CN102565111B - Method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions - Google Patents
Method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions Download PDFInfo
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Abstract
The invention relates to the field of detection and analysis of heavy metal ions in water solution, and particularly discloses a method for simultaneous enrichment and analysis of heavy metal lead, cadmium and mercury ions, which adopts diethyl disulfide sodium formate or dithizone as a complexing agent, so as to realize complexation with the lead, cadmium and mercury ions to form metal complex, wherein the metal complex is extracted and enriched through the dispersive liquid phase micro-extraction technology, and qualitative and quantitative analysis is simultaneously performed on the lead, cadmium and mercury ions in the water solution through the X-ray fluorescence spectrum technology. The enrichment multiples of the lead, cadmium and mercury ions in the water solution are high, the enrichment is complete, the operation is simple and quick, and the simultaneous qualitative and quantitative analysis on the lead, cadmium and mercury ions is realized.
Description
Technical field
The present invention relates to the detection analysis field of heavy metal ion in aqueous solution, the while of relating to a kind of particularly, heavy metal ion lead, cadmium and mercury carry out the method for enrichment and analysis.
Background technology
In article and environment, the harm of heavy metal element is subject to the understanding of the whole society day by day, and focus hazardous events emerges in an endless stream, as a lot of area occurs that blood lead exceeds standard event etc.Maximum with the harm of lead, cadmium and mercury in heavy metal element in environment, also institute of society is cognitive the most, and its detection method and standard are also a lot.In article articles for children due to children's intimate contact, heavy metal contained by it is sucked by Among Children, add lane, the behavioural habits such as to swallow brings in human body by harmful element, heavy metal can be put aside in vivo for a long time, serious harm is produced like this by the health of children, so its heavy metal limit is also strict, as International Toy Safety standard-Part III: migration (the ISO 8124-3 of element-specific, second edition 2010-04-01) give lead, cadmium and mercury migration limitation, be respectively plumbous 90mg/kg, cadmium 50mg/kg and mercury 25mg/kg; China's national toy technical specification of security (GB 6675-2003), European Union EN71-3:1994/AC:2002(toy safety the 3rd part: the migration of element-specific), American National Toy Safety Standards (ASTM F963-08 Standard Consumer Safety Specification for Toy Safety) and Japanese Toy Safety Standards (ST 2002 TOY SAFETY STANDARD) give also identical limitation requirement.The harm approach of plumbous in article and environment, cadmium and mercury is mainly through aqueous solution transmission, therefore the content detection of lead, cadmium and mercury in aqueous solution is absolutely necessary, its extracting and enriching and detection method varied, extraction and enrichment method is as Solid-Phase Extraction, molecular engram, solid-phase microextraction, hanging drop micro-extraction and the liquid-phase micro-extraction etc. based on hollow fiber, and detection method is as spectrophotometric method, flame atomic absorption method, inductively coupled plasma transmitting or mass spectroscopy etc.The meticulous detection method of constituent content has atom extinction spectrum method (conventional has graphite furnace, flame and hydride generation method etc.), atomic fluorescence spectrometry, inductively coupled plasma emission spectrography, inductively coupled plasma mass spectrometry etc.According to respective technical specifications requirement, at present except icp ms, other type analysis equipment is difficult to the detection directly completing above-mentioned element.But icp ms is expensive, operation and maintenance cost is high, and a lot of laboratory is difficult to bear, and causes popularity rate lower.In addition, the rapid screening method that simultaneously can detect these three kinds of elements has wavelength dispersion X-ray fluorescence spectrometer, energy-dispersion X-ray fluorescence spectrometer, laser ablation sample introduction-plasma light spectral technology (LA-ICP) and laser ablation sample introduction-plasma mass technology (LA-ICP/MS) etc.In these techniques, energy-dispersion X-ray fluorescence spectrometer is due to without the need to sample preparation, the advantage such as easy and simple to handle and being widely used.But rapid screening mode especially x ray fluorescence spectrometry has to be strengthened in accurate quantitative analysis, its detection limit is than meticulous method generally low 1 number magnitude, and sensitivity more and more cannot meet the requirement that the increasingly strict poisonous and harmful element of content detects.
