CN110075606B - Rapid adsorption filtering device and method for infrared full-automatic oil measurement method - Google Patents
Rapid adsorption filtering device and method for infrared full-automatic oil measurement method Download PDFInfo
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- CN110075606B CN110075606B CN201910378399.XA CN201910378399A CN110075606B CN 110075606 B CN110075606 B CN 110075606B CN 201910378399 A CN201910378399 A CN 201910378399A CN 110075606 B CN110075606 B CN 110075606B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D24/00—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof
- B01D24/02—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof with the filter bed stationary during the filtration
- B01D24/10—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof with the filter bed stationary during the filtration the filtering material being held in a closed container
- B01D24/12—Downward filtration, the filtering material being supported by pervious surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/003—Filters in combination with devices for the removal of liquids
- B01D36/008—Means to filter or treat the separated liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/02—Combinations of filters of different kinds
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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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Abstract
The invention discloses a rapid filtering and adsorbing method for full-automatic oil measurement, which comprises the steps of filtering and adsorbing through a filtering device and an adsorbing device, wherein the filtering and adsorbing device comprises a bottle body, a sample injection air pipe is arranged above the bottle body and comprises an outer pipe and an inner pipe, the inner pipe is made of polytetrafluoroethylene material, the outer pipe is made of silica gel material and is connected with a nitrogen gas source, the inner pipe is a reagent pipeline, the outer pipe is a gas pipeline, and the sample injection air pipe is connected to the inlet of the bottle body through a frosted port; the three-stage filter or the adsorbent with single granularity is sequentially arranged in the bottle body from top to bottom, the bottom of the bottle body is sealed by the sand core filter plate, and the bottom is connected with the oil outlet pipe through the detachable frosted opening.
Description
Technical Field
The invention relates to a quick adsorption and filtration device for full-automatic oil measurement, which is used for adsorption and filtration of water and impurities by a full-automatic infrared oil measurement instrument and belongs to the technical field of pretreatment of analytical chemical samples.
Background
With the development of social economy and the continuous improvement of industrialization level, the water resource pollution condition in the human living environment is increasingly serious and gets more and more attention, the oil pollution from industrial production activities such as oil exploitation and processing, petrochemical industry and the like in the pollution source in the current environmental water occupies a considerable proportion, the detection of the oil content in the environmental water area is also more and more important, and the current detection mainly utilizes an infrared oil detector and adopts an infrared method for detection. In the detection method, anhydrous sodium sulfate is used for isolating impurities and moisture, and a solution of oil and carbon tetrachloride is separated to determine the oil content of the total extract; and removing polar substances such as animal and vegetable oil by using magnesium silicate adsorption, and determining the content of petroleum oil. In conventional testing methods, the prepared anhydrous sodium sulfate or magnesium silicate is typically added to a ground conical flask, shaken, allowed to stand, and filtered. Aiming at the existing full-automatic infrared oil measuring instrument, how to improve the speed and efficiency of adsorption filtration is one of the keys for improving the performance of the instrument. The traditional adsorption filtering device adopts gravity supply, which consumes long time and has low efficiency; or external suction filtration, a suction filter needs to be added, the cost is increased, and the volume of the instrument is increased. Therefore, it is necessary to develop a rapid adsorption filtering device which is suitable for a full-automatic infrared oil level meter and can significantly improve the adsorption filtering speed and efficiency.
Disclosure of Invention
In order to solve the technical problems, the invention provides a rapid adsorption and filtration device and a rapid adsorption and filtration method for an infrared full-automatic oil measurement method.
The complete technical scheme of the invention comprises the following steps:
a full-automatic oil measurement fast filtering and adsorbing method adopts a filtering device and an adsorbing device with similar structures to carry out filtering and adsorbing, wherein the filtering device comprises a bottle body, a sample injection air pipe is arranged above the bottle body and comprises an outer pipe and an inner pipe, the inner pipe is made of polytetrafluoroethylene material, the outer pipe is made of silica gel material and is connected with a nitrogen gas source, the inner pipe is a reagent pipeline, the outer pipe is a gas pipeline, and the sample injection air pipe is connected with the inlet of the bottle body through a frosted port; the first-stage filtering agent, the second-stage filtering agent and the third-stage filtering agent are sequentially arranged in the bottle body from top to bottom, the third-stage filtering agent is respectively composed of anhydrous sodium sulfate with different particle sizes, the bottom of the bottle body is sealed by a sand core filtering plate, the size of the sand core filtering plate is G3-G4, and the bottom is connected with an oil outlet pipe through a detachable frosted opening;
the filtering method comprises the following steps: sample reagent passes through the inner tube and gets into the bottle, open the nitrogen gas air supply simultaneously, make the nitrogen gas of 0.15MPa pressure get into the bottle, sample reagent filters moisture and impurity wherein through the different anhydrous sodium sulfate of tertiary granularity, the granularity of first order anhydrous sodium sulfate is 80 meshes, can filter the great impurity of size and partial moisture fast, the pressure of nitrogen gas is 0.15MPa and control makes the pressure linear decline in this time control bottle, make sample reagent pass through first order anhydrous sodium sulfate relatively rapidly under the effect of gravity and the nitrogen pressure of linear decline. When the sample reagent enters the second-stage anhydrous sodium sulfate, the nitrogen pressure is reduced to 0.12MPa, the granularity of the second-stage anhydrous sodium sulfate is 120 meshes, impurities with small sizes and other water in the sample are filtered, and the nitrogen pressure is continuously controlled to be linearly reduced. When the sample reagent enters the third-stage anhydrous sodium sulfate, the pressure drop of the gas in the bottle is 0.1MPa, the granularity of the third-stage anhydrous sodium sulfate is 200 meshes, the residual small-size impurities are filtered, and the residual small-size impurities flow out through the oil outlet pipe after the filtration is finished.
