CN112113810A - High-pressure oxidation treatment device for organic samples - Google Patents
High-pressure oxidation treatment device for organic samples Download PDFInfo
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- CN112113810A CN112113810A CN202010800748.5A CN202010800748A CN112113810A CN 112113810 A CN112113810 A CN 112113810A CN 202010800748 A CN202010800748 A CN 202010800748A CN 112113810 A CN112113810 A CN 112113810A
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- reactor
- oxidation treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention belongs to the technical field of elemental analysis, and relates to a high-pressure oxidation treatment device for an organic sample. The device comprises an oxygen cylinder, an air inlet pipeline, a reactor and an ignition resistance wire, wherein oxygen stored in the oxygen cylinder is introduced into the sealed reactor through the air inlet pipeline, and after the ignition resistance wire in the reactor is ignited, the organic sample put into the reactor is subjected to high-pressure oxidation treatment. The high-pressure oxidation treatment device for the organic sample can be used for treating the organic sample for analyzing the metal elements or the radionuclides at a higher speed, in a shorter time and with less acid consumption.
Description
Technical Field
The invention belongs to the technical field of elemental analysis, and relates to a high-pressure oxidation treatment device for an organic sample.
Background
In order to analyze metal elements or radionuclides in organic samples, ashing oxidation treatment is generally required for the samples. The ashing oxidation treatment of the organic sample generally includes a heating oxidation treatment, a wet oxidation treatment, and the like.
In the open sample heat oxidation process, if the loss of the organic sample (heavy metal or radionuclide) to be analyzed is small and the loss amount can be determined by an auxiliary method, the organic sample can be treated by the open heat oxidation method. When the organic substance in the sample and the analyte exist in the form of an organic complex, or the analyte is easily volatilized, or the sample component is easily volatilized, the open heating oxidation method cannot be used. For example: polonium is easy to volatilize above 100 ℃, polonium and organic matter can be complexed, and thus polonium in the organic sample cannot be subjected to open-type heating oxidation treatment; analysis of natural radionuclides in samples such as petroleum, natural gas, asphalt and the like needs to consider the influence of volatilization.
The wet oxidation treatment is mainly an open oxidation treatment. In the open oxidation treatment, a reagent such as an oxidizing agent is added to a sample in a certain temperature range by controlling the temperature of a heating device (e.g., an electric hot plate). Open type oxidation treatment is to open type oxidize the sample by controlling the temperature, because the treatment temperature is relatively low, the sample needs to be repeatedly treated by concentrated acid (nitric acid, hydrochloric acid, perchloric acid) and hydrogen peroxide, in the treatment, because the ignition point of perchloric acid is relatively low, the temperature must be strictly controlled, otherwise, ignition can occur, and the experiment fails. In addition, in the open oxidation treatment, the sample needs to be repeatedly treated, so that a large amount of acid is consumed, and much time is consumed.
Disclosure of Invention
The invention aims to provide a high-pressure oxidation treatment device for organic samples, which can process the organic samples for analyzing metal elements or radionuclides more quickly, in shorter time and with less acid.
To achieve the object, in a basic embodiment, the present invention provides a high-pressure oxidation treatment device for organic samples, which comprises an oxygen cylinder, an air inlet pipeline, a reactor and an ignition resistance wire,
the oxygen stored in the oxygen cylinder is introduced into the sealed reactor through the air inlet pipeline, and after the ignition resistance wire in the reactor is ignited, the organic sample put into the reactor is subjected to high-pressure oxidation treatment.
In a preferred embodiment, the present invention provides an apparatus for high-pressure oxidation treatment of an organic sample, wherein the apparatus further comprises a pressure reducing valve, a safety valve, and an air inlet valve, which are sequentially disposed on the air inlet line.
In a preferred embodiment, the present invention provides an apparatus for high pressure oxidative treatment of an organic sample, wherein said apparatus further comprises a pressure gauge for measuring the pressure in said reactor.
