CN103499538A - Method for measuring trace copper in water through ultrasonic extraction-atomic spectrum - Google Patents
Method for measuring trace copper in water through ultrasonic extraction-atomic spectrum Download PDFInfo
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Abstract
The invention provides a method for measuring trace copper in water through ultrasonic extraction-atomic spectrum. The method is characterized in that the cloud point extraction of traditional water bath heating is replaced by ultrasonic vibration extraction, the ultrasonic technology is combined with the cloud point extraction technology, ultrasonic assisted extraction is realized, the movement frequency and speed of substance molecules are increased under the cavitation effect of the ultrasonic, and as a result, the penetrating power of an extracting agent is improved and the dissolving-out speed of copper is increased, and moreover, the content of impurity in the extract can be reduced while the extraction time is shortened, and the extraction rate is increased. The method provided by the invention simultaneously has the advantages of low detection limit, high accuracy and high analysis speed.
Description
Technical field
The present invention relates to a kind of quantitative analysis method of measuring copper trace in water body, be specifically related to the method for copper trace in a kind of body of the Water by Flame Atomic Absorption Spectrometry by ultrasonic extraction.
Background technology
Copper is one of nutrient of needed by human, activity and human endocrine to hematopoietic cell growth, some enzyme have certain physiological action, but intake too much can cause various diseases, comprise acute copper poisoning, hepatolenticular degeneration, children's intrahepatic cholestasis etc.Along with industrial expansion, copper pollutes day by day serious mistake, and in environment, the mensuration of copper content has become one of project of national environmental protection department emphasis monitoring.Regulation in drinking water sanitary standard (GB5749-2006), in Drinking Water, copper content must not surpass 1mg/L, and therefore, in the mensuration water body, copper trace is significant.
Current modal analysis means mainly contains atomic absorption spectrophotometry, flow injection light scattering method, GFAAS (graphite furnace atomic absorption spectrometry), flame atomic absorption spectrometry, and wherein flame atomic absorption spectrometry is because its rapid and convenient, accuracy are high, favorable repeatability becomes one of common method of trace element determination and analysis.Simultaneously, measure sensitivity and accuracy often by certain extraneous means in order to improve in the mensuration process, such as, micro-wave digestion, cloud point extraction etc., cloud point extraction is the most frequently used abstraction technique of present stage, it does not use volatile organic solvent, do not affect environment, take the dissolubility of neutral surface active agent's micellar aqueous solution and cloud point phenomenon is basis, changing the experiment parameter initiation is separated, lyophobic dust is separated with hydroaropic substance, by measuring the content of the surfactant phase solution acquisition trace element that just energy is accurate sensitive.But, in order to reach cloud point temperature, need to be in water-bath long-time heating, increased the time that experiment expends when extraction efficiency is low, therefore, be necessary in this respect to do further improvement.
Summary of the invention
In order to solve the deficiency in background technology, the object of the invention is to overcome the defect of background technology, a kind of method that extraction efficiency is high, can shorten copper trace in the experiment mensuration of the atomic spectroscopy by ultrasonic extraction water body consuming time is provided.
For achieving the above object, the technical solution used in the present invention is: a kind of ultrasonic extraction-atomic spectroscopy is measured the method for copper trace in water body, it is characterized in that: comprise the following steps:
A. the sample micro-wave digestion is processed: get water sample to be measured in clean dry micro-wave diminishing pot, add and clear up solvent, the described solvent of clearing up is 70% nitric acid that volume ratio is 3:1, the mixed solvent of 30% hydrogen peroxide, prepare blank solution simultaneously, put into microwave digestion device after sealing and clear up 20～30min, after clearing up end, take out counteracting tank and be cooled to room temperature, solution is transferred in polytetrafluoroethylene beaker, clean counteracting tank with a small amount of water and be incorporated to beaker for several times, be placed in heating on electric hot plate and catch up with acid, when solution is evaporated to quick-drying, take off beaker cooling and shift test solution to volumetric flask, dilute constant volume with redistilled water, obtain sample solution,
B. sample solution ultrasonic extraction enrichment is processed: the sample solution quantitatively obtained in removing step a is in centrifuge tube, the 1-(2-pyridylazo that adds 10mmol/L)-2 naphthols (PAN) ethanolic solutions, shaking up after standing the pH value that adds NaAc_HAc buffer solution that the pH value is 9.0 to regulate mixed solution is 5.0, then add 4.5% TritonX-114 solution, centrifuge tube is placed in to ultrasonic cleaning instrument vibration extraction, the rear centrifugal 3min(4600r/min while hot that takes out of extraction end) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, to lower floor's surfactant, add the nital of 0.1mol/L to be settled to 0.5mL in mutually, obtain testing sample solution,
C. 1% the nitric acid of take is thinning agent, the copper titer is mixed with to the series standard solution of variable concentrations, successively through micro-wave digestion process, the ultrasonic extraction enrichment measures the absorbance of series standard solution after processing, set up regression equation or drawing curve;
D. measure the absorbance of testing sample solution, according to the content of copper in regression equation or working curve calculating testing sample solution.
Preferably, in step b, the time of vibration extraction is 10～20min.
Preferably, in step b, the frequency of operation of ultrasonic cleaning instrument is 80kHz.
Preferably, the 1-(2-pyridylazo added in step b) volume ratio of-2 naphthols (PAN) ethanolic solutions and 4.5% TritonX-114 solution is 5:4.
Preferably, this method sensing range is: 1.0 * 10
-4g/L～3.0 * 10
-3g/L, be limited to 1.0 * 10 under detection
-4g/L.
Preferably, in step a, in water body, copper content is prescribed a time limit under detecting lower than this method, after the water sample low-temperature evaporation is concentrated, clears up again; When contained the suspension particulate in water sample, first after the membrane filtration in 0.45um aperture, sample again.
Preferably, in step c and steps d, all adopt flame atomic absorption spectrophotometer to measure absorbance, its condition determination is:
Analytical wavelengths: 324.8nm
Lamp current: 3.0mA
Spectral band-width: 0.4nm
Burner height: 7mm
Acetylene gas flow: 2.3L/min
Air mass flow: air mass flow: 9.5mL/min.
Usefulness of the present invention is: ultrasonic extraction of the present invention-atomic spectroscopy is measured the method for copper trace in water body, in sample solution ultrasonic extraction enrichment treatment step, ultrasonic technique is combined with Cloud-Point Extraction Technique, ultrasonic auxiliary extraction, utilize hyperacoustic cavitation to increase motion frequency and the speed of material molecule, increase the penetration power of extractant, improve the dissolution rate of copper, when shortening extraction time, can reduce impurity content in extract, improve percentage extraction.Method of the present invention has advantages of that detection limit is low, accuracy is high, analysis speed is fast simultaneously.
Embodiment
In order to make those skilled in the art person understand better the present invention program, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with embodiment, the present invention is further detailed explanation.
The present invention proposes following ultrasonic extraction-atomic spectroscopy and measure the method for copper trace in water body:
1, equipment and reagent
(1) AA6800 flame atomic absorption spectrophotometer (attached computing machine and printer);
(2) copper hollow cathode lamp;
(3) pH-3C type acidometer;
(4) LD5-2A type hydro-extractor;
(5) electric hot plate;
(6) NaAc_HAc buffer solution that the pH value is 9.0; The PAN ethanolic solution of 10mmol/L; 4.5% TritonX-114 solution; 0.1mol/L nital; 70% salpeter solution; 30% hydrogen peroxide; 1% salpeter solution;
(7) preparation of copper series standard solution: get respectively different volumes, concentration is the copper standard solution of 5ug/mL in volumetric flask, and the nitric acid dilution constant volume with 1%, shake up.Obtain as required the series standard solution of 0.1～2.5ug/mL during use with 1% nitric acid stepwise dilution.
2, the atomic absorption spectrometry condition is as follows:
Analytical wavelengths: 324.8nm
Lamp current: 3.0mA
Spectral band-width: 0.4nm
Burner height: 7mm
Acetylene gas flow: 2.3L/min
Air mass flow: air mass flow: 9.5mL/min.