Dispersive liquid-liquid microextraction (dispersive liquid-liquid microextraction, DLLME) be a kind of novel sample pretreatment, by RezaeeM etc., (RezaeeM is proposed first for 2006, A ssad iY, Milan iHosse in iM R, Aghaee E, Ahmadi F, Berijani S. J. Chromatogr. A, 2006,1116:1 ~ 9), the method centralized procurement sample, extract and concentrate in one, be a kind of simple to operate, quick, low cost, bioaccumulation efficiency are high and environment amenable Sample Pretreatment Technique.First the method adds several tens of microliters extractant and certain volume spreading agent in sample solution, namely mixed liquor forms the emulsion system of a water/spreading agent/extractant after vibrating gently, again through centrifugal layering, take out extractant with regard to direct injection analysis with microsyringe.At present, it is little that this technology is applied to metal element analyse in sample, and especially multielement Sync enrichment is not reported, only has the paper of certain ultimate analysis, as cadmium (Zeini Jahromi E, BidariA, AssadiY, Milani Hosseini M R, Jamali M R. Anal. Ch im. Acta, 2007,585:305 ~ 311) and plumbous (Liang P, Sang H B. Anal. Biochem., 2008,380:21 ~ 25).
The invention solves that the detection sensitivity existed in prior art detection method is limited, detection method is high and cannot realize carrying out the defects such as detection analysis to various heavy to equipment requirement simultaneously, the while of proposing a kind of, plumbous, the cadmium of heavy metal ion and mercury carry out the method for enrichment and analysis.The inventive method detects that the time limit is short, detection sensitivity is high, can realize carrying out tens of extremely enrichment of hundreds of times to more than one contents of many kinds of heavy metal ion, and carries out qualitative and quantitative detecting analysis.
Summary of the invention
The while of the present invention proposes a kind of, heavy metal ion lead, cadmium and mercury carry out the method for enrichment and analysis, with diethyl-dithio sodium formate or dithizone for complexing agent, the metal complex being insoluble in water is formed with the complexing simultaneously of lead, cadmium and mercury ion, adopt dispersive liquid-liquid microextraction technology to carry out extracting and enriching to described metal complex, and adopt X-ray fluorescence spectra technology to carry out qualitative and quantitative analysis to lead, cadmium and mercury ion in extraction solution simultaneously.
Wherein, when complexing agent is diethyl-dithio sodium formate, complexing agent forms the course of reaction of the metal complex being insoluble in water as shown in the formula shown in (I) with the complexing simultaneously of lead, cadmium and mercury ion:
Wherein, M is lead, cadmium, mercury.
Wherein, when complexing agent is dithizone, complexing agent forms the course of reaction of the metal complex being insoluble in water as shown in the formula shown in (II) with the complexing simultaneously of lead, cadmium and mercury ion:
Wherein, M is lead, cadmium, mercury.
Wherein, under pH 2.5-5 condition, extracting and enriching is carried out to described metal complex.
Wherein, described method using acetone, methyl alcohol, ethanol as spreading agent, using zellon as extractant.Described method using acetone, methyl alcohol, ethanol as spreading agent, using zellon as extractant.
Wherein, adopt described X-ray fluorescence spectra technology to carry out qualitative detection to the lead in dispersive liquid-liquid microextraction organic phase, cadmium and mercury ion simultaneously.
Wherein, the content of lead, cadmium and mercury ion in described X-ray fluorescence spectra technology Simultaneously test dispersive liquid-liquid microextraction organic phase is adopted.
Wherein, the enrichment times of described method is tens of to hundreds of times.
Wherein, the detection limit of described method to lead, cadmium and mercury ion is respectively 0.10 mg/L.
The present invention proposes a kind of XRF Simultaneous multi element analysis method of lead, cadmium and mercury in Sync enrichment aqueous phase, this method first with diethyl-dithio sodium formate (DDTC) or dithizone (HDZ) for complexing agent, under pH 2.5-5 condition, plumbous in complexing agent and aqueous solution, cadmium and mercury ion complexing simultaneously, form corresponding with three metal ion species three kinds of metal complexs being insoluble in water respectively; Adopt dispersive liquid-liquid microextraction technology again, add to these three kinds of metal complex solubleness far above the extractant of water, utilize the formation of micro emulsion liquid phase, realize the transfer of metal complex to extractant, thus reach the extraction of heavy metal ion and the object of high multiple enrichment.This method adopts the common extractants such as common spreading agent and zellon such as acetone, complex compound is belonged to GOLD FROM PLATING SOLUTION and carries out decades of times to the extracting and enriching of hundreds of times simultaneously, adopt energy color dispersing X fluorescent spectrometer directly to go out peak to lead, cadmium and mercury ion scanning in extraction solution to carry out qualitative and quantitative analysis, whole analytic process is no more than 10 minutes simultaneously.
