CN105891245A - Solid-phase extraction and XFR combined method and device for detecting heavy metal in water - Google Patents
Solid-phase extraction and XFR combined method and device for detecting heavy metal in water Download PDFInfo
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- CN105891245A CN105891245A CN201610244996.XA CN201610244996A CN105891245A CN 105891245 A CN105891245 A CN 105891245A CN 201610244996 A CN201610244996 A CN 201610244996A CN 105891245 A CN105891245 A CN 105891245A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/22—Investigating 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
- G01N23/223—Investigating 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/22—Investigating 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
- G01N23/2202—Preparing specimens therefor
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Abstract
The invention relates to the technical field of water quality analysis, in particular to a solid-phase extraction and XFR combined method and device for detecting heavy metal in water. The detection method comprises steps as follows: filtration, metal enrichment, detection of fluorescence intensity, preparation of a series of standard solutions of different heavy metals, drawing of a concentration-fluorescence intensity standard curve and comparison. The detection device comprises a pre-treatment device, an XFR detection instrument and a solid-phase extraction device. By means of the detection method, the detection problem about heavy metal elements in water is effectively solved, the complicated pretreatment process is avoided, the testing cost is greatly reduced, a trace quantity of heavy metal elements in the water are automatically and rapidly analyzed, and the detection limit can reach the ppb level. The detection device can detect concentrations of multiple heavy metal elements, and the detection data are accurate; besides, equipment runs stably, and the operability is high.
Description
Technical field
The present invention relates to water analysis technical field, be specifically related to water associated with a kind of SPE and XFR
Middle heavy metal detection method, detection device.
Background technology
Heavy metal element in water body is an important content of water quality monitoring, measures in water environment at present
The method of heavy metal element is mainly atomic absorption spectrography (AAS) and inductively coupled plasma mass spectrometry.This
The pretreatment process of two kinds of methods is the most complicated, and analytical instrument is expensive, and the testing cost of sample is higher,
It is not suitable for being used as the method for monitoring water quality on line.
Xray fluorescence spectrometer is capable of the on-line checking to detection device for multi metallic elements, and pre-treatment letter
Single, quickly, the testing cost of sample is low in operation, but owing to X-ray diffraction has the higher scattering back of the body
Scape, the detection limit causing the method is of a relatively high, it is impossible to reach the requirement of water quality monitoring.
Summary of the invention
It is an object of the invention to provide heavy metal detection method in water associated with a kind of SPE and XFR,
The method efficiently solves the test problems of heavy metal element in water quality, it is to avoid complicated pretreatment process,
Significantly reduce testing cost, it is achieved the automatically and rapidly analysis to underwater trace heavy metal element, and
Detection limit can reach ppb level.
The present invention also aims to provide a kind of detection device, this device makes a huge sum of money in water by enrichment sheet
Directly detected by XFR detector after belonging to enrichment, it is to avoid the pretreatment process of complexity, technique stream
Journey is short, and equipment cost is low.Additionally this device can detect detection device for multi metallic elements concentration simultaneously, detects data
Accurately.
In order to realize object above, the present invention adopts the following technical scheme that
Heavy metal detection method in water associated with a kind of SPE and XFR, comprises the following steps:
(1) water sample to be detected is processed through pretreating device, filter out solid particle therein;
(2) water sample to be measured after filtering is placed in solid phase extraction device so that it is in heavy metal element rich
Combine on the metal enrichment sheet in solid-phase extraction device;
(3) the metal enrichment sheet XFR detector being enriched with heavy metal is detected, obtain described
The fluorescence intensity level of heavy metal element in water sample to be measured;
(4) take multiple different heavy metal, be configured to the titer of a series of variable concentrations respectively, and use
Heavy metal therein is enriched with by metal enrichment sheet, then detects with XFR detector, draws not
Same heavy metal, the fluorescence intensity level of variable concentrations, and draw the concentration of this heavy metal-glimmering according to concentration
Light intensity standard curve, every kind of corresponding calibration curve of element;
(5) by the fluorescence intensity of the fluorescence intensity of step (3) gained Yu step (4) gained standard liquid
Compare, draw kind and the concentration of heavy metal in described water sample to be measured.
Optionally, described metal enrichment sheet is resin sheet.
Optionally, described resin sheet use ion exchange resin, specially cationic ion-exchange resin or the moon from
Sub-exchange resin.
Optionally, multiple different heavy metals described in step (4) be lead, chromium, cadmium, mercury, arsenic, selenium,
Antimony, barium.
