CN105606553A - Method for detecting content of lead in water by means of solid-phase extraction-atomic absorption spectrum - Google Patents
Method for detecting content of lead in water by means of solid-phase extraction-atomic absorption spectrum Download PDFInfo
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- CN105606553A CN105606553A CN201610121666.1A CN201610121666A CN105606553A CN 105606553 A CN105606553 A CN 105606553A CN 201610121666 A CN201610121666 A CN 201610121666A CN 105606553 A CN105606553 A CN 105606553A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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Abstract
The invention discloses a method for detecting the content of lead in water by means of solid-phase extraction-atomic absorption spectrum. According to the method, simple Nafion with the high adsorption efficiency is adopted for wrapping glass fiber cotton to be used as lead enrichment materials. It proves that the method is high in detection repeatability and sensitivity for tap water samples and can meet the requirement for determining lead in the tap water samples through a test for the tap water samples. The detection method has the advantages of being high in sensitivity, high in analysis speed, good in mechanical repeatability, high in selectivity, little in operation, easy to operate, low in cost and the like.
Description
Technical field
The present invention relates to the detection method of trace lead in water, relate in particular to a kind of by SPE-atomic absorption spectrumDetect the method for lead content in water.
Background technology
Lead is that one common are look heavy metal, has widely and distributes at nature. Along with industrial expansion, plumbous and leadedChemicals is widely applied in industry, agricultural and daily life. But the thing followed is the generation of leaded refuse, exampleAs the discharge of the burning of doped fuel and waste gas, the discharge of lead-containing industrial wastewater, waste residue etc., severe contamination atmosphere, soil andWater body. Vertical connecing in water body affects aquatile lead content, the safety of the drinking water of serious threat simultaneously. In addition, in water bodyLead can pass through again food chain enrichment, causes the lead of animals and human beings to be accumulated with poisoning. Plumbous enrichment meeting in human body cause acute orSlow poisoning, main toxic action shows nervous system, the aspects such as hemopoietic system. Saturnine animals can show gaitShakiness, muscle twitch, roars, and eats dishes without rice or wine to chew, and the nervous symptoms such as hyperesthesia, also can affect animal growth simultaneously. In addition,Plumbous embryonic development and sexal maturity to animal reproductive system, all toxic effects of multiple links that the life such as fecundity are grown up.
At present, be plumbously used as a kind of conventional pollutant and carried out strict management and limit at food and water body secure contextSystem. Plumbous mensuration has plasma emission spectroscopy method, anodic stripping voltammetry, AAS etc., generally all first sample is disappearedThen solution is measured, and method detectability is higher, and the relative standard deviation of replication is larger. China divides for lead content standard in waterAnalysis method be " the mensuration atomic absorption spectrophotometry of Copper in Water, zinc, lead, cadmium " (GB7475-87), its detectable concentration modelEnclose the g/L for 10-200 μ. The method detects and can not meet the demands for the lower lead content of concentration, thereby, cannot realize water bodyIn the mensuration of low content lead more.
Summary of the invention
For above-mentioned prior art present situation, the invention provides a kind of SPE pretreatment technology and Atomic Absorption SpectrometerMethod for combined use, is intended to realize the mensuration of trace lead in water.
In the method, utilize a kind of simple cation-exchange membrane-Nafion doped-glass cellucotton as enrichment materialMaterial, fills online solid phase extraction column, utilizes the method for flow injection to complete enrichment, the elution process of water body example, in water bodyLead carry and be enriched on solid phase extraction column by peristaltic pump, utilize small size nitric acid wash-out, realize plumbous separation and richnessCollection. Can reduce the detection limit of atomic absorption spectrum direct-detection lead by this method, and effectively reduce in environment waterInterfering ion, raising atomic absorption spectrum detects the antijamming capability of lead element, and having solved Determination of Trace Lead in Environmental Samples cannot determineThe problem that amount detects. Realize highly sensitive, the high selectivity of trace lead in environmental water sample, simple, rapid analysis.
SPE provided by the present invention-atomic absorption spectrum detects the method for lead content in water, comprises followingStep:
Step 1, the water sample of collection is filtered to pre-treatment;
Step 2, utilize solid-phase extraction column to carry out SPE water sample after treatment;
Step 3, with nitric acid by the plumbous wash-out being adsorbed in solid-phase extraction column;
Step 4, utilize Atomic absorption to analyze mensuration to wash-out solution out;
Step 5, utilize nitric acid and deionized water to carry out the regeneration of solid-phase extraction column.
