CN109569262A - The method, apparatus and application of chlorosilane in a kind of removal polysilicon tail gas - Google Patents

The method, apparatus and application of chlorosilane in a kind of removal polysilicon tail gas Download PDF

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Publication number
CN109569262A
CN109569262A CN201811594353.3A CN201811594353A CN109569262A CN 109569262 A CN109569262 A CN 109569262A CN 201811594353 A CN201811594353 A CN 201811594353A CN 109569262 A CN109569262 A CN 109569262A
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China
Prior art keywords
tail gas
chlorosilane
polysilicon tail
polysilicon
absorbent module
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CN201811594353.3A
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Chinese (zh)
Inventor
安军林
田润朝
曹岩德
周慧娟
乔琳琳
王海礼
魏东亮
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Asia Silicon Qinghai Co Ltd
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Asia Silicon Qinghai Co Ltd
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Priority to CN201811594353.3A priority Critical patent/CN109569262A/en
Publication of CN109569262A publication Critical patent/CN109569262A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/81Solid phase processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/68Halogens or halogen compounds
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004Gaseous mixtures, e.g. polluted air
    • G01N33/0009General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/20Halogens or halogen compounds
    • B01D2257/204Inorganic halogen compounds

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Biomedical Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present invention relates to technical field of polysilicon production, disclose a kind of method for removing chlorosilane in polysilicon tail gas, including following treatment process: collecting, collect polysilicon tail gas;The polysilicon tail gas being collected into is carried out condensation process, makes it that part chlorosilane be precipitated by condensation;It absorbs, by the polysilicon tail gas after condensation process by adsorbent, continues to be adsorbed and removed remaining chlorosilane in tail gas.Also disclose a kind of device for removing chlorosilane in polysilicon tail gas, including sampling assemble and deep cooling mechanism;Pipeline is connected on the sampling assemble, pipeline passes through deep cooling mechanism and is connected with absorbent module after cooling, is filled with adsorbent in absorbent module;The absorbent module has outlet.The method and device of chlorosilane can remove the chlorosilane in tail gas in this removal polysilicon tail gas, easy to operate effectively to protect detection device in detecting tail gas when trace phosphine gas content, prolong its service life, reduction testing cost.