The present invention utilizes diethyl-dithio sodium formate (DDTC) to be complexing agent, under pH 2.5-5 buffer solution condition, metal complex is formed with lead, cadmium and mercury ion complexing simultaneously in the aqueous solution of certain volume, add the spreading agent of several tens of microliters zellon extractant and certain volume, through centrifugal layering after ultrasonic process, Xray fluorescence spectrometer carries out qualitative and quantitative analysis to lead, cadmium and mercury element in lower floor's extraction solution simultaneously, and whole analytic process is no more than 10 minutes.
The present invention utilizes dithizone (HDZ) to be complexing agent, under pH 2.5-5 buffer solution condition, metal complex is formed with lead, cadmium and mercury ion complexing simultaneously in the aqueous solution of certain volume, add the spreading agent of several tens of microliters zellon extractant and certain volume, through centrifugal layering after ultrasonic process, Xray fluorescence spectrometer carries out qualitative and quantitative analysis to lead, cadmium and mercury element in lower floor's extraction solution simultaneously, and whole analytic process is no more than 10 minutes.
The present invention utilizes dispersive liquid-liquid microextraction technology to extract plumbous in solution, cadmium and mercury metal complex, and according to the ratio of selected extractant and aqueous phase volume, the enrichment times scope of the inventive method heavy metal ion is that decades of times arrives hundreds of times.
The present invention utilizes dispersive liquid-liquid microextraction technology to extract lead, cadmium and mercury metal complex in solution, Xray fluorescence spectrometer carries out qualitative and quantitative analysis, and set up relevant work curve, this method can reach 0.10 mg/L respectively to the detection limit of various heavy metal ion.
The present invention utilizes dispersive liquid-liquid microextraction technology can the advantage of high multiple enriched sample, and partial metal complex is insoluble in the character of water, construct and described three heavy metal species ions are transferred to extractant from aqueous phase simultaneously, and by the method for enrichment 100 times.Meanwhile, under the prerequisite that concentration of heavy metal ion improves greatly, achieve and use X fluorescence spectrum method rapid screening and sensitive test soluble heavy metal ions concentration.Propose a kind of heavy metal Element Lead simultaneously, cadmium and mercury carry out the method for enrichment and analysis, with diethyl-dithio sodium formate (DDTC) or dithizone (HDZ) for complexing agent, under pH 2.5-5 condition, plumbous in complexing agent and aqueous solution, cadmium and mercury ion complexing simultaneously, formed on metal complex basis, dispersive liquid-liquid microextraction technology is adopted to extract, select common spreading agent and the zellons etc. such as acetone and common extractant, complex compound is belonged to GOLD FROM PLATING SOLUTION and carries out decades of times to the extracting and enriching of hundreds of times simultaneously, finally adopt Xray fluorescence spectrometer to plumbous in extraction solution, cadmium and mercury element carry out qualitative and quantitative analysis simultaneously, whole analytic process is no more than 10 minutes.The inventive method enrichment analyzing detect concentration of heavy metal ion have with low cost, simply, advantage maintain good specificity and high sensitivity fast.
Accompanying drawing explanation
Fig. 1 be the inventive method using dithizone as complexing agent time enrichment three heavy metal species ion process schematic.Wherein, two points of samples in Fig. 1 (a) are respectively blank water sample and standard solution (wherein three heavy metal species ion concentrations are 1.0mg/L); Two parts of samples of Fig. 1 (b) are the micro emulsion liquid phase formed after adding spreading agent and extractant; Fig. 1 (c) is extractant and aqueous phase layering after centrifugal 5min, and extractant is sunken to centrifuge tube lower end.
