CN220207552U - Germanium dioxide analysis and detection reaction device - Google Patents
Germanium dioxide analysis and detection reaction device Download PDFInfo
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- CN220207552U CN220207552U CN202320895220.XU CN202320895220U CN220207552U CN 220207552 U CN220207552 U CN 220207552U CN 202320895220 U CN202320895220 U CN 202320895220U CN 220207552 U CN220207552 U CN 220207552U
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- Prior art keywords
- absorption
- germanium dioxide
- pipe
- gas
- absorption bottle
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- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229940119177 germanium dioxide Drugs 0.000 title claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 41
- 238000001514 detection method Methods 0.000 title claims abstract description 21
- 238000004458 analytical method Methods 0.000 title claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 67
- 230000001681 protective effect Effects 0.000 claims abstract description 55
- 239000007789 gas Substances 0.000 claims abstract description 53
- 238000005485 electric heating Methods 0.000 claims abstract description 17
- 239000012670 alkaline solution Substances 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- 229910052757 nitrogen Inorganic materials 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 22
- 239000010453 quartz Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000002474 experimental method Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- 239000012495 reaction gas Substances 0.000 abstract description 3
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical group Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 239000003517 fume Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- BAEIUCDXXHCJQG-UHFFFAOYSA-N germanium;hydrate Chemical compound O.[Ge] BAEIUCDXXHCJQG-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052729 chemical element Inorganic materials 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- FNIHDXPFFIOGKL-UHFFFAOYSA-N disodium;dioxido(oxo)germane Chemical compound [Na+].[Na+].[O-][Ge]([O-])=O FNIHDXPFFIOGKL-UHFFFAOYSA-N 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model relates to a germanium dioxide analysis detection reaction device, and belongs to the field of analysis detection. The reaction device comprises a reaction main body device and an absorption device; the reaction main body device comprises an electric heating plate, a beaker, a protective cover, an air inlet pipe, an elbow pipe and a protective gas device, and the absorption device comprises an absorption bottle filled with alkaline solution and an air outlet pipe; the beaker is placed on the electric hot plate, and in electric hot plate and the beaker were placed the safety cover, safety cover one side set up the intake pipe, and the intake pipe is connected with the shielding gas device, lets in shielding gas, and the opposite side of safety cover sets up the return bend of gas outlet, and the return bend is connected with the absorption bottle, and the absorption bottle still is provided with the outlet duct. The reaction device can avoid the pollution of the environment to the sample to a great extent in the experimental process of dissolving germanium dioxide, improve the detection accuracy and ensure the purity of the germanium dioxide sample; the reaction gas generated in the experiment is absorbed, so that the corrosion of experimental equipment and the pollution to the environment are avoided.
Description
Technical Field
The utility model relates to a germanium dioxide analysis detection reaction device, which belongs to the field of analysis detection, in particular to the field of metallurgical analysis detection.
Background
Germanium dioxide is an inorganic compound with a molecular formula of GeO 2 Is a germanium dioxide. Germanium dioxide is mainly widely used for preparing fluorescent powder, catalysts, infrared optics and electronic devices, and high-purity germanium dioxide is mainly used for preparing high-purity metal germanium. Different application fields have different requirements on the purity of germanium dioxide.
According to the product standard GB/T11069 of germanium dioxide, the germanium dioxide brands are two, namely 5N germanium dioxide and 6N germanium dioxide, and the product standard clearly specifies the requirements of chemical components, granularity and electrochemical performance of the two brands of germanium dioxide. Of these, the most important is the requirement of the chemical composition, which is the most important factor in determining the purity of high purity germanium dioxide. GB/T11069 requires the determination of the content of twelve chemical elements in germanium dioxide, each As, fe, cu, ni, pb, ca, mg, si, co, in, zn, al. Because the purity of germanium dioxide is higher, the content of twelve chemical elements is lower, the chemical components in the germanium dioxide are mainly determined by a separation and enrichment method, after the germanium dioxide is heated and decomposed by pure hydrochloric acid, the germanium and the hydrochloric acid are evaporated and removed in a germanium tetrachloride form, and after residues are dissolved by nitric acid, the chemical components are determined by an inductively coupled plasma mass spectrometer.
