CN102706847A - Method for measuring arsenic and mercury in water by hydride generation-atomic fluorescence spectrometry - Google Patents
Method for measuring arsenic and mercury in water by hydride generation-atomic fluorescence spectrometry Download PDFInfo
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- CN102706847A CN102706847A CN2012101997761A CN201210199776A CN102706847A CN 102706847 A CN102706847 A CN 102706847A CN 2012101997761 A CN2012101997761 A CN 2012101997761A CN 201210199776 A CN201210199776 A CN 201210199776A CN 102706847 A CN102706847 A CN 102706847A
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Abstract
The invention belongs to the field of water environment monitoring methods, in particular to a method for measuring arsenic and mercury in water by hydride generation-atomic fluorescence spectrometry. The method comprises the following steps of: a) preparing a mixed sample solution which contains the arsenic and the mercury; b) generating arsine vapor and mercury vapor by using the mixed sample solution and a potassium borohydride solution; and c) introducing the arsine vapor and the mercury vapor into an atomizer by using a carrier gas, exciting the arsine vapor and the mercury vapor by using a special hollow cathode light source to generate atomic fluorescence, detecting the intensity of the atomic fluorescence, and calculating the content of the corresponding components in the sample solution by utilizing the direct proportion relationship of the fluorescence intensity with the content of the arsenic and the mercury in the solution. By using the method, the content of the arsenic and the mercury in environmental water can be measured at the same time; the method is operated simply and quickly; and labor, time and reagents are saved.
Description
Technical field
The invention belongs to monitoring water environment method field, be specifically related to the method that a kind of hydride generation atomic fluorescence spectrometry is measured arsenic and mercury in the water.
Background technology
Arsenic, mercury are the toxicologic index in the various water bodys, and the content to arsenic, mercury in all kinds of water quality standards of China has all carried out strict regulation.Arsenic in the Environmental Water and mercury be environmental monitoring require must survey project.The mensuration of arsenic was many in the past with atomic absorption spectrography (AAS), atomic fluorescence spectrometry and inductively coupled plasma emission spectrography.And the mensuration of mercury then is the atomic fluorescence spectrometry with stannous chloride or potassium borohydride reduction, and the dithizone photometry etc.The content of arsenic or mercury is generally separated measuring in the prior art Environmental Water, and cost plenty of time and manpower also consume more reagent, equipment, influence finding speed, therefore design the content of measuring arsenic in the water environment, mercury simultaneously and have outstanding realistic meaning.
Advantages such as hydride generation atomic fluorescence spectrometry is a kind of new trace analysis technology, and tool is highly sensitive, coexistence elements disturb less, method is simply quick.The invention provides two pass atom fluorescent luminosity method and measure arsenic and the assay method of mercury in the water body simultaneously; Can measure arsenic and the content of mercury in the water sample fast simultaneously; Realized that hydride generation atomic fluorescence spectrometry measures arsenic and mercury in the Environmental Water simultaneously; Make operation become more easy to be quick, the tool saving of work and time is economized advantages such as reagent.
Summary of the invention
The objective of the invention is to overcome the problems referred to above, provide a kind of realize hydride generation atomic fluorescence spectrometry measure simultaneously arsenic and mercury in the Environmental Water, easy and simple to handle fast, the saving of work and time hydride generation atomic fluorescence spectrometry of economizing reagent measures the method for arsenic and mercury in the water.
For realizing above-mentioned purpose, the technical scheme that the present invention adopted is: the method for arsenic and mercury in the hydride generation atomic fluorescence spectrometry mensuration water, it is characterized in that, and comprise the steps: that a) preparation is mercurous and contain arsenic recombined sample solution; B) recombined sample solution and solution of potassium borohydride generate arsenic hydride steam and mercury vapour; C) arsenic hydride and mercury vapour import atomizer by carrier gas, via exciting of extraordinary hollow cathode lamp source, produce atomic fluorescence, detect the intensity of atomic fluorescence.
The method of arsenic and mercury in the aforesaid hydride generation atomic fluorescence spectrometry mensuration water, the concentration of described solution of potassium borohydride is 15gL
-1
The method of arsenic and mercury is utilized the proportional relation that arsenic, mercury content were in fluorescence intensity and the solution in the aforesaid hydride generation atomic fluorescence spectrometry mensuration water, calculates the content of arsenic, mercury in the sample solution.
The method of arsenic and mercury in the aforesaid hydride generation atomic fluorescence spectrometry mensuration water, in the described sample solution, the content range of mercury is 0.05～5.00 μ gL
-1, the content range of arsenic is 0.50 ~ 50.0 μ gL
-1
Arsenic in the sample solution and potassium borohydride are reflected at and generate arsenic hydride in the hydride generating system; Mercury and potassium borohydride reaction generate the atomic state mercury vapour; Arsenic hydride and mercury vapour are directly imported in the quartz atomizer by carrier gas (argon gas), so in argon-hydrogen flame atomization.Ground state atom receives exciting of extraordinary hollow cathode lamp source, produces atomic fluorescence, through detecting the intensity of atomic fluorescence, utilizes the proportional relation of arsenic, mercury content in fluorescence intensity and the solution, calculates the content of corresponding composition in the sample solution.This method can be measured the content of arsenic and mercury in the Environmental Water simultaneously, easy and simple to handle fast, saving of work and time is economized reagent.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is done further explain.
1.1 principle
Environmental Water sample (underground water and the surface water that refer to cleaning especially), arsenic in the sample solution and potassium borohydride are reflected at and generate arsenic hydride in the hydