CN109342474A - Solid phase extraction concentration device and with its associated with XRF - Google Patents

Solid phase extraction concentration device and with its associated with XRF Download PDF

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Publication number
CN109342474A
CN109342474A CN201710644663.0A CN201710644663A CN109342474A CN 109342474 A CN109342474 A CN 109342474A CN 201710644663 A CN201710644663 A CN 201710644663A CN 109342474 A CN109342474 A CN 109342474A
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China
Prior art keywords
cavity cylinder
enriching column
adsorbent
solid phase
propeller
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CN201710644663.0A
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Chinese (zh)
Inventor
滕飞
田世玉
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BEIJING ANCHOR WISDOM TECHNOLOGY Co Ltd
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BEIJING ANCHOR WISDOM TECHNOLOGY Co Ltd
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Priority to CN201710644663.0A priority Critical patent/CN109342474A/en
Publication of CN109342474A publication Critical patent/CN109342474A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202Preparing specimens therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/07Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076X-ray fluorescence

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The embodiment of the invention discloses a kind of solid phase extraction concentration device and with its associated with XRF, the device includes the enriching column (200) with cavity cylinder, the top of enriching column is inlet, cavity cylinder bottom is built-in with the enrichment piece (300) for always penetrating fluidity adsorbent material, and the cavity inboard wall of cylinder sealing of the enrichment piece (300) and enriching column (200) cooperates;Device further includes a propeller (100) that cavity cylinder can be entered and left from inlet;Propeller (100) one end is the cock body (110) in the cavity cylinder for being slidably disposed in the enriching column and with cavity cylinder sealing cooperation, and liquid permeability adsorbent material is anion exchange resin or cation exchange resin.The present invention can make trace gold in water category ion enrichment in adsorbent material by solid phase extraction concentration device, so that XRF is passed through detection adsorbent material micro to trace heavy metal contents level in aqueous solution to analyze.

Description

Solid phase extraction concentration device and with its associated with XRF
Technical field
The invention belongs to water analysis technical field, more particularly to a kind of solid phase extraction concentration device and with its associated with XRF。
Background technique
Heavy metal element in water body is an important content of water quality monitoring, measures the heavy metal member in water environment at present The method of element is mainly atomic absorption spectrography (AAS) and inductively coupled plasma mass spectrometry.
The pretreatment process of both methods is complicated, and analysis instrument is expensive, and the testing cost of sample is higher, is not suitable for The frequent or long term monitoring of water quality uses.
Xray fluorescence spectrometer (X Ray Fluorescence, abbreviation XRF), which is able to achieve, exists to detection device for multi metallic elements Line detection, have many advantages, such as that easy to operate, testing cost is low, detection accuracy is high, but in surface water, underground water and seawater to Check weighing tenor is very low (such as ppb grades), far below the detection limit of XRF spectrometer, to limit XRF heavy metal in water Application in pollution determination.
Summary of the invention
The technical problem that the embodiment of the present invention solves is: provide a kind of solid phase extraction concentration device and with its associated with XRF, solid phase extraction concentration device can make trace gold in water category ion enrichment in adsorbent material, so that XRF passes through measurement absorption It is micro to trace heavy metal content in material analysis water.
According to an aspect of an embodiment of the present invention, a kind of Solid Phase Extraction SPE (Solid-Phase is provided Extraction) enriching apparatus, comprising: the enriching column (200) with cavity cylinder, the top of enriching column are inlet, cavity Cylinder bottom is built-in with and always penetrates the enrichment piece (300) of fluidity adsorbent material, the enrichment piece (300) and enriching column (200) The sealing cooperation of cavity inboard wall of cylinder;Device further includes a propeller (100) that cavity cylinder can be entered and left from inlet;Propeller (100) one end is the plug in the cavity cylinder for being slidably disposed in the enriching column and with cavity cylinder sealing cooperation Body (110), liquid permeability adsorbent material are Anion-adsorption resin or Cation adsorption resin.
Another aspect according to an embodiment of the present invention provides a kind of XRF, comprising: the extraction of solid phase described in above-described embodiment Take SPE enriching apparatus.
Solid Phase Extraction SPE enriching apparatus provided by the invention, the device are inhaling heavy metal accumulation in water by being enriched with piece On enclosure material, adsorbent material is detected by XRF, measures the content of beary metal being wherein enriched with, not only avoids complexity Pretreatment process has the advantages that easy to operate, process flow is short, equipment cost is low etc.;Also, compared to target in initial water sample The concentration of analyte, the analyte concentration after enrichment improve 2 orders of magnitude or higher, make detection of the XRF to heavy metal in water Limit reaches ppb grades.Effectively solve the test problems of heavy metal element in water quality.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the Solid Phase Extraction SPE enriching apparatus of the present invention;
XRF of the Fig. 2 for the present invention comprising Solid Phase Extraction SPE enriching apparatus uses schematic diagram.
Specific embodiment
Carry out the various exemplary embodiments of detailed description of the present invention now with reference to attached drawing.It should also be noted that unless in addition having Body explanation, the positioned opposite of the component otherwise illustrated in these embodiments, numerical expression and the unlimited system of numerical value are of the invention Range.
The embodiment of the invention provides a kind of solid phase extraction concentration devices, as shown in Figure 1, including the richness with cavity cylinder Clustered column (200), the top of enriching column are inlet, and cavity cylinder bottom is built-in with the enrichment piece for always penetrating fluidity adsorbent material (300), the enrichment piece (300) and the cavity inboard wall of cylinder of enriching column (200), which seal, cooperates;Device further includes one can be from inlet Enter and leave the propeller (100) of cavity cylinder;Propeller (100) one end is the cavity column for being slidably disposed in the enriching column The cock body (110) cooperated in vivo and with cavity cylinder sealing.
Using solid phase extraction concentration device of the invention, test water sample need to be only injected into enriching column (200), then be pushed away Enter propeller downlink, so that test water sample flows out enriching column (200) by the adsorbent material in enrichment piece (200), to make Heavy metal element is enriched in adsorbent material, then uses XRF technical testing adsorbent material, can be realized to water sample content of beary metal Detection.Solid phase extraction concentration device of the invention, using needle tube type structure, have easy to operate, process flow is short, equipment at This low advantage.
The present invention does not limit the adsorbent material structure in enrichment piece, as shown in Figure 1, enrichment piece (300) includes to have sealing The connector (320) of property and adsorbent (310) with taper, adsorbent (310) through connector (320) center and with The connector is slidingly sealed cooperation, and adsorbent includes liquid permeability adsorbent material.
It is equally also fitted using the adsorbent of other up big and down small structures such as the adsorbent of small one and large one two cylindrical structures Answer the application.
Further, adsorbent (310) is frustum cone structure, and adsorbent and connector are tightly connected, and is enriched with piece (300) and rich When clustered column (200) connects, the bottom surface (313) of rotary table is towards propeller cock body.Using the adsorbent of up big and down small structure, so that inhaling Attached body can efficiently be enriched with the object ion in water sample, and will not be detached from enrichment piece in propeller downward storke.
In Fig. 1, adsorbent rotary table (310) with a thickness of at least 2mm, preferably 2-10mm, rotary table (310) bottom surface Diameter is at least 2mm, preferably 2-8mm.