3, determination and analysis method
(1) the sample micro-wave digestion is processed:
As copper content in water body detects lower limit lower than this method, water sample is carried out to evaporation and concentration; As contain the suspension particulate in advance through the membrane filtration in 0.45um aperture.Pipette water sample to be measured in clean dry micro-wave diminishing pot, add and clear up solvent, the described solvent of clearing up is 70% nitric acid that volume ratio is 3:1, the mixed solvent of 30% hydrogen peroxide, prepare blank solution simultaneously, put into microwave digestion device after sealing and clear up 20～30min, after clearing up end, take out counteracting tank and be cooled to room temperature, solution is transferred in polytetrafluoroethylene beaker, clean counteracting tank with a small amount of water and be incorporated to beaker for several times, be placed in heating on electric hot plate and catch up with acid, when solution is evaporated to quick-drying, take off beaker cooling and shift test solution to volumetric flask, dilute constant volume with redistilled water, obtain sample solution,
(2) sample solution ultrasonic extraction enrichment is processed:
The sample solution quantitatively obtained in removing step a is in centrifuge tube, the 1-(2-pyridylazo that adds 10mmol/L)-2 naphthols (PAN) ethanolic solutions, shaking up after standing the pH value that adds NaAc_HAc buffer solution that the pH value is 9.0 to regulate mixed solution is 5.0, then add 4.5% TritonX-114 solution, herein, the 1-(2-pyridylazo added) volume ratio of-2 naphthols (PAN) ethanolic solutions and 4.5% TritonX-114 solution is 5:4; Centrifuge tube is placed in to ultrasonic cleaning instrument vibration extraction, and the frequency of operation of ultrasonic cleaning instrument is 80kHz herein, and the vibration extraction time is 10～20min; The rear centrifugal 3min(4600r/min while hot that takes out of extraction end) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, to lower floor's surfactant, add the nital of 0.1mol/L to be settled to 0.5mL in mutually, obtain testing sample solution;
(3) preparation series standard solution drawing curve:
The copper standard solution that pipette respectively 0.5,2.5,5.0,7.5,10.0,12.5,15mL is 5ug/mL in concentration is in the 25mL volumetric flask, with 1% nitric acid dilution constant volume, obtain the series standard solution that cupric concentration A is respectively 0.1ug/mL, 0.5ug/mL, 1.0ug/mL, 1.5ug/mL, 2.0ug/mL, 2.5ug/mL, 3.0ug/mL, then measure respectively the absorbance C of series standard solution according to above-mentioned atomic absorption spectrometry condition, as follows: C=6.61,34.39,69.11,103.83,138.56,173.28.
According to the corresponding relation of A and C, obtain an equation of linear regression by Mathematical Fitting, as follows:
A=0.0144C(ug/mL)+0.0048, related coefficient is r=0.9997.
Embodiment 1: the mensuration of copper content in Suzhou City's TAIHU LAKE
The sample micro-wave digestion is processed and is obtained sample solution:
Gather the 5mL TAIHU LAKE in clean dry micro-wave diminishing pot, add 6mL70% nitric acid, 2mL30% hydrogen peroxide, put into microwave digestion device after sealing and clear up 20～30min, after clearing up end, take out counteracting tank and be cooled to room temperature, solution is transferred in the 50mL polytetrafluoroethylene beaker, clean counteracting tank with a small amount of water and be incorporated to beaker for several times, be placed in heating on electric hot plate and catch up with acid, when solution evaporation 2mL, take off beaker cooling and shift test solution to the 25mL volumetric flask, with redistilled water, dilute constant volume, obtain sample solution;
Sample solution ultrasonic extraction enrichment is processed:
Pipette the 6mL sample solution in the 15mL centrifuge tube, the 1-(2-pyridylazo that adds 0.1mL10mmol/L)-2 naphthols (PAN) ethanolic solutions, shaking up after standing the pH value that adds NaAc_HAc buffer solution that the 1.5mLpH value is 9.0 to regulate mixed solution is 5.0, then the TritonX-114 solution that adds 0.08mL4.5%, centrifuge tube is placed in to the ultrasonic cleaning instrument vibration extraction 15min that frequency of operation is 80kHz, the rear centrifugal 3min(4600r/min while hot that takes out of extraction end) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, to lower floor's surfactant, add the nital of 0.1mol/L to be settled to 0.5mL in mutually, obtain testing sample solution,
The mensuration of sample absorbance:
Carry out the mensuration of testing sample solution absorbance under above-mentioned same parameters arranges, prepare 6 parts of parallel testing sample solutions, calculate respectively the content of copper in this 6 duplicate samples according to equation of linear regression, average.The copper content recorded is respectively: 327.8ug/mL, 329.3ug/mL, 327.6ug/mL, 328.9ug/mL, 327.7ug/mL, 329.1ug/mL, calculating mean value is 328.4ug/mL, meets the copper content Cmax of regulation in drinking water sanitary standard (GB5749-2006).
Recovery experiment:
For recovery experiment has been carried out in method of inspection accuracy, in the actual sample analytic process, this step is omitted.
Pipette respectively testing sample solution 5.0mL sample liquid in conical flask, then the copper standard solution 1mL that adds respectively three kinds of variable concentrations in each conical flask, measured by experimental technique of the present invention, do blank and recovery testu simultaneously, result is as following table 1-1:
Table 1-1
| The concentration numbering | Add scalar/(ug/L) | Measured value/(ug/L) | The recovery/% |
| 1 | 10 | 10.42 | 104.2 |
| 2 | 15 | 14.2 | 94.7 |
| 3 | 20 | 19.6 | 96.5 |
Can find out that by table 1-1 with the recovery of standard addition of method mensuration Copper in Water Samples content of the present invention be between 94.7～104.2%, calculating relative standard deviation is 2.7%, highly sensitive, accurate, quick.
