CN103743655B - Method for determining inorganic arsenic in soil or water body based on diffusive gradients in thin-films technique - Google Patents
Method for determining inorganic arsenic in soil or water body based on diffusive gradients in thin-films technique Download PDFInfo
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- CN103743655B CN103743655B CN201410049733.4A CN201410049733A CN103743655B CN 103743655 B CN103743655 B CN 103743655B CN 201410049733 A CN201410049733 A CN 201410049733A CN 103743655 B CN103743655 B CN 103743655B
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Abstract
The invention discloses a method for determining inorganic arsenic in soil or a water body (comprising precipitates) based on DGT (Diffusive Gradients in Thin-Films Technique); gel films (Zr-oxide films) prepared by adopting zirconium dioxide as adsorbent are fixed films based on the diffusive gradients in thin-films principle; the gel films, diffusion films and the like are assembled to a DGT device; after the DGT device is contacted with the soil or a water body (comprising precipitates) for 1-6 days, the Zr-oxide films in the device are taken out to extract and measure the accumulation of the inorganic arsenic in the Zr-oxide films; the concentration of the inorganic arsenic is calculated according to the Fick first diffusion law. The method applies the Zr-oxide films to the DGT determination method of the inorganic arsenic; compared with the existing ferrihydrite DGT and Metsorb DGT methods, the method has the characteristics of high volume, long storage time and strong PO43-interference resistance.
Description
Technical field
The present invention relates to a kind of to soil, water body（Including deposit）Deng the assay method of inorganic arsenic in surrounding medium, can
A+E for the migratory activity of inorganic arsenic, biological effectiveness, pollution risk etc. in surrounding medium.
Background technology
Diffusive gradients in thin-films（Diffusive Gradients in Thin Films, DGT）Technology is a kind of new shape
State analytical technology, is mainly grown up in the mid-90 in last century by Lancaster university of Britain Davison and Zhang etc..
This technology is based on ion diffusion principle, by object ion in the diffusion defining diffusion layer and association process research, obtains
Obtain ion activated information in media as well.The device of DGT determination techniques is made up of fixed layer and diffusion layer superposition, and ion is to spread
Mode passes through diffusion layer, immediately fixed layer capture, and forms linear gradient distribution on diffusion layer, and it is near fixing film one end
Ion concentration be maintained zero, contact the concentration of one end with medium（）For：
In above formulaMAccumulation (mol cm for ion on fixing film-2),For thickness of diffusion layer (cm), DgExist for ion
Diffusion rate (cm in diffusion barrier2s-1), t is diffusion time（s）.It is standing time section by putting down that DGT analysis obtains
All concentration (mol L-1).
Ion migration in DGT diffusion process and actual environment and bioadsorption processes have comparability, and this technology is
As a kind of new morphological analyses means, be gradually applied to water body, soils and sediments research in, object of study is from conventional
Metallic element expands to yttrium and nonmetalloid etc..
Arsenic（As）Organized by international cancer（IARC）It is classified as a class carcinogen.Multiple natures and human activity cause in a large number
Arsenic spreads so that arsenic pollution has become international environmental problem in earth's surface and underground environment.Especially underground water outlet arsenic is exceeded
With Oryza sativa L. arsenic pollution, due to being related to the diet of billions of populations, safe drinking water it is considered to be the environmental disaster in 20-21 century.
Arsenic in the environment mainly presented in inorganic ionss, with trivalent inorganic arsenic in the reducing environments such as rice soil, deposit（As
(III)）Based on.Toxicity due to inorganic arsenic is higher than organo-arsenic, is the important prerequisite evaluating arsenic pollution risk to its Accurate Determining.
DGT technology has been used for the mensure of inorganic arsenic in soil and water body, and main technology has two kinds：（1）A kind of method
It is to utilize（Hydrogen）Ferrum oxide（ferrihydrite）The gel film made for adsorbent, as fixing film, is prepared according to fixing film
Method divides into sludge-type and sedimentation type, and the former is business-like material at present, but exists and measure that capacity is low, storage time is short（6
Individual month）Etc. defect；The latter is measured capacity compared with the former and has and improves by a small margin, but storage time shortens to 38 days.（2）Another kind of
Method is to utilize titanium dioxide（Trade name Metsorb）The gel film made for adsorbent is as fixing film.This fixing film
Technical performance is relatively stable, and storage time is not still reported, but is only the 37% of mud sections film to the mensure capacity of As (III),
Therefore can not be applied in the reducing environments such as rice soil, the deposit of high As (III) content.