Fig. 2 is that before extraction, water sample scans spectrogram with the energy color dispersing X fluorescent spectrometer of the rear extractant of extraction.Wherein, Fig. 2 (a) is water sample spectrogram before extraction, and at spectrum peak position corresponding to Pb, Cd, Hg tri-kinds of elements without corresponding peak, Fig. 2 (b) is the spectrogram of lower floor's extractant after extraction, has obviously go out peak at the spectrum peak position that Pb, Cd, Hg tri-kinds of elements are corresponding.
Fig. 3 be the inventive method using dithizone as complexing agent time, X fluorescence spectrometer response to be mapped the canonical plotting obtained to concentration of heavy metal ion in aqueous phase.In water sample, the concentration of Pb, Cd, Hg heavy metal ion is identical, is 0 ~ 2.0mg/L.
Fig. 4 be the inventive method using diethyl-dithio sodium formate as complexing agent time, X fluorescence spectrometer response to be mapped the canonical plotting obtained to concentration of heavy metal ion in aqueous phase.In water sample, the concentration of Pb, Cd, Hg heavy metal ion is identical, is 0 ~ 2.0mg/L.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Under the spirit and scope not deviating from inventive concept, the change that those skilled in the art can expect and advantage are all included in the present invention, and are protection domain with appended claims.
embodiment 1:
It is as follows that the inventive method comprises experimental procedure, and described condition is the result after optimization.Present invention uses two heavy metal species complexing agents, be respectively dithizone (HDZ) and diethyl-dithio sodium formate (DDTC).
The experimental procedure that employing dithizone implements the inventive method is as follows: first, by the Pb containing 1mg/L concentration
2+, Cd
2+, Hg
2+water sample adjust ph is after 4.0, and the water sample taking out 5mL volume adds (as shown in Figure 1a) in centrifuge tube.Then, using the dithizone solution (wherein the concentration of dithizone is 0.1% massfraction) of 50 μ L zellons and 500 μ L acetone (as spreading agent, also methyl alcohol can be used, ethanol etc. are soluble in water, also the reagent dissolved each other with zellon) mix after, use one-shot injector to be added in water sample fast by mixed liquor, and immediately ultrasonic to formed homogeneous microemulsion liquid (ultrasonic time 15s, as shown in Figure 1 b).Finally, by centrifugal 5 minutes of the microemulsion formed, zellon is separated (as illustrated in figure 1 c).Abandoning supernatant, lower floor's zellon is mutually to be tested.The non-complexing of dithizone in blank water sample, microemulsion is aobvious green, and shows the redness of complex state containing dithizone in the microemulsion of the water sample of heavy metal ion.Through centrifuging, the zellon containing dithizone is sunken to bottom test tube mutually.
The experimental procedure that employing diethyl-dithio sodium formate implements the inventive method is as follows: first, will containing certain density Pb
2+, Cd
2+, Hg
2+water sample adjust ph is after 4.0, and the water sample taking out 5mL volume adds in centrifuge tube, adds the DDTC aqueous solution of 20g/L in this water sample, shakes up to leave standstill 1 minute afterwards.Using 50 μ L zellons and 500 μ L ketones (as spreading agent, also acetone can be used, ethanol etc. are soluble in water, also the reagent dissolved each other with zellon) mix after, one-shot injector is used to be added in water sample fast by mixed liquor, and ultrasonic to forming homogeneous microemulsion liquid (ultrasonic time 15s) immediately.Finally, by centrifugal 5 minutes of the microemulsion formed, abandoning supernatant, lower floor's zellon is mutually to be tested.
Because the heavy metal complex state of DDTC is water white transparency shape, experimental phenomena is not obvious, therefore does not take pictures.Blank water sample and see Fig. 2 containing the XRF scanning result of heavy metal water sample.Fig. 2 a is the zellon scanning phase result not adding DDTC, at spectrum peak position corresponding to Pb, Cd, Hg tri-kinds of elements without corresponding peak; Fig. 2 b is the zellon scanning phase result adding DDTC, has obviously go out peak at the spectrum peak position that Pb, Cd, Hg tri-kinds of elements are corresponding.After DDTC complexing, obviously can see Pb, the characteristic peak of Hg, Cd, the heavy metal ion illustrating in solution can be formed metal complex after DDTC complexing and be precipitated to zellon mutually in.Therefore, the inventive method is utilized can to realize simultaneously to enrichment and the qualitative analysis detection of contents of many kinds of heavy metal ion.
