CN101581675A - Method of simultaneously measuring mercury and cadmium - Google Patents
Method of simultaneously measuring mercury and cadmium Download PDFInfo
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- CN101581675A CN101581675A CNA2008100114153A CN200810011415A CN101581675A CN 101581675 A CN101581675 A CN 101581675A CN A2008100114153 A CNA2008100114153 A CN A2008100114153A CN 200810011415 A CN200810011415 A CN 200810011415A CN 101581675 A CN101581675 A CN 101581675A
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- cadmium
- mercury
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- measuring
- testing sample
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Abstract
The invention relates to a method of simultaneously measuring heavy metals of mercury and cadmium, in particular to a method of simultaneously measuring mercury and cadmium. The method of simultaneously measuring the mercury and the cadmium comprises the following steps: a red composition is generated by simultaneous sensitive color development reactions of the mercury and the cadmium with carboxyl phenyl diazoamino azo under an alkaline condition and the existence of TritonX-100, has the maximum absorption wavelength of 520 nm and absorbency which presents obvious additivity property while the mercury and the cadmium simultaneously exist; the cadmium is successfully masked by adding sodium pyrophosphate as a masking agent so as to measure the mercury; and then, a light absorption value of the mercury is subtracted from a sum light absorption value of the mercury and the cadmium to obtain an absorption value of the cadmium. The method has the mercury detection limit of 0.01 mg/L and the cadmium detection limit of 0.005 mg/L, is simple and rapid to operate and has accurate measuring results.
Description
Technical field
The present invention relates to the determination techniques of heavy metal Hg and cadmium, specifically is a kind of method of measuring mercury and cadmium simultaneously.
Background technology
Heavy metal Hg and cadmium are to be the important pollutant that receives much attention always, can be at human body, and accumulation in the animal body has carcinogenic, teratogenesis, mutagenesis, therefore detects the attention that has been subjected to more and more widely by its pollution that causes and supervision.The water sample of mercurous usually, cadmium pollution or treating fluid all adopt under test condition separately, measure its content respectively, and sample preparation and determination step are comparatively loaded down with trivial details, and be consuming time longer.At the detection of this two heavy metal species, at present the most frequently used is large-scale instrument analytic approachs such as atomic absorption and atomic fluorescence, needs the operating personnel of expensive instrument and equipment and specialty.Next is to be the spectrophotometric method of representative with the dithizone method, dithizone less stable in this method, and need to use harmful organic solvent such as Lu side, and because dithizone and multiple metallic ion all can develop the color, measure disturb more.
Summary of the invention
The object of the invention has been to provide that a kind of convenience is quick, cost is low, measure the method for mercury and cadmium good stability the time.
For achieving the above object, the technical solution used in the present invention is:
Measure the method for mercury and cadmium simultaneously: with 1-5mL Na
2B
4O
7-NaOH buffer solution and 0.5-3mL chromogenic reagent solution join in the 10-50mL testing sample, shake up, and behind the static 20-40min, mensuration obtains adding and absorbance M of mercury, cadmium at spectrophotometer 520nm place; Then in addition with 1-5mLNa
2B
4O
7-NaOH buffer solution, 5～50mg sodium pyrophosphate and 0.5-3mL chromogenic reagent solution add in the 10-50mL testing sample, shake up, and behind the static 20-40min, measure the absorbance N that obtains mercury in the testing sample at spectrophotometer 520nm place; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing the adjacent carboxyl phenyl diazoamino of 5～40mg azobenzene it is dissolved among 0.5～5g TritonX-100, be settled to 100mL with alcohol or ketone solution.Described Na
2B
4O
7-NaOH buffer solution pH=10.6.Described when measuring absorbance at spectrophotometer 520nm place the reagent blank with distilled water be reference.Obtain adding and the absorbance N of absorbance M, mercury and the absorbance M-N of cadmium of mercury, cadmium by measuring at spectrophotometer 520nm place, draw the typical curve of mercury and cadmium, the difference that realizes the two is quantitative, the linear determination scope of its mercury and cadmium is 0.02-0.6mg/L, the detection of mercury is limited to 0.01mg/L, and the detection of cadmium is limited to 0.005mg/L.