Additionally, DGT is to PO4 3-There is Competition in the absorption with inorganic arsenic ion.Due to PO in environment4 3-Content generally than
Inorganic arsenic exceeds the 1-2 order of magnitude, and DGT technical measurement arsenic will be produced with great interference.Existing two kinds of DGT technology
（Ferrihydrite DGT and Metsorb DGT）Low to the mensure capacity of arsenic, therefore anti-PO4 3-Interference performance is weak.
Content of the invention
It is an object of the present invention to provide a kind of be based on DGT technical measurement soil and water body（Including deposit）The side of middle inorganic arsenic
Method, can overcome existing DGT technology short, anti-for not enough, the fixing film storage time of installed capacity present in inorganic arsenic mensure
PO4 3-A series of defects such as interference performance is weak.
Above-mentioned purpose of the present invention is achieved through the following technical solutions：One kind is based on nothing in DGT technical measurement soil or water body
The method of machine arsenic is it is characterised in that described method is fixing film using zirconium dioxide for the gel film that adsorbent is made.
Preferably, the gel film that described fixing film is configured to using polyacrylamide and Zirconium dioxide powder（Below
Referred to as " Zr-oxide film "）, relevant Zr-oxide film and preparation method thereof, detailed technology content can be found in Chinese invention patent
CN200910183047.5.
As well known to those skilled in the art, DGT measures the structure being provided with fixing film, diffusion barrier and permeable membrane superposition in device.
DGT method is based on diffusive gradients in thin-films principle, DGT mensure device is put into and extracts determinand in surrounding medium and by fixing film
Capture, i.e. the method measuring inorganic arsenic in soil or water body of the present invention, using the DGT device comprising Zr-oxide film, by it
With soil or water body（Including deposit）Contact, after placing 1-6 days, Zr-oxide film in withdrawing device, extracts and measures Zr-
The accumulation of inorganic arsenic in oxide film, is calculated the concentration of inorganic arsenic according to Fick first diffusion law.
About DGT device, the fixing recovery of film or the place of section, the extraction of inorganic arsenic ion and mensure and determination data
Reason etc., all can realize according to DGT technology in prior art.
Specifically, described method comprises the following steps：
(1) DGT device assembling：It is assembled into DGT device after Zr-oxide film, diffusion barrier, permeable membrane are sequentially overlapped；
(2) nitrogen charging：DGT device is put in the container filling deionized water, is filled with pure nitrogen gas in water and removes DGT device
In the oxygen that contains；
(3) DGT device is placed：DGT device is put into soil（Add water in advance moistening）, in water body or deposit, during placement
Between be 1-6 days；
(4) Zr-oxide film reclaims and cuts into slices：After DGT device is taken out, take out Zr-oxide film deionized water punching
Put in container after washing；For the mensure of arsenic in deposit, first Zr-oxide film is cut into slices, then by each Zr-oxide
Film section is respectively put in container；
(5) arsenic extracts：Compare 1 according to Zr-oxide film with extracting liquid volume:10 to 1:100 add extracting solution in container,
Vibrate 24 hours under room temperature；Extracting solution can adopt 1.0 M NaOH（Mensure for fresh water system）Or 1.0 M NaOH and 1.0
M H2O2Mixed liquor（Mensure for sea water or brine system）；
(6) arsenic measures：From step（5）Each container in draw appropriate extracting solution, after dilution, using hydride occur-
Atomic fluorescence spectrum（HG-AFS）Or inductivity coupled plasma mass spectrometry (ICP-MS) method measures the arsenic in extracting solution
Concentration；
(7) arsenic accumulation (M) conversion on Zr-oxide film：Calculated according to below equation,
WhereinC eIt is the concentration of inorganic arsenic in extracting solution,V e It is extracting liquid volume after dilution,V g It is Zr-oxide membrane volume,f e It is the extraction ratio of arsenic, be 87.7% when using 1.0 M NaOH for extracting solution, using 1.0 M NaOH and 1.0 M H2O2Mixed
Close liquid for being 91.7% during extracting solution；
(8) DGT concentration conversion：Calculated according to Fick First Law,
In above formula,For spreading film thickness, unit is cm；For diffusion coefficient in diffusion barrier for the inorganic arsenic ion,
Unit is cm2/s（25 DEG C is 8.69 × 10-6cm2/s）；For DGT device exposed area, unit is cm2；T is standing time,
Unit is the second,For the concentration of inorganic arsenic ion, unit is g/L.
Gel film with zirconium dioxide as adsorbent（Zr-oxide film）The method being generally used for DGT technical measurement phosphorus
In, Zr-oxide film is used in the DGT assay method of inorganic arsenic the present invention, with existing ferrihydrite DGT and
Metsorb DGT method is compared, and has capacity height, storage time length, anti-PO4 3-The strong feature of interference performance.