Description

The method, apparatus and application of chlorosilane in a kind of removal polysilicon tail gas
Technical field
The present invention relates to technical field of polysilicon production, more particularly to a kind of side of chlorosilane in removal polysilicon tail gas Method, device and application.
Background technique
Electronic-grade polycrystalline silicon is the basic material of generation information technology industry and photovoltaic industry, with high-efficiency solar electricity The fast development progress of pool technology, more stringent requirements are proposed for quality and appearance to polycrystalline silicon for photovoltaic use.In production of polysilicon In, the impurity content in tail gas can embody the clean level of whole system, and impurity mainly has chloride, boride, arsenic Object, phosphide, carbohydrate etc..Wherein boron, phosphorus compound seriously affect polysilicon product quality, especially influence resistivity Size and stability.For this purpose, measuring phosphorus in silicon wafer by detecting to the phosphine gas generated in polysilicon production process Content, to be monitored and instruct to technique.About detection, generally using trace in flame photometric detector detection tail gas Phosphine gas.And due to containing a certain amount of HCl, SiH in the tail gas of recycling2Cl2、SiHCl3And SiCl4, especially chlorine silicon The presence of alkane gas can make detector photomultiplier tube by a degree of damage, cause testing result inaccurate.Therefore, The invention proposes a kind of method of chlorosilane in removal polysilicon tail gas and the devices of application this method.
Summary of the invention
The present invention is intended to provide the method, apparatus of chlorosilane and application are in a kind of removal polysilicon tail gas to solve existing skill Above-mentioned technical problem in art.
The technical solution adopted by the present invention are as follows:
A kind of method of chlorosilane in removal polysilicon tail gas, including following treatment process:
It collects, collects polysilicon tail gas;
The polysilicon tail gas being collected into is carried out condensation process, makes it that part chlorosilane be precipitated by condensation;
It absorbs, by the polysilicon tail gas after condensation process by adsorbent, continues to be adsorbed and removed remaining chlorine silicon in tail gas Alkane.
The method of chlorosilane in the removal polysilicon tail gas provided according to the present invention, finally, collecting by absorbing processing Polysilicon tail gas.
According to the method for chlorosilane in above-mentioned removal polysilicon tail gas, polysilicon tail gas is used after this method is handled The content of trace hydrogen phosphide in measurement tail gas.
The device of chlorosilane in a kind of removal polysilicon tail gas, including sampling assemble and deep cooling mechanism;The sampling assemble On be connected with pipeline, pipeline passes through deep cooling mechanism and is connected with absorbent module after cooling, is filled with adsorbent in absorbent module;Institute Stating absorbent module has outlet.
The device of chlorosilane in the removal polysilicon tail gas provided according to the present invention, the outlet of the absorbent module is connected with Collection assembly is connected with aspiration pump between collection assembly and absorbent module;The sampling assemble is sampling bag, and collection assembly is to receive Collect bag.
The device of chlorosilane in the removal polysilicon tail gas provided according to the present invention, the absorbent module are accommodating cylinder, One end is import, and the other end is outlet;The adsorbent elements filled in it are NaOH.
The device of chlorosilane, the deep cooling mechanism are cold-trap device in the removal polysilicon tail gas provided according to the present invention, It is loaded with refrigerant with refrigerating chamber in refrigerating chamber, fixation is coated with heat insulation layer outside refrigerating chamber.
The device of chlorosilane, further includes being connected on pipeline, and set in the removal polysilicon tail gas provided according to the present invention Condenser pipe between sampling assemble and absorbent module, condenser pipe are placed in deep cooling mechanism.
The device of chlorosilane, further includes being set to deep cooling survey within the organization in the removal polysilicon tail gas provided according to the present invention Temperature meter, thermometric are calculated as temperature sensor.
According to the device of chlorosilane in above-mentioned removal polysilicon tail gas, polysilicon tail gas is used after device processing The content of trace hydrogen phosphide in measurement tail gas.
Beneficial effects of the present invention:
It collects in polysilicon tail gas to sampling assemble, and places it in cold-trap mechanism and condense, make that part chlorosilane is precipitated; Then, continue the polysilicon tail gas after condensation process through absorbent module, in adsorbent be adsorbed and removed in tail gas again Remaining chlorosilane is discharged from the outlet of absorbent module later.
The method and device of chlorosilane can remove the chlorosilane in tail gas in this removal polysilicon tail gas, easy to operate to have Effect.Polysilicon tail gas removes chlorosilane gas, measures the trace phosphatization in the tail gas later after this method or device processing Hydrogen can avoid it from being polluted corrosion and damage by chlorosilane in measurement with effective protection detection device, and extension detection device uses the longevity Life reduces testing cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the device of chlorosilane in removal polysilicon tail gas provided in an embodiment of the present invention;
In figure:
1, sampling assemble 2, pipeline 3, deep cooling mechanism 4, condenser pipe
5, heat insulation layer 6, absorbent module 7, aspiration pump 8, collection assembly
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with attached drawing, to the present invention into One step is described in detail.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments. Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts all Other embodiments shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical", The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation or Person is constructed and operated in a specific orientation, therefore it is not considered as limiting the invention.In addition, term " first ", " the Two ", " third " is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected;When Right, it can also be mechanical connection, be also possible to be electrically connected;In addition, it can also be and be connected directly, be also possible to pass through centre Medium is indirectly connected, or can be the connection inside two elements.For the ordinary skill in the art, Ke Yigen The concrete meaning of above-mentioned term in the present invention is understood according to concrete condition.