In a preferred embodiment, the present invention provides an apparatus for high pressure oxidation treatment of organic samples, wherein the apparatus further comprises a gas outlet pipeline connected to the reactor and a gas outlet valve disposed on the gas outlet pipeline.
In a preferred embodiment, the present invention provides an apparatus for high pressure oxidative treatment of an organic sample, wherein said apparatus further comprises a quartz cup disposed in said reactor below and in close proximity to said ignition resistance wire for placement of said organic sample.
In a preferred embodiment, the present invention provides an apparatus for high pressure oxidation treatment of organic samples, wherein said apparatus further comprises a flange and a screw, and said reactor is sealed with said flange and said screw at the top.
In a preferred embodiment, the invention provides a high-pressure oxidation treatment device for organic samples, wherein the device further comprises a low-voltage power supply which is arranged outside the reactor and connected with the ignition resistance wire, and the low-voltage power supply is used for driving the ignition resistance wire to ignite the samples.
The invention has the advantages that the high-pressure oxidation treatment device for the organic sample can be used for treating the organic sample for analyzing the metal elements or the radionuclides at higher speed, in shorter time and with less acid consumption.
In the analysis of metal elements or radionuclides, the composition and structure of an organic sample are different from those of an inorganic sample, so that the ashing and oxidation treatment of the organic sample by using a strong oxidant is slow in treatment speed and needs repeated treatment, so that the consumption of acid is large and the time consumption is long. The high-pressure oxidation treatment device provided by the invention is used for treating the organic sample, the treatment capacity of the sample at one time is twice of that of the ashing oxidation treatment method of the strong oxidant, the reagents such as acid are saved by more than 80%, the time is saved by more than 80%, and various organic samples including flammable and explosive organic samples such as crude oil, gasoline, asphalt, latex and the like can be treated.
Drawings
FIG. 1 is a schematic view showing the constitution of an exemplary high-pressure oxidation apparatus for treating an organic sample according to the present invention.
Detailed Description
The composition structure of an exemplary high-pressure oxidation treatment device for organic samples of the invention is shown in fig. 1, and comprises an oxygen cylinder 1, an air inlet pipeline, an air outlet pipeline, a pressure reducing valve 2, a safety valve 3, an air inlet valve 4, a pressure gauge 5, an air outlet valve 6, a screw 7, a low-voltage power supply 8(1-12 volts), a flange 9, a reactor 10, an ignition resistance wire 11 and a quartz cup 12.
Oxygen stored in the oxygen cylinder 1 is introduced into a sealed reactor 10 through an air inlet pipeline (the reactor 10 is sealed with a screw 7 through a flange 9 positioned at the top), after an ignition resistance wire 11 in the reactor 10 is ignited (the ignition resistance wire 11 is driven by a low-voltage power supply 8 which is arranged outside the reactor 10 and connected with the ignition resistance wire 11 to ignite a sample), an organic sample in a quartz cup 12 (the quartz cup 12 is positioned below the ignition resistance wire 11 and is close to the ignition resistance wire 11) placed in the reactor 10 is subjected to high-pressure oxidation treatment.
The air inlet pipeline is sequentially provided with a pressure reducing valve 2, a safety valve 3 and an air inlet valve 4.
The pressure gauge 5 is used to measure the pressure in the reactor 10.
An air outlet pipeline connected with the reactor 10 is provided with an air outlet valve 6.
The device utilizes sufficient oxygen in a high-pressure (30-100 atmospheric pressures) reactor, ignites organic matters through an ignition device, enables the organic matters to be fully combusted in the reactor, and collects gas and combustion residues for further analysis.
The operation method of the above-described exemplary high-pressure oxidation treatment apparatus for organic samples of the present invention is as follows.