Table 1
aBennett et al., (2011);bPrice et al., (2013);cLuo et al.,(2010);d
Panther et al.,(2008);eHuynh et al.,(2012).
Table 1 be the Capacity Ratio of three kinds of DGT technology relatively, the capacity data of wherein Zr-oxide film DGT method is applicant
Practical measurement obtains, and ferrihydrite DGT and Metsorb DGT capacity data are collected from document report.Permissible from table 1
Find out, Zr-oxide film DGT method is other two kinds of DGT methods to the mensure capacity of As (III) and As (V) in fresh water system
5-19 times, be 3-13 times of other two kinds of DGT methods to the mensure capacity of As in seawer system (III) and As (V).Application
The research of people shows（Fig. 1-Fig. 7）, compared with existing DGT method, the assay method of inorganic arsenic of the present invention is measuring capacity, is being suitable for
PH scope, fixing film storage time, anti-PO4 3-The aspects such as interference performance all increase significantly.
In a word, the inventive method at least has advantages below and beneficial effect：
（1）The Zr-oxide film that the present invention adopts can store more than 24 months at normal temperatures, and existing arsenic measures DGT and fixes
Film can only store 6 months；
（2）The inventive method adopts Zr-oxide film to be used for arsenic ion DGT method for measuring, and the pH scope of adaptation is
2.0-9.1, existing DGT device may be only available for the surrounding medium that pH is 3.0-8.5；
（3）The inventive method is 159 to the mensure capacity of As (III) inorganic in fresh water system and As (V)µG and 434µ
G, is 5-19 times of existing DGT technology, and the mensure capacity to As (III) inorganic in seawer system and As (V) is 94µG and 152µG, is 3-13 times of existing DGT technology；
（4）The inventive method is to PO4 3-There is very strong capacity of resisting disturbance, in tolerable environment, there is more than 10mg P/L
Phosphate anion, existing DGT device only allows-0.5 mg P/L（When measuring As (III)）With 2.5 mg P/L（Measure As
(V) when）.
Brief description
Fig. 1 is effective storage time of Zr-oxide film（>24 months）.WhereinC SOLDense for arsenic ion inorganic in solution
Degree,C DGTMeasure the inorganic arsenic ion concentration obtaining for Zr-oxide DGT, when both ratios coincide（I.e.C DGT/C SOLRatio exists
Between 0.9-1.1）, illustrate that Zr-oxide DGT measures accurately.As can be seen from Figure 1, after Zr-oxide film stored to 24 months,
The DGT of assembling still can be with the inorganic arsenic ion concentration in Accurate Determining solution（I.e.C DGT/C SOLRatio is between 0.9-1.1）.
Fig. 2 is that Zr-oxide DGT measures the pH scope adapting to（2.0-9.1）.When pH changes between 2.0-9.1,
Zr-oxide DGT measures and keeps accurately（I.e.C DGT/C SOLRatio is between 0.9-1.1）.
Fig. 3 is to PO during three kinds of DGT technical measurement As (III)4 3-Capacity of resisting disturbance.Work as PO4 3-Concentration increases to 10mg/
During L, Zr-oxide DGT measured value keeps accurately.Work as PO4 3-When concentration is 0.25 and 0.50 mg/L, ferrihydrite DGT
Reduce with Metsorb DGT measured value（I.e.C DGT/C SOLRatio is less than 0.9）, PO is described4 3-Both DGT mensure is produced aobvious
The impact writing.
Fig. 4 is to PO during three kinds of DGT technical measurement As (V)4 3-Capacity of resisting disturbance.Work as PO4 3-Concentration increases to 10mg/L
When, Zr-oxide DGT measured value keeps accurately.Work as PO4 3-Concentration be 0.50 and 2.5 mg/L when, ferrihydrite DGT and
Metsorb DGT measured value starts to reduce（I.e.C DGT/C SOLRatio is less than 0.9）, PO is described4 3-Both DGT are measured and produces
Significant impact.
Fig. 5 is the comparison of three kinds of DGT technical measurement sea water inorganic arsenics.When DGT device standing time extends to 100h, Zr-
Oxide DGT measured value keeps accurately.When being respectively 24h and 48h between when left, ferrihydrite DGT and Metsorb
DGT measured value starts to reduce, and two kinds of DGT finite capacities is described, the absorption to arsenic ion quickly reaches saturation.