Optionally, calibration curve described in step (4) be according to heavy metal concentration in described standard liquid by
Little form to big or descending drafting.
Detection device used by heavy metal detection method in water associated with above-mentioned SPE and XFR, depends on
Secondary including is provided with one below pretreating device and XFR detector, described pretreating device and XFR detector
Mobile platform, also includes the solid-phase extraction device being arranged on described mobile platform, will by mobile platform
Solid-phase extraction device is delivered to below pretreating device and XFR detector;
There is in described pretreating device the filter for filtering the solid particle in water sample to be measured, described
Solid phase extraction device is provided with the metal enrichment sheet for enriching heavy metal.
Optionally, perfusor, described pretreating device and perfusor it are additionally provided with below described pretreating device
Upper end is equipped with injection port, and lower end is equipped with outlet, the outlet of described pretreating device and perfusor
Injection port connection, be provided with sample feeding pipe, described solid-phase extraction device at the injection port of described pretreating device
The metal enrichment sheet placed including the sampler being arranged on mobile platform and sampler top.
Optionally, described sampler top is additionally provided with memory, is used for storing metal enrichment sheet, described XFR
Detector is positioned at the right side of described pretreating device, and described memory is positioned at the left side of described pretreating device.
Optionally, described metal enrichment sheet is resin sheet.
Optionally, described resin sheet use ion exchange resin, specially cationic ion-exchange resin or the moon from
Sub-exchange resin.
The XFR detector that the present invention uses, uses Mo target or Rh target or Ag target X-ray tube,
Crystal is Ge crystal or Si crystal, for extracting the K α characteristic X-ray of Mo or Rh or Ag element.
Heavy metal detection method in water associated with the SPE of present invention offer and XFR, by preparation one
The heavy metal standard liquid of series variable concentrations, and the detection method provided by the present invention, molten to standard
Heavy metal in liquid uses XFR detector to detect it after being enriched with, and draws the mark of concentration known
The fluorescence intensity level of heavy metal element in quasi-solution, and by a series of variable concentrations of this heavy metal element
The different fluorescence intensity levels that solution detection obtains are depicted as calibration curve.Above-mentioned heavy metal standard liquid includes
Water generally contains the heavy metal that maybe may contain, specifically include as lead, chromium, cadmium, mercury, arsenic, selenium,
Antimony, barium.After the method using the present invention to provide the most again carries out filtration treatment to water sample to be measured, put
Be placed in solid-phase extraction device so that it is in heavy metal accumulation on heavy metal accumulation sheet, use the most again
It is detected by XFR device, draws the metallic element fluorescence intensity level in testing sample, then should
Fluorescence intensity level is compared with calibration curve, can draw heavy metal element kind in testing sample and
Concentration value.
The detection device that the present invention provides, is carried out the solid particle in water sample to be measured by pretreating device
After filtration, moved by mobile platform and move to, below pretreating device, make by solid phase extraction device
Water sample after filter flows through metal enrichment sheet, makes the heavy metal accumulation in water sample to be measured in solid phase extraction device
Metal enrichment sheet on, then by the movement of mobile platform, metal enrichment sheet is delivered under XFR detector
Side, detects.
The detection device that the present invention provides, it is to avoid complicated pretreatment process, technological process is short, equipment
Low cost.And this device can detect detection device for multi metallic elements concentration simultaneously, detection data are accurate.Meanwhile,
This stable equipment operation, workable.
The detection device that the present invention provides, resin sheet has three positions in the course of the work, is first storage
In memory, it is positioned at above sampler, then moves with mobile platform and extract to perfusor
With the enrichment of metal, finally, then resin sheet is moved detect to XFR detector.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation detecting device that the embodiment of the present invention 1 provides.
Detailed description of the invention
Embodiment 1
A kind of detection device as described in Figure 1, include successively the memory 1 for storing metal enrichment sheet,
Pretreating device and XFR detection fill 7 and put, and described XFR detector is positioned at the right side of described pretreating device,
Described memory is positioned at the left side of described pretreating device.
It is provided with a mobile platform 8 below described pretreating device and XFR detector and is arranged at described platform
On solid-phase extraction device, by mobile platform, solid-phase extraction device is delivered to pretreating device and XFR
Below detector;There is in described pretreating device the filtration for filtering the solid particle in water sample to be measured
Device 6, is additionally provided with perfusor 4, described pretreating device and perfusor upper end equal below described pretreating device
Being provided with injection port, lower end is equipped with outlet, the outlet of described pretreating device and the sample introduction of perfusor
Mouth connection, is provided with sample feeding pipe 5 at the injection port of described pretreating device.Described solid-phase extraction device includes setting
The metal enrichment sheet 2 that the sampler 3 being placed on mobile platform and sampler top are placed.