Realize the further description of the object of the invention: because mercury and cadmium are congeners, chemical property is close, realize the independent mensuration of mercury, and cadmium can produce serious disturbance.Must or shelter its removal.Screening at the cadmium screening agent, sodium pyrophosphate, sodium tartrate, sodium fluoride, potassium iodide, nitrilotriacetic acid, sodium thiosulfate, EDTA etc. have been attempted, the result shows that the masking effect of sodium pyrophosphate is best in this method, can successfully shelter cadmium and does not influence the mensuration of mercury.The screening ability test shows, for the standard solution of mercurous 2 μ g, adds sodium pyrophosphate 5-50mg, measures in light absorption value error ± 5% scope of solution, allows coexisting ion amount (μ g): Cd
2+(10), Pb
2+(40), Zn
2+(5), Mg
2+(20), Cl
-(60), Na
+, K
+, Ca
2+, NO
3 -, F
-, Cl
-, SO
4 2-, CO
3 2-, PO
4 3-(20000), NH
4 +, Mg
2+, As
3+, C
2O
4 2-(1000), Al
3+(800), Fe
3+(600), Cr
3+(400), Mn
2+(100).
Principle of the present invention is based on alkali condition and TritonX-100 exists down, and mercury, cadmium with adjacent carboxyl phenyl diazoamino azo sensitive chromogenic reaction take place simultaneously, generate red complex.The maximum absorption wavelength of this complex is 520nm, and when mercury, cadmium existed simultaneously, its absorbance presented tangible additive property.By adding sodium pyrophosphate as screening agent, successfully cadmium is sheltered, realize the mensuration of mercury; From the light absorption value that deducts mercury with light absorption value that adds of the two, obtain the absorption value of cadmium then.By on measure respectively when can realize mercury and cadmium.
The advantage that the present invention had:
1. simple to operate.As long as parallelly get two parts of test solutions to be measured, according to the inventive method operation, the difference by absorption value subtracts calculating, can measure wherein mercury and cadmium respectively, reaches the two simultaneously quantitative purpose.
2. good stability.Use reagent stability good in the inventive method, the normal temperature sealing was preserved the term of validity greater than 6 months.Colour developing back complex absorbance reaches maximal value and stable within 20～90min, the tester can operate calmly.
3. fast convenient.The present invention's operation is used with portable direct-reading tintmeter, and is quantitative when only needing 25～30min can finish mercury and cadmium.
Embodiment
Embodiment 1
Get the 10mL testing sample in the 10mL color comparison tube, add the Na of 1mL pH=10.6
2B
4O
7-NaOH buffer solution and 1mL chromogenic reagent solution shake up, and obtain adding and absorbance M of mercury, cadmium in spectrophotometer 520nm place mensuration behind the static 20min; Then get the 10mL testing sample in addition in the 10mL color comparison tube, add the Na of 1mL pH=10.6 simultaneously
2B
4O
7-NaOH buffer solution, 5mg sodium pyrophosphate and 1mL chromogenic reagent solution shake up, and obtain the absorbance N of mercury in the testing sample behind the static 20min in spectrophotometer 520nm place mensuration; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing adjacent carboxyl phenyl diazoamino azobenzene of 5mg and 0.5gTritonX-100, be settled to 100mL with 95% ethanol; When spectrophotometer 520nm place measures absorbance, be reference with the reagent blank of distilled water.
Obtain adding and the absorbance N of absorbance M, mercury and the absorbance M-N of cadmium of mercury, cadmium by measuring, draw the typical curve of mercury and cadmium, realize that the difference of the two is quantitative at spectrophotometer 520nm place.
The range of linearity of measuring mercury and cadmium according to method of the present invention is 0.02-0.6mg/L, draws the typical curve of mercury and cadmium, regression equation, coefficient R
2ε is respectively with apparent molar absorption coefficient:
A
Hg=0.8731C
Hg(mg/L)+0.0021, coefficient R 2=0.9998, ε
Hg=1.75x105L/ (molcm)
A
Cd=1.679C
Cd(mg/L)+0.0102, coefficient R 2=0.9994, ε
Cd=1.89x105L/ (molcm)
The detection of mercury is limited to 0.01mg/L among the present invention, and the detection of cadmium is limited to 0.005mg/L, can satisfy the assay determination of little Trace Hg, cadmium.
Embodiment 2
Get the 50mL testing sample in color comparison tube, add the Na of 5mL pH=10.6
2B
4O
7-NaOH buffer solution and 3mL chromogenic reagent solution shake up, and obtain adding and absorbance M of mercury, cadmium in spectrophotometer 520nm place mensuration behind the static 40min; Then get the 50mL testing sample in addition in color comparison tube, add the Na of 5mL pH=10.6 simultaneously
2B
4O
7-NaOH buffer solution, 50mg sodium pyrophosphate and 3mL chromogenic reagent solution shake up, and obtain the absorbance N of mercury in the testing sample behind the static 40min in spectrophotometer 520nm place mensuration; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing adjacent carboxyl phenyl diazoamino azobenzene of 40mg and 5gTritonX-100, be settled to 100mL with acetone.
