CN100424493C - Automatic analysis of cadmium and mercury in seawater, surface water and sewage - Google Patents
Automatic analysis of cadmium and mercury in seawater, surface water and sewage Download PDFInfo
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- CN100424493C CN100424493C CNB2005100210848A CN200510021084A CN100424493C CN 100424493 C CN100424493 C CN 100424493C CN B2005100210848 A CNB2005100210848 A CN B2005100210848A CN 200510021084 A CN200510021084 A CN 200510021084A CN 100424493 C CN100424493 C CN 100424493C
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Abstract
The present invention relates to an automatic analysis method for cadmium and mercury in sea water, surface water and industrial sewage, which adopts flow injection analysis and spectrophotometric detection. The present invention uses a NaCl solution as propelling liquid, uses the mixed liquid of potassium iodide, ascorbic acid, polyvinyl alcohol and citric acid or the mixed liquid of potassium iodide, ascorbic acid, polyvinyl alcohol and thiourea as reaction liquid, and uses an ethyl violet solution as chromogenic liquid, wherein the propelling liquid in an analysis detecting flow path is mixed with the reaction liquid entering the flow path. The mixed liquid is mixed with the chromogenic liquid entering the flow path to generate a base line which is measured and drawn, and a guide sample or a sample enters the analysis detecting flow path through a sample flow path and is mixed with the reaction liquid entering the sample flow path in the analysis detecting flow path to react and then is mixed with the chromogenic liquid entering the flow path under the propelling of the propelling liquid to react for generating spectrograms which are measured and drawn. The relative standard deviation of parallel analysis in the method is less than-5% to +5%, and one time of analysis only needs 2 to 5 minutes; the present invention is especially suitable for field analysis.
Description
Technical field
The invention belongs to the analytical approach of contained cadmium, mercury in seawater, surface water and the industrial sewage, particularly a kind of automatic analysis method.
Background technology
Cadmium, mercury are harmful accumulative toxicants, have stronger teratogenesis, carcinogenic, mutagenesis, therefore are used as the routine monitoring project of environment water.Analytical approach about cadmium, mercury in seawater, surface water and the industrial sewage, external at present main inductively coupled plasma emission spectrography (ICP), the inductively coupled plasma atomic emission one mass spectrometry analytic approach (ICP-MS) of adopting, domestic except that adopting said method, also adopt manual colourimetry.ICP method and the not only used analytical instrument of ICP-MS coupling method cost an arm and a leg, and are used for difficulty of on-the-spot on-line analysis.Though manual colourimetry analysis cost is lower, many, the complex operation of step is not suitable for on-the-spot on-line analysis.
Publication number is the automatic analysis method that the Chinese patent application of CN 1560623A discloses a kind of seawater, river mouth underwater trace metallic element, and this method is undertaken sample to adopt the low-voltage ion chromatography analysis after the online treatment by instrument.The sample online treatment has dual mode: a kind of steps in sequence of mode for concentrate, cleaning and desorb; The steps in sequence of another kind of mode is complexing, concentrate, cleaning and desorb.Though this kind analytical approach can make the analytical instrument miniaturization, can carry out on-line automatic analysis to the trace metal element in seawater, the river mouth water easily, but owing to will handle and adopt the low-voltage ion chromatography analysis to sample, analysis cost is still higher, and once analyzing needs about 20 minutes.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the automatic analysis method of cadmium, mercury in a kind of seawater, surface water and the industrial sewage is provided, with further reduction analysis cost and be convenient to on-the site analysis.
The method of the invention adopts Flow Injection Analysis and spectrophotomelric assay, and measuring principle is as follows: in sulfuric acid medium, under the condition that polyvinyl alcohol (PVA) exists, and cadmium iodine complex anion [CdI
4]
2-Or mercury iodine complex anion [HgI
4]
2-Can form comparatively stable blue associated matter with ethyl violet.Detected device detected when this blueness associated matter passed through flow cell, its light absorption value passes through recording device records Cheng Fengzhuan figure after being converted into electric signal, the peak height of working sample spectrogram can be found the middle cadmium of tested sample or the content of mercury on concentration-peak height working curve.
