CN112213176A - In-situ rapid enrichment device for water phosphate and using method - Google Patents
In-situ rapid enrichment device for water phosphate and using method Download PDFInfo
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- CN112213176A CN112213176A CN202010987864.2A CN202010987864A CN112213176A CN 112213176 A CN112213176 A CN 112213176A CN 202010987864 A CN202010987864 A CN 202010987864A CN 112213176 A CN112213176 A CN 112213176A
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- chromatographic column
- zeolite
- water
- phosphate
- rubber tube
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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
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
Abstract
The invention discloses an in-situ rapid enrichment device for water phosphate, which comprises a chromatographic column, wherein the chromatographic column is fixed on a chromatographic column frame, zirconium-loaded zeolite is filled at the bottom in the chromatographic column, rubber tubes are connected to the top and the bottom of the chromatographic column respectively, the front end of the rubber tube at the bottom of the chromatographic column is a water outlet, the front end of the rubber tube at the top of the chromatographic column is connected with the output end of a small-sized rechargeable water pump, the input end of the small-sized rechargeable water pump is also connected with the rubber tube, the front end of the rubber tube at the input end of the small-sized rechargeable water pump is a; the device can realize the in-situ rapid enrichment of phosphate in rivers or lakes and the high-efficiency elution in laboratories, and finally obtain high-purity and high-concentration phosphorusAcid salt solution, thereby being beneficial to subsequent high-purity Ag3PO4Generating; compared with the traditional phosphate oxygen isotope pretreatment method, the method can avoid the collection and transportation of a large amount of overlying water samples.
Description
Technical Field
The invention relates to a water phosphate oxygen isotope determination technology, in particular to a water phosphate in-situ rapid enrichment device and a use method thereof.
Background
The phosphate oxygen isotope technology is an effective tool for tracing river phosphorus sources and a circulation process, and aiming at an experimental method of the phosphate oxygen isotope technology, at present, a considerable amount of environmental samples are mainly collected, and phosphate in the samples is completely converted into Ag through a pretreatment method (enrichment, separation and purification)3PO4Due to the complex components of the sample in nature, especially the existence of organic matters and other oxygen-containing substances, the Ag can be interfered3PO4The generation of (2) also interferes with the measurement result of a stable isotope ratio mass spectrometer, so that the pretreatment of the sample is particularly important.
However, the existing sample pretreatment method has complicated steps and large sample collection amount, and the development and application of the phosphate oxygen isotope technology are severely restricted. For this reason, many scientists have been around increasing Ag in recent years3PO4The purification rate, the pretreatment steps are simplified, the sample collection amount is reduced, the phosphate oxygen isotope pretreatment methods under different application scenes (seawater, fresh water, sediment and soil) are optimized, most of the processes enrich phosphate in the sample by a magnesium-induced phosphate coprecipitation method in a laboratory, then impurity ions and organic matters are removed by adopting a series of methods according to the characteristics of the sample, and finally Ag with relatively higher purity is obtained by washing for multiple times3PO4And (3) a solid. However, these optimized methods still require the collection of a large number of environmental samples, the experimental procedure is still rather cumbersome, and Ag3PO4The purification rate of (A) is more difficult to ensure, and the convenience of the method is not completely changed.
Therefore, a new optimization idea is needed for optimizing the phosphate oxygen isotope pretreatment method in rivers or lakes to improve Ag content3PO4Based on the purification rate and the simplified experimental steps, the method is further developedThe collection amount of samples is reduced, and the convenience of the method is improved.
Disclosure of Invention
The invention aims to provide an in-situ rapid enrichment device for water phosphate and a using method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a quick enrichment device of water phosphate normal position, includes the chromatography column, and the chromatography column is fixed on the chromatography column frame, and the bottom packing has zirconium load zeolite in the chromatography column, all is connected with the rubber tube in chromatography column top and bottom, and the front end of chromatography column bottom rubber tube is the delivery port, and chromatography column top rubber tube front end is connected with the output of small-size rechargeable water pump, is connected with the rubber tube equally at the input of small-size rechargeable water pump, the front end of the input rubber tube of small-size rechargeable water pump is the water inlet, water inlet department parcel has the non-woven fabrics.
The use method of the in-situ rapid water phosphate enrichment device comprises three steps of zeolite pretreatment, in-situ on-site enrichment and laboratory elution.