Embodiment 2
Heavy metal detection method in water associated with a kind of SPE and XFR, it uses embodiment 1 to provide
Detection device carry out, specifically comprise the following steps that
(1) water sample to be detected is processed through pretreating device, filter out it through filter 6 therein
In solid particle;
(2) being moved by mobile platform 8, make sampler 3 be positioned at below perfusor, make after filtration is to be measured
Water sample flows through resin sheet 2 so that it is in heavy metal element be enriched on the resin sheet in solid-phase extraction device;
(3) mobile platform 8 is moved, make the resin sheet being enriched with heavy metal move to XFR inspection
Survey below instrument 7, and detected by XFR detector, obtain heavy metal element in described water sample to be measured
Fluorescence intensity level;
(4) take multiple different heavy metal, be configured to the titer of a series of variable concentrations respectively, and use
Heavy metal therein is enriched with by resin sheet, then detects with XFR detector, draws different weight
Metal, the fluorescence intensity level of variable concentrations, and according to the concentration of concentration this heavy metal of ascending drafting-glimmering
Light intensity standard curve, every kind of corresponding calibration curve of element;
(5) by the fluorescence intensity of the fluorescence intensity of step (3) gained Yu step (4) gained standard liquid
Compare, draw kind and the concentration of heavy metal in described water sample to be measured.
Described multiple different heavy metals are lead, chromium, cadmium, mercury, arsenic, selenium, antimony, barium.
Metal enrichment sheet described in embodiment 1-2 is resin sheet, is specifically exchanged by the ion with active group
Resin and forming agent are mixed in the certain mass ratio than 1-2:1.The thickness of resin sheet used is about
4-6mm, diameter is about 6-8mm, and selected resin is Dowex ion exchange resin.
Test example
The concrete method of testing of heavy metal element Hg and test result in water sample:
Related reagent and Preparatory work of experiment
(1) preparation of Hg standard liquid.Concentration is become to be 0,0.01 by the storing solution stepwise dilution of 1ppm,
0.02,0.04,0.1,0.2ppm standard liquid.
(2) the detection device that embodiment 1 provides.
(3) the Hg water sample to be measured of standard value and uncertainty is indicated.
Two, the testing procedure of sample
Hg standard liquid is ready to, connects pipeline, open machine, proceed by test.
The first step: open control software, is sucked 50mL distilled water by auto injection pipe and fills SPE
Put and be carried out.
Second step: input calibration curve title to be set up and corresponding concentration point in software.Test one
The Hg element fluorescence intensity of series standard solution, concentration is tested from low to high, after having surveyed sample, uses every time
50mL distilled water flushing.
3rd step: use glimmering to the heavy metal element in water sample to be measured of detection method that embodiment 2 provides
Luminous intensity is tested.
4th step: storage data, contrasts the concentration range of test result with water sample to be measured.
Table 1 is the result tested by apparatus and method of the present invention water sample to be measured to Hg.From table 1
In it can be seen that the test result of the present invention accurately and reliably.
Table 1.Hg water sample to be measured test result
Index | Linearly (R2) | Repeatability (RSD%) | Water sample concentration range to be measured | Experiment test value |
Result | 0.99927 | 6.17 | 9.46±0.9ppb | 9.98ppb |
Above example only in order to technical scheme to be described, is not intended to limit;Although with reference to signing
The present invention has been described in detail by administration's embodiment, it will be understood by those within the art that: its
Still the technical scheme described in described embodiment can be modified, or to wherein portion of techniques
Feature carries out equivalent;And these amendments or replacement.It it is not the essence disengaging of appropriate technical solution
The present invention respectively implements the spirit and scope of technical scheme.