The automatic analysis method of cadmium in seawater of the present invention, surface water and the industrial sewage is provided with sample flow path, promotion liquid stream, reactant liquor stream, colour developing liquid stream and analyzing and testing stream in the analytical instrument; Promoting liquid is NaCl solution, and reactant liquor is potassium iodide-ascorbic acid-polyvinyl alcohol (PVA)-citric acid mixed liquor, and colour developing liquid is ethyl violet solution; Promote liquid and enter the analyzing and testing stream through promoting the liquid stream, mix with the reactant liquor that enters this stream in the analyzing and testing stream, above-mentioned mixed liquor mixes back generation baseline and is surveyed and drawn with the colour developing liquid that enters this stream; Standard specimen or sample enter the analyzing and testing stream through sample flow path, produce spectrogram with the living reaction of the colour developing liquid hybrid concurrency that enters this stream back with the living reaction of the reactant liquor hybrid concurrency that enters this stream back under the promotion that promotes liquid and surveyed and drawn in the analyzing and testing stream.
In order to improve sensitivity for analysis, the drift limit of standard specimen, sample and promotion liquid is 0.8～1.0ml/min, and the drift limit of reactant liquor and colour developing liquid is 0.2～0.5ml/min.
The optimization proportioning that said method promotes liquid, reactant liquor and colour developing liquid is: promote in the liquid, the weight/volume percentage of NaCl is 1～3%.In the reactant liquor, the weight/volume percentage of potassium iodide is 2～6%, and the weight/volume percentage of ascorbic acid is 0.2～0.6%, and the weight/volume percentage of polyvinyl alcohol (PVA) is 0.2～0.5%, the weight/volume percentage of citric acid is 0.1～0.5%, and the concentration of sulfuric acid is 5～13 * 10
-3Mol/L.In the colour developing liquid, the weight/volume percentage of ethyl violet is 4～8 * 10
-3%.
The automatic analysis method of mercury in seawater of the present invention, surface water and the industrial sewage is provided with sample flow path, promotion liquid stream, reactant liquor stream, colour developing liquid stream and analyzing and testing stream in the analytical instrument; Promoting liquid is NaCl solution, and reactant liquor is potassium iodide-ascorbic acid-polyvinyl alcohol (PVA)-thiocarbamide mixed liquor, and colour developing liquid is ethyl violet solution; Promote liquid and enter the analyzing and testing stream through promoting the liquid stream, mix with the reactant liquor that enters this stream in the analyzing and testing stream, above-mentioned mixed liquor mixes back generation baseline and is surveyed and drawn with the colour developing liquid that enters this stream; Standard specimen or sample enter the analyzing and testing stream through sample flow path, produce spectrogram with the living reaction of the colour developing liquid hybrid concurrency that enters this stream back with the living reaction of the reactant liquor hybrid concurrency that enters this stream back under the promotion that promotes liquid and surveyed and drawn in the analyzing and testing stream.
In order to improve sensitivity for analysis, the drift limit of standard specimen, sample and promotion liquid is 0.8～1.0ml/min, and the drift limit of reactant liquor and colour developing liquid is 0.2～0.5ml/min.
The optimization proportioning that said method promotes liquid, reactant liquor and colour developing liquid is: promote in the liquid, the weight/volume percentage of NaCl is 1～3%.In the reactant liquor, the weight/volume percentage of potassium iodide is 2～6%, and the weight/volume percentage of ascorbic acid is 0.2～0.6%, and the weight/volume percentage of polyvinyl alcohol (PVA) is 0.2～0.5%, the weight/volume percentage of thiocarbamide is 0.2～1.5%, and the concentration of sulfuric acid is 5～13 * 10
-3Mol/L.In the colour developing liquid, the weight/volume percentage of ethyl violet is 4～8 * 10
-3%.
The analytical approach of cadmium and mercury belongs to a total inventive concept, and their difference only is the difference of reactant liquor, when analyzing cadmium, contain mercury screening agent citric acid in the reactant liquor, when analyzing mercury, contain cadmium screening agent thiocarbamide in the reactant liquor, to obtain the single cadmium or the spectrogram of mercury.