The adsorption device comprises a bottle body, wherein a sample injection air pipe is arranged above the bottle body and comprises an outer pipe and an inner pipe, the inner pipe is made of polytetrafluoroethylene materials, the outer pipe is made of silica gel materials and connected with a nitrogen gas source, the inner pipe is a reagent pipeline, the outer pipe is a gas pipeline, and the sample injection air pipe is connected to the inlet of the bottle body through a frosted opening; magnesium silicate is arranged in the bottle body, the bottom of the bottle body is sealed by a sand core filter plate, the size of the sand core filter plate is G3-G4, and the bottom is connected with an oil outlet pipe through a detachable frosted opening;
the adsorption method comprises the following steps: the sample reagent enters the bottle body through the inner tube, meanwhile, a nitrogen gas source is started, nitrogen gas with the pressure of 0.1MPa enters the bottle body, the sample reagent adsorbs polar substances such as animal and vegetable oil through magnesium silicate, the granularity of the magnesium silicate is 200 meshes, the pressure of the nitrogen gas in the bottle is controlled to be 0.1MPa, the pressure is linearly reduced, the sample reagent passes through the magnesium silicate under the action of gravity and the linearly reduced nitrogen gas pressure, the nitrogen gas pressure is reduced to 0.02MPa when the sample reagent reaches the bottom of the bottle body, and the sample reagent flows out through the oil outlet pipe after adsorption is completed.
Compared with the prior art, the invention has the advantages that:
1. the sample (gas) inlet pipe is internally and externally provided with two layers, the inner pipe is made of hydrophobic polytetrafluoroethylene materials, non-specific adsorption to a target object is avoided, and the outer pipe is made of a silicone tube and can protect the inner pipe.
2. A small amount of nitrogen with pressure is introduced into the outer pipe, and the filter is properly pressurized, so that the filtering speed is accelerated; in addition, the antibacterial agent also plays a role in inhibiting the growth of bacteria.
3. The interfaces at the two ends of the filter are frosted openings, so that the filter can be detached, the adsorbent can be conveniently replaced, and the leakage and volatilization of carbon tetrachloride can be prevented.
4. By adopting a multi-stage filtration mode, oil can rapidly pass through filtering agents at all stages, the efficiency is improved, and the filtering efficiency and the effect are taken into consideration by linearly reduced nitrogen pressure.
Drawings
FIG. 1 is a schematic view of a rapid adsorption filtration device for an infrared full-automatic oil measurement method.
In the figure: 1-bottle body, 2-outer tube, 3-inner tube, 4-frosted opening, 5-first-stage filtering agent, 6-second-stage filtering agent, 7-third-stage filtering agent, 8-sand core and 9-oil outlet pipe.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
The utility model provides a full-automatic quick adsorption filtration device who surveys oil, includes similar filter equipment and adsorption equipment of structure to filter equipment is the example, and its structure includes bottle 1, and the bottle top is equipped with advances the trachea, should advance the trachea and include outer tube 2 and inner tube 3, and the inner tube is polytetrafluoroethylene material, and the outer tube is silica gel material to connect the nitrogen gas source, and the inner tube is the reagent pipeline, and the outer tube is the gas pipeline, advances the trachea and passes through dull polish 4 connections in bottle entrance.
The interior of the bottle body is provided with a multistage adsorption material which specifically comprises a first-stage filtering agent 5, a second-stage filtering agent 6 and a third-stage filtering agent 7, wherein the third-stage filtering agent is composed of anhydrous sodium sulfate with different particle sizes, the bottom of the bottle body is sealed by a sand core filter plate 8, the sand core filter plate is in specification G3-G4, and the bottom of the bottle body is connected with an oil outlet pipe 9 through a frosted opening. The dull polish mouth can be dismantled, prevents the leakage and the volatilization of adsorption process sample.