Embodiment 2:
With the difference of embodiment 1, only be: centrifuge tube is placed in to the ultrasonic cleaning instrument vibration extraction 10min that frequency of operation is 80kHz.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel testing sample solutions, calculates respectively the content of copper in this 6 duplicate samples according to equation of linear regression, averages.The copper content recorded is respectively: 316.9ug/mL, 317.1ug/mL, 316.8ug/mL, 315.7ug/mL, 315.9ug/mL, 316.3ug/mL, calculating mean value is 316.45ug/mL.With respect to embodiment 1, draw, vibration extraction 15min increases to some extent than 10min absorbance.
Embodiment 3:
With the difference of embodiment 1, only be: centrifuge tube is placed in to the ultrasonic cleaning instrument vibration extraction 20min that frequency of operation is 80kHz.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel testing sample solutions, calculates respectively the content of copper in this 6 duplicate samples according to equation of linear regression, averages.The copper content recorded is respectively: 327.1ug/mL, 328.3ug/mL, 326.4ug/mL, 326.9ug/mL, 327.3ug/mL, 328.8ug/mL, calculating mean value is 327.47ug/mL, with respect to embodiment 1-3, draw, 15min is optimum extraction time.
Embodiment 4:
With the difference of embodiment 1, only be: in sample solution ultrasonic extraction enrichment processing procedure, the process that does not add the ultrasound wave auxiliary extraction, add after the TritonX-114 solution of 0.08mL4.5% the water-bath that centrifuge tube is placed in to 90 ℃ to heat 50min, the rear centrifugal 3min(4600r/min while hot that takes out of extraction end) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, to lower floor's surfactant, add the nital of 0.1mol/L to be settled to 0.5mL in mutually, obtain testing sample solution;
Prepare 6 parts of parallel testing sample solutions, calculate respectively the content of copper in this 6 duplicate samples according to equation of linear regression, average.The copper content recorded is respectively: 328.3ug/mL, 328.6ug/mL, 327.9ug/mL, 329.2ug/mL, 326.5ug/mL, 327.2ug/mL, calculating mean value is 327.95ug/mL.
Recovery experiment:
Pipette respectively testing sample solution 5.0mL sample liquid in conical flask, then the copper standard solution 1mL that adds respectively three kinds of variable concentrations in each conical flask, measured by experimental technique of the present invention, do blank and recovery testu simultaneously, result is as following table 1-2:
Table 1-2
| The concentration numbering | Add scalar/(ug/L) | Measured value/(ug/L) | The recovery/% |
| 1 | 10 | 10.2 | 102 |
| 2 | 15 | 13.86 | 92.4 |
| 3 | 20 | 20.2 | 101 |
Can find out that by table 1-2 with the recovery of standard addition of the method for embodiment 4 mensuration Copper in Water Samples content be between 92.4～102%, calculating relative standard deviation is 2.8%.
Comparing embodiment 1 and embodiment 4, the value of the copper content that two kinds of methods record reaches unanimity, the recovery of embodiment 1 and relative standard deviation have a little raising with respect to embodiment 4, but only need vibration extraction 15min in embodiment 1, and need in the water-bath of 90 ℃, heat 50min in embodiment 4, that is to say in the situation that the result obtained is consistent, measure the time that has shortened 35min with method quantitative test of the present invention, therefore, method of the present invention is under the prerequisite that guarantees percentage extraction, can shorten greatly the time of experimental expenses, there is detection limit low simultaneously, accuracy is high, the advantage that analysis speed is fast.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify and all should be equivalent substitute mode, within being included in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (7)
1. a ultrasonic extraction-atomic spectroscopy is measured the method for copper trace in water body, it is characterized in that: comprise the following steps:
A. the sample micro-wave digestion is processed: get water sample to be measured in clean dry micro-wave diminishing pot, add and clear up solvent, the described solvent of clearing up is 70% nitric acid that volume ratio is 3:1, the mixed solvent of 30% hydrogen peroxide, prepare blank solution simultaneously, put into microwave digestion device after sealing and clear up 20 ~ 30min, after clearing up end, take out counteracting tank and be cooled to room temperature, solution is transferred in polytetrafluoroethylene beaker, clean counteracting tank with a small amount of water and be incorporated to beaker for several times, be placed in heating on electric hot plate and catch up with acid, when solution is evaporated to quick-drying, take off beaker cooling and shift test solution to volumetric flask, dilute constant volume with redistilled water, obtain sample solution,
B. sample solution ultrasonic extraction enrichment is processed: the sample solution quantitatively obtained in removing step a is in centrifuge tube, the 1-(2-pyridylazo that adds 10mmol/L)-2 naphthols (PAN) ethanolic solutions, shaking up after standing the pH value that adds NaAc_HAc buffer solution that the pH value is 9.0 to regulate mixed solution is 5.0, then add 4.5% Triton X-114 solution, centrifuge tube is placed in to ultrasonic cleaning instrument vibration extraction, the rear centrifugal 3min(4600r/min while hot that takes out of extraction end) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, to lower floor's surfactant, add the nital of 0.1mol/L to be settled to 0.5mL in mutually, obtain testing sample solution,
C. 1% the nitric acid of take is thinning agent, the copper titer is mixed with to the series standard solution of variable concentrations, successively through micro-wave digestion process, the ultrasonic extraction enrichment measures the absorbance of series standard solution after processing, set up regression equation or drawing curve;
D. measure the absorbance of testing sample solution, according to the content of copper in regression equation or working curve calculating testing sample solution.