It is in order to eliminate the interference of contained NaCl to analyzing in the seawater that promotion liquid is selected NaCl solution for use, NaCl content in surface water and the industrial sewage is lower than seawater, the weight/volume percentage that promotes the NaCl in the liquid should select lower bound, also can add certain NaCl in sample and standard specimen.
The present invention has following beneficial effect:
1, analytical precision height, the parallel analysis relative standard deviation is less than ± 5%.
2, do not need sample is handled, the volume of analytical instrument is little, and analysis speed is fast, and once only analyzing needs 2～5 minutes, thereby is specially adapted to on-the site analysis.
3, few, simple in structure with the supporting analytical instrument stream of this method, reduce with respect to existing analytical instrument manufacturing cost, help reducing analysis cost.
4, save chemical reagent, required chemical reagent only is 3～5% of manual analysis.
Description of drawings
Fig. 1 is a kind of structure diagram with the analytical instrument of the method for the invention coupling, also is a kind of workflow diagram of the method for the invention;
Fig. 2 is the precision test spectrogram that cadmium in the seawater is analyzed;
Fig. 3 is the precision test spectrogram that mercury in the seawater is analyzed.
Among the figure, 1-low-lift pump, 2-sampling valve, 3-mixer, 4-reacting ring, 5-mixer, 6-reacting ring, 7-optical flow cell, 8-fluorescence detector, 9-computer processing system, 10-cross-over valve, S-sample or standard specimen, C-promote liquid, R1
CdReactant liquor, the R1 of-analysis cadmium
Hg-the reactant liquor, the R2-that the analyze mercury liquid that develops the color.
Embodiment
Embodiment 1: analyze the cadmium in the seawater
1, the preparation of standard specimen
Take by weighing caddy (CdCl
22.5H
2O) 0.203lg is dissolved in after the low amounts of water and moves in the 100ml volumetric flask, is diluted with water to scale, is mixed with the stock solution that concentration is 1.00mg/ml.With the stock solution dilution, be mixed with a series of standard specimens, the concentration of each standard specimen cadmium is respectively 1.00 μ g/L, 2.00 μ g/L, 4.00 μ g/L, 8.00 μ g/L, 10.00 μ g/L.
2, reactant liquor R1
CdPreparation
Take by weighing potassium iodide, that ascorbic acid is mixed with 20% potassium iodide-2% ascorbic acid stock solution is standby, pipettes the H of 4.5mol/L
2SO
4In volumetric flask, add 20% potassium iodide-2% ascorbic acid stock solution, add polyvinyl alcohol (PVA) and citric acid again, last dilute with water, in the reactant liquor of being prepared, the weight/volume percentage of potassium iodide is 5%, the weight/volume percentage of ascorbic acid is 0.6%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.4%, and the weight/volume percentage of citric acid is 0.2%, and the concentration of sulfuric acid is 10 * 10
-3Mol/L.
3, the preparation of colour developing liquid
Take by weighing ethyl violet 0.03g in volumetric flask, thin up, the weight/volume percentage that makes ethyl violet is 6 * 10
-3%.
4, promote the preparation of liquid
Take by weighing the 7.5g anhydrous NaCl in volumetric flask, thin up, the weight/volume percentage that makes NaCl is 2.5%.
5, the testing and drawing of sample spectrogram
Employing is tested by the automatic analyzer of technical flow design shown in Figure 1, low-lift pump 1 is selected the four-way constant flow pump for use, the drift limit of standard specimen, sample and promotion liquid is 0.9ml/min, the drift limit of reactant liquor and colour developing liquid is 0.4ml/min, optical flow cell is the 20mm light path, and the detection wavelength is 530nm.