Wherein, the solid-phase extraction column of use is the polytetrafluoroethylene (PTFE) of the homemade glass fibre cotton that is filled with Nafion parcelPipe, the Atomic absorption instrument of use is HITACHI-Z5700 model.
Wherein, the water sample in above-mentioned steps 1 is the water sample that does not contain particle, and pre-treating method is by 4.5 μ by water sampleThe filtering with microporous membrane in m aperture, water sample is running water, pure water etc.
Wherein, the method for SPE in above-mentioned steps 2, specifically comprises: the nitric acid and the ultrapure moisture of 5mL that use 5mL1MNot successively flow through solid-phase extraction column emptying, carry out extraction column activation; Measure 10mL filter after water sample, then by water sample withThe flow velocity of 2mL/min carries out adsorption and enrichment by solid-phase extraction column to lead, after enrichment finishes, utilizes peristaltic pump to pump into air rowRemain in to the greatest extent the sample in post.
Wherein, in above-mentioned steps 3, specifically comprise: adopt the 1M salpeter solution of 0.2mL to carry out the lead to adsorbing in extraction columnCarry out wash-out, and collect eluent and put into sample introduction cup.
Wherein, the service condition of Atomic absorption instrument is: drying time 40s, ashing time 20s, atomization time 3s, clearClean time 2s, cool time 17s, sampling volume be 20 microlitres/time;
Wherein, in above-mentioned steps 5, utilize the nitric acid of 1mL1M and 2mL deionized water successively to pass through solid-phase extraction column, carry out solid phaseExtraction column regeneration, finally utilizes air emptying, prepares to carry out next enrichment use.
Compared with prior art, the method that detects lead content in water by SPE-Atomic absorption of the present invention, hasFollowing advantage:
1, the Atomic absorption specifying with national standard method detects plumbous technology and compares, and this method can significantly reduce the inspection of lead contentRising limit, detection limit of the present invention can reach 0.005 μ g/L.
2, the material environmental pollution that the present invention adopts is little, high to plumbous bioaccumulation efficiency.
3, the rate of recovery of the present invention is high, reproducible, adopts flow injection method to carry out SPE and wash-out, greatly disappearsExcept manual error.
Brief description of the drawings
Fig. 1 is the calibration curve of the Instrumental Analysis that records through this method of the plumbous standard liquid of 7 concentration standards.
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the invention are described in further detail.
In embodiments of the invention, adopt self-control solid-phase extraction column and Atomic Absorption Spectrometer (HITACHI-Z5700) to carry outRelated experiment and test.
Wherein, the service condition of above-mentioned Atomic Absorption Spectrometer is: drying time 40s, ashing time 20s, when atomizationBetween 3s, cleaning time 2s, cool time 17s, sampling volume be 20 microlitres/time.
Wherein, the preparation method of above-mentioned solid phase extraction column is: get 5%Nafion(CAS:31175-20-9) stoste is 60DEG C evaporating solvent obtains Nafion solid, and a certain amount of Nafion solid is melted in dimethyl sulfoxide (DMSO) (DMSO), be made into 40 ~70% Nafion solution, is added drop-wise to this solution in glass fibre cotton, to soak glass fibre cotton completely as standard, then willBe placed under infrared lamp and dry immersed with the glass fibre cotton of Nafion; Get three sections of poly fourfluoroplastics pipes, caliber and length are respectively againFor mono-of 3.175*1.6*30mm, two of 1.6*0.8*50mm, are assembled into together, and the glass fibre cotton containing Nafion is filled intoIn relatively thick pipe, use quartz glass spraying tampon to live in the polytetrafluoroethylplastic plastic Guan Erduan of packing material, with Anti-lost.The solid-phase extraction column assembling is connected in peristaltic pump, carries out example enrichment.
Embodiments of the invention, according to the quantitative absorption peak strength of atomic absorption spectrum, with calibration curve comparison, calculate water outletThe concentration of lead in sample. Computing formula is as follows:
A=kc(1)
Wherein: the concentration of c-lead, μ g/L; The absorbance of A-quota ion; The slope of k-calibration curve;
Wherein, the method for drafting of calibration curve is: the plumbi nitras storing solution that is 1g/L with the nitric acid preparation lead concentration of 1M is for subsequent use, soObtain corresponding standard liquid with ultra-pure water dilution storing solution afterwards. The concentration of standard solution using in the present invention is respectively 0.01 μ g/L, 0.02 μ g/L, 0.05 μ g/L, 0.10 μ g/L, 0.20 μ g/L, 0.50 μ g/L and a 1.00 μ g/L7 concentration standardPlumbous standard liquid carries out absorbance test, and drawing standard curve, and titer absorbance test result result is as shown in the table:
Table 1 standard curve determination result
| # | Concentration (μ g/L) | Absorbance |
| 1 | 0.01 | 0.0020 |
| 2 | 0.02 | 0.0050 |
| 3 | 0.05 | 0.0207 |
| 4 | 0.1 | 0.0264 |
| 5 | 0.2 | 0.6000 |
| 6 | 0.5 | 0.1236 |
| 7 | 1.0 | 0.2738 |
Corresponding absorbance and lead concentration carry out linear fit and obtain working curve: Y=0.2682c+0.0010, wherein, R=0.0098,Wherein Y-axis is absorbance, and X-axis is lead concentration. Detect lead content in water by SPE-Atomic absorption as can be seen from Figure 1Method to measure the working curve correlation of plumbous concentration fine.
SPE that what the embodiment of the present invention provided pass through-Atomic absorption detects the method for lead content in water, comprises followingStep:
Step 1, the water sample of obtaining is filtered to pre-treatment;
Step 2, the sample of handling well is carried out to SPE by solid-phase extraction column;
Step 3, will be adsorbed on plumbous wash-out in extraction column out with nitric acid;
Step 4, utilize Atomic Absorption Spectrometer to analyze mensuration to wash-out solution out;
Step 5, utilize nitric acid and deionized water to carry out the regeneration of solid-phase extraction column.
Embodiment 1
Take from water sample through filtering after purification process, get 10mL and carry out plumbous absorption by solid-phase extraction column, use subsequently1M nitric acid 200 μ L carry out wash-out to the solid-phase extraction column after adsorbing, and collect eluent. Repeat aforesaid operations 7 times, obtain 7 parts and put downRow sample, analyzes sample by Atomic Absorption Spectrometer, testing result is as shown in the table:
Determination of Pb in table 2 drinking water sample
As shown in Table 2, in running water, lead content is about 0.099 μ g/L.
Get 6 parts of autogamy standard liquids and measure plumbous content by method provided by the invention, result is as shown in the table:
Comparative example
Get 5 parts of autogamy standard liquids and measure plumbous content by method provided by the invention, prepare 2 kinds of contrast SPEs simultaneouslyPost, the 1st kind with 5%Nafion(CAS:31175-20-9) stoste is directly added drop-wise in glass fibre cotton, contrasts post 1; The 2ndPlant according to same sample preparation method carbonated hydroxyapatite (carbonatedhydroxyapatite, CHA) is replaced to NafionPrepare solid-phase extraction column, contrast post 2. Three kinds of solid-phase extraction columns are processed respectively after same sample, with same Atomic absorptionSpectrometer detects. Comparative test result shows, Nafion film is to Pb2+The ability of enrichment be weaker than CHA, but Nafion film warpCross dimethyl sulfoxide (DMSO) (DMSO) process after to Pb2+Accumulation ability better than CHA, analyze data as shown in the table:
Detect content plumbous in water by SPE-Atomic absorption detection method, measurement result is comparatively desirable, and the rate of recovery existsBetween 0.050%-0.200%, relative standard deviation is 0.7%-1.5%, and detection limit can reach 0.005 μ g/L. Working curve is at 0-1.00 μ g/L coefficient correlation is 0.9980, linear good. The Atomic absorption specifying with national standard method detects plumbous technology phaseRatio, this method can significantly reduce the detection limit of lead content, and the material environmental pollution that the present invention adopts is little, to plumbous bioaccumulation efficiencyHigh; The rate of recovery of the present invention is high, reproducible, adopts flow injection method to carry out SPE and wash-out, has greatly eliminated handThe error of work operation.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention does not limitBe formed on specific embodiment described above. To those skilled in the art, any equivalent modifications that the present invention is carried out andSubstitute also all among category of the present invention. Therefore the equalization conversion, done without departing from the spirit and scope of the invention andAmendment, all should contain within the scope of the invention.