Embodiment 3
Get the 30mL testing sample in color comparison tube, add the Na of 3mL pH=10.6
2B
4O
7-NaOH buffer solution and 0.5mL chromogenic reagent solution shake up, and obtain adding and absorbance M of mercury, cadmium in spectrophotometer 520nm place mensuration behind the static 30min; Then get the 30mL testing sample in addition in color comparison tube, add the Na of 3mL pH=10.6 simultaneously
2B
4O
7-NaOH buffer solution, 20mg sodium pyrophosphate and 0.5mL chromogenic reagent solution shake up, and obtain the absorbance N of mercury in the testing sample behind the static 30min in spectrophotometer 520nm place mensuration; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing adjacent carboxyl phenyl diazoamino azobenzene of 20mg and 2gTritonX-100, be settled to 100mL with acetone.
Embodiment 4
Get the 20mL testing sample in color comparison tube, add the Na of 2mL pH=10.6
2B
4O
7-NaOH buffer solution and 2mL chromogenic reagent solution shake up, and obtain adding and absorbance M of mercury, cadmium in spectrophotometer 520nm place mensuration behind the static 35min; Then get the 20mL testing sample in addition in color comparison tube, add the Na of 2mL pH=10.6 simultaneously
2B
4O
7-NaOH buffer solution, 10mg sodium pyrophosphate and 2mL chromogenic reagent solution shake up, and obtain the absorbance N of mercury in the testing sample behind the static 35min in spectrophotometer 520nm place mensuration; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing adjacent carboxyl phenyl diazoamino azobenzene of 15mg and 0.8gTritonX-100, be settled to 100mL with acetone.
Embodiment 5
Get the 40mL testing sample in color comparison tube, add the Na of 2.5mL pH=10.6
2B
4O
7-NaOH buffer solution and 1.5mL chromogenic reagent solution shake up, and obtain adding and absorbance M of mercury, cadmium in spectrophotometer 520nm place mensuration behind the static 25min; Then get the 40mL testing sample in addition in color comparison tube, add the Na of 2.5mL pH=10.6 simultaneously
2B
4O
7-NaOH buffer solution, 15mg sodium pyrophosphate and 1.5mL chromogenic reagent solution shake up, and obtain the absorbance N of mercury in the testing sample behind the static 25min in spectrophotometer 520nm place mensuration; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing adjacent carboxyl phenyl diazoamino azobenzene of 25mg and 1gTritonX-100, be settled to 100mL with absolute ethyl alcohol.
Embodiment 6
Get the 15mL testing sample in color comparison tube, add the Na of 4.5mLpH=10.6
2B
4O
7-NaOH buffer solution and 2.5mL chromogenic reagent solution shake up, and obtain adding and absorbance M of mercury, cadmium in spectrophotometer 520nm place mensuration behind the static 20min; Then get the 15mL testing sample in addition in color comparison tube, add the Na of 4.5mL pH=10.6 simultaneously
2B
4O
7-NaOH buffer solution, 35mg sodium pyrophosphate and 2.5mL chromogenic reagent solution shake up, and obtain the absorbance N of mercury in the testing sample behind the static 20min in spectrophotometer 520nm place mensuration; The absorbance M-N of cadmium in the testing sample.
Described chromogenic reagent solution is: take by weighing among adjacent carboxyl phenyl diazoamino azobenzene of 30mg and the 3gTritonX-100, be settled to 100mL with 95% ethanol.
Application examples
The precision of analysis result and accuracy:
Measure according to mercury of the present invention, cadmium method for measuring simultaneously, at 0.02mg/L, 0.08mg/L adds mercury and cadmium respectively on three concentration levels of 0.20mg/L in tap water and two rivers with standard addition method, do parallel recovery test five times, measurement result sees Table 1.
The table 1 mark-on test recovery (%)
As seen, 0.02,0.08, on three mark-on levels of 0.20mg/L, the recovery 85%～109% of mercury and cadmium, relative deviation 1.9%～5.2%.
Therefore, use method of the present invention and distinguish mercury and cadmium in the quantitative test solution to be measured simultaneously, can obtain fast, stable, reliable result.
Claims (5)
1. a method of measuring mercury and cadmium simultaneously is characterized in that: with 1-5mL Na
2B
4O
7-NaOH buffer solution and 0.5-3mL chromogenic reagent solution join in the 10-50mL testing sample, shake up, and behind the static 20-40min, mensuration obtains adding and absorbance M of mercury, cadmium at spectrophotometer 520nm place; Then in addition with 1-5mL Na
2B
4O
7-NaOH buffer solution, 5～50mg sodium pyrophosphate and 0.5-3mL chromogenic reagent solution add in the 10-50mL testing sample, shake up, and behind the static 20-40min, measure the absorbance N that obtains mercury in the testing sample at spectrophotometer 520nm place; The absorbance M-N of cadmium in the testing sample.