Optionally, adsorbent (310) is connect with connector (320) slidable sealing, after water quality enrichment, is enriched with piece (300) it can be detached from enriching column (200), adsorbent (310) can also be detached from enrichment piece (300).So can be with, using adsorbent as Consumptive material, the recyclable Reusability of the other component of solid phase extraction concentration device improve Solid Phase Extraction richness of the present invention to maximize The utilization rate of acquisition means saves test material, reduces the wasting of resources.
In the present invention, water penetration adsorbent material is resin, and resin preferred ion exchanger resin is handed over including cation Change resin or anion exchange resin.
For the ease of recording the volume of water sample, in the present invention it is possible to indicate scale on the outside of enriching column (200).
Using solid phase extraction concentration device of the present invention, when injection water sample only accounts for the partial volume of enriching column, push-in is promoted There is air cock body (110) front end of device, propeller, so that propeller friction in down stroke is larger, is unfavorable for pushing propeller, in order to The air of cock body front end is discharged, in solid phase extraction concentration device of the invention, can be equipped in propeller coaxial direction logical Air column makes ventilating column be in aeration status when being pushed into propeller, separate in propeller after the air before cock body is substantially discharged The end of cock body will ventilate column sealing, continue to press on propeller downlink, water sample is squeezed out adsorbent.
In the present invention, enrichment piece (300) is connect with enriching column (200) removable seal, wherein enrichment piece can be glue Body material;Or sealing screw thread is set in enrichment column bottom, enrichment piece lateral body sets external seal screw thread, and enrichment piece and enriching column pass through sealing It is threadedly coupled.Further, in order to improve sealing effect, cock body lateral body can be equipped at least one leakage-proof ring.
Testing water sample includes the water samples such as drinking water, underground water and waste water, can be straight if it is not high to fix granule content in water sample It connects using solid phase extraction concentration device of the present invention, if it is higher to fix granule content in water sample, is using solid phase of the present invention extraction Before taking enriching apparatus, filter device can be used, processing first is filtered to water sample, to reduce solid particle to adsorbent (310) pollution.
In addition, including solid phase extraction concentration shown in any of the above-described embodiment the embodiment of the invention also provides a kind of XRF Device.
As shown in Fig. 2, detecting water sample tenor using XRF, it may include following steps:
(1) water sample to be detected is handled through pretreating device, filters out solid therein through filter therein (201) Particle.
(2) water sample enters perfusor (202) after filtering.
(3) enriching column of solid phase extraction concentration device (203) is moved to perfusor (202) position by sample injector (204), note A certain amount of filtered water sample is injected the enriching column of solid phase extraction concentration device (203) by sample device (202).
(4) sample injector (204) removes the enriching column of solid phase extraction concentration device (203), and pushes solid phase extraction concentration The propeller of device (203) makes water sample to be measured be enriched in solid phase by being enriched with piece adsorbent, the heavy metal element in water sample to be measured On resin sheet (adsorbent) in extraction equipment;It is enriched with piece and is detached from solid-phase extraction device.
(4) the mobile enrichment piece for being enriched with heavy metal of sample injector (204) is to XRF spectroanalysis instrument (205) sample bin.And lead to It crosses XRF spectroanalysis instrument (205) to detect the heavy metal of enrichment, obtains the fluorescence of heavy metal element in the water sample to be measured Intensity value.
(5) a variety of different heavy metals are taken, are configured to a series of titer of various concentrations respectively, and using enrichment piece to it In heavy metal be enriched with, then detected with XRF spectroanalysis instrument, obtain the fluorescence of different heavy metals, various concentration Intensity value, and according to the ascending concentration-Standardization curve for fluorescence intensity for drawing the heavy metal of concentration, every kind of element is one corresponding Standard curve.
(6) step (4) resulting fluorescence intensity is compared with the fluorescence intensity of standard solution obtained by step (5), is obtained The type and concentration of heavy metal in the water sample to be measured out.
Heavy metal in the detectable water quality of the present invention includes lead, chromium, cadmium, mercury, arsenic, selenium, antimony, barium etc..
Solid Phase Extraction SPE enriching apparatus provided by the invention, the device are consolidating heavy metal accumulation in water by being enriched with piece On phase resin, solid-phase resin is detected by XRF, measures the content of beary metal being wherein enriched with, not only avoids complexity Pretreatment process has the advantages that easy to operate, process flow is short, equipment cost is low etc.;Also, compared to target in initial water sample The concentration of analyte, the analyte concentration after enrichment improve 2 orders of magnitude or higher, make detection of the XRF to heavy metal in water Limit reaches ppb grades, effectively solves the test problems of heavy metal element in water quality.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with its The difference of its embodiment, the same or similar part cross-reference between each embodiment.
Description of the invention is given for the purpose of illustration and description, and is not exhaustively or will be of the invention It is limited to disclosed form.Many modifications and variations are obvious for the ordinary skill in the art.It selects and retouches It states embodiment and is to more preferably illustrate the principle of the present invention and practical application, and those skilled in the art is enable to manage The solution present invention is to design various embodiments suitable for specific applications with various modifications.