At first carry out the baseline mapping, promote liquid C and under the driving of low-lift pump 1, enter the analyzing and testing stream, in the analyzing and testing stream with by low-lift pump 1, drive the reactant liquor R1 that enters this stream through promoting liquid stream and sampling valve 2
CdIn mixer 3, mix, in reactor 4, further mix, above-mentioned mixed liquor mixes in mixer 5, further mixes the back by optical flow cell 7 in reactor 6 with the colour developing liquid R2 that is entered this stream by low-lift pump 1 driving, and fluorescence detector 8 is transferred to computer processing system 9 with signal and promptly draws a baseline on computer display.After the baseline mapping is finished, sample S enters the analyzing and testing stream through sample flow path and sampling valve 2 under the driving of low-lift pump 1, meanwhile, low-lift pump 1 drives promotion liquid C and enters the analyzing and testing stream by sampling valve 2, under the promotion that promotes liquid, sample and the reactant liquor R1 that enters the analyzing and testing stream by low-lift pump 1 driving
CdHybrid concurrency is given birth to reaction in mixer 3, further hybrid concurrency is given birth to reaction in reactor 4, above-mentioned mixed liquor is given birth to reaction with the colour developing liquid R2 hybrid concurrency in mixer 5 that is entered this stream by low-lift pump 1 driving under the promotion of promotion liquid, further hybrid concurrency is given birth to and reacted the back by optical flow cell 7 in reactor 6, fluorescence detector 8 is transferred to computer processing system 9 is promptly drawn cadmium in the tested sample on computer display spectrogram with signal, and its precision test spectrogram as shown in Figure 2.
6, the testing and drawing of standard specimen spectrogram
The used instrument of testing and drawing standard specimen spectrogram, promote the used instrument of liquid, reactant liquor, colour developing liquid and testing and drawing sample spectrogram, promote liquid, reactant liquor, colour developing liquid phase be same, method of testing is also identical.The standard specimen of being prepared is analyzed from thin to thick successively, promptly got the series of standards spectrogram.
7, the sample testing result calculates
Sample spectrogram and the standard spectrogram drawn are compared, then can calculate the cadmium content in the sample.
Embodiment 2: analyze the cadmium in the surface water
1, the preparation of standard specimen
Identical with embodiment 1.
2, reactant liquor R1
CdPreparation
Take by weighing potassium iodide, that ascorbic acid is mixed with 20% potassium iodide-2% ascorbic acid stock solution is standby, pipettes the H of 4.5mol/L
2SO
4In volumetric flask, add 20% potassium iodide-2% ascorbic acid stock solution, add polyvinyl alcohol (PVA) and citric acid again, last dilute with water, in the reactant liquor of being prepared, the weight/volume percentage of potassium iodide is 3%, the weight/volume percentage of ascorbic acid is 0.3%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.3%, and the weight/volume percentage of citric acid is 0.3%, and the concentration of sulfuric acid is 8 * 10
-3Mol/L.
3, the preparation of colour developing liquid
Take by weighing ethyl violet 0.03g in volumetric flask, thin up, the weight/volume percentage that makes ethyl violet is 4 * 10
-3%.
4, promote the preparation of liquid
Take by weighing the 7.5g anhydrous NaCl in volumetric flask, thin up, the weight/volume percentage that makes NaCl is 1%.
5, the testing and drawing of sample spectrogram
Employing is tested by the automatic analyzer of technical flow design shown in Figure 1, low-lift pump 1 is selected the four-way constant flow pump for use, the drift limit of standard specimen, sample and promotion liquid is 1.0ml/min, the drift limit of reactant liquor and colour developing liquid is 0.3ml/min, optical flow cell is the 20mm light path, and the detection wavelength is 530nm.
The test operation method is identical with embodiment 1.
6, the testing and drawing of standard specimen spectrogram
The used instrument of testing and drawing standard specimen spectrogram, promote the used instrument of liquid, reactant liquor, colour developing liquid and testing and drawing sample spectrogram, promote liquid, reactant liquor, colour developing liquid phase be same, method of testing is also identical.The standard specimen of being prepared is analyzed from thin to thick successively, promptly got the series of standards spectrogram.
7, the sample testing result calculates
Sample spectrogram and the standard spectrogram drawn are compared, then can calculate the cadmium content in the sample.
Embodiment 3: the cadmium in the analytical industry sewage
1, the preparation of standard specimen
Identical with embodiment 1.
