further, the four groups of thermistors have the same resistance value at the same temperature.
The embodiment of the invention has the following advantages:
the device for detecting the content of the single constant impurity gas in the neon provided by the embodiment of the invention is based on the principle of gas thermal conductivity, the thermal conductivity of the mixed gas to be detected is changed relative to the pure neon due to the existence of the impurity gas (such as nitrogen, helium, hydrogen or oxygen) in the neon, the resistance value change of the thermistor caused by the change of the thermal conductivity is detected through a Wheatstone bridge, and the thermal conductivity of the mixed gas to be detected is calculated, so that the content of the impurity gas in the neon is obtained, the online detection of the content of the single constant impurity gas in the neon can be realized, compared with a chromatographic separation detection mode, the cost is greatly saved, the real-time detection purpose is achieved, and the problem of difficulty in flow control is solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary and that other implementation drawings may be derived from the provided drawings by those of ordinary skill in the art without inventive effort.
FIG. 1 is a schematic structural diagram of an apparatus for detecting the content of a single-term constant impurity gas in neon provided in example 1 of the present invention;
fig. 2 is a schematic structural diagram of a detection unit of an apparatus for detecting the content of a single-term constant impurity gas in neon provided in embodiment 1 of the present invention;
fig. 3 is a schematic structural diagram of a measuring cell of an apparatus for detecting the content of a single-term constant impurity gas in neon according to embodiment 1 of the present invention.
In the figure: the detection unit 100, the calculation unit 200, the thermostatic device 110, the reference cell 120, the measurement cell 130, the gas inlet 131 and the gas outlet 132.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in fig. 1, the apparatus for detecting the content of a single-term constant impurity gas in neon proposed in the present embodiment comprises a detection unit 100 and a calculation unit 200.
As shown in fig. 2, the detection unit 100 includes four sets of constant temperature thermal conductivity cells with the same specification and size, and the four sets of constant temperature thermal conductivity cells are disposed in the constant temperature device 110 to provide a constant temperature T. All be provided with thermistor in four groups constant temperature thermal conductance ponds, four groups thermistor resistance value under the same temperature are the same and its material, specification, size are all the same. Two of the four groups of constant temperature thermal conductivity cells are used as reference cells 120, the other two groups are used as measurement cells 130, reference gas is packaged in the reference cells 120, gas to be measured flows in the measurement cells 130, the gas to be measured is neon gas containing single constant impurity gas, as shown in fig. 3, two ends of the measurement cells 130 are respectively provided with a gas inlet 131 and a gas outlet 132, and the gas to be measured flows in through the gas inlet 131 and flows out through the gas outlet 132.
The reference gas may be pure neon or neon containing a known amount of a single-term, constant impurity gas, which may be any of nitrogen, helium, oxygen, or hydrogen. When the reference gas is pure neon, the measuring cell 130 can be used for measuring neon containing any one of the above single constant impurity gases; where the reference gas is neon containing a known amount of a certain single-term constant impurity gas, the measurement cell 130 is used to measure neon containing the same type of single-term constant impurity gas as that in the reference gas. For example, when the reference gas is neon containing known amounts of helium impurity gas, the measurement cell 130 is used to measure neon containing helium impurity gas; when the reference gas is neon containing a known content of nitrogen impurity gas, the measuring cell 130 is used for measuring the neon containing the nitrogen impurity gas; when the reference gas is neon containing a known amount of oxygen impurity gas, the measurement cell 130 is used to measure neon containing oxygen impurity gas; where the reference gas is neon containing a known amount of hydrogen impurity gas, the measurement cell 130 is configured to measure neon containing hydrogen impurity gas. By adjusting the content of the single constant impurity gas such as nitrogen, helium, oxygen or hydrogen contained in the neon in the reference cell, the measurement range and the measurement precision of the corresponding impurity gas with unknown content near the content can be increased.
The four sets of thermistors form a wheatstone bridge, the thermistors of the two sets of reference cells 120 or the thermistors of the two sets of measurement cells 130 are arranged opposite to each other, and a constant current I is conducted in the wheatstone bridge. Specifically, the thermistors of the two reference cells 120 are respectively R1 and R2, the thermistors of the two measurement cells 130 are respectively R3 and R4, and the series branch of the thermistor R1 and the thermistor R3 is connected in parallel with the series branch of the thermistor R2 and the thermistor R4 to form a Wheatstone bridge. Thermistors R1 and R2 in two reference cells 120 in a Wheatstone bridge circuit serve as reference arms, and thermistors R3 and R4 in two measurement cells 130 serve as measurement arms. The node between the thermistor R1 and the thermistor R3 is a first output end, the node between the thermistor R2 and the thermistor R4 is a second output end, and the unbalanced potential output by the Wheatstone bridge is the potential difference Vout between the first output end and the second output end.
