CN105606553B - A kind of method that Solid Phase Extraction-atomic absorption spectrum detects lead content in water - Google Patents
A kind of method that Solid Phase Extraction-atomic absorption spectrum detects lead content in water Download PDFInfo
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- CN105606553B CN105606553B CN201610121666.1A CN201610121666A CN105606553B CN 105606553 B CN105606553 B CN 105606553B CN 201610121666 A CN201610121666 A CN 201610121666A CN 105606553 B CN105606553 B CN 105606553B
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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
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- G01N1/405—Concentrating samples by adsorption or absorption
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Abstract
The invention discloses the methods of lead content in a kind of Solid Phase Extraction-atomic absorption spectrum detection water, present invention employs enrichment material of the Nafion package glass fibre cottons as lead simply with high adsorption efficiency, by proving that this method is all very high for the detection repeatability of originally water sample and sensitivity to the experiment of originally water sample, the requirement that lead measures in originally water sample disclosure satisfy that.The detection method of the present invention has the features such as high sensitivity, analyze speed are very fast, machinery is reproducible, method choice is strong, pollution is small, operation is relatively easy, at low cost.
Description
Technical field
The present invention relates to the detection methods of trace lead in water, more particularly to one kind passing through Solid Phase Extraction-atomic absorption spectrum
The method for detecting lead content in water.
Background technology
Lead is that one kind common are color heavy metal, has extensive distribution in nature.With the development of industry, lead with it is leaded
Chemicals is widely applied in industry, agricultural and daily life.But the thing followed is the generation of lead bearing waste, example
Such as the burning of doped fuel and the discharge of exhaust gas, the discharge etc. of lead-containing industrial wastewater, waste residue, seriously polluted air, soil and
Water body.Lead in water body directly affects aquatile lead content, while seriously threatening the safety of drinking water.In addition, in water body
Lead can be enriched with again by food chain, and the lead of animals and human beings is caused to accumulate and be poisoned.Enrichment of the lead in human body can cause it is acute or
Slow poisoning, main toxic action show nervous system, hemopoietic system etc..The animals of lead poisoning can show gait
Shakiness, muscle ballism, roars, and eats dishes without rice or wine to chew, the nervous symptoms such as hyperesthesia, while can also influence animal growth.In addition,
Embryonic development and sexal maturity of the lead to animals' reproduction system, all toxic effect of multiple links of the life such as fecundity growth.
Currently, lead is carried out stringent management and limit as a kind of Conventional pollution in food and water body secure context
System.The measurement of lead has plasma emlssion spectrometry, anodic stripping voltammetry, spectrophotometry etc., and generally all first sample disappears
Then solution measures, method detection limit is higher, and the relative standard deviation of replication is larger.China is for lead content standard scores in water
Analysis method is《Copper in Water, zinc, lead, Cadmium detrmination atomic absorption spectrophotometry》(GB 7475-87), detectable concentration model
It encloses for 10-200 μ g/L.This method cannot meet the requirements the detection of concentration lower lead content, thus, it cannot achieve water body
The measurement of middle lower loading lead.
Invention content
Present situation for the above-mentioned prior art, a kind of Solid Phase Extraction pretreatment technology of present invention offer and Atomic Absorption Spectrometer
Method for combined use, it is intended to realize the measurement of trace lead in water.
In the method, using a kind of simple cation-exchange membrane-Nafion doped-glasses cellucotton as enrichment material
Material, fills online solid phase extraction column, the enrichment of water body example, elution process is completed using the method for flow injection, in water body
Lead conveyed and be enriched on solid phase extraction column by peristaltic pump, using small size nitric acid elute, realize separation and the richness of lead
Collection.Atomic absorption spectrum can be reduced by this method and directly detects the detection limit of lead, and is effectively reduced in environment water
Interfering ion improves the anti-interference ability of atomic absorption spectrum detection lead element, solves Determination of Trace Lead in Environmental Samples without legal
The problem of amount detection.Realize highly sensitive, highly selective, simple, the quick analysis of the trace lead in environmental water sample.