Fig. 6 and Fig. 7 is the comparison of three kinds of DGT technical measurement soil inorganic arsenic.Have chosen 29 kinds of different soil of total arsenic content
Earth is tested, when Zr-oxide DGT absorbtivity is 10µWhen below g As/ device, ferrihydrite DGT and
The absorbtivity of Metsorb DGT is consistent with Zr-oxide DGT（Fig. 6）；When Zr-oxide DGT absorbtivity reaches 23µg
During As/ device, ferrihydrite DGT absorbtivity starts reduction；When Zr-oxide DGT absorbtivity reaches 78µg As/
During device, reducing occurs in Metsorb DGT absorbtivity（Fig. 7）.Above Discrepancy Description ferrihydrite DGT and Metsorb
DGT is lower than Zr-oxide DGT to the absorptive capacity of arsenic in soil.
Fig. 8 is to measure inorganic arsenic ion in the Taihu Lake Sediment obtaining using the inventive method by Zr-oxide DGT to contain
The profile of amount.
Specific embodiment
Analyzed as example with the DGT of inorganic arsenic in Taihu Lake Sediment below, the present invention will be further described.
Zr-oxide film adopts with zirconium dioxide as adsorbent, by acrylamide, Zirconium dioxide powder is made gel thin
Film, the method preparation specifically disclosing according to Chinese invention patent CN200910183047.5.
According to the present invention, Zr-oxide film DGT device is put in Lake Taihu deposit, take out after 48 hours, fortune
Return laboratory, the arsenic on fixing film is analyzed, obtained in core sediments by the accumulation conversion of arsenic on fixing film and live
The content of property arsenic and spatial distribution（Fig. 8）.
Concrete operations include：
(1) DGT device assembling：It is assembled into DGT device after Zr-oxide film, diffusion barrier, permeable membrane are sequentially overlapped；
(2) nitrogen charging：DGT device is put in the container filling deionized water, is filled with pure nitrogen gas in water and removes DGT device
In the oxygen that contains；
(3) DGT device is placed：DGT device is saved in sealing container, after being transported to lake region scene, device is vertically inserted
Enter in deposit, standing time is 4 days；
(4) Zr-oxide film reclaims：After device is taken out, open permeable membrane and diffusion barrier successively, Zr-oxide film is used
After deionized water rinsing, put into preprepared plastic containers（Generally centrifuge tube）In；
(5) Zr-oxide film section：To part below fixing film water/sediment interface, pressed one-dimensional with microtome knife（Deposit
Vertical）The strip fragment of 2mm width is cut in direction, and each fragment is chosen, and puts in the plastic centrifuge tube of 1.0ml；
(6) arsenic extracts：Compare 1 according to Zr-oxide film with extracting liquid volume:10 add 1.0MNaOH in each centrifuge tube,
Vibrate 24 hours under room temperature；
(7) arsenic measures：From step（6）Each centrifuge tube in draw the solution of 0.2ml, after appropriate dilution, adopt
Hydride generation-atomic fluorescence spectrometry spectrophotography（HG-AFS）Measure the arsenic concentration in extracting solution；
(8) arsenic accumulation (M) conversion on Zr-oxide film：Calculated according to below equation,
WhereinC eIt is the concentration of inorganic arsenic in extracting solution,V e It is extracting liquid volume（After dilution）,V g It is Zr-oxide membrane volume
（0.15ml）,f e It is the extraction ratio (87.7%) of arsenic；
(9) DGT concentration conversion：Calculated according to Fick First Law,
In above formula,For diffusion film thickness (0.093cm)；For diffusion coefficient in diffusion barrier for the inorganic arsenic ion（25
DEG C be 8.69 × 10-6cm2/s）；A is DGT device exposed area (0.16cm2/ fragment)；T is standing time (345600 seconds),For the concentration of active phosphorus or ferrum, unit is g/L.
Fig. 8 is to measure the inorganic arsenic ion Soil profile obtaining, and finds arsenic ion content from interface（Sediment depth labelling
For 0）Increase sharply to about -20mm, be in subsequently reduction trend.Arsenic ion is probably that ferrum combines in the increase of near interface content
Release under the internal reducing condition of deposit for the state arsenic causes, and subsequent reduction should be the precipitation of arsenic and the metal ions such as calcium
Absorption with metalliferous mineral causes.
Claims (4)
1. a kind of method based on inorganic arsenic in DGT technical measurement soil or water body is it is characterised in that described method adopts two
Zirconium oxide is fixing film for the gel film that adsorbent is made；Described fixing film be using 200910183047.5 disclosed by
The gel film that polyacrylamide and Zirconium dioxide powder are configured to, as fixing film, is designated as Zr-oxide film.