Claims (10)

1. a kind of solid phase extraction concentration device, including the enriching column (200) with cavity cylinder, the top of enriching column is feed liquor Mouthful, which is characterized in that
Cavity cylinder bottom is built-in with the enrichment piece (300) for always penetrating fluidity adsorbent material, the enrichment piece (300) and institute State the cavity inboard wall of cylinder sealing cooperation of enriching column (200);
Described device further includes a propeller (100) that cavity cylinder can be entered and left from inlet;Propeller (100) one end To be slidably disposed in the cock body (110) in the cavity cylinder of the enriching column and with cavity cylinder sealing cooperation;
The liquid permeability adsorbent material is anion exchange resin or cation exchange resin.
2. the apparatus according to claim 1, which is characterized in that enrichment piece (300) includes the connection with leakproofness Body (320) and adsorbent (310) with taper, the adsorbent (310) through the connector (320) center and with The connector is slidingly sealed cooperation, and the adsorbent includes the liquid permeability adsorbent material.
3. the apparatus of claim 2, which is characterized in that the adsorbent is frustum cone structure, the outsole of the rotary table Cock body of the face (311) towards the propeller.
4. the apparatus of claim 2, which is characterized in that the thickness of the rotary table is at least 2mm, the rotary table bottom surface Diameter be at least 2mm.
5. device according to claim 4, which is characterized in that the diameter of the rotary table bottom surface is 2-10mm, the rotary table With a thickness of 2-8mm.
6. the apparatus according to claim 1, which is characterized in that enriching column (200) outer surface is labeled with scale.
7. the apparatus according to claim 1, which is characterized in that propeller (100) coaxial direction is equipped with salable logical Air column.
8. the apparatus according to claim 1, which is characterized in that the connector of enrichment piece (300) is colloidal materials, or Enrichment piece (300) and the cavity cylinder of the enriching column (200) are threadedly engaged by sealing.
9. the apparatus according to claim 1, which is characterized in that the cock body (110) is equipped at least one leakage-proof ring.
10. a kind of XRF, which is characterized in that include solid phase extraction concentration device described in claim 1 to 9 any one.
CN201710644663.0A 2017-08-01 2017-08-01 Solid phase extraction concentration device and with its associated with XRF Pending CN109342474A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112649454A (en) * 2019-10-09 2021-04-13 清华苏州环境创新研究院 Method for detecting concentration of heavy metal in liquid
CN113552151A (en) * 2020-04-23 2021-10-26 北京安科慧生科技有限公司 X-ray fluorescence spectrometer and ion enrichment device thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202869877U (en) * 2012-11-02 2013-04-10 陕西出入境检验检疫局检验检疫技术中心 Sample purifying and filtering device
CN105891245A (en) * 2016-04-19 2016-08-24 北京安科慧生科技有限公司 Solid-phase extraction and XFR combined method and device for detecting heavy metal in water
CN205656174U (en) * 2016-05-25 2016-10-19 中南大学 System for be used for detecting trace metal ion content
CN207318386U (en) * 2017-08-01 2018-05-04 北京安科慧生科技有限公司 Solid phase extraction concentration device and with its associated with XRF
CN216410841U (en) * 2021-08-26 2022-04-29 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) Enrichment device of elements in on-site water sample

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202869877U (en) * 2012-11-02 2013-04-10 陕西出入境检验检疫局检验检疫技术中心 Sample purifying and filtering device
CN105891245A (en) * 2016-04-19 2016-08-24 北京安科慧生科技有限公司 Solid-phase extraction and XFR combined method and device for detecting heavy metal in water
CN205656174U (en) * 2016-05-25 2016-10-19 中南大学 System for be used for detecting trace metal ion content
CN207318386U (en) * 2017-08-01 2018-05-04 北京安科慧生科技有限公司 Solid phase extraction concentration device and with its associated with XRF
CN216410841U (en) * 2021-08-26 2022-04-29 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) Enrichment device of elements in on-site water sample

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112649454A (en) * 2019-10-09 2021-04-13 清华苏州环境创新研究院 Method for detecting concentration of heavy metal in liquid
CN113552151A (en) * 2020-04-23 2021-10-26 北京安科慧生科技有限公司 X-ray fluorescence spectrometer and ion enrichment device thereof
CN113552151B (en) * 2020-04-23 2024-04-19 北京安科慧生科技有限公司 X-ray fluorescence spectrometer and ion enrichment device thereof

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