The method of lead content in Solid Phase Extraction provided by the present invention-atomic absorption spectrum detection water, including it is following
Step：
The water sample of acquisition is filtered pre-treatment by step 1；
Step 2, by treated, water sample utilizes solid-phase extraction column to carry out Solid Phase Extraction；
Step 3 is eluted the lead being adsorbed in solid-phase extraction column with nitric acid；
Step 4 carries out analysis measurement using Atomic absorption to the solution being eluted out；
Step 5, the regeneration that solid-phase extraction column is carried out using nitric acid and deionized water.
Wherein, the solid-phase extraction column used is the polytetrafluoroethylene (PTFE) of the homemade glass fibre cotton filled with Nafion packages
Pipe, the Atomic absorption instrument used are HITACHI-Z5700 models.
Wherein, the water sample in above-mentioned steps 1 is the water sample without containing particulate matter, and pre-treating method is that water sample is passed through 4.5 μ
The filtering with microporous membrane in the apertures m, water sample are tap water, pure water etc..
Wherein, in above-mentioned steps 2 Solid Phase Extraction method, specifically include：Use the ultrapure moisture of nitric acid and 5mL of 5mL 1M
It does not flow through solid-phase extraction column successively and empties, carry out extraction column activation；Measure the filtered water samples of 10mL, then by water sample with
The flow velocity of 2 mL/min carries out adsorption and enrichment by solid-phase extraction column to lead, after enrichment, is pumped into air using peristaltic pump and arranges
Remain in the sample in column to the greatest extent.
Wherein, it is specifically included in above-mentioned steps 3：The lead to being adsorbed in extraction column is carried out using the 1M salpeter solutions of 0.2mL
It is eluted, and collects eluent and be put into sample introduction cup.
Wherein, the use condition of Atomic absorption instrument is：Drying time 40s, ashing time 20s, atomization time 3s, clearly
Clean time 2s, cooling time 17s, sampling volume be 20 microlitres/time；
Wherein, successively pass through solid-phase extraction column, progress using the nitric acid of 1mL 1M and 2mL deionized waters in above-mentioned steps 5
Solid Phase Extraction column regeneration finally utilizes air to empty, and is ready for enrichment next time and uses.
Compared with prior art, the method for the invention for detecting lead content in water by Solid Phase Extraction-Atomic absorption, has
Following advantages：
1, compared with Atomic absorption as defined in national standard method detects the technology of lead, this method can significantly reduce lead content
Detection limit, detection limit of the invention is up to 0.005 μ g/L.
2, the material environmental pollution that the present invention uses is small, high to lead bioaccumulation efficiency.
3, the rate of recovery of the invention is high, reproducible, carries out Solid Phase Extraction and elution using flow injection method, disappears significantly
In addition to manually operated error.
Description of the drawings
Fig. 1 is the standard curve for the Instrumental Analysis that the lead standard solution of 7 concentration standards is measured by this method.
Specific implementation mode
The embodiment of the present invention is described in further detail below in conjunction with attached drawing.
Using self-control solid-phase extraction column and Atomic Absorption Spectrometer in the embodiment of the present invention（HITACHI-Z5700）It carries out
Related experiment and test.
Wherein, the use condition of above-mentioned Atomic Absorption Spectrometer is：Drying time 40s, ashing time 20s, when atomization
Between 3s, cleaning time 2s, cooling time 17s, sampling volume be 20 microlitres/time.
Wherein, the preparation method of above-mentioned solid phase extraction column is：Take 5% Nafion（CAS: 31175-20-9）Stoste is 60
DEG C evaporation solvent obtain Nafion solids, a certain amount of Nafion solids are melted into dimethyl sulfoxide (DMSO)（DMSO）In, it is made into 40 ~
The solution is added drop-wise in glass fibre cotton by 70% Nafion solution, to be completely soaked glass fibre cotton as standard, then will
It is placed under infrared lamp and dries immersed with the glass fibre cotton of Nafion；Three sections of poly fourfluoroplastics pipes, caliber and length difference are taken again
It is assemblied together for 3.175*1.6*30mm mono-, 1.6*0.8*50mm two, the glass fibre cotton containing Nafion is filled into
In relatively thick pipe, the polytetrafluoroethylplastic plastic Guan Erduan of packing material is lived using quartz glass spraying tampon, with Anti-lost.
