CN100465618C - Method for measuring trace copper ion by using light absorption ratio difference and continuous-flow - Google Patents
Method for measuring trace copper ion by using light absorption ratio difference and continuous-flow Download PDFInfo
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- CN100465618C CN100465618C CNB2007100371251A CN200710037125A CN100465618C CN 100465618 C CN100465618 C CN 100465618C CN B2007100371251 A CNB2007100371251 A CN B2007100371251A CN 200710037125 A CN200710037125 A CN 200710037125A CN 100465618 C CN100465618 C CN 100465618C
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Abstract
It is an optical absorption ratio difference continuous flow determination trace amounts copper ion method, relating to a continuous flow analysis and optical absorption ratio difference linked water samples determination trace amounts copper ion concentration method. Prepare 0.04mmol/l chromium naphthalene green G and pH 4~5 acetate - sodium acetate buffer solution mixture as color solution; use peristaltic pump, mixed reactor, circulation pool an spectrophotometer to determine the water sample. The peristaltic pump uses 1000r/min speed to pump simultaneously the copper ion samples and color solution into a self-designed mixed reactor, and passing through the circulation pool, using the spectrophotometer to measure the copper ion sample concentration of 0-0.0180mg/l scope and 508nm wavelength and 586nm absorbance, to calculate the absorbance ratio, and draw the line; use the same method to determine absorbency of measured water samples; compare the line to calculate the copper ions concentration in water sample. The invention is fast, efficient and reproducible, and it can be online monitoring and continuous determination. It is suitable for rapid determination and online analysis for trace copper ions in drinking water, surface water, and other natural waters.
Description
Technical field
The present invention relates to a kind of Continuous Flow Analysis and the coupling of light absorption ratio and measure the method for trace copper ion concentration in the water sample, this method can fast, efficiently be monitored trace copper ion concentration in the water sample, belongs to the environmental analysis field.
Background technology
Copper ion is a kind of important metallic ion that extensively exists in the water body, and its existence all has great importance to the animals and plants and the mankind.But excessive copper ion enters water body, can cause serious environmental to pollute, and influences human beings'health and vegeto-animal procreation existence.Therefore copper ion concentration in the water body is carried out rapidly and efficiently the monitoring ten parts of necessity and urgent that just seem.The main method of measuring copper ion concentration in the water sample at present has: graphite oven atomic absorption, inductively coupled plasma emission spectrometry, electrochemical methods and spectrophotometric method etc.
Graphite oven atomic absorption (AAS) is to utilize graphite furnace that sample is gasified, and working sample is to the absorption of copper ion characteristic spectral line then, thus the copper ion concentration in the test sample.This method is more succinct than faster, is disturbed lessly, and water sample is easily handled, but institute's use instrument costliness, complicated operation, reappearance are poor, and can not realize on-line monitoring.
Inductively coupled plasma emission spectrometry (ICP-AES) is to utilize inductance coupling device with sample gasification earlier, thereby continue to improve the temperature ionization, measure the intensity of the copper ion characteristic spectral line that the later sample of ionization launches then, the quantitative measurement copper ion concentration.Inductively coupled plasma emission spectrometry institute test sample product are simple, can realize simultaneous determination of multiponents, yet the inductively coupled plasma emission spectrometer is quite expensive, and repeatability is poor, and can't on-line monitoring.
Electrochemical methods: the electrochemical analysis method of present due mensuration copper ion mainly contains oscilloscopic polarography and anodic stripping voltammetry.The former utilizes electron oscillograph to observe electric current-voltage curve in the polarogram electrolytic process, thereby carries out quantitative test; Make copper ion on microelectrode, carrying out enrichment under the suitable condition earlier on the latter is then main, then in of the burning stripping of the method for utilizing the change electrode potential with enrichment, and the record oxidation wave, finally carry out quantitatively.Galvanochemistry operation more complicated is disturbed by external condition than being easier to.