The zeolite pretreatment step comprises: a. 20g of zeolite with the particle size of 1-2mm is placed in 500mL of 1mol/L hydrochloric acid solution, and the mixture is subjected to microwave oscillation for 4 hours; b. placing the zeolite after acid treatment in 500mL of 1mol/L sodium hydroxide solution, and performing microwave oscillation for 4 hours; c. washing zeolite with a large amount of deionized water for later use; d. putting zeolite into 100mL of 1mol/L sodium hydroxide, performing microwave oscillation for 2 hours, and performing magnetic stirring for 30 min; e. under the condition of magnetic stirring, inserting a pH tester, and slowly dripping zirconium oxychloride octahydrate until the pH is 7; f. and aging the solution for 24h, taking out the zeolite, putting the zeolite into a drying oven at 105 ℃ for drying, and generating the zirconium-loaded zeolite after drying.
The in situ enrichment step comprises the following steps: h. fixing a chromatographic column on a chromatographic column frame, and placing 20g of zirconium-loaded zeolite in the chromatographic column; i. fixing the non-woven filter cloth in front of the water inlet of the rubber tube by using a rubber band, placing the water inlet in a river, and connecting the other end of the rubber tube with the water inlet; j. starting a small-sized charging type water pump, filtering overlying water of the river by non-woven filter cloth, then entering a chromatographic column, and flowing through zirconium-loaded zeolite in the chromatographic column and then returning to the river or lake; k. after 20 minutes the mini-charge pump was turned off and the zirconium loaded zeolite in the column was removed and placed in a self-sealing bag and brought back to the laboratory.
The laboratory elution step comprises: l, putting the zirconium-loaded zeolite subjected to in-situ enrichment on site into 50mL of sodium hydroxide with the concentration of 1mol/L, and performing microwave oscillation for 4 hours to elute phosphate in the zirconium-loaded zeolite to finally obtain 50mL of high-concentration and high-purity phosphate solution, wherein the solution can be subjected to subsequent purification treatment to realize high-purity Ag3PO4And (4) preparing.
As a preferred embodiment of the present invention: and a rubber band is sleeved outside the non-woven filter cloth and used for ensuring the fixation of the non-woven filter cloth and the rubber tube.
Compared with the prior art, the invention has the beneficial effects that: the device can realize the in-situ rapid enrichment of phosphate in rivers or lakes and the high-efficiency elution in laboratories to finally obtain the high-purity and high-concentration phosphate solution, thereby being beneficial to the subsequent high-purity Ag3PO4Generating; compared with the traditional phosphate oxygen isotope pretreatment method, the method can avoid the collection and transportation of a large number of overlying water samples and improve the Ag of the final product3PO4The purification rate is high, the method is simple and convenient, and repeated and complicated enrichment processes of samples are not needed like the traditional method; meanwhile, the device has a simple structure, the preparation process of the phosphate selective adsorption material is mature, the parts are convenient to assemble on site, the phosphate in the river or lake covering water can be quickly enriched in situ in about 20min, and a large amount of time is saved compared with the traditional method.
Drawings
FIG. 1 is a schematic view of the structure of the enrichment apparatus of the present invention.
In the figure, 1-a chromatographic column frame, 2-a chromatographic column, 3-a small-sized charging type water pump, 4-zirconium loaded zeolite, 5-a rubber tube, 6-a rubber band, 7-non-woven filter cloth, 8-a water outlet and 9-a water inlet.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, an in-situ rapid water phosphate enrichment device comprises a chromatographic column 2, wherein the chromatographic column 2 is fixed on a chromatographic column frame 1, zirconium-loaded zeolite 4 is filled at the bottom of the chromatographic column 2, rubber tubes 5 are connected to the top and the bottom of the chromatographic column 2, a water outlet 8 is arranged at the front end of the rubber tube 5 at the bottom of the chromatographic column 2, the front end of the rubber tube 5 at the top of the chromatographic column 2 is connected with an output end of a small-sized rechargeable water pump 3, the input end of the small-sized rechargeable water pump 3 is also connected with the rubber tube 5, a water inlet 9 is arranged at the front end of the rubber tube 5 at the input end of the small-sized rechargeable.
The use method of the device comprises three steps of zeolite pretreatment, on-site in-situ enrichment and laboratory elution.