At a fixed temperature T, the content of nitrogen or helium in the neon nitrogen or neon helium mixed gas to be detected determines the thermal conductivity of the mixed gas to be detected, and the content of nitrogen or helium in the mixed gas to be detected can be calculated by measuring the thermal conductivity.
In the constant temperature thermal conductivity cell with the temperature T, constant current I flows through the thermistor, and the temperature of the thermistor is T. When pure neon gas slowly circulates in the constant temperature thermal conductivity cell, the heat of the thermistor is conducted out by the passing pure neon gas, after the thermal balance is achieved, the temperature of the thermistor is changed from t to t1, and after the pure neon is doped with impurity gases such as nitrogen or helium, the pure neon is mixed with the gas to be detected, because the thermal conductivity of the impurity gases such as nitrogen or helium is different from that of the pure neon (the difference is larger), the thermal conductivity of the mixed gas to be detected is changed relative to the pure neon, so that the thermal balance in the constant temperature thermal conductivity cell is changed, and the temperature of the thermistor is changed from t1 to t 2. Because t1 and t2 are different, the resistance value of the thermistor can be changed, the matched Wheatstone bridge circuit is unbalanced, micro current is generated, the resistance value of the thermistor in thermal balance can be obtained through the potential change, the change of the thermal conductivity of the neon nitrogen or neon helium mixed gas to be detected is measured, and finally the content of nitrogen or helium in the mixed gas to be detected is obtained.
When the concentration of the neon nitrogen or neon helium mixed gas to be measured introduced into the measurement cell 130 is consistent with the concentration of pure neon (or mixed gas to be measured) encapsulated in the reference cell 120, the thermal conductivity of the gas to be measured is the same as that of the encapsulating gas, the output voltage of the bridge circuit is zero, and when the concentration of the neon nitrogen (or neon helium) mixed gas to be measured introduced into the measurement cell 130 is different from that of the gas encapsulated in the reference cell 120, the thermal conductivity of the gas to be measured is also different from that of the encapsulating gas, so that the resistance value of the measurement arm is changed during thermal balance, and the bridge outputs unbalanced potential.
The calculating unit 200 is configured to calculate a resistance value of the thermistor in the measuring cell 130 according to the unbalanced potential output by the wheatstone bridge, calculate a thermal conductivity of the gas to be measured according to the resistance value, and calculate a content C of the impurity gas in the gas to be measured according to the following thermal conductivity calculation formulaM
CM=CM1+CR-CM1·CR (1)
λM=CM1·λX+(1-CM1)·λT (2)
Figure BDA0002160672740000061
Wherein:
CMthe content of impurity gas in the gas to be detected;
CM1suppose that the reference gas is gas one, the pure impurity gas is gas two, CM1Is in the gas-phase
The content of the second gas in the mixed gas to be detected consisting of the second gas;
CRthe content of single constant impurity gas in the gas of the reference cell;
λMmeasuring the thermal conductivity of the gas to be measured in the thermal conductivity cell when the temperature T is fixed by the thermal conductivity cell;
λTWhen the temperature T of the thermal conductivity cell is fixed, the thermal conductivity of reference gas of the reference cell;
λXthermal conductivity at pure impurity gas temperature T;
k is an instrument constant which is related to the structure of the thermal conductivity cell and is measured by tests;
R0the resistance value of the thermistor at 0 ℃;
alpha is the temperature coefficient of the thermistor;
i, current flowing through the thermistor;
Voutunbalanced potential differences output by the wheatstone bridge.
The device for detecting the content of the single constant impurity gas in the neon provided by the embodiment is based on the principle of gas thermal conductivity, the thermal conductivity of the mixed gas to be detected is changed relative to the pure neon due to the existence of the impurity gas (such as helium or nitrogen) in the neon, the resistance value change of the thermistor caused by the change of the thermal conductivity is detected through a Wheatstone bridge, and the thermal conductivity of the mixed gas to be detected is calculated, so that the content of the impurity gas in the neon is obtained, the online detection of the content of the single constant impurity gas in the neon can be realized, compared with a chromatographic separation detection mode, the cost is greatly saved, the purpose of real-time detection is achieved, and the problem of difficulty in flow control is solved.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (8)

1. The device for detecting the content of the single constant impurity gas in the neon is characterized by comprising a detection unit and a calculation unit;
the detection unit comprises four groups of constant temperature thermal conductivity cells, wherein thermistors are arranged in the constant temperature thermal conductivity cells, two groups of the four groups of constant temperature thermal conductivity cells are used as reference cells, the other two groups of constant temperature thermal conductivity cells are used as measurement cells, reference gas is packaged in the reference cells, gas to be measured flows in the measurement cells, the gas to be measured is neon containing single constant impurity gas, the four groups of thermistors form a Wheatstone bridge, the thermistors of the two groups of reference cells or the thermistors of the two groups of measurement cells are arranged oppositely, and constant current is communicated in the Wheatstone bridge;
the calculating unit is used for calculating the resistance value of a thermistor in the measuring cell according to the unbalanced potential output by the Wheatstone bridge, calculating the thermal conductivity of the gas to be measured according to the resistance value, and calculating the content of impurity gas in the gas to be measured according to the thermal conductivity;
the thermistors of the two groups of reference cells are respectively R1 and R2, the thermistors of the two groups of measuring cells are respectively R3 and R4, and a series branch of the thermistor R1 and the thermistor R3 is connected with a series branch of the thermistor R2 and the thermistor R4 in parallel to form a Wheatstone bridge;
The node between the thermistor R1 and the thermistor R3 is a first output end, the node between the thermistor R2 and the thermistor R4 is a second output end, and the unbalanced potential output by the Wheatstone bridge is the potential difference between the first output end and the second output end.
2. The apparatus as claimed in claim 1, wherein said measuring cell has a gas inlet and a gas outlet at opposite ends thereof, and said gas to be measured flows in through said gas inlet and out through said gas outlet.
3. The apparatus of claim 1, wherein said constant temperature thermal conductivity cells are located in a constant temperature device.
4. The apparatus of claim 1 wherein said reference gas is pure neon and said gas to be tested is neon containing a single constant impurity gas.
5. The device for detecting the content of the single-term constant impurity gas in neon according to claim 1, wherein the reference gas is neon containing a known content of the single-term constant impurity gas, and the gas to be detected is neon containing the same kind of the single-term constant impurity gas as the reference gas.
6. The apparatus of claim 5 wherein the amount of the single-term, constant impurity gas contained in the neon gas as the reference gas is varied to vary the range and accuracy of the measurement of the corresponding single-term impurity gas.
7. The apparatus for detecting the content of the single-term constant impurity gas in neon according to claim 4, 5 or 6, wherein said single-term constant impurity gas is any one of nitrogen, helium, oxygen or hydrogen.
8. The apparatus of claim 1 wherein said four sets of thermistors have the same resistance at the same temperature.
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US2751777A (en) * 1951-03-08 1956-06-26 Saint Gobain Gas analysis apparatus
CN1037967A (en) * 1988-05-16 1989-12-13 通用电气公司 Binary gas analyzer instrument and analytical approach
US5265459A (en) * 1991-08-22 1993-11-30 The Perkin Elmer Corporation Single-element thermal conductivity detector
CN2572404Y (en) * 2002-10-14 2003-09-10 安徽省电力试验研究所 Hydroge purity detector with heat conductive pool
CN101377469A (en) * 2008-07-15 2009-03-04 华南理工大学 Method and apparatus for real-time detecting mixing gas component content by thermal conductivity detector
CN201600347U (en) * 2009-07-28 2010-10-06 贝士德仪器科技(北京)有限公司 Nitrogen concentration detector

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2751777A (en) * 1951-03-08 1956-06-26 Saint Gobain Gas analysis apparatus
CN1037967A (en) * 1988-05-16 1989-12-13 通用电气公司 Binary gas analyzer instrument and analytical approach
US5265459A (en) * 1991-08-22 1993-11-30 The Perkin Elmer Corporation Single-element thermal conductivity detector
CN2572404Y (en) * 2002-10-14 2003-09-10 安徽省电力试验研究所 Hydroge purity detector with heat conductive pool
CN101377469A (en) * 2008-07-15 2009-03-04 华南理工大学 Method and apparatus for real-time detecting mixing gas component content by thermal conductivity detector
CN201600347U (en) * 2009-07-28 2010-10-06 贝士德仪器科技(北京)有限公司 Nitrogen concentration detector

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