2. ultrasonic extraction according to claim 1-atomic spectroscopy is measured the method for copper trace in water body, it is characterized in that: in step b, the time of vibration extraction is 10 ~ 20min.
3. ultrasonic extraction according to claim 1 and 2-atomic spectroscopy is measured the method for copper trace in water body, and it is characterized in that: in step b, the frequency of operation of ultrasonic cleaning instrument is 80kHz.
4. the method for copper trace in water body is measured in ultrasonic extraction according to claim 3-atomic spectroscopy, it is characterized in that: the 1-(2-pyridylazo added in step b) volume ratio of-2 naphthols (PAN) ethanolic solutions and 4.5% Triton X-114 solution is 5:4.
5. ultrasonic extraction according to claim 1-atomic spectroscopy is measured the method for copper trace in water body, and it is characterized in that: this method sensing range is: 1.0 * 10
-4g/L ~ 3.0 * 10
-3g/L, be limited to 1.0 * 10 under detection
-4g/L.
6. ultrasonic extraction according to claim 5-atomic spectroscopy is measured the method for copper trace in water body, it is characterized in that: in step a, in water body, copper content is prescribed a time limit under detecting lower than this method, after the water sample low-temperature evaporation is concentrated, clears up again; When contained the suspension particulate in water sample, first after the membrane filtration in 0.45um aperture, sample again.
7. ultrasonic extraction according to claim 1-atomic spectroscopy is measured the method for copper trace in water body, it is characterized in that: in step c and steps d, all adopt flame atomic absorption spectrophotometer to measure absorbance, its condition determination is:
Analytical wavelengths: 324.8nm
Lamp current: 3.0mA
Spectral band-width: 0.4nm
Burner height: 7mm
Acetylene gas flow: 2.3 L/min
Air mass flow: air mass flow: 9.5mL/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104406926A (en) * | 2014-11-28 | 2015-03-11 | 苏州东辰林达检测技术有限公司 | Detection method of trace methylmercury in alga |
| CN105861826A (en) * | 2016-05-19 | 2016-08-17 | 昆明理工大学 | Method for extracting copper ions through ultrasonic wave channelization |
| CN105973824A (en) * | 2016-08-13 | 2016-09-28 | 浙江杭康检测技术有限公司 | Method for detecting heavy metals in wastewater |
| CN108871917A (en) * | 2018-08-29 | 2018-11-23 | 重庆科技学院 | The analysis method of heavy metal element chromium and lead in a kind of quick detection vegetable oil |
| CN110441243A (en) * | 2018-05-02 | 2019-11-12 | 天津工业大学 | It is a kind of based on film enrichment and UV-vis DRS spectrum underwater trace copper ion quantitative analysis method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104406926A (en) * | 2014-11-28 | 2015-03-11 | 苏州东辰林达检测技术有限公司 | Detection method of trace methylmercury in alga |
| CN105861826A (en) * | 2016-05-19 | 2016-08-17 | 昆明理工大学 | Method for extracting copper ions through ultrasonic wave channelization |
| CN105973824A (en) * | 2016-08-13 | 2016-09-28 | 浙江杭康检测技术有限公司 | Method for detecting heavy metals in wastewater |
| CN110441243A (en) * | 2018-05-02 | 2019-11-12 | 天津工业大学 | It is a kind of based on film enrichment and UV-vis DRS spectrum underwater trace copper ion quantitative analysis method |
| CN108871917A (en) * | 2018-08-29 | 2018-11-23 | 重庆科技学院 | The analysis method of heavy metal element chromium and lead in a kind of quick detection vegetable oil |
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Application publication date: 20140108 |