In the process of analyzing and detecting germanium dioxide, the experimental process of preparing the analysis test solution in the early stage is mainly divided into two steps. The first step is that germanium dioxide reacts with hydrochloric acid in a heating state to generate volatile germanium tetrachloride and water; and in the second step, germanium tetrachloride volatilizes, and the matrix is separated and impurities are enriched. Since germanium dioxide has a relatively high purity, the content of twelve impurity elements is relatively low, and is 0.x or 0.0x mug/g. Contamination in the whole experimental process can seriously affect the content of impurity elements, so that the avoidance of contamination is the most important link, and the requirements on the experimental environment and the cleaning degree of vessels are higher. In the whole analysis and detection process, the two steps of dissolving germanium dioxide samples and volatilizing the matrix are easier to introduce contamination, and if no protective measures are added, experiments are directly carried out in a fume hood, and the experiment environment can pollute the samples so as to influence the purity of the germanium dioxide. The germanium tetrachloride which is easy to volatilize is a chemical product with strong corrosiveness, and can corrode chemical experiment devices such as metal, plastic and the like. Experiments are carried out in a fume hood, if no protective measures are added, the fume hood and the fume duct are corroded for a long time, and certain damage is caused.
Disclosure of Invention
Aiming at the possible problems in the experimental process, the utility model provides an experimental device for analyzing and detecting germanium dioxide, which is environment-friendly and can avoid environmental pollution. The experimental reaction device is provided with a protective cover around the germanium dioxide sample, so that the environmental pollution to the sample is prevented; the gas path inlet pipeline is additionally arranged on one side of the protective cover, protective gas nitrogen is introduced into the protective cover, the gas outlet pipeline is arranged on the other side of the protective cover, and the nitrogen and gas generated by reaction enter the gas absorption device to prevent the experiment from generating strong corrosive gas germanium tetrachloride to discharge and corrode experimental apparatus equipment and pollute the environment. The reaction device can avoid the pollution of the environment to the sample to a great extent in the germanium dioxide experiment process, improve the detection accuracy and ensure the purity of the germanium dioxide sample; the reaction gas generated in the experiment is absorbed, so that the corrosion of experimental equipment and the pollution to the environment are avoided.
In order to solve the technical problems, the utility model is realized by the following technical scheme:
the germanium dioxide analysis and detection reaction device comprises a reaction main body device and an absorption device; the reaction main body device comprises an electric heating plate, a beaker, a protective cover, an air inlet pipe, an elbow pipe and a protective gas device, and the absorption device comprises an absorption bottle filled with alkaline solution and an air outlet pipe; the beaker is placed on the electric heating plate, the electric heating plate and the beaker are placed in the protective cover, an air inlet pipe is arranged on one side of the protective cover, the air inlet pipe is connected with the protective gas device, protective gas is introduced, an elbow pipe of a gas outlet is arranged on the other side of the protective cover, the elbow pipe is connected with the absorption bottle, and an air outlet pipe is further arranged on the absorption bottle.
The electric heating plate is a graphite electric heating plate.
The beaker and the protective cover are made of quartz materials with corrosion resistance and high cleanliness.
The protective cover is made of quartz. The two sides of the protective cover are provided with air passage pipes. One side is provided with a protective gas inlet pipe, nitrogen is introduced into the pipeline, and the nitrogen is introduced into the protective cover. The other side is provided with a protective gas outlet bent pipe which is connected into the absorption bottle. The germanium dioxide is heated to react with hydrochloric acid to generate germanium tetrachloride and water. Under the condition that graphite plate heats, germanium tetrachloride and water are heated and evaporated, steam volatilizes to the top of the quartz cover, and the steam is condensed on the inner wall, and if nitrogen is not added at this moment, liquid drops condensed on the inner wall of the cover drop down along with the growth of experimental time, and the sample can be polluted in the beaker where the sample is located with great probability, so that the error of experimental results is caused. If after the nitrogen is introduced, the evaporated mixed gas can be discharged into the absorption bottle along with the passing of the nitrogen from the air outlet pipe on the left side of the quartz cover, and the steam is completely discharged, so that the steam cannot be condensed on the inner wall of the quartz cover, and the possibility of the sample being polluted by the steam dripping is further reduced.
On the protective cover, the height of the air inlet pipe is lower than that of the bent pipe, so that the evaporated germanium tetrachloride gas is taken away by nitrogen.
The protective gas is nitrogen, the purity of the nitrogen is 5N-6N, and the higher the purity is, the lower the impurity element content in the nitrogen is, so that the germanium dioxide sample is not polluted.
The absorption device comprises an absorption bottle, a plug, an air outlet pipe, absorption liquid and the like, wherein the absorption bottle is sealed by the plug, the air outlet pipe and the bent pipe extend into the absorption bottle through holes formed in the plug, and alkaline absorption liquid is filled in the absorption bottle. The bent pipe is longer, the air outlet pipe is shorter, the bent pipe is inserted below the liquid level of the absorption liquid, is close to the bottom but does not contact the bottom of the absorption bottle, and the tail end of the air outlet pipe is above the liquid level of the absorption liquid.
The absorption liquid is sodium hydroxide solution with the volume fraction of 5-10%.
The air inlet pipe of the absorption bottle and the air outlet pipe of the protective cover are the same bent pipe, the air inlet bent pipe of the absorption bottle is inserted below the liquid level of the dilute sodium hydroxide, and the air outlet pipe of the absorption bottle is inserted above the liquid level. Germanium tetrachloride gas enters the absorption bottle from the protective cover along with nitrogen through the bent pipe and is subjected to chemical reaction when meeting alkali, and GeCl 4 +6NaOH=4NaCl+Na 2 GeO 3 +3H 2 O, forming non-volatile sodium germanate, sodium chloride and water. And nitrogen which does not react with alkali is discharged through an air outlet pipe of the absorption bottle. The strong corrosive germanium tetrachloride generated by the chemical reaction in the protective cover is absorbed by the alkali solution, so that the experimental equipment is prevented from being corroded, and the environment is prevented from being polluted.
The utility model has the following beneficial effects:
1. the experimental reaction device is characterized in that a protective cover is arranged around a germanium dioxide sample, and the protective cover is arranged on a graphite plate to protect a quartz beaker and prevent the sample from being polluted by the environment; the detection accuracy is improved, and the purity of the germanium dioxide sample is ensured.
2. The experimental reaction device is characterized in that a gas path inlet pipeline is additionally arranged on one side of a protective cover, protective gas high-purity nitrogen is introduced into the protective cover, and a gas outlet elbow is arranged on the other side of the protective cover. An orderly gas flow is formed in the protective cover, and volatilized germanium tetrachloride gas cannot condense at the top of the inner side of the protective cover. The method reduces the dripping of the impurity element into a quartz beaker for reaction of germanium dioxide samples, ensures the accuracy of the impurity element and improves the accuracy of the oxidation or purity.
3. The nitrogen in the protecting cover and germanium tetrachloride generated by the reaction in the experimental reaction device enter the gas absorption device, so that the experiment is prevented from generating strong corrosive gas germanium tetrachloride to discharge and corrode experimental apparatus equipment and pollute the environment. The reaction device enables the experimental generated reaction highly corrosive gas to be absorbed, and avoids corroding experimental equipment and polluting the environment.
Drawings
FIG. 1 is a schematic diagram of a germanium dioxide reaction apparatus according to the present utility model.
The main reference numerals illustrate:
1-an electric heating plate; 2-beaker; 3-protecting cover; 4-an air inlet pipe; 5-bending the pipe; 6-an air outlet pipe; 7-an absorption bottle; 8-a shielding gas device.
Detailed Description
The technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model.
Referring to fig. 1, the present utility model is a germanium dioxide reaction apparatus, which includes a reaction main body apparatus and an absorption apparatus. The reaction main body device comprises an electric heating plate 1, a beaker 2, a protective cover 3, an air inlet pipe 4, an elbow pipe 5 and a protective gas device 8. The absorption device comprises an absorption bottle 7 filled with alkaline solution and an air outlet pipe 6. Wherein, safety cover 3 one side sets up intake pipe 4, intake pipe 4 and shielding gas device 8, lets in shielding gas, and the opposite side of safety cover 3 sets up the return bend 5 of gas outlet, and return bend 5 is connected with absorption bottle 7, and absorption bottle 7 still is provided with outlet duct 6. A series of beakers 2 are arranged on the electric heating plate 1, and a protective cover 3 is covered outside the electric heating plate 1 and the beakers 2.
The electric heating plate 1 is a graphite electric heating plate. The electric heating plate 1 is made of graphite material and has the characteristics of corrosion resistance, high temperature resistance, uniform heating and the like. In the reaction process of the germanium dioxide sample and the concentrated hydrochloric acid, strong corrosive germanium tetrachloride can be generated, and the graphite electric heating plate can prevent the germanium tetrachloride from corroding the surface of the heating plate 1.
Beaker 2 is a quartz beaker. The quartz material has the characteristics of corrosion resistance and high cleanliness. Quartz beakers are generally used for samples with relatively high purity and low impurity element content. The method is suitable for analysis of high-purity germanium dioxide samples.
The protective cover 3 is a cover made of quartz, and the left side and the right side are provided with air channel pipes. The right side is provided with a protective gas inlet pipe 4, nitrogen is introduced into the pipeline, and the nitrogen is introduced into the protective cover 3. The left side is provided with a shielding gas outlet elbow 5, and the outlet elbow 5 is connected into an absorption bottle 7.
On the protective cover 3, the height of the air inlet pipe 4 is slightly lower than that of the outlet elbow pipe 5, so that the evaporated germanium tetrachloride gas can be taken away by nitrogen. The bent pipe 5 connects the protective cover 3 and the absorption bottle 7.