2. by the described method of measuring mercury and cadmium simultaneously of claim 1, it is characterized in that: described chromogenic reagent solution is: take by weighing the adjacent carboxyl phenyl diazoamino of 5～40mg azobenzene it is dissolved among 0.5～5gTritonX-100, be settled to 100mL with alcohol or ketone solution.
3. by the described method of measuring mercury and cadmium simultaneously of claim 1, it is characterized in that: described Na
2B
4O
7-NaOH buffer solution pH=10.6.
4. by the described method of measuring mercury and cadmium simultaneously of claim 1, it is characterized in that: described when measuring absorbance at spectrophotometer 520nm place the reagent blank with distilled water be reference.
5. by the described method of measuring mercury and cadmium simultaneously of claim 1, it is characterized in that: obtain adding and the absorbance N of absorbance M, mercury and the absorbance M-N of cadmium of mercury, cadmium by measuring at spectrophotometer 520nm place, draw the typical curve of mercury and cadmium, the difference that realizes the two is quantitative, the linear determination scope of its mercury and cadmium is 0.02-0.6mg/L, the detection of mercury is limited to 0.01mg/L, and the detection of cadmium is limited to 0.005mg/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100114153A CN101581675A (en) | 2008-05-15 | 2008-05-15 | Method of simultaneously measuring mercury and cadmium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100114153A CN101581675A (en) | 2008-05-15 | 2008-05-15 | Method of simultaneously measuring mercury and cadmium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101581675A true CN101581675A (en) | 2009-11-18 |
Family
ID=41363918
Family Applications (1)
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|---|---|---|---|
| CNA2008100114153A Pending CN101581675A (en) | 2008-05-15 | 2008-05-15 | Method of simultaneously measuring mercury and cadmium |
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| Country | Link |
|---|---|
| CN (1) | CN101581675A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487390A (en) * | 2013-09-18 | 2014-01-01 | 深圳市绿恩环保技术有限公司 | Testing method for cadmium content in water body |
| WO2014075385A1 (en) * | 2012-11-13 | 2014-05-22 | 北京吉天仪器有限公司 | Method and instrument for simultaneously measuring mercury and cadmium by direct sample injection |
| CN104897590A (en) * | 2015-06-03 | 2015-09-09 | 常州大学 | Method for quickly detecting content of petroleum hydrocarbon and thallus in oily sewage treatment system |
| CN109781721A (en) * | 2019-03-15 | 2019-05-21 | 中南大学 | Test system optimization method that is a kind of while measuring copper cobalt ferronickel content in zinc electrolyte |
| CN110361343A (en) * | 2019-08-20 | 2019-10-22 | 贵州大学 | A kind of heavy metal colorimetric detection method based on oligonucleotide regulation mangano-manganic oxide catalytic activity |
-
2008
- 2008-05-15 CN CNA2008100114153A patent/CN101581675A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014075385A1 (en) * | 2012-11-13 | 2014-05-22 | 北京吉天仪器有限公司 | Method and instrument for simultaneously measuring mercury and cadmium by direct sample injection |
| JP2016503500A (en) * | 2012-11-13 | 2016-02-04 | 北京吉天儀器有限公司 | Method and instrument technology for measuring mercury and cadmium at the same time as introducing a sample directly |
| CN103487390A (en) * | 2013-09-18 | 2014-01-01 | 深圳市绿恩环保技术有限公司 | Testing method for cadmium content in water body |
| CN104897590A (en) * | 2015-06-03 | 2015-09-09 | 常州大学 | Method for quickly detecting content of petroleum hydrocarbon and thallus in oily sewage treatment system |
| CN109781721A (en) * | 2019-03-15 | 2019-05-21 | 中南大学 | Test system optimization method that is a kind of while measuring copper cobalt ferronickel content in zinc electrolyte |
| CN109781721B (en) * | 2019-03-15 | 2020-04-14 | 中南大学 | Test system optimization method for determining content of copper, cobalt and nickel and iron in zinc electrolyte |
| CN110361343A (en) * | 2019-08-20 | 2019-10-22 | 贵州大学 | A kind of heavy metal colorimetric detection method based on oligonucleotide regulation mangano-manganic oxide catalytic activity |
| CN110361343B (en) * | 2019-08-20 | 2022-03-22 | 贵州大学 | Heavy metal colorimetric detection method for regulating catalytic activity of mangano-manganic oxide based on oligonucleotide |
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Application publication date: 20091118 |