2, reactant liquor R1
CdPreparation
Take by weighing potassium iodide, that ascorbic acid is mixed with 20% potassium iodide-2% ascorbic acid stock solution is standby, pipettes the H of 4.5mol/L
2SO
4In volumetric flask, add 20% potassium iodide-2% ascorbic acid stock solution, add polyvinyl alcohol (PVA) and citric acid again, last dilute with water, in the reactant liquor of being prepared, the weight/volume percentage of potassium iodide is 6%, the weight/volume percentage of ascorbic acid is 0.5%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.5%, and the weight/volume percentage of citric acid is 0.4%, and the concentration of sulfuric acid is 6 * 10
-3Mol/L.
3, the preparation of colour developing liquid
Take by weighing ethyl violet 0.03g in volumetric flask, thin up, the weight/volume percentage that makes ethyl violet is 8 * 10
-3%.
4, promote the preparation of liquid
Take by weighing the 7.5g anhydrous NaCl in volumetric flask, thin up, the weight/volume percentage that makes NaCl is 1.5%.
5, the testing and drawing of sample spectrogram
Employing is tested by the automatic analyzer of technical flow design shown in Figure 1, low-lift pump 1 is selected the four-way constant flow pump for use, the drift limit of standard specimen, sample and promotion liquid is 0.8ml/min, the drift limit of reactant liquor and colour developing liquid is 0.25ml/min, optical flow cell is the 20mm light path, and the detection wavelength is 530nm.
The test operation method is identical with embodiment 1.
6, the testing and drawing of standard specimen spectrogram
The used instrument of testing and drawing standard specimen spectrogram, promote the used instrument of liquid, reactant liquor, colour developing liquid and testing and drawing sample spectrogram, promote liquid, reactant liquor, colour developing liquid phase be same, method of testing is also identical.The standard specimen of being prepared is analyzed from thin to thick successively, promptly got the series of standards spectrogram.
7, the sample testing result calculates
Sample spectrogram and the standard spectrogram drawn are compared, then can calculate the cadmium content in the sample.
Embodiment 4: analyze the mercury in the seawater
1, the preparation of standard specimen
Take by weighing mercuric chloride HgCl
20.1353g, be dissolved in after the low amounts of water and move in the 100ml volumetric flask, be diluted with water to scale, be mixed with the stock solution that concentration is 1.00mg/mL.With the stock solution dilution, be mixed with a series of standard specimens, the concentration of each standard specimen cadmium is respectively 2.00 μ g/L, 4.00 μ g/L, 8.00 μ g/L, 16.00 μ g/L, 20.00 μ g/L.
2, reactant liquor R1
HgPreparation
Take by weighing potassium iodide, that ascorbic acid is mixed with 20% potassium iodide-2% ascorbic acid stock solution is standby, pipettes the H of 4.5mol/L
2SO
4In volumetric flask, add 20% potassium iodide-2% ascorbic acid stock solution, add polyvinyl alcohol (PVA) and thiocarbamide again, last dilute with water, in the reactant liquor of being prepared, the weight/volume percentage of potassium iodide is 4%, the weight/volume percentage 0.3% of ascorbic acid, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.4%, and the weight/volume percentage of thiocarbamide is 1.2%, and the concentration of sulfuric acid is 8 * 10
-3Mol/L.
3, the preparation of colour developing liquid
Take by weighing ethyl violet 0.03g in volumetric flask, thin up, the weight/volume percentage that makes ethyl violet is 5 * 10
-3%.
4, promote the preparation of liquid
Take by weighing the 7.5g anhydrous NaCl in volumetric flask, thin up, the weight/volume percentage that makes NaCl is 3%.
5, the testing and drawing of sample spectrogram
Employing is tested by the automatic analyzer of technical flow design shown in Figure 1, low-lift pump 1 is selected the four-way constant flow pump for use, the drift limit of standard specimen, sample and promotion liquid is 0.9ml/min, the drift limit of reactant liquor and colour developing liquid is 0.35ml/min, optical flow cell is the 20mm light path, and the detection wavelength is 530nm.