Claims (10)
1. heavy metal detection method in water associated with a SPE and XFR, it is characterised in that bag
Include following steps:
(1) water sample to be detected is processed through pretreating device, filter out solid particle therein;
(2) water sample to be measured after filtering is placed in solid phase extraction device so that it is in heavy metal element rich
Combine on the metal enrichment sheet in solid-phase extraction device;
(3) the metal enrichment sheet XFR detector being enriched with heavy metal is detected, obtain described
The fluorescence intensity level of heavy metal element in water sample to be measured;
(4) take multiple different heavy metal, be configured to the titer of a series of variable concentrations respectively, and use
Heavy metal therein is enriched with by metal enrichment sheet, then detects with XFR detector, draws not
Same heavy metal, the fluorescence intensity level of variable concentrations, and draw the concentration of this heavy metal-glimmering according to concentration
Light intensity standard curve, every kind of corresponding calibration curve of element;
(5) by the fluorescence intensity of the fluorescence intensity of step (3) gained Yu step (4) gained standard liquid
Compare, draw kind and the concentration of heavy metal in described water sample to be measured.
Heavy metal analysis in water associated with a kind of SPE the most according to claim 1 and XFR
Method, it is characterised in that described metal enrichment sheet is resin sheet.
Heavy metal analysis in water associated with a kind of SPE the most according to claim 2 and XFR
Method, it is characterised in that described resin sheet uses ion exchange resin, specially cationic ion-exchange resin
Or anion exchange resin.
Heavy metal analysis in water associated with a kind of SPE the most according to claim 1 and XFR
Method, it is characterised in that multiple different heavy metals described in step (4) be lead, chromium, cadmium, mercury, arsenic,
Selenium, antimony, barium.
Heavy metal analysis in water associated with a kind of SPE the most according to claim 1 and XFR
Method, it is characterised in that calibration curve described in step (4) is according to heavy metal in described standard liquid
Ascending or the descending drafting of concentration forms.
6. heavy metal analysis side in water associated with a SPE as claimed in claim 1 and XFR
Detection device used by method, it is characterised in that include pretreating device and XFR detector successively, described
It is provided with a mobile platform below pretreating device and XFR detector, also includes being arranged at described mobile platform
On solid-phase extraction device, by mobile platform, solid-phase extraction device is delivered to pretreating device and XFR
Below detector;
There is in described pretreating device the filter for filtering the solid particle in water sample to be measured, described
Solid phase extraction device is provided with the metal enrichment sheet for enriching heavy metal.
Detection device used by heavy metal detection method in water the most according to claim 6, its feature
It is, is additionally provided with perfusor, described pretreating device and perfusor upper end below described pretreating device equal
Being provided with injection port, lower end is equipped with outlet, the outlet of described pretreating device and the sample introduction of perfusor
Mouth connection, is provided with sample feeding pipe at the injection port of described pretreating device, described solid-phase extraction device includes setting
The metal enrichment sheet that the sampler being placed on mobile platform and sampler top are placed.
Detection device used by heavy metal detection method in water the most according to claim 7, its feature
Being, described sampler top is additionally provided with memory, is used for storing metal enrichment sheet, and described XFR detects
Instrument is positioned at the right side of described pretreating device, and described memory is positioned at the left side of described pretreating device.
Detection device used by heavy metal detection method in water the most according to claim 6, its feature
Being, described metal enrichment sheet is resin sheet.
Detection device used by heavy metal detection method in water the most according to claim 9, it is special
Levying and be, described resin sheet uses ion exchange resin, specially cationic ion-exchange resin or anion to hand over
Change resin.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107271469A (en) * | 2017-06-08 | 2017-10-20 | 上海市环境科学研究院 | The heavy metal in water semi-quantitative analysis method analyzed based on X-ray fluorescence spectra |
CN108910419A (en) * | 2018-05-03 | 2018-11-30 | 北京安科慧生科技有限公司 | Resin sheet taking device, element ion enrichment device and resin sheet |
CN109342474A (en) * | 2017-08-01 | 2019-02-15 | 北京安科慧生科技有限公司 | Solid phase extraction concentration device and with its associated with XRF |
CN110068589A (en) * | 2019-04-28 | 2019-07-30 | 天津迪沃特生物电子科技有限公司 | The device and method of heavy metal in a kind of on-line analysis water |
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 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107271469A (en) * | 2017-06-08 | 2017-10-20 | 上海市环境科学研究院 | The heavy metal in water semi-quantitative analysis method analyzed based on X-ray fluorescence spectra |
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CN108910419A (en) * | 2018-05-03 | 2018-11-30 | 北京安科慧生科技有限公司 | Resin sheet taking device, element ion enrichment device and resin sheet |
CN110068589A (en) * | 2019-04-28 | 2019-07-30 | 天津迪沃特生物电子科技有限公司 | The device and method of heavy metal in a kind of on-line analysis water |
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 |
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Application publication date: 20160824 |