2. the method measuring inorganic arsenic in soil or water body according to claim 1 is it is characterised in that using comprising Zr-
The DGT device of oxide film, it is contacted with soil or water body, after placing 1-6 days, Zr-oxide film in withdrawing device, extracts
And measure the accumulation of inorganic arsenic in Zr-oxide film, it is calculated the concentration of inorganic arsenic according to Fick first diffusion law.
3. the method measuring inorganic arsenic in soil or water body according to claim 2 is it is characterised in that described method bag
Include following steps：
（1）DGT device assembles：It is assembled into DGT device after Zr-oxide film, diffusion barrier, permeable membrane are sequentially overlapped；
（2）Nitrogen charging：DGT device is put in the container filling deionized water, is filled with water in pure nitrogen gas removal DGT device and contains
Some oxygen；
（3）DGT device is placed：DGT device is put in the damp soil that adds water in advance, water body or deposit, standing time is
1-6 days；
（4）Zr-oxide film reclaims and cuts into slices：After DGT device is taken out, after taking out Zr-oxide film deionized water flushing
Put in container；For the mensure of arsenic in deposit, first Zr-oxide film is cut into slices, then each Zr-oxide film is cut
Piece is respectively put in container；
（5）Arsenic extracts：Compare 1 according to Zr-oxide film with extracting liquid volume:10 to 1:100 add extracting solution, room temperature in container
Lower vibration 24 hours；
（6）Arsenic measures：From step（5）Each container in draw appropriate extracting solution, after dilution, using hydride generation-atomic
Fluorescence spectrophotometry or inductivity coupled plasma mass spectrometry method measure the arsenic concentration in extracting solution；
（7）Arsenic accumulation (M) conversion on Zr-oxide film：Calculated according to below equation,
WhereinC eIt is the concentration of inorganic arsenic in extracting solution,V e It is extracting liquid volume after dilution,V g It is Zr-oxide membrane volume,f e It is arsenic
Extraction ratio；
（8）DGT concentration conversion：Calculated according to Fick First Law,
In above formula,For spreading film thickness, unit is cm；For diffusion coefficient in diffusion barrier for the inorganic arsenic ion, unit is
cm2/s；A is DGT device exposed area, and unit is cm2；For standing time, unit is the second,Dense for inorganic arsenic ion
Degree, unit is g/L.
4. the method measuring inorganic arsenic in soil or water body according to claim 3 is it is characterised in that described extracting solution
1.0 M NaOH solution are adopted to the mensure of fresh water system, 1.0 M NaOH and 1.0 are adopted to the mensure of sea water or brine system
M H2O2Mixed liquor.
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| CN104198405B (en) * | 2014-08-11 | 2016-08-24 | 渤海大学 | A kind of biologically effective phosphorus yield method in soil |
| CN104492376A (en) * | 2014-12-19 | 2015-04-08 | 南京大学 | Preparation method of activated carbon adsorption film and method for measuring bisphenol substances in wetland soil or sediment based on thin-film diffusion gradient technique |
| CN104568673B (en) * | 2014-12-25 | 2017-02-22 | 安徽建筑大学 | Mg(OH)2-based phosphorus binding film as well as preparation and application thereof |
| CN106290785B (en) * | 2016-07-29 | 2019-01-11 | 农业部环境保护科研监测所 | A method of soil heavy metals of different forms is separated using DGT technology |
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| CN108680726B (en) * | 2018-05-08 | 2020-06-26 | 中国科学院地球化学研究所 | DGT enrichment membrane for determining bioavailability Hg (II) of paddy field soil solution and preparation method thereof |
| US11319225B2 (en) | 2018-10-24 | 2022-05-03 | Savannah River Nuclear Solutions, Llc | Modular system and method for mercury speciation in a fluid sample |
| CN109580762A (en) * | 2018-11-28 | 2019-04-05 | 南京维申环保科技有限公司 | A kind of method of biomembrane DGT device and simultaneous quantitative detection target bio-available Zn concentration and cytogenetic toxicity |
| CN110849776A (en) * | 2019-11-26 | 2020-02-28 | 中国科学院城市环境研究所 | Method for measuring content of effective silicon in water body and soil |
| CN114152543B (en) * | 2021-11-15 | 2024-01-02 | 东南大学 | Device and method for researching migration and diffusion of in-situ injection medicament in soil layer |
| CN115758690B (en) * | 2022-11-07 | 2023-11-24 | 中国科学院烟台海岸带研究所 | Site soil arsenic bioavailability prediction model, construction method and application thereof |
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