Embodiment 1
The embodiment provides a kind of methods of chlorosilane in removal polysilicon tail gas, including following processing work Sequence:
It collects, collects polysilicon tail gas;Specifically, sample collection bag, which can be used, is collected storage.
The polysilicon tail gas being collected into is carried out condensation process, makes it that part chlorosilane be precipitated by condensation;Specifically, by upper The sample collection bag stated, which is placed in the refrigerants such as liquid nitrogen, carries out condensation process, so that its temperature is dropped to -40 DEG C or so, polysilicon tail gas In chlorosilane can be precipitated.It should be noted that can be defeated by pipeline 2 by the polysilicon tail gas in it in sample collection bag During being sent to collecting bag, condensation process is carried out to polysilicon tail gas.
It absorbs, by the polysilicon tail gas after condensation process by adsorbent, continues to be adsorbed and removed remaining chlorine silicon in tail gas Alkane.Specifically, continuing through adsorbent through the above-mentioned polysilicon tail gas by condensation process and part chlorosilane of going out, adsorb Agent continues to absorb remaining chlorosilane in it.Adsorbent is usually NaOH particle.The polysilicon of processing is absorbed by NaOH particle Tail gas, in chlorosilane be substantially achieved removing or content is extremely low, to the detection device of later period measurement trace hydrogen phosphide Corrosion and damage is extremely low.
Finally, collecting the polysilicon tail gas by absorbing processing.Specifically, collecting processed polysilicon using collecting bag Tail gas.
Embodiment 2
Based on inventive concept same as Example 1, the embodiment provides in above-mentioned removal polysilicon tail gas A kind of application mode of the method for chlorosilane, polysilicon tail gas is after this method is handled, for measuring trace phosphatization in tail gas The content of hydrogen.Specifically, being detected with flame photometric detector to Phosphine content in polysilicon tail gas.
Embodiment 3
As shown in Figure 1, the embodiment provides a kind of removal is more based on inventive concept same as Example 1 The device of chlorosilane in crystal silicon tail gas, including sampling assemble 1 and deep cooling mechanism 3;It is connected with pipeline 2 on the sampling assemble 1, manages Road 2 passes through deep cooling mechanism 3 and is connected with absorbent module 6 after cooling, is filled with adsorbent in absorbent module 6;The absorbent module 6 With outlet.
Polysilicon tail gas 2 conveying by the road in sampling assemble 1, first passes through 3 cooling treatment of deep cooling mechanism, is condensed out part Chlorosilane adsorbs remaining chlorosilane using absorbent module 6, is finally discharged from the outlet of absorbent module 6.
The outlet of absorbent module 6 is connected with collection assembly 8, and aspiration pump 7 is connected between collection assembly 8 and absorbent module 6; The sampling assemble 1 is sampling bag, and collection assembly 8 is collecting bag.Aspiration pump 7 can aspirate the polysilicon tail gas in sampling bag defeated It is sent in collecting bag.Common micro-suction pump 7 can meet using purpose.Micro-suction pump 7 (also known as minipump) Model ZQ370-02PM, voltage rating DC 12V, flow 2L/min, manufacturer is the really suitable limited public affairs of electronics of Dongguan City Department.
Absorbent module 6 is accommodating cylinder, and one end is import, and the other end is outlet;Adsorbent elements of filling are in it NaOH。
Polysilicon tail gas is passed through from the import of absorbent module 6, is discharged after NaOH adsorption treatment, and from its outlet.It inhales Attached dose is usually NaOH particle.
Deep cooling mechanism 3 is cold-trap device, and with refrigerating chamber, refrigerant, fixed cladding outside refrigerating chamber are loaded in refrigerating chamber There is heat insulation layer 5.
It further include the condenser pipe 4 for being connected on pipeline 2, and being set between sampling assemble 1 and absorbent module 6, condenser pipe 4 is set In in deep cooling mechanism 3.
Condenser pipe 4 is stainless steel material, diameter 6mm, long 20cm.Appropriate liquid nitrogen is added in deep cooling mechanism 3, condenser pipe 4 is set Enter in liquid nitrogen, when the temperature of polysilicon tail gas drops to -40 DEG C, in chlorosilane can be precipitated.
It further include the thermo detector in deep cooling mechanism 3, thermometric is calculated as temperature sensor.
Thermo detector is used to detect the temperature of condensation polysilicon tail gas, common thermocouple temperature sensor may be selected, this is Commercially available common temperature measurement tool, range is preferably at -200~200 DEG C.
Embodiment 4
Based on inventive concept same as Example 3, the embodiment provides in above-mentioned removal polysilicon tail gas A kind of application mode of the device of chlorosilane, polysilicon tail gas is after device processing, for measuring trace phosphatization in tail gas The content of hydrogen.Specifically, being detected with flame photometric detector to Phosphine content in polysilicon tail gas.
Finally, it should be noted that the above various embodiments is only preferred embodiment of the invention to illustrate skill of the invention Art scheme, rather than its limitations, when being less limitation the scope of the patents of the invention;Although referring to foregoing embodiments to the present invention It is described in detail, those skilled in the art should understand that: it still can be to recorded in foregoing embodiments Technical solution modify, or equivalent substitution of some or all of the technical features;And these modification or Replacement, the range for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution;In addition, by of the invention Technical solution it is direct or indirect be used in other related technical areas, similarly include in scope of patent protection of the invention It is interior.