Spectrophotometric method is based between developer and the copper ion and specific chromogenic reaction to take place comes copper ion concentration in the working sample.At present the copper developer that uses mainly is dithizone and new cuprous spirit, the former directly and copper ion generate the material that characteristic color is arranged, react and the latter mainly is and pass through the cuprous ion that oxammonium hydrochloride reduces, the both will use a large amount of organic solvents to extract.Though spectrophotometric method has instrument simple cheap, operation characteristics such as succinct, the method ratio is easier to be subjected to other ion interference, and sensitivity is not enough to accurately measure the trace copper ion that concentration in the natural water is lower than 0.01mg/l.And early stage light absorption ratio method mainly is manually-operated, can't robotization and online detection, and required time long (about 20min), analysis efficiency is low.
Therefore seek that quick, efficient, simple and direct, easy robotization, favorable reproducibility and the environment amenable method of trace copper ion concentration determination become the problem that the environmentalist presses for solution in a kind of suitable environment water.
Summary of the invention
The object of the present invention is to provide a kind of direct mensuration concentration to be lower than the high-sensitivity method of the copper trace of 0.01mg/l, to realize the detection rapidly and efficiently of trace copper ion in the water sample.
For achieving the above object, the present invention will analyze continuously, fast, efficiently with the characteristics and the light absorption ratio method high sensitivity advantages of good reproducibility, realize the rapid and accurate determination of copper ion concentration in the water sample.
Concrete steps are as follows:
The first step: the screening of color development system
The naphthalene chrome green G of obvious chromogenic reaction can take place as developer in selection and copper ion, adding developer in pH4～5 acetate-sodium acetate buffer reacts, the mixed solution of the acetate-sodium acetate buffer of preparation 0.04mmol/l naphthalene chrome green G and pH=4～5 is colour developing liquid, and be the reference scanning optical spectrum with blank standard specimen separately, relatively the operation wavelength of difference maximum is 508nm and 586nm between crest and the trough;
Second step: copper ion standard specimen absorbance is measured in light absorption ratio-continuous flow coupling
Earlier with the solution of the one group copper ions of concentration in the 0-0.0180mg/l scope as the copper ion standard specimen, and the colour developing liquid of first step preparation, be connected with two interfaces (import) of mixing reactor respectively, peristaltic pump makes copper ion standard specimen and colour developing liquid enter mixing reactor with 1000r/min simultaneously then, copper ion standard specimen and colour developing liquid are fully mixed, carry out pumping into flow cell after the chromogenic reaction, spectrophotometer carries out spectral scan and measures operation wavelength 508nm and the absorbance A of the copper ion standard specimen at 586nm place
508And A
586The interface that is connected with the copper ion standard specimen with mixing reactor in spectrophotometer scanning inserts in the another one copper ion standard specimen, repeats said process; Variable concentrations copper ion standard specimen (0mg/l is blank standard specimen) is measured one by one and is finished, and obtains different absorbance A respectively
508And A
586After, by controlling and operation, calculate absorbance automatically and compare A with the computer that peristaltic pump is connected with spectrophotometer
586/ A
508Poor Δ A with the absorbance ratio
r=A
586/ A
508-A
0 586/ A
0 508A wherein
0 508And A
0 586For blank standard specimen in 508nm and 586nm place absorbance; With Δ A
rTo the copper ion concentration mapping, draw graticule (typical curve abbreviation graticule) automatically;
The 3rd step: water determination
Earlier water sample to be measured is surveyed water sample (the clarification water sample directly uses) through the spy that 0.45 μ m membrane filtration becomes clarification.The water sample to be measured that to clarify again replaces the copper ion standard specimen in second step, uses and identical method of second step, measures the absorbance A of the water sample to be measured at wavelength 508nm and 586nm place
508And A
586Calculate the Δ A of water sample
r
The 4th step: copper ion concentration calculates in the water sample
Δ A with the 3rd step water sample that obtain of water determination
r, in the graticule of the copper ion standard specimen in second step of substitution, calculate and obtain copper ion concentration in the water sample.
The present invention uses peristaltic pump as power pump, and peristaltic pump and spectrophotometer can control and operate by computer, so solution flow rate is stable, and good reproducibility can be realized robotization fully.
The present invention has used the mixing reactor that two cascade reaction chambeies are arranged of design voluntarily, and the reaction chamber volume is than pipeline much bigger (the reaction chamber internal diameter is than taking over the big 4-6 of caliber doubly), make color development system and water sample that twice mixing be arranged, in mixed process, constantly carry out chromogenic reaction, help the mensuration of trace copper ion in the water sample.
