CN109211785A - Eliminate the element sulphur analysis Auxiliary Processing Unit and method of high content nitrogen element influences - Google Patents
Eliminate the element sulphur analysis Auxiliary Processing Unit and method of high content nitrogen element influences Download PDFInfo
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- CN109211785A CN109211785A CN201810631867.5A CN201810631867A CN109211785A CN 109211785 A CN109211785 A CN 109211785A CN 201810631867 A CN201810631867 A CN 201810631867A CN 109211785 A CN109211785 A CN 109211785A
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- China
- Prior art keywords
- element sulphur
- sample gas
- high content
- influences
- processing unit
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000005864 Sulphur Substances 0.000 title claims abstract description 78
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 31
- 238000012545 processing Methods 0.000 title claims abstract description 15
- 238000004458 analytical method Methods 0.000 title abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 2
- 230000008030 elimination Effects 0.000 abstract description 6
- 238000003379 elimination reaction Methods 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 abstract description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 28
- 238000002795 fluorescence method Methods 0.000 description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 4
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 241000255964 Pieridae Species 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
Abstract
The present invention provides the element sulphur analysis Auxiliary Processing Unit and method of a kind of elimination high content nitrogen element influences, including threeway reaction tube, the first entrance of threeway reaction tube is connected with ozone supplied source, its second entrance is connected with sample gas inlet pipeline, for accessing the sample gas after high-temperature S removal, the outlet of threeway reaction tube then connects sample gas outlet pipeline, for sample gas to be sent into element sulphur detection device.It can be reacted with the sample gas for entering threeway reaction tube by second entrance by the ozone that first entrance enters threeway reaction tube, the sample gas after reaction is entered into element sulphur detection by the outlet of threeway reaction tube again, the influence to testing result of nitrogen can be eliminated.
Description
Technical field
The present invention relates to it is a kind of with ultraviolet fluorescence method principle realize element sulphur analyzer pre-procesor and method,
Sample middle and high concentration nitrogen can be eliminated to the analysis result of sulfur content.
Background technique
The method of the element sulphur analysis of current petrochemical industry product has very much, main to have: GB/T 380-1977
(2004) " oil product sulphur content determination method (Ignition Lamp Method) ", GB/T 387-1990 " deep color petroleum product sulphur content determination method
(tube oven method) ", GB/T 388-1964 " oil product sulphur content determination method (bomb method) ", SH/T 0689-2000 " light hydrocarbon
And the total sulfur content measuring method (ultraviolet fluorescence method) of engine fuel and other oil products ", GB/T 11140-2008 " oil product
The measurement Single wavelength dispersive x-ray fluorescence spectroscopic methodology of sulfur content ", SH/T 17040-2008 " oil product sulphur content determination method
(energy-dispersion X-ray fluorescence spectrometry) " etc..
Ultraviolet fluorescence method element sulphur analysis method is unique arbitration side in numerous specifications of surveys and standard method
Method;Corresponding international standard is: " ASTM D5453-09 light hydrocarbons, spark-ignition engine fuel, diesel engine combustion
Total sulfur content measuring method (ultraviolet fluorescence method) in material and engine lubricating oil ".
Currently, ultraviolet fluorescence method element sulphur analyzer is for high-content in above-mentioned sample, (nitrogen mass fraction is greater than
0.3%) nitrogen is to analyzing influence brought by low content element sulphur without effectively eliminating and inhibit processing method and special
Device.Also contain a large amount of nitrogen in above-mentioned sample other than containing element sulphur to be analyzed, in ultraviolet fluorescence method sulphur member
Element sulphur in sample is carried out catalysis oxidation by the mode that the sample in plain analyzer is all made of Pintsch process, to generate to be measured
Contain sulfur dioxide (SO2) sample gas.But the nitrogen in sample is also under identical condition by catalysis oxygen in the process
Turn to nitrogen oxides (mainly nitric oxide (NO) and nitrogen dioxide (NO2)), wherein nitric oxide is in UV vluorescent tester
In can also be excited under the irradiation of ultraviolet light, fluorescence can be issued when turning again to stable state, this part light (interference signal)
Fluorescence (useful signal) is formed by with element sulphur eventually arrives at photoelectric converter together and form total electric signal exported.In this way
With regard to the serious final result for affecting element sulphur analysis, measured value can be substantially higher.