About the enrichment times of the inventive method, computing method are as follows,
Enrichment times=aqueous phase volume (μ L)/final phenixin phase volume (μ L)
Aqueous phase volume is that the phenixin phase volume of 5000 μ L, HDZ and DDTC is 30 μ L, therefore theoretical enrichment times is 167 times.As calculated, the actual enrichment times of the present embodiment experimental result is 143 times.Consider the loss in test operation, therefore, actual enrichment times may be slightly less than theoretical values.
embodiment 2:
the step of Criterion curve is:
The water sample that 5mL pH value is 4.0 is added respectively, wherein Pb in 6 25mL glass centrifuge tube
2+, Cd
2+, Hg
2+concentration be respectively 0,0.2,0.5,1.0,1.5,2.0mg/L;
(1) operate according to the step of embodiment 1, prepare two groups respectively with the zellon standard solution that HDZ and DDTC is complexing agent;
(2) get 20 μ L zellon phases, be placed in XRF sample cell, under 1000mV voltage, entirely compose scanning, sweep time 100s.Read the L α of Pb, the K α of the K α of Cd, Hg composes peak response value, and makes typical curve, sees shown in Fig. 3, Fig. 4;
Wherein, dithizone and DDTC available from Sigma, Pb (NO
3)
2, Cd (NO
3)
2solid is available from Sigma also, is mixed with 1000mg/L stock solution with ultrapure water (18M Ω), and the used time dilutes.Hg
2+standard solution available from Sigma, concentration is 1000mg/L, and the used time dilutes.Energy color dispersing X fluorescent spectrometer used is Horiba Products, and model is 1000WR.
In obtained typical curve, with variable concentrations heavy metal ion, XRF response is mapped;
The pre-service of testing sample: for fluid sample, uses 1mol/L NaOH or HNO after filtering
3adjust ph to 4.0; For solid sample, use nitric acid-hydrogen peroxide (7mL+1.5mL) micro-wave digestion, catch up with acid and use 1mol/LNaOH adjust ph to 4.0 after filtration.Get a certain amount of gained sample solution and replace standard solution, by step (1) ~ (3) operation, read XRF response.
According to the response of testing sample, look into typical curve, try to achieve content of beary metal in testing sample.
Pb in the inventive method
2+, Cd
2+, Hg
2+the determination limit of ion concentration is respectively 0.10mg/L, can meet laboratory routine testing needs completely.
embodiment 3: solubility Pb in toy sample
2+
, Cd
2+
, Hg
2+
the mensuration of ion
Normative reference: EN71-3:1994+A1:2001
The present embodiment is depicted as situation when testing sample is toy, all tests all parts of touching in toy sample.
sample preparation
For the toy of the types such as weaving face fabric, plastics or rubber, with scissors or pliers, material is cut into the fritter of 5mm × 5mm as testing sample.
For the toy with paint, ink or similar coatings, with clean blade using scraping part as testing sample.
For the toy for liquid paint or ink, get part and to be applied on clean glass plate after at room temperature natural drying, scrape as testing sample.As testing sample can not be at room temperature dry, then press serviceability temperature in drying in oven, scrape acquisition testing sample.
All powdery testing samples must use the sieved sieve of stainless steel metal that aperture is 0.5mm.
For the toy containing grease, oils, wax or similar material, sample is wrapped in toughened filter paper, after using normal heptane contained grease and analogous components to be removed by dissolution extraction, obtain testing sample.
pre-service before the acid extractants of testing sample and sample detection
By load weighted testing sample be equivalent to testing sample quality 50 times, temperature is 37 ± 2 DEG C, and concentration is the combined of 0.07 mol/L.Potpourri is shaken 1min, and checks its acidity.If pH value is greater than 1.5, shake potpourri, dropwise add 2 mol/L hydrochloric acid until pH value is between 1.0 ~ 1.5 on one side.Make potpourri lucifuge, at 37 ± 2 DEG C, stir 1h, then leave standstill 1h at 37 ± 2 DEG C.