Putting an organic sample into a quartz cup 12, covering a flange 9, screwing a screw 7, closing an air outlet valve 6, closing a safety valve 3, opening an air inlet valve 4, opening an oxygen cylinder 1 and adjusting a pressure reducing valve 2. When the pressure gauge 5 displays that the pressure reaches the preset requirement, the oxygen cylinder 1 is closed, the air inlet valve 4 is closed, and the safety valve 3 is opened. When the safety valve 3 does not exhaust any more, the safety valve 3 is closed, the pressure reducing valve 2 is closed, the low-voltage power supply 8 is opened, and the ignition resistance wire 11 generates heat to ignite a sample. When the pressure gauge 5 shows that the pressure is stable and does not change, the gas outlet valve 6 is opened to collect gas. After the gas collection is completed, the screw 7 is unscrewed, the flange 9 is removed, the quartz cup 12 is taken out, and the combustion residue is collected.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (7)
1. A high-pressure oxidation processing device of an organic sample is characterized in that: the device comprises an oxygen cylinder, an air inlet pipeline, a reactor and an ignition resistance wire,
the oxygen stored in the oxygen cylinder is introduced into the sealed reactor through the air inlet pipeline, and after the ignition resistance wire in the reactor is ignited, the organic sample put into the reactor is subjected to high-pressure oxidation treatment.
2. The apparatus of claim 1, wherein: the device also comprises a pressure reducing valve, a safety valve and an air inlet valve which are arranged on the air inlet pipeline in sequence.
3. The apparatus of claim 1, wherein: the device also comprises a pressure gauge for measuring the pressure in the reactor.
4. The apparatus of claim 1, wherein: the device also comprises an air outlet pipeline connected with the reactor and an air outlet valve arranged on the air outlet pipeline.
5. The apparatus of claim 1, wherein: the device also comprises a quartz cup which is arranged in the reactor, is positioned below the ignition resistance wire and is close to the ignition resistance wire and is used for placing the organic sample.
6. The apparatus of claim 1, wherein: the device also comprises a flange and a screw, and the reactor is sealed by the flange and the screw which are positioned at the top.
7. The apparatus of claim 1, wherein: the device also comprises a low-voltage power supply which is arranged outside the reactor and connected with the ignition resistance wire and is used for driving the ignition resistance wire to ignite the sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010800748.5A CN112113810A (en) | 2020-08-11 | 2020-08-11 | High-pressure oxidation treatment device for organic samples |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010800748.5A CN112113810A (en) | 2020-08-11 | 2020-08-11 | High-pressure oxidation treatment device for organic samples |
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| CN112113810A true CN112113810A (en) | 2020-12-22 |
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| CN202010800748.5A Pending CN112113810A (en) | 2020-08-11 | 2020-08-11 | High-pressure oxidation treatment device for organic samples |
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2020
- 2020-08-11 CN CN202010800748.5A patent/CN112113810A/en active Pending
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| US20040047766A1 (en) * | 2002-09-11 | 2004-03-11 | The Regents Of The University Of California | System for trapping and storing gases for subsequent chemical reduction to solids |
| WO2007141718A2 (en) * | 2006-06-09 | 2007-12-13 | Firmenich Sa | Method and apparatus for providing samples of volatiles to analysis using a multi-port valve and cryo-modulation |
| CN102713557A (en) * | 2009-11-03 | 2012-10-03 | 7685297加拿大有限公司 | Systems and methods for preparing samples for chemical analysis |
| CN201664413U (en) * | 2010-03-30 | 2010-12-08 | 赵卫东 | Automatic temperature-control smokeless moxibustion instrument |
| CN201773515U (en) * | 2010-07-21 | 2011-03-23 | 黄本东 | Teaching tool for physical experiments |
| CN202584512U (en) * | 2012-04-12 | 2012-12-05 | 雷海平 | Short circuit and fuse effect experimental device |
| CN205582885U (en) * | 2016-03-31 | 2016-09-14 | 东华理工大学 | Supplementary surperficial desorption ordinary pressure chemical ionization mass spectrum device of gas heat and ionization source thereof |
| CN105973666A (en) * | 2016-05-04 | 2016-09-28 | 新奥科技发展有限公司 | Chlorine and sulfur extraction and determination method and apparatus thereof |
| CN110848966A (en) * | 2019-11-04 | 2020-02-28 | 湖南鑫长星机械设备有限公司 | Environment-friendly boiler |
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Application publication date: 20201222 |