At first carry out the baseline mapping, promote liquid C and under the driving of low-lift pump 1, enter the analyzing and testing stream, in the analyzing and testing stream with by low-lift pump 1, drive the reactant liquor R1 that enters this stream through promoting liquid stream and sampling valve 2
HgIn mixer 3, mix, in reactor 4, further mix, above-mentioned mixed liquor mixes in mixer 5, further mixes the back by optical flow cell 7 in reactor 6 with the colour developing liquid R2 that is entered this stream by low-lift pump 1 driving, and fluorescence detector 8 is transferred to computer processing system 9 with signal and promptly draws a baseline on computer display.After the baseline mapping is finished, sample S enters the analyzing and testing stream through sample flow path and sampling valve 2 under the driving of low-lift pump 1, meanwhile, low-lift pump 1 drives promotion liquid C and enters the analyzing and testing stream by sampling valve 2, under the promotion that promotes liquid, sample and the reactant liquor R1 that enters the analyzing and testing stream by low-lift pump 1 driving
HgHybrid concurrency is given birth to reaction in mixer 3, further hybrid concurrency is given birth to reaction in reactor 4, above-mentioned mixed liquor is given birth to reaction with the colour developing liquid R2 hybrid concurrency in mixer 5 that is entered this stream by low-lift pump 1 driving under the promotion of promotion liquid, further hybrid concurrency is given birth to and reacted the back by optical flow cell 7 in reactor 6, fluorescence detector 8 is transferred to computer processing system 9 is promptly drawn mercury in the tested sample on computer display spectrogram with signal, and its precision test spectrogram as shown in Figure 3.
6, the testing and drawing of standard specimen spectrogram
The used instrument of testing and drawing standard specimen spectrogram, promote the used instrument of liquid, reactant liquor, colour developing liquid and testing and drawing sample spectrogram, promote liquid, reactant liquor, colour developing liquid phase be same, method of testing is also identical.The standard specimen of being prepared is analyzed from thin to thick successively, promptly got the series of standards spectrogram.
7, the sample testing result calculates
Sample spectrogram and the standard spectrogram drawn are compared, then can calculate the mercury content in the sample.
Embodiment 5: analyze the mercury in the surface water
1, the preparation of standard specimen
Identical with embodiment 1.
2, reactant liquor R1
HgPreparation
Take by weighing potassium iodide, that ascorbic acid is mixed with 20% potassium iodide-2% ascorbic acid stock solution is standby, pipettes the H of 4.5mol/L
2SO
4In volumetric flask, add 20% potassium iodide-2% ascorbic acid stock solution, add polyvinyl alcohol (PVA) and citric acid again, last dilute with water, in the reactant liquor of being prepared, the weight/volume percentage of potassium iodide is 3.5%, the weight/volume percentage of ascorbic acid is 0.4%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.3%, and the weight/volume percentage of thiocarbamide is 1.0%, and the concentration of sulfuric acid is 5 * 10
-3Mol/L.
3, the preparation of colour developing liquid
Take by weighing ethyl violet 0.03g in volumetric flask, thin up, the weight/volume percentage that makes ethyl violet is 3 * 10
-3%.
4, promote the preparation of liquid
Take by weighing the 7.5g anhydrous NaCl in volumetric flask, thin up, the weight/volume percentage that makes NaCl is 1%.
5, the testing and drawing of sample spectrogram
Employing is tested by the automatic analyzer of technical flow design shown in Figure 1, low-lift pump 1 is selected the four-way constant flow pump for use, the drift limit of standard specimen, sample and promotion liquid is 1.0ml/min, the drift limit of reactant liquor and colour developing liquid is 0.45ml/min, optical flow cell is the 20mm light path, and the detection wavelength is 530nm.
The test operation method is identical with embodiment 4.
6, the testing and drawing of standard specimen spectrogram
The used instrument of testing and drawing standard specimen spectrogram, promote the used instrument of liquid, reactant liquor, colour developing liquid and testing and drawing sample spectrogram, promote liquid, reactant liquor, colour developing liquid phase be same, method of testing is also identical.The standard specimen of being prepared is analyzed from thin to thick successively, promptly got the series of standards spectrogram.