Advantage of the present invention is as follows:
1, owing to use light absorption ratio method deal with data among the present invention, different with the data processing mode in the spectrophotometric method of traditional mensuration copper ion, the therefore sensitivity that can improve method helps the mensuration of trace copper ion concentration in the water body.
2, use the mixing reactor of the secondary mixing of design voluntarily among the present invention, improve mixing efficiency, help the complete reaction between naphthalene chrome green G and the copper ion, thus the trace copper ion concentration that is lower than 0.01mg/l in the better working sample.
3, use the peristaltic pump sample introduction among the present invention, can carry out the online acquisition of water sample and the METHOD FOR CONTINUOUS DETERMINATION and the online detection of carrying, so having realized sample continuously, remedied some classic methods such as electrochemical process and atomic absorption method deficiency in this respect.
4, peristaltic pump sample introduction among the present invention and absorbance measurement can be controlled and operate by computer, therefore mixing in the whole process, colour developing and concentration are calculated and all can be realized robotization, measure a sample and approximately only need 3 minutes, compare with traditional light absorption ratio method, can improve finding speed and analysis efficiency greatly;
5, compare with GFAAS (graphite furnace atomic absorption spectrometry) and inductively coupled plasma emission spectrometry, institute's use instrument simple cheap among the present invention, but portability, therefore easy to operate easy maintenance is suitable for the field monitoring and the field measuring of natural water.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention
Fig. 2 is that sample analysis of the present invention is measured process
Fig. 3 is a self-designed mixed reactor synoptic diagram of the present invention
Embodiment
Embodiment 1
Measure copper ion concentration in the Yangtze River Water.
Consult Fig. 1,2 and 3.In triangular flask, the acetate-sodium acetate buffer and the naphthalene chrome green G that add pH=4.0 respectively react earlier, preparation 0.04mmol/l colour developing liquid.Get a series of 10ml color comparison tubes then, totally 7, add the copper ion of variable concentrations respectively, make copper ion concentration finally be respectively 0; 0.0030mg/L; 0.0060mg/l; 0.0090mg/l; 0.0120mg/l; 0.0150mg/l and 0.0180mg/l.The triangular flask of colour developing liquid (developer and damping fluid) and an interface of mixing reactor will be housed link to each other, and the color comparison tube of the copper ion standard specimen (solution) of above-mentioned variable concentrations will be linked to each other with another interface respectively.Utilize the peristaltic pump Control Software to start peristaltic pump, peristaltic pump moves with 1000r/ minute speed, and operational mode is: move 2 minutes, stop 1 minute, and then move 2 minutes, stop 1 minute again, so circulate 2-3 time.Colour developing liquid and copper ion standard specimen enter mixing reactor simultaneously under the effect of peristaltic pump, two reaction chambers of flowing through constantly mix and react, pond then circulates, this moment, peristaltic pump stopped operating, and spectrophotometer carries out spectral scan automatically under function software control, measure absorbance A
508And A
586, calculate absorbance and compare A
r, A
r=A
586/ A
508The spectrophotometer operational mode is: temporal mode, run-down was composed entirely in per 3 minutes, exported absorbance A simultaneously automatically
508And A
586And absorbance compares A
rInterface with mixing reactor in spectral scan inserts in the another one copper ion standard specimen, repeats said process.Variable concentrations copper ion standard specimen sample introduction finishes, and system provides graticule automatically.
Water determination and above-mentioned similar, water sample be through the membrane filtration of 0.45 μ m, in the 10ml color comparison tube of packing into, mixing reactor another one interface (above-mentioned be connected with the copper ion standard specimen) is connected with this color comparison tube, repeats said process, and computer calculates A automatically
rWith Δ A
r, copper ion concentration is 0.0113mg/l in the output water sample.As a comparison, utilize the result of inductively coupled plasma emission spectrographic determination to be 0.010mg/l in addition, experimental result is very identical.
Embodiment 2
Measure copper ion concentration in the Yangtze River Water.