The method for filtering the sample reagent by adopting the full-automatic oil measurement quick adsorption filtering device disclosed by the invention comprises the following steps:
sample reagent passes through the inner tube and gets into the bottle, open the nitrogen gas air supply simultaneously, make the nitrogen gas of 0.15MPa pressure get into the bottle, sample reagent filters moisture and impurity wherein through the different anhydrous sodium sulfate of tertiary granularity, the granularity of first order anhydrous sodium sulfate is 80 meshes, can filter the great impurity of size and partial moisture fast, the pressure of nitrogen gas is 0.15MPa and control makes the pressure linear decline in this time control bottle, make sample reagent pass through first order anhydrous sodium sulfate relatively rapidly under the effect of gravity and the nitrogen pressure of linear decline. When the sample reagent enters the second-stage anhydrous sodium sulfate, the nitrogen pressure is reduced to 0.12MPa, the granularity of the second-stage anhydrous sodium sulfate is 120 meshes, impurities with small sizes and other water in the sample are filtered, and the nitrogen pressure is continuously controlled to be linearly reduced. When the sample reagent enters the third-stage anhydrous sodium sulfate, the pressure drop of the gas in the bottle is 0.1MPa, the granularity of the third-stage anhydrous sodium sulfate is 200 meshes, the residual small-size impurities are filtered, and the residual small-size impurities flow out through the oil outlet pipe after the filtration is finished.
The invention adopts the structure and the method, and the consideration factors are mainly that in the traditional filtering method, the anhydrous sodium sulfate is added into a ground conical flask, the flask is oscillated, stood and filtered, the sample passes through the anhydrous sodium sulfate under the action of self gravity, the sample amount is small in the initial stage, the static pressure is not large enough, the passing speed is slow, the efficiency is reduced, the granularity of the anhydrous sodium sulfate is not changed, and the larger impurity molecules in the initial stage can block gaps among adsorption filtering agents, so that the passing time of the sample is prolonged. Therefore, the invention adopts the filtering agent with the particle size gradient distribution, firstly adopts the larger-particle adsorption filtering agent to remove the larger-size impurities, at the moment, the sample can smoothly pass through because the gaps between the filtering agents are larger, and the problem of insufficient static pressure of the sample at the moment is solved by adopting larger pressure, so that the filtering can be rapidly carried out. When entering the second and third grade adsorption filtration agent, because the sample static pressure can be gradually increased, the nitrogen pressure is gradually reduced at the moment, so that the sample can not pass through the adsorption filtration agent too fast, certain adsorption filtration time is ensured, and the adsorption filtration efficiency is improved.
The structure of the adsorption device is similar to that of the filtering device, except that magnesium silicate with single granularity is arranged in the bottle.
The adsorption method comprises the following steps: the sample reagent enters the bottle body through the inner tube, meanwhile, a nitrogen gas source is started, nitrogen gas with the pressure of 0.1MPa enters the bottle body, the sample reagent adsorbs polar substances such as animal and vegetable oil through magnesium silicate, the granularity of the magnesium silicate is 200 meshes, the pressure of the nitrogen gas in the bottle is controlled to be 0.1MPa, the pressure is linearly reduced, the sample reagent passes through the magnesium silicate under the action of gravity and the linearly reduced nitrogen gas pressure, the nitrogen gas pressure is reduced to 0.02MPa when the sample reagent reaches the bottom of the bottle body, and the sample reagent flows out through the oil outlet pipe after adsorption is completed.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (1)
1. A full-automatic oil measurement fast filtering and adsorbing method is characterized in that a filtering device and an adsorbing device which are similar in structure are adopted for filtering and adsorbing, the filtering device comprises a bottle body, a sample injection air pipe is arranged above the bottle body and comprises an outer pipe and an inner pipe, the inner pipe is made of polytetrafluoroethylene materials, the outer pipe is made of silica gel materials and is connected with a nitrogen gas source, the inner pipe is a reagent pipeline, the outer pipe is a gas pipeline, and the sample injection air pipe is connected to the inlet of the bottle body through a frosted port; the bottle body is internally provided with a first-stage filtering agent, a second-stage filtering agent and a third-stage filtering agent in sequence from top to bottom, the third-stage filtering agent is composed of anhydrous sodium sulfate with different granularities, the bottom of the bottle body is sealed by a sand core filtering plate, the size of the sand core filtering plate is G3-G4, and the bottom is connected with an oil outlet pipe through a detachable frosted opening;