If using complicated sample chemical pretreatment mode, one side high operation requirements, process complexity;Another party
Face also can have an impact and lose to element sulphur to be measured while to sample treatment, finally can not accurately be measured
As a result.
Summary of the invention
The present invention provides the element sulphur analysis Auxiliary Processing Unit and method of a kind of elimination high content nitrogen element influences, solves
Above-mentioned technical problem.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of element sulphur analysis Auxiliary Processing Unit for eliminating high content nitrogen element influences, it is characterized in that including:
Ozone generator;
Threeway reaction tube, first entrance are connected with the outlet of the ozone generator, and second entrance is connected with sample
Gas inlet pipe road, for accessing the sample gas after high-temperature S removal, the outlet of threeway reaction tube then connects sample gas and goes out
Mouth pipeline, for sample gas to be sent into element sulphur detection device.
The element sulphur of the elimination high content nitrogen element influences analyzes Auxiliary Processing Unit, in which: the ozone occurs
The oxygen inlet pipeline of the entrance connection of device is equipped with current limiting tube.
The element sulphur of the elimination high content nitrogen element influences analyzes Auxiliary Processing Unit, in which: the oxygen inlet
Piping connection is to oxygen bottle.
The element sulphur of the described elimination high content nitrogen element influences analyzes Auxiliary Processing Unit, in which: the sample gas into
Mouth piping connection is in the Pintsch process of element sulphur analyzer and the downstream of equipment for drying, the sample gas outlet piping connection
In the upstream of the element sulphur detection device of the element sulphur analyzer.
The present invention also provides a kind of element sulphurs for eliminating high content nitrogen element influences to analyze aid in treatment method, and feature exists
In: the sample gas after high-temperature S removal is reacted with ozone, sulphur member then is carried out to the sample gas by reaction
Element detection.
The element sulphur of the elimination high content nitrogen element influences analyzes aid in treatment method, in which: described to pass through high temperature
Sample gas after catalysis oxidation be element sulphur analyzer Pintsch process and be dried link caused by, the element sulphur
Detecting step is carried out in the element sulphur detection of the element sulphur analyzer.
The present invention by the sample gas (gas molecule containing NO) generated by elemental analyser by with O3(ozone) is in room temperature
Under reaction, be completely converted into will not ultraviolet light irradiation under generate fluorescence NO2(+N2) etc. ingredients, to eliminate nitrogen pair
The influence of element sulphur signal, while also the character of element sulphur is not had an impact.
The present invention connects pipeline and circuit, and without operation and control, opening power supply can be used, compact-sized, pipe
Road is clear, and used component is simple, reliable performance, long service life.In addition present apparatus compatibility very well, can connect not
The element sulphur analyzer of same type.
Detailed description of the invention
Fig. 1 is that the structure of the element sulphur analysis Auxiliary Processing Unit provided by the invention for eliminating high content nitrogen element influences is former
Reason figure.
Description of symbols: 1- element sulphur analyzer;2- sample gas inlet pipeline;3- threeway reaction tube;4- ozone occurs
Device;5- current limiting tube;6 oxygen inlet pipelines;7- oxygen bottle;8- sample gas outlet pipeline.
Specific embodiment
As shown in Figure 1, the present invention provides a kind of element sulphur analysis Auxiliary Processing Unit for eliminating high content nitrogen element influences,
Comprising:
Oxygen inlet pipeline 6, for supplying oxygen;It in the present embodiment, is to supply oxygen with oxygen bottle 7;
Current limiting tube 5, one end are connected with the oxygen inlet pipeline 6;
Ozone generator 4, entrance is connected with the other end of the current limiting tube 5, for converting the oxygen to ozone;
Threeway reaction tube 3, first entrance are connected with the outlet of the ozone generator 4, and second entrance is connected with sample
Gas inlet pipe road 2, the outlet of threeway reaction tube 3 then connect sample gas outlet pipeline 8;
Wherein, the sample gas inlet pipeline 2 is for accessing the sample gas after high-temperature S removal;Existing sulphur member
Plain analyzer 1 is designed with high-temperature S removal device, thus can directly be accessed from element sulphur analyzer 1 sample gas into
Mouth pipeline 2;The sample gas outlet pipeline 8 then takes back element sulphur analyzer 1, carries out element sulphur detecting step.
Therefore, the present invention also provides a kind of element sulphurs for eliminating high content nitrogen element influences to analyze aid in treatment method, is
Sample gas after high-temperature S removal is reacted with ozone, element sulphur inspection then is carried out to the sample gas by reaction
It surveys.In preferred embodiment, the sample gas after high-temperature S removal be element sulphur analyzer 1 Pintsch process and
It is dried caused by link, the element sulphur detecting step is the element sulphur detection in the element sulphur analyzer 1
Middle progress.
The working principle of the invention is that present invention addition in 1 Pintsch process of element sulphur analyzer and is dried link
Between (equipment) and element sulphur detection (equipment), enable by first entrance enter the ozone of threeway reaction tube 3 with by
The sample gas that second entrance enters threeway reaction tube 3 reacts, and eliminates the influence of nitrogen, then by the sample gas after reaction by
The outlet of threeway reaction tube 3 enters element sulphur detection.
Wherein, it is as follows to eliminate the basic principle that nitrogen influences by the present invention:
R-N+O2→NO+NO2+N2O+CO2+H2O (1)
NO+O3→NO2(+N2)+O2 (2)
Reaction equation (1) is that the nitrogen compound of high-content in sample is generated each after the reaction of Pintsch process Guan Zhongyu oxygen
Kind substance.If these gases (in addition to water, having moisture in de-watering apparatus removal sample) can be as carrier gas be direct without the present invention
Into in Ultraluminescence element sulphur detector, wherein NO gas molecule is excited under the irradiation of the ultraviolet source of detector, quilt
The NO gas molecule of excitation can issue fluorescence when returning to stable state, be received by the photoelectric converter in element sulphur detector, shape
At very big interference signal, here it is the basic processes of high concentration N element sample interference element sulphur detection.
The present invention passes through the principle of reaction equation (2), the sample gas (gas molecule containing NO) that will be generated by elemental analyser
By with O3The reaction of (ozone) at normal temperature is completely converted into the NO that fluorescence will not be generated under ultraviolet light irradiation2(+N2) etc.
Ingredient to eliminate influence of the nitrogen to element sulphur signal, while also not having an impact the character of element sulphur, is finally reached
The purpose of the present invention.
Wherein, the pressure in the threeway reaction tube 3 is determined by the sample air pipe (carrier gas) of element sulphur analyzer 1 substantially
(generally all between 0.1-0.3MPa), carrier gas flux are usually no more than 600ml/min, the ozone flow that this equipment uses for
20-30ml/min or so.
Practical effect of the invention is as shown in the table:
Sample (ppm) | Testing result (ppm) | Remarks |
S5 | 5.01 | Without apparatus of the present invention |
S10 | 9.98 | Without apparatus of the present invention |
S5 | 4.97 | There are apparatus of the present invention |
S10 | 9.95 | There are apparatus of the present invention |
N500 | 12.1 | Without apparatus of the present invention |
N500 | 0.02 | There are apparatus of the present invention |
S5+N500 | 16.8 | Without apparatus of the present invention |
S10+N500 | 21.9 | Without apparatus of the present invention |
S5+N500 | 5.11 | There are apparatus of the present invention |
S10+N500 | 10.2 | There are apparatus of the present invention |
Illustrate:
1. S5: concentration is the element sulphur standard sample of 5mg/L
2. S10: concentration is the element sulphur standard sample of 10mg/L
3. N500: concentration is the nitrogen standard sample of 500mg/L
4. standard sample is Research Institute of Petro-Chemical Engineering's production
In contrast, the present invention has the advantage that
The present invention uses the gas source for preparing of pure oxygen (cylinder oxygen, purity requirement 99.99%) as ozone, and corona mode produces
Raw ozone so that the ozone concentration of preparation is very high, and prepares speed and fully meets sample gas flowing velocity, can guarantee ozone with
Nitrogen oxides in sample reacts completely, so that nitrogen oxides fluorescence interference of the sample in UV vluorescent tester drops to
Minimum, this technical solution is more direct compared with the prior art, more thorough, simpler;And sample loss and secondary will not be brought
Pollution.
Apparatus of the present invention also use simple mode direct, low in cost, reliable for operation in structure realization.To guarantee
The reflection speed that ozone flow velocity caused by ozone generator 4 is all satisfied sample gas and nitrogen oxides with concentration matches,
The flow for flowing into ozone generator 4 is set up by the way of current limiting tube 5 at oxygen intake.In addition, in order to avoid sample
Loss (SO2Gas is easy to react or adsorbed by it with metal under given conditions), pipeline (containing connector etc.) is in material
Select inertia nonmetallic (PEEK, polytetrafluoroethylene (PTFE), quartz etc.) in matter, to greatest extent reduce due to the present apparatus introducing and
The error of bring test data.
In conclusion the present invention connects pipeline and circuit, without operation and control, opening power supply can be used, and be tied
Structure is compact, pipeline is clear, and used component is simple, reliable performance, long service life.In addition present apparatus compatibility is fine,
Different types of element sulphur analyzer 1 can be connected.
Claims (7)
1. a kind of element sulphur for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit, it is characterized in that including:
Threeway reaction tube, first entrance are connected with ozone supplied source, and second entrance is connected with sample gas inlet pipeline, is used for
Sample gas after high-temperature S removal is accessed, the outlet of threeway reaction tube then connects sample gas outlet pipeline, for will be with
Sample gas after ozone reaction is sent into element sulphur detection device.
2. the element sulphur according to claim 1 for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit, feature
Be: the first entrance of threeway reaction tube is connected to the outlet of ozone generator.
3. the element sulphur according to claim 2 for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit, feature
Be: the oxygen inlet pipeline of the entrance connection of the ozone generator is equipped with current limiting tube.
4. the element sulphur according to claim 3 for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit, feature
It is: the oxygen inlet piping connection to oxygen bottle.
5. the element sulphur according to claim 1 for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit, feature
Be: the sample gas inlet piping connection is described in the Pintsch process of element sulphur analyzer and the downstream of equipment for drying
Sample gas outlet piping connection is in the upstream of the element sulphur detection device of the element sulphur analyzer.
6. a kind of element sulphur for eliminating high content nitrogen element influences analyzes aid in treatment method, it is characterised in that: high temperature will be passed through
Sample gas after catalysis oxidation reacts with ozone, then carries out element sulphur detection to the sample gas by reaction.
7. the element sulphur according to claim 6 for eliminating high content nitrogen element influences analyzes aid in treatment method, feature
Be: the sample gas after high-temperature S removal is the Pintsch process and drying process link institute in element sulphur analyzer
It generates, the element sulphur detecting step is carried out in the element sulphur detection of the element sulphur analyzer.
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CN201810631867.5A CN109211785A (en) | 2018-06-19 | 2018-06-19 | Eliminate the element sulphur analysis Auxiliary Processing Unit and method of high content nitrogen element influences |
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CN201810631867.5A CN109211785A (en) | 2018-06-19 | 2018-06-19 | Eliminate the element sulphur analysis Auxiliary Processing Unit and method of high content nitrogen element influences |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110208319A (en) * | 2019-06-05 | 2019-09-06 | 北京诺德泰科仪器仪表有限公司 | A kind of Dumars azotometer reaction tube |
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CN202869975U (en) * | 2012-10-24 | 2013-04-10 | 中国石油化工股份有限公司 | Online automatic testing device for liquid or gas sulfur content |
CN208206779U (en) * | 2018-06-19 | 2018-12-07 | 北京诺德泰科仪器仪表有限公司 | The element sulphur for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit |
-
2018
- 2018-06-19 CN CN201810631867.5A patent/CN109211785A/en active Pending
Patent Citations (2)
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CN202869975U (en) * | 2012-10-24 | 2013-04-10 | 中国石油化工股份有限公司 | Online automatic testing device for liquid or gas sulfur content |
CN208206779U (en) * | 2018-06-19 | 2018-12-07 | 北京诺德泰科仪器仪表有限公司 | The element sulphur for eliminating high content nitrogen element influences analyzes Auxiliary Processing Unit |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110208319A (en) * | 2019-06-05 | 2019-09-06 | 北京诺德泰科仪器仪表有限公司 | A kind of Dumars azotometer reaction tube |
CN110208319B (en) * | 2019-06-05 | 2022-03-04 | 北京诺德泰科仪器仪表有限公司 | Dumas azotometer reaction tube |
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