The protective gas is nitrogen, the purity of the nitrogen is 5N-6N, and the higher the purity is, the lower the impurity element content in the nitrogen is, so that the germanium dioxide sample is not polluted. The shielding gas device 8 may be a nitrogen cylinder.
The absorption device comprises an absorption bottle 7, a plug, an air outlet pipe 6 and absorption liquid, wherein the plug is arranged at the sealing part of the absorption bottle 7, and the air outlet pipe 6 and the bent pipe 5 are respectively arranged in the middle of the plug. One side of the absorption bottle 7 is provided with a gas inlet pipe, namely a gas outlet elbow pipe 5 of the protective cover 3; the other side is provided with a gas outlet pipe 6. The bent pipe 5 is longer, and the air outlet pipe 6 is shorter. The bent pipe 5 is inserted below the liquid level of the dilute sodium hydroxide of the absorption liquid in the absorption bottle 7, and is positioned at a lower position, so that the gas is absorbed by the absorption liquid. The air outlet pipe 6 is inserted into the absorption bottle 7, and the tail end of the air outlet pipe 6 is above the liquid level, so that nitrogen which is not absorbed by the absorption liquid is ensured to be discharged out of the absorption bottle 7.
The absorption bottle 7 is filled with dilute sodium hydroxide solution, and the concentration is 5-10% by volume. Germanium tetrachloride gas enters an absorption bottle 7 from a protective cover 3 along with nitrogen through a bent pipe 5 and is subjected to chemical reaction when meeting alkali, and GeCl 4 +6NaOH=4NaCl+Na 2 GeO 3 +3H 2 O, forming non-volatile sodium germanate, sodium chloride and water. While nitrogen that does not react with the base is removed through the outlet pipe 6 of the absorption bottle 7.
According to the germanium dioxide analysis detection reaction device, the protective cover is arranged around the germanium dioxide sample, so that the environmental pollution to the sample can be prevented; and a gas path inlet pipeline is additionally arranged on one side of the protective cover, protective gas nitrogen is introduced into the protective cover, and the nitrogen and gas generated by reaction enter the gas absorption device, so that the experiment is prevented from generating strong corrosive gas germanium tetrachloride to discharge and corrode experimental apparatus equipment and pollute the environment. The reaction device can avoid the pollution of the environment to the sample to a great extent in the experimental process of dissolving germanium dioxide, improve the detection accuracy and ensure the purity of the germanium dioxide sample; the reaction gas generated in the experiment is absorbed, so that the corrosion of experimental equipment and the pollution to the environment are avoided.
Claims (7)
1. The germanium dioxide analysis and detection reaction device is characterized in that: comprises a reaction main body device and an absorption device; the reaction main body device comprises an electric heating plate, a beaker, a protective cover, an air inlet pipe, an elbow pipe and a protective gas device, and the absorption device comprises an absorption bottle filled with alkaline solution and an air outlet pipe; the beaker place on the electric plate, electric plate and beaker arrange in the safety cover, safety cover one side set up the intake pipe, intake pipe and protection gas device be connected, let in the protection gas, the opposite side of safety cover set up the return bend of gas outlet, the return bend be connected with the absorption bottle, the absorption bottle still be provided with the outlet duct.
2. The germanium dioxide analysis detection reaction device according to claim 1, wherein: the electric heating plate is a graphite electric heating plate.
3. The germanium dioxide analysis detection reaction device according to claim 1, wherein: the beaker and the protective cover are made of quartz.
4. The germanium dioxide analysis detection reaction device according to claim 1, wherein: on the protective cover, the height of the air inlet pipe is lower than that of the bent pipe.
5. The germanium dioxide analysis detection reaction device according to claim 1, wherein: the protective gas is nitrogen, and the purity of the nitrogen is 5N-6N.
6. The germanium dioxide analysis detection reaction device according to claim 1, wherein: the absorption device comprises an absorption bottle, a plug, an air outlet pipe and absorption liquid, wherein the absorption bottle is sealed by the plug, the air outlet pipe and the bent pipe extend into the absorption bottle through holes formed in the plug, and the absorption liquid is filled in the absorption bottle.
7. The germanium dioxide analysis and detection reaction device according to claim 6, wherein: the bent pipe is inserted below the liquid level of the absorption liquid, and the tail end of the air outlet pipe is above the liquid level of the absorption liquid.
Priority Applications (1)
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CN202320895220.XU CN220207552U (en) | 2023-04-20 | 2023-04-20 | Germanium dioxide analysis and detection reaction device |
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CN202320895220.XU CN220207552U (en) | 2023-04-20 | 2023-04-20 | Germanium dioxide analysis and detection reaction device |
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