Claims (9)
1. a method that detects lead content in water by SPE-Atomic absorption, is characterized in that, comprises following stepRapid:
Step 1, the water sample of obtaining is filtered to pre-treatment;
Step 2, utilize solid-phase extraction column to carry out SPE water sample after treatment described step 1;
Step 3, with nitric acid by the plumbous wash-out being adsorbed in solid-phase extraction column;
Step 4, utilize Atomic Absorption Spectrometer to analyze mensuration to wash-out solution out;
Step 5, utilize nitric acid and deionized water to carry out the regeneration of solid-phase extraction column;
Wherein, in described step 2, water sample after treatment carries out SPE, described solid-phase extraction column by self-control solid-phase extraction columnPreparation method be: get 5%Nafion stoste and obtain Nafion solid at 60 DEG C of evaporating solvents, Nafion solid is melted into diformazanIn base sulfoxide, be made into the Nafion solution of 40 ~ 70wt%, described Nafion solution be added drop-wise in glass fibre cotton, to soak completelyBulb glass cellucotton is standard, then will be placed under infrared lamp and dry immersed with the glass fibre cotton of Nafion, then be packaged in poly-In tetrafluoroethene pipe.
2. SPE according to claim 1-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, the water sample in described step 1 is the water sample that does not contain particle, described filtration pre-treatment is by 4.5 μ m by described water sampleThe filtering with microporous membrane in aperture.
3. SPE according to claim 2-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, described water sample is running water, pure water etc.
4. SPE according to claim 1-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, in described step 2, to cross the flow velocity of solid-phase extraction column be 1mL/min to aqueous sample stream.
5. SPE according to claim 1-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, the concentration of nitric acid of the use in described step 5 is 0.1M.
6. SPE according to claim 1-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, the method for SPE in described step 2, concrete steps comprise: use the each 5mL of nitric acid of ultra-pure water and 0.1M to flow respectivelyCross solid-phase extraction column and carry out the activation of extraction column, and residual liquid in emptying extraction column; Measure the water sample after 10mL purifying, soAfter water sample is carried out to adsorption and enrichment by solid-phase extraction column to lead with the flow velocity of 1mL/min, after end of the sample, continue to flow through 1minAir, to drain the moisture remaining in post as far as possible.
7. SPE according to claim 1-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, the lead that adopts the 0.1M salpeter solution of 0.2mL to carry out adsorbing in extraction column in described step 3 carries out wash-out, and collects and washDe-liquid is put into sample introduction cup.
8. SPE according to claim 1-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, the service condition of described Atomic Absorption Spectrometer is: drying time 40s, ashing time 20s, atomization time 3s, when cleanBetween 2s, cool time 17s, sampling volume be 20 microlitres/time.
9. SPE according to claim 2-atomic absorption spectrum detects the method for lead content in water, and its feature existsIn, in described step 5, use the nitric acid of 1mL1M and 2mL deionized water successively to pass through solid-phase extraction column, carry out solid-phase extraction columnRegeneration.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106353267A (en) * | 2016-08-29 | 2017-01-25 | 浙江中检测研究院股份有限公司 | Method for detecting content of lead in blood by aid of nanometer cerium oxide-atomic absorption spectra |
| CN108195781A (en) * | 2018-01-23 | 2018-06-22 | 山东省食品药品检验研究院 | The detection method of lead content in a kind of grape wine |
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| CN103512854A (en) * | 2013-09-23 | 2014-01-15 | 桂林理工大学 | Flame atomic absorption spectrometry method for separating, enriching and detecting trace plumbum in water sample by utilizing thiobarbituric-acid-modified silica gel |
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| 孙博思等: "浊点萃取高分辨连续光源石墨炉原子吸收光谱法测定环境水样中的痕量铅", 《光谱学与光谱分析》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106353267A (en) * | 2016-08-29 | 2017-01-25 | 浙江中检测研究院股份有限公司 | Method for detecting content of lead in blood by aid of nanometer cerium oxide-atomic absorption spectra |
| CN108195781A (en) * | 2018-01-23 | 2018-06-22 | 山东省食品药品检验研究院 | The detection method of lead content in a kind of grape wine |
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Denomination of invention: A Method for Determination of Lead in Water by Solid Phase Extraction Atomic Absorption Spectrometry Effective date of registration: 20221027 Granted publication date: 20181026 Pledgee: China Construction Bank Co.,Ltd. Ningbo housing and urban construction sub branch Pledgor: ZHEJIANG ZHONGYI TESTING INSTITUTE CO.,LTD. Registration number: Y2022980019870 |
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