7, the sample testing result calculates
Sample spectrogram and the standard spectrogram drawn are compared, then can calculate the mercury content in the sample.
Embodiment 6: the mercury in the analytical industry sewage
1, the preparation of standard specimen
Identical with embodiment 1.
2, reactant liquor R1
HgPreparation
Take by weighing potassium iodide, that ascorbic acid is mixed with 20% potassium iodide-2% ascorbic acid stock solution is standby, pipettes the H of 4.5mol/L
2SO
4In volumetric flask, add 20% potassium iodide-2% ascorbic acid stock solution, add polyvinyl alcohol (PVA) and citric acid again, last dilute with water, in the reactant liquor of being prepared, the weight/volume percentage of potassium iodide is 5%, the weight/volume percentage of ascorbic acid is 0.5%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.5%, and the weight/volume percentage of thiocarbamide is 0.6%, and the concentration of sulfuric acid is 10 * 10
-3Mol/L.
3, the preparation of colour developing liquid
Take by weighing ethyl violet 0.03g in volumetric flask, thin up, the weight/volume percentage that makes ethyl violet is 7 * 10
-3%.
4, promote the preparation of liquid
Take by weighing the 7.5g anhydrous NaCl in volumetric flask, thin up, the weight/volume percentage that makes NaCl is 1.2%.
5, the testing and drawing of sample spectrogram
Employing is tested by the automatic analyzer of technical flow design shown in Figure 1, low-lift pump 1 is selected the four-way constant flow pump for use, the drift limit of standard specimen, sample and promotion liquid is 0.8ml/min, the drift limit of reactant liquor and colour developing liquid is 0.25ml/min, optical flow cell is the 20mm light path, and the detection wavelength is 530nm.
The test operation method is identical with embodiment 4.
6, the testing and drawing of standard specimen spectrogram
The used instrument of testing and drawing standard specimen spectrogram, promote the used instrument of liquid, reactant liquor, colour developing liquid and testing and drawing sample spectrogram, promote liquid, reactant liquor, colour developing liquid phase be same, method of testing is also identical.The standard specimen of being prepared is analyzed from thin to thick successively, promptly got the series of standards spectrogram.
7, the sample testing result calculates
Sample spectrogram and the standard spectrogram drawn are compared, then can calculate the mercury content in the sample.
Claims (4)
1. the automatic analysis method of cadmium in a seawater, surface water and the industrial sewage is characterized in that:
(1) adopts Flow Injection Analysis and spectrophotomelric assay, be provided with sample flow path, promotion liquid stream, reactant liquor stream, colour developing liquid stream and analyzing and testing stream in the analytical instrument;
(2) promoting liquid is NaCl solution, promotes in the liquid, and the weight/volume percentage of NaCl is 1～3%; Reactant liquor is potassium iodide-ascorbic acid-polyvinyl alcohol (PVA)-citric acid mixed liquor, in the reactant liquor, the weight/volume percentage of potassium iodide is 2～6%, the weight/volume percentage of ascorbic acid is 0.2～0.6%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.2～0.5%, the weight/volume percentage of citric acid is 0.1～0.5%, and the concentration of sulfuric acid is 5～13 * 10
-3Mol/L; Colour developing liquid is ethyl violet solution, and in the colour developing liquid, the weight/volume percentage of ethyl violet is 4～8 * 10
-3%;
(3) promote liquid and enter the analyzing and testing stream through promoting the liquid stream, mix with the reactant liquor that enters this stream in the analyzing and testing stream, above-mentioned mixed liquor mixes back generation baseline and is surveyed and drawn with the colour developing liquid that enters this stream;
(4) standard specimen or sample enter the analyzing and testing stream through sample flow path, produce spectrogram with the living reaction of the colour developing liquid hybrid concurrency that enters this stream back with the living reaction of the reactant liquor hybrid concurrency that enters this stream back under the promotion that promotes liquid and surveyed and drawn in the analyzing and testing stream.
2. the automatic analysis method of cadmium in seawater according to claim 1, surface water and the industrial sewage, the flow velocity that it is characterized in that standard specimen, sample and promotion liquid is 0.8～1.0ml/min, the flow velocity of reactant liquor and colour developing liquid is 0.2～0.5ml/min.