The zeolite pretreatment step comprises: a. 20g of zeolite with the particle size of 1-2mm is placed in 500mL of 1mol/L hydrochloric acid solution, and the mixture is subjected to microwave oscillation for 4 hours; b. placing the zeolite after acid treatment in 500mL of 1mol/L sodium hydroxide solution, and performing microwave oscillation for 4 hours; c. washing zeolite with a large amount of deionized water for later use; d. putting zeolite into 100mL of 1mol/L sodium hydroxide, performing microwave oscillation for 2 hours, and performing magnetic stirring for 30 min; e. under the condition of magnetic stirring, inserting a pH tester, and slowly dripping zirconium oxychloride octahydrate until the pH is 7; f. and aging the solution for 24h, taking out the zeolite, putting the zeolite into a drying oven at 105 ℃ for drying, and generating the zirconium-loaded zeolite after drying.
The in situ enrichment step comprises the following steps: h. fixing a chromatographic column 2 on a chromatographic column frame 1, and placing 20g of zirconium-loaded zeolite 4 in the chromatographic column 2; i. fixing the non-woven filter cloth 7 in front of a water inlet 9 of a rubber tube 5 by using a rubber band 6, placing the water inlet 9 in a river, and connecting the other end of the rubber tube 5 with the water inlet 9; j. starting a small-sized charging type water pump 3, filtering the overlying water of the river by non-woven filter cloth 7, then entering a chromatographic column 2, flowing through zirconium-loaded zeolite 4 in the chromatographic column 2, and then returning to the river or lake; k. after 20 minutes the mini-charge pump 3 was turned off and the zirconium loaded zeolite 4 in the column 2 was removed and placed in a self-sealing bag and brought back to the laboratory.
The laboratory elution step comprises: l, putting the zirconium-loaded zeolite 4 subjected to in-situ enrichment on site into 50mL of sodium hydroxide with the concentration of 1mol/L, and performing microwave oscillation for 4 hours to elute phosphate in the zirconium-loaded zeolite 4 to obtain 50mL of high-concentration and high-purity phosphate solution, wherein the solution can be subjected to subsequent purification treatment to realize high-purity Ag3PO4And (4) preparing.
The device can realize the in-situ rapid enrichment of phosphate in rivers or lakes and the high-efficiency elution in laboratoriesFinally obtaining high-purity and high-concentration phosphate solution, thereby being beneficial to follow-up high-purity Ag3PO4Generating; compared with the traditional phosphate oxygen isotope pretreatment method, the method can avoid the collection and transportation of a large number of overlying water samples and improve the Ag of the final product3PO4The purification rate is high, the method is simple and convenient, and repeated and complicated enrichment processes of samples are not needed like the traditional method; meanwhile, the device has a simple structure, the preparation process of the phosphate selective adsorption material is mature, the parts are convenient to assemble on site, the phosphate in the river or lake covering water can be quickly enriched in situ in about 20min, and a large amount of time is saved compared with the traditional method.
Example 2:
on the basis of the embodiment 1, the rubber band 6 is sleeved outside the non-woven filter cloth 7 to ensure the fixation of the non-woven filter cloth 7 and the rubber tube 5.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The utility model provides a quick enrichment device of water phosphate normal position, includes chromatographic column (2), a serial communication port, chromatographic column (2) are fixed on chromatography column frame (1), the bottom packing has zirconium load zeolite (4) in chromatographic column (2), all be connected with rubber tube (5) at chromatographic column (2) top and bottom, the front end of chromatography column (2) bottom rubber tube (5) is delivery port (8), chromatographic column (2) top rubber tube (5) front end is connected with the output of small-size rechargeable water pump (3), be connected with rubber tube (5) at the input of small-size rechargeable water pump (3) equally, the front end of input rubber tube (5) of small-size rechargeable water pump (3) is water inlet (9).
2. The in-situ rapid phosphate enrichment device for the water body according to claim 1, wherein the water inlet (9) is wrapped with a non-woven filter cloth (7).
3. The in-situ rapid phosphate enrichment device for the water body according to claim 2, wherein a rubber band (6) is sleeved outside the non-woven filter cloth (7) to ensure the fixation of the non-woven filter cloth (7) and the rubber tube (5).