Use filter membrane (aperture is 0.45 μm) to filter, gained filtrate is with 1 mol/L NaOH adjust pH to 4.0.
content of beary metal measures
With reference to the experimental procedure (1) in embodiment 1, (2) operate, and gained zellon uses XRF to scan mutually, read response, and try to achieve content of beary metal according to the typical curve of DDTC and HDZ set up in embodiment 2.
When selected toy sample uses HDZ as complexing agent, the response of reading is Pb 11.29cps/mA, Cd 5.76 cps/mA, Hg 3.08cps/mA.Corresponding concentration is respectively Pb 0.61mg/L, Cd 0.43mg/L, Hg 0.18mg/L; When using DDTC as complexing agent, the response of reading is Pb 13.85cps/mA, Cd 6.09 cps/mA, Hg 4.11cps/mA.Corresponding concentration is Pb 0.67mg/L, Cd 0.44mg/L, Hg 0.22mg/L.
From above embodiment 1-3, utilize the inventive method with DDTC or HDZ for complexing agent, the metal complex being insoluble in water is formed with lead, cadmium and mercury ion complexing simultaneously in aqueous phase, through the extraction of dispersive liquid-liquid microextraction technology, achieve and decades of times is carried out to the extracting and enriching of hundreds of times to metal complex in aqueous phase simultaneously.Through Xray fluorescence spectrometer, qualitative and quantitative analysis is carried out to lead, cadmium and mercury element simultaneously, obtain above qualitative and quantitative detection result.Whole analytic process is no more than 10 minutes.As can be seen here, the inventive method enrichment analyzing detect concentration of heavy metal ion have with low cost, simply, advantage maintain good specificity and high sensitivity fast.
Claims (8)
1. one kind simultaneously plumbous, the cadmium of heavy metal ion and mercury carry out the method for enrichment and analysis, it is characterized in that, described method with diethyl-dithio sodium formate or dithizone for complexing agent, the metal complex being insoluble in water is formed with the complexing simultaneously of lead, cadmium and mercury ion, adopt dispersive liquid-liquid microextraction technology to utilize the relatively described metal complex of microemulsion formed to carry out extracting and enriching, and adopt X-ray fluorescence spectra technology to carry out qualitative and quantitative analysis to lead, cadmium and mercury ion in described micro emulsion liquid phase simultaneously; Wherein, the enrichment times of described method is tens of to hundreds of times; Described micro emulsion liquid phase is the emulsion system of water/spreading agent/extractant.
2. the method for claim 1, is characterized in that, when complexing agent is diethyl-dithio sodium formate, complexing agent forms the course of reaction of the metal complex being insoluble in water as shown in the formula shown in (I) with the complexing simultaneously of lead, cadmium and mercury ion:
Wherein, M is lead, cadmium, mercury.
3. the method for claim 1, is characterized in that, when complexing agent is dithizone, complexing agent forms the course of reaction of the metal complex being insoluble in water as shown in the formula shown in (II) with the complexing simultaneously of lead, cadmium and mercury ion:
Wherein, M is lead, cadmium, mercury.
4. the method for claim 1, is characterized in that, carries out extracting and enriching to described metal complex under pH2.5-5 condition.
5. the method for claim 1, is characterized in that, described method using acetone, methyl alcohol, ethanol as spreading agent, using zellon as extractant.
6. the method for claim 1, is characterized in that, adopts described X-ray fluorescence spectra technology to carry out qualitative detection to the lead in dispersive liquid-liquid microextraction organic phase, cadmium and mercury ion simultaneously.
7. the method for claim 1, is characterized in that, adopts the content of lead, cadmium and mercury ion in described X-ray fluorescence spectra technology Simultaneously test dispersive liquid-liquid microextraction organic phase.
8. the method for claim 1, is characterized in that, the detection limit of described method to lead, cadmium and mercury ion is respectively 0.10mg/L.
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| CN104764762A (en) * | 2014-01-02 | 2015-07-08 | 广州市怡文环境科技股份有限公司 | Chemical sample preparation method used for determining content of arsenic in soil and waste water |
| CN104764762B (en) * | 2014-01-02 | 2020-07-03 | 广州市怡文环境科技股份有限公司 | Chemical sample preparation method for testing content of arsenic element in soil and sewage |
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