the filtering method comprises the following steps: a sample reagent enters the bottle body through the inner tube, a nitrogen gas source is started at the same time, nitrogen gas with the pressure of 0.15MPa enters the bottle body, the sample reagent filters moisture and impurities in the sample reagent through anhydrous sodium sulfate with different three-level granularity, the granularity of the first-level anhydrous sodium sulfate is 80 meshes, the impurities with larger size and part of moisture can be quickly filtered, the pressure of the nitrogen gas in the bottle is controlled to be 0.15MPa, the pressure is controlled to be linearly reduced, and the sample reagent can rapidly pass through the first-level anhydrous sodium sulfate under the action of gravity and the linearly reduced nitrogen gas pressure; when the sample reagent enters the second-stage anhydrous sodium sulfate, the nitrogen pressure is reduced to 0.12MPa, the granularity of the second-stage anhydrous sodium sulfate is 120 meshes, impurities with smaller sizes and other water in the sample are filtered, and the nitrogen pressure is continuously controlled to be linearly reduced; when the sample reagent enters the third-stage anhydrous sodium sulfate, the pressure drop of the gas in the bottle is 0.1MPa, the granularity of the third-stage anhydrous sodium sulfate is 200 meshes, the residual small-size impurities are filtered, and the filtered small-size impurities flow out through an oil outlet pipe;
the adsorption device comprises a bottle body, wherein a sample injection air pipe is arranged above the bottle body and comprises an outer pipe and an inner pipe, the inner pipe is made of polytetrafluoroethylene materials, the outer pipe is made of silica gel materials and connected with a nitrogen gas source, the inner pipe is a reagent pipeline, the outer pipe is a gas pipeline, and the sample injection air pipe is connected to the inlet of the bottle body through a frosted opening; magnesium silicate is arranged in the bottle body, the bottom of the bottle body is sealed by a sand core filter plate, the size of the sand core filter plate is G3-G4, and the bottom of the sand core filter plate is connected with an oil outlet pipe through a detachable frosted opening;
the adsorption method comprises the following steps: the sample reagent enters the bottle body through the inner pipe, meanwhile, a nitrogen gas source is started, nitrogen gas with the pressure of 0.1MPa enters the bottle body, the sample reagent adsorbs animal and vegetable oil through magnesium silicate, the granularity of the magnesium silicate is 200 meshes, the pressure of the nitrogen gas in the bottle is controlled to be 0.1MPa, the pressure is linearly reduced, the sample reagent passes through the magnesium silicate under the action of gravity and the pressure of the linearly reduced nitrogen gas, the pressure of the nitrogen gas is reduced to 0.02MPa when the sample reagent reaches the bottom of the bottle body, and the sample reagent flows out through the oil outlet pipe after adsorption is completed.
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| US7473369B2 (en) * | 2002-02-14 | 2009-01-06 | The Trustees Of The Stevens Institute Of Technology | Methods of preparing a surface-activated titanium oxide product and of using same in water treatment processes |
| CN201444157U (en) * | 2009-04-03 | 2010-04-28 | 泰安市科瑞光学仪器有限公司 | Full-automatic infrared oil tester |
| CN201399261Y (en) * | 2009-04-16 | 2010-02-10 | 泰安市科瑞光学仪器有限公司 | Full-automatic extraction apparatus |
| CN102798605A (en) * | 2012-06-29 | 2012-11-28 | 苏州国环环境检测有限公司 | Method for determining oil substances in water sample according to infrared spectrophotometry |
| CN203552871U (en) * | 2013-11-01 | 2014-04-16 | 上海雷波尔企业发展股份有限公司 | Oil service intelligent processing system for large transformer |
| CN108115917A (en) * | 2018-01-30 | 2018-06-05 | 江苏光辉包装材料有限公司 | A kind of rush plasticizing type polyester fondant filter device |
| CN208525894U (en) * | 2018-05-14 | 2019-02-22 | 河南省政院检测研究院有限公司 | It is a kind of for Petroleum Determination except solid-phase extraction device is used in conjunction in animals and plants greases |
| CN208505734U (en) * | 2018-07-27 | 2019-02-15 | 浙江谱创仪器有限公司 | A kind of petroleum separation of animal and vegetable oils device |
| CN109444070A (en) * | 2018-12-06 | 2019-03-08 | 宁波然诺科学仪器有限公司 | Oil content all automatic measurement instrument in water |
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Inventor after: Guo Bo Inventor after: Hu Dedong Inventor after: Wang Xinjun Inventor after: Lin Zhenqiang Inventor after: Zhang Sen Inventor after: Zhang Zheng Inventor after: Liu Chuanrong Inventor after: Sui Feng Inventor after: Xu Aihua Inventor after: Zheng Peng Inventor before: Zhang Sen Inventor before: Guo Bo Inventor before: Lin Zhenqiang Inventor before: Zhang Zheng Inventor before: Sui Feng Inventor before: Xu Aihua Inventor before: Zheng Peng |
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