Assembled solid-phase extraction column is connected in peristaltic pump, example enrichment is carried out.
The embodiment of the present invention is according to atomic absorption spectrum quantitative adsorption peak intensity, compared with standard curve, calculates water outlet
The concentration of lead in sample.Calculation 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-standard curve；
Wherein, the method for drafting of standard curve is：It is standby that the plumbi nitras storing solution that lead concentration is 1g/L is prepared with the nitric acid of 1M
With, then with ultra-pure water dilution storing solution obtain corresponding standard solution.The concentration of standard solution used 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 1.00 μ g/L 7 are dense
The lead standard solution of scale standard carries out absorbance test, and draws standard curve, and titer absorbance test result result is as follows
Shown in table：
1 standard curve determination result of table
| # | 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.It is detected in water by Solid Phase Extraction-Atomic absorption as can be seen from Figure 1
The working curve correlation that the method for lead content measures the concentration of lead is fine.
The method provided in an embodiment of the present invention that lead content in water is detected by Solid Phase Extraction-Atomic absorption, including it is following
Step：
The water sample of acquirement is filtered pre-treatment by step 1；
The sample handled well is carried out Solid Phase Extraction by step 2 by solid-phase extraction column；
The lead being adsorbed in extraction column is eluted out by step 3 with nitric acid；
Step 4 carries out analysis measurement using Atomic Absorption Spectrometer to the solution being eluted out；
Step 5, the regeneration that solid-phase extraction column is carried out using nitric acid and deionized water.
Embodiment 1
It is derived from and carrys out water sample after Purification by filtration is handled, take absorption of the 10mL by solid-phase extraction column into quadrat, then
The solid-phase extraction column after absorption is eluted using 200 μ L of 1M nitric acid, collects eluent.It repeats aforesaid operations 7 times, obtains 7
Part parallel sample, sample is analyzed by Atomic Absorption Spectrometer, testing result is as shown in the table：
Determination of Pb in 2 Drinking Water Samples of table
As shown in Table 2, lead content is about 0.099 μ g/L in tap water.
6 parts of autogamy standard solution are taken to measure the content of lead by method provided by the invention, the results are shown in table below：
Comparative example
It takes 5 parts of autogamy standard solution to measure the content of lead by method provided by the invention, while preparing 2 kinds of control solid phase extractions
Take column, the 1st kind with 5% Nafion（CAS: 31175-20-9）Stoste is directly added drop-wise in glass fibre cotton, that is, compares column 1；The
2 kinds according to same sample preparation method by carbonated hydroxyapatite（carbonated hydroxyapatite, CHA）Instead of Nafion
Solid-phase extraction column is prepared, that is, compares column 2.After three kinds of solid-phase extraction columns handle same sample respectively, with same Atomic absorption
Spectrometer is detected.Comparative test result shows Nafion membrane to Pb2+The ability of enrichment be weaker than CHA, but Nafion membrane passes through
Cross dimethyl sulfoxide (DMSO)（DMSO）To Pb after processing2+Accumulation ability ratio CHA it is more preferable, analysis data it is as shown in the table：
The content of lead in water is detected by Solid Phase Extraction-Atomic absorption detection method, measurement result is ideal, and the rate of recovery exists
Between 0.050%-0.200%, relative standard deviation 0.7%-1.5%, detection limit is up to 0.005 μ g/L.Working curve is in 0-
1.00 μ g/L related coefficients are 0.9980, linear good.The technology phase of lead is detected with Atomic absorption as defined in national standard method
Than this method can significantly reduce the detection limit of lead content, and the material environmental pollution that the present invention uses is small, to lead bioaccumulation efficiency
It is high；The rate of recovery of the present invention is high, reproducible, carries out Solid Phase Extraction and elution using flow injection method, eliminates hand significantly
The error of work operation.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by impartial conversion and
Modification, all should be contained within the scope of the invention.
Claims (8)
1. the method for lead content in a kind of Solid Phase Extraction-atomic absorption spectrum detection water, which is characterized in that including following step
Suddenly：
The water sample of acquirement is filtered pre-treatment by step 1；
The step 1 treated water sample is utilized solid-phase extraction column to carry out Solid Phase Extraction by step 2；
Step 3 is eluted the lead being adsorbed in solid-phase extraction column with nitric acid；
Step 4 carries out analysis measurement using Atomic Absorption Spectrometer to the solution being eluted out；
Step 5, the regeneration that solid-phase extraction column is carried out using nitric acid and deionized water；
Wherein, treated in the step 2, and water sample carries out Solid Phase Extraction, the solid-phase extraction column by making solid-phase extraction column by oneself
Preparation method be：It takes 5%Nafion stostes to evaporate solvent at 60 DEG C and obtains Nafion solids, Nafion solids are melted into diformazan
In base sulfoxide, it is made into the Nafion solution of 40~70wt%, the Nafion solution is added drop-wise in glass fibre cotton, with complete
Immersion glass fibre cotton is standard, then will be placed under infrared lamp and dries immersed with the glass fibre cotton of Nafion, then is packaged in
In polyfluortetraethylene pipe；
Wherein, in the step 2 Solid Phase Extraction method, specific steps include：Use each 5mL of the nitric acid of ultra-pure water and 0.1M points
Solid-phase extraction column is not flowed through and carries out the activation of extraction column, and is vented the residual liquid in extraction column；It measures 10mL and filters pre-treatment
Then water sample is carried out adsorption and enrichment by water sample afterwards by solid-phase extraction column with the flow velocity of 1mL/min to lead, after end of the sample,
1min air is continued to flow through, to drain the moisture remained in column as possible.
2. the method for lead content, feature exist in Solid Phase Extraction according to claim 1-atomic absorption spectrum detection water
In the water sample in the step 1 is the water sample without containing particulate matter, and the filtering pre-treatment is that the water sample is passed through 4.5 μm
The filtering with microporous membrane in aperture.
3. the method for lead content, feature exist in Solid Phase Extraction according to claim 2-atomic absorption spectrum detection water
In the water sample is tap water, pure water.
4. the method for lead content, feature exist in Solid Phase Extraction according to claim 1-atomic absorption spectrum detection water
In the flow velocity that water sample flows through solid-phase extraction column in the step 2 is 1mL/min.
5. the method for lead content, feature exist in Solid Phase Extraction according to claim 1-atomic absorption spectrum detection water
In the concentration of nitric acid used in the step 5 is 0.1M.
6. the method for lead content, feature exist in Solid Phase Extraction according to claim 1-atomic absorption spectrum detection water
In using the 0.1M salpeter solutions of 0.2mL elute the lead adsorbed in extraction column in the step 3, and collect and wash
De- liquid is put into sample introduction cup.
7. the method for lead content, feature exist in Solid Phase Extraction according to claim 1-atomic absorption spectrum detection water
In the use condition of the Atomic Absorption Spectrometer is：Drying time 40s, ashing time 20s, atomization time 3s, when cleaning
Between 2s, cooling time 17s, sampling volume be 20 microlitres/time.
8. the method for lead content, feature exist in Solid Phase Extraction according to claim 2-atomic absorption spectrum detection water
In successively passing through solid-phase extraction column using the nitric acid of 1mL 1M and 2mL deionized waters in the step 5, carry out solid-phase extraction column
Regeneration.
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| 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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| JPS5868643A (en) * | 1981-10-19 | 1983-04-23 | Toyota Motor Corp | Determining method for atom absorbance of microzinc by palladium coprecipitation separation |
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| CN102262060A (en) * | 2010-05-27 | 2011-11-30 | 上海光谱仪器有限公司 | Method and device for analyzing heavy metal elements by on-line enrichment and atomic absorption spectrum |
| 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 |
| CN103822885A (en) * | 2014-01-21 | 2014-05-28 | 中华人民共和国淮安出入境检验检疫局 | Separation and enrichment as well as detection method for trace lead and cadmium ions in edible salt |
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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 |