Claims (10)

1. a kind of method of chlorosilane in removal polysilicon tail gas, which is characterized in that including following treatment process:
It collects, collects polysilicon tail gas;
The polysilicon tail gas being collected into is carried out condensation process, makes it that part chlorosilane be precipitated by condensation;
It absorbs, by the polysilicon tail gas after condensation process by adsorbent, continues to be adsorbed and removed remaining chlorosilane in tail gas.
2. the method for chlorosilane in removal polysilicon tail gas according to claim 1, which is characterized in that finally, collecting warp Cross the polysilicon tail gas for absorbing processing.
3. the method for chlorosilane in the removal polysilicon tail gas as described in any in claim 1,2, polysilicon tail gas is by being somebody's turn to do After method processing, for measuring the content of trace hydrogen phosphide in tail gas.
4. the device of chlorosilane in a kind of removal polysilicon tail gas, which is characterized in that including sampling assemble and deep cooling mechanism;It is described Pipeline is connected on sampling assemble, pipeline passes through deep cooling mechanism and is connected with absorbent module after cooling, filling in absorbent module There is adsorbent;The absorbent module has outlet.
5. the device of chlorosilane in removal polysilicon tail gas according to claim 4, which is characterized in that the absorbent module Outlet be connected with collection assembly, aspiration pump is connected between collection assembly and absorbent module;The sampling assemble is sampling bag, Collection assembly is collecting bag.
6. the device of chlorosilane in removal polysilicon tail gas according to claim 4, which is characterized in that the absorbent module To accommodate cylinder, one end is import, and the other end is outlet;The adsorbent elements filled in it are NaOH.
7. the device of chlorosilane in removal polysilicon tail gas according to claim 4, which is characterized in that the deep cooling mechanism Refrigerant is loaded in refrigerating chamber with refrigerating chamber for cold-trap device, fixation is coated with heat insulation layer outside refrigerating chamber.
8. the device of chlorosilane in removal polysilicon tail gas according to claim 4, which is characterized in that further include being connected to On pipeline, and the condenser pipe being set between sampling assemble and absorbent module, condenser pipe are placed in deep cooling mechanism.
9. the device of chlorosilane in removal polysilicon tail gas according to claim 4, which is characterized in that further include being set to deeply Cold thermo detector within the organization, thermometric are calculated as temperature sensor.
10. the device of chlorosilane in the removal polysilicon tail gas as described in any in claim 4-9, polysilicon tail gas is by being somebody's turn to do After device processing, for measuring the content of trace hydrogen phosphide in tail gas.
CN201811594353.3A 2018-12-25 2018-12-25 The method, apparatus and application of chlorosilane in a kind of removal polysilicon tail gas Pending CN109569262A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110918001A (en) * 2019-12-13 2020-03-27 亚洲硅业(青海)股份有限公司 Method and apparatus for separating high boiling substance

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102009955A (en) * 2010-12-23 2011-04-13 江西嘉柏新材料有限公司 Method for recovering hydrogen chloride from trichlorosilane tail gas
CN202070281U (en) * 2011-03-14 2011-12-14 蒋超 Tail gas recovery and purification treatment device for polycrystalline silicon production line
CN204536066U (en) * 2015-04-22 2015-08-05 陕西天宏硅材料有限责任公司 For the rapid sampling attachment of containing chlorosilane in polysilicon production waste gas
CN106621757A (en) * 2017-02-21 2017-05-10 德山化工(浙江)有限公司 Recovery treatment device and treatment method of chlorosilane analysis waste gases
CN106644660A (en) * 2016-11-21 2017-05-10 天津大学 A sample pretreatment device and method for measuring the trace phosphorous impurity content in chlorosilane
CN206535403U (en) * 2017-02-21 2017-10-03 德山化工(浙江)有限公司 Chlorosilane analyzes waste gas recovery processing unit

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102009955A (en) * 2010-12-23 2011-04-13 江西嘉柏新材料有限公司 Method for recovering hydrogen chloride from trichlorosilane tail gas
CN202070281U (en) * 2011-03-14 2011-12-14 蒋超 Tail gas recovery and purification treatment device for polycrystalline silicon production line
CN204536066U (en) * 2015-04-22 2015-08-05 陕西天宏硅材料有限责任公司 For the rapid sampling attachment of containing chlorosilane in polysilicon production waste gas
CN106644660A (en) * 2016-11-21 2017-05-10 天津大学 A sample pretreatment device and method for measuring the trace phosphorous impurity content in chlorosilane
CN106621757A (en) * 2017-02-21 2017-05-10 德山化工(浙江)有限公司 Recovery treatment device and treatment method of chlorosilane analysis waste gases
CN206535403U (en) * 2017-02-21 2017-10-03 德山化工(浙江)有限公司 Chlorosilane analyzes waste gas recovery processing unit

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110918001A (en) * 2019-12-13 2020-03-27 亚洲硅业(青海)股份有限公司 Method and apparatus for separating high boiling substance

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