4. The use method of the in-situ rapid water phosphate enrichment device adopts the in-situ rapid water phosphate enrichment device in claim 1 or 2, and comprises three steps of zeolite pretreatment, in-situ on-site enrichment and laboratory elution.
5. The use method of the in-situ rapid water phosphate enrichment device according to claim 4, wherein the zeolite pretreatment step comprises: a. 20g of zeolite with the particle size of 1-2mm is placed in 500mL of 1mol/L hydrochloric acid solution, and the mixture is subjected to microwave oscillation for 4 hours; b. placing the zeolite after acid treatment in 500mL of 1mol/L sodium hydroxide solution, and performing microwave oscillation for 4 hours; c. washing zeolite with a large amount of deionized water for later use; d. putting zeolite into 100mL of 1mol/L sodium hydroxide, performing microwave oscillation for 2 hours, and performing magnetic stirring for 30 min; e. under the condition of magnetic stirring, inserting a pH tester, and slowly dripping zirconium oxychloride octahydrate until the pH is 7; f. and aging the solution for 24h, taking out the zeolite, putting the zeolite into a drying oven at 105 ℃ for drying, and generating the zirconium-loaded zeolite after drying.
6. The use method of the in-situ rapid water phosphate enrichment device according to claim 5, wherein the in-situ enrichment step comprises the following steps: h. fixing a chromatographic column (2) on a chromatographic column frame (1), and placing 20g of zirconium-loaded zeolite (4) in the chromatographic column (2); i. fixing the non-woven filter cloth (7) in front of a water inlet (9) of the rubber tube (5) by a rubber band (6), placing the water inlet (9) in a river, and connecting the other end of the rubber tube (5) with the water inlet (9); j. starting a small-sized charging type water pump (3), filtering the water covered on the river by non-woven filter cloth (7), then entering a chromatographic column (2), and flowing back to the river or lake after flowing through zirconium-loaded zeolite (4) in the chromatographic column (2); k. after 20 minutes the mini-charge pump (3) was turned off and the zirconium loaded zeolite (4) in the column (2) was removed and placed in a self-sealing bag and brought back to the laboratory.
7. The use method of the in-situ rapid water phosphate enrichment device according to claim 6, wherein the laboratory elution step comprises: l, putting the zirconium-loaded zeolite (4) subjected to in-situ enrichment on site into 50mL of sodium hydroxide with the concentration of 1mol/L, and performing microwave oscillation for 4 hours to elute phosphate in the zirconium-loaded zeolite (4) to finally obtain 50mL of high-concentration and high-purity phosphate solution, wherein the solution can be subjected to subsequent purification treatment to realize high-purity Ag3PO4And (4) preparing.
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| CN202010987864.2A CN112213176A (en) | 2020-09-18 | 2020-09-18 | In-situ rapid enrichment device for water phosphate and using method |
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| CN202010987864.2A CN112213176A (en) | 2020-09-18 | 2020-09-18 | In-situ rapid enrichment device for water phosphate and using method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113109126A (en) * | 2021-03-09 | 2021-07-13 | 中国环境科学研究院 | Phosphate oxygen isotope enrichment equipment, method and device |
| CN115108648A (en) * | 2022-05-23 | 2022-09-27 | 西南交通大学 | Water body in-situ phosphate enrichment device |
| CN115824724A (en) * | 2022-12-08 | 2023-03-21 | 中国地质科学院 | Novel preparation of radium isotope test sample device |
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| US9322014B1 (en) * | 2012-11-28 | 2016-04-26 | Sandia Corporation | Multiplexed microfluidic approach for nucleic acid enrichment |
| CN206583677U (en) * | 2017-03-07 | 2017-10-24 | 中国科学院寒区旱区环境与工程研究所 | The device of organic matter and nitrate in a kind of On-site sampling concentration glacier |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113109126A (en) * | 2021-03-09 | 2021-07-13 | 中国环境科学研究院 | Phosphate oxygen isotope enrichment equipment, method and device |
| CN115108648A (en) * | 2022-05-23 | 2022-09-27 | 西南交通大学 | Water body in-situ phosphate enrichment device |
| CN115108648B (en) * | 2022-05-23 | 2023-10-20 | 西南交通大学 | Water normal position enrichment phosphate device |
| CN115824724A (en) * | 2022-12-08 | 2023-03-21 | 中国地质科学院 | Novel preparation of radium isotope test sample device |
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Application publication date: 20210112 |