Consult Fig. 1,2 and 3.In triangular flask, the acetate-sodium acetate buffer and the naphthalene chrome green G that add pH=5.0 respectively react earlier, preparation 0.04mmol/l colour developing liquid.Adopt program and the method mensuration copper ion concentration identical finally to be respectively 0,0.0030mg/L, 0.0060mg/l then with embodiment 1,0.0090mg/l, 0.0120mg/l the copper ion standard specimen of 0.0150mg/l and 0.0180mg/l obtains the absorbance A of above-mentioned variable concentrations copper ion standard specimen
508And A
586, calculate absorbance and compare A
r, A
r=A
586/ A
508Poor Δ A with the absorbance ratio
r=A
586/ A
508-A
0 586/ A
0 508A wherein
0 508And A
0 586For blank standard specimen (copper ion concentration is 0), in 508nm and 586nm place absorbance; With Δ A
rTo the copper ion concentration mapping, system provides graticule automatically.
Water determination and above-mentioned similar, water sample, insert mixing reactor another one interface in this color comparison tube in the 10ml color comparison tube of packing into through the membrane filtration of 0.45 μ m, repeat said process, and computer calculates A automatically
rWith Δ A
r, copper ion concentration is in the output water sample: 0.0105mg/l.As a comparison, utilize the result of inductively coupled plasma emission spectrographic determination to be 0.010mg/l in addition, experimental result is still very identical.
Claims (2)
1. the method for measuring trace copper ion by using light absorption ratio difference and continuous-flow is characterized in that:
The first step: the screening of color development system
Select naphthalene chrome green G as developer, the acetate-sodium acetate buffer solution mixture of preparation 0.04mmol/l naphthalene chrome green G and pH=4～5 is as colour developing liquid;
Second step: copper ion standard specimen absorbance is measured in light absorption ratio-continuous flow coupling
Earlier with the one group copper ion solution of concentration in the 0-0.0180mg/1 scope as standard specimen, and the colour developing liquid that is mixed with of the first step, be connected with two interfaces of mixing reactor by peristaltic pump respectively, peristaltic pump makes copper ion standard specimen and colour developing liquid enter mixing reactor with the speed of 1000r/min simultaneously then, copper ion standard specimen and colour developing liquid are fully mixed, carry out flowing into flow cell after the chromogenic reaction, spectrophotometer carries out spectral scan and measures operation wavelength 508nm and the absorbance A of the copper ion standard specimen at 586nm place
508And A
586The interface that is connected with the copper ion standard specimen with mixing reactor in spectrophotometer scanning inserts in the another one copper ion standard specimen, repeats said process, and variable concentrations copper ion standard specimen is measured and finished, and obtains different absorbance A respectively
508And A
586After, by controlling and operation, calculate absorbance automatically and compare A with the computer that peristaltic pump is connected with spectrophotometer
586/ A
508Poor Δ A with the absorbance ratio
r=A
586/ A
508-A
0 586/ A
0 508A wherein
0 508And A
0 586For blank standard specimen reagent in 508nm and 586nm place absorbance; With Δ A
rTo the copper ion concentration mapping, draw graticule; Above-mentioned blank standard specimen reagent is that concentration is the copper ion standard specimen of 0mg/l;
The 3rd step: water determination
Earlier water sample to be measured is become the water sample to be measured of clarification through 0.45 μ m membrane filtration; The water sample to be measured that to clarify again replaces the copper ion standard specimen in second step, uses and identical method of second step, measures the absorbance A of the water sample to be measured at wavelength 508nm and 586nm place
508And A
586Obtain the Δ A of water sample
r
The 4th step: copper ion concentration calculates in the water sample
Δ A with the 3rd step water sample that calculate automatically of water determination
r, in the graticule of the copper ion standard specimen in second step of substitution, calculate copper ion concentration in the water sample.
2. the method for measuring trace copper ion by using light absorption ratio difference and continuous-flow according to claim 1, it is characterized in that: make copper ion standard specimen and colour developing liquid fully mix the process of carrying out chromogenic reaction and be through mixing reactor, both are through flow through two entrance sleeves of mixing reactor of two interfaces of mixing reactor, behind the big 4-6 of the caliber reaction chamber doubly of the internal diameter of two series connection in the middle of entering simultaneously than two entrance sleeves, in first reaction chamber, fully stop earlier and carry out chromogenic reaction, enter second reaction chamber then and stop once more and carry out chromogenic reaction, improved mixing and reaction efficiency.
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