3. the automatic analysis method of mercury in a seawater, surface water and the industrial sewage is characterized in that:
(1) adopts Flow Injection Analysis and spectrophotomelric assay, be provided with sample flow path, promotion liquid stream, reactant liquor stream, colour developing liquid stream and analyzing and testing stream in the analytical instrument;
(2) promoting liquid is NaCl solution, promotes in the liquid, and the weight/volume percentage of NaCl is 1～3%; Reactant liquor is potassium iodide-ascorbic acid-polyvinyl alcohol (PVA)-thiocarbamide mixed liquor, in the reactant liquor, the weight/volume percentage of potassium iodide is 2～6%, the weight/volume percentage of ascorbic acid is 0.2～0.6%, the weight/volume percentage of polyvinyl alcohol (PVA) is 0.2～0.5%, the weight/volume percentage of thiocarbamide is 0.2～1.5%, and the concentration of sulfuric acid is 5～13 * 10
-3Mol/L; Colour developing liquid is ethyl violet solution, and in the colour developing liquid, the weight/volume percentage of ethyl violet is 4～8 * 10
-3%;
(3) promote liquid and enter the analyzing and testing stream through promoting the liquid stream, mix with the reactant liquor that enters this stream in the analyzing and testing stream, above-mentioned mixed liquor mixes back generation baseline and is surveyed and drawn with the colour developing liquid that enters this stream;
(4) standard specimen or sample enter the analyzing and testing stream through sample flow path, produce spectrogram with the living reaction of the colour developing liquid hybrid concurrency that enters this stream back with the living reaction of the reactant liquor hybrid concurrency that enters this stream back under the promotion that promotes liquid and surveyed and drawn in the analyzing and testing stream.
4. the automatic analysis method of mercury in seawater according to claim 3, surface water and the industrial sewage, the flow velocity that it is characterized in that standard specimen, sample and promotion liquid is 0.8～1.0ml/min, the flow velocity of reactant liquor and colour developing liquid is 0.2～0.5ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100210848A CN100424493C (en) | 2005-06-15 | 2005-06-15 | Automatic analysis of cadmium and mercury in seawater, surface water and sewage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100210848A CN100424493C (en) | 2005-06-15 | 2005-06-15 | Automatic analysis of cadmium and mercury in seawater, surface water and sewage |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1712934A CN1712934A (en) | 2005-12-28 |
| CN100424493C true CN100424493C (en) | 2008-10-08 |
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| CNB2005100210848A Expired - Fee Related CN100424493C (en) | 2005-06-15 | 2005-06-15 | Automatic analysis of cadmium and mercury in seawater, surface water and sewage |
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| CN101975777A (en) * | 2010-10-28 | 2011-02-16 | 四川大学 | Automatic analysis method of chlorate in water sample |
| CN102830117A (en) * | 2012-09-18 | 2012-12-19 | 国家海洋局天津海水淡化与综合利用研究所 | Device and method for carrying out continuous flow detection on bicarbonates in water |
| CN104569457B (en) * | 2015-01-13 | 2016-08-24 | 四川大学 | The automatic analysis method of trace nickelous in water sample |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1983003057A1 (en) * | 1982-03-09 | 1983-09-15 | Roald-Franch Walle | Transmission of small volumes of liquid samples |
| CN1419118A (en) * | 2002-12-12 | 2003-05-21 | 施文健 | Novel method for investigating cadmium and mercury |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1983003057A1 (en) * | 1982-03-09 | 1983-09-15 | Roald-Franch Walle | Transmission of small volumes of liquid samples |
| CN1419118A (en) * | 2002-12-12 | 2003-05-21 | 施文健 | Novel method for investigating cadmium and mercury |
Non-Patent Citations (2)
| Title |
|---|
| 交替注入流动注射分光光度法同时测定镉和汞. 陈菊，赵书林.冶金分析，第20卷第3期. 2000 |
| 交替注入流动注射分光光度法同时测定镉和汞. 陈菊，赵书林.冶金分析，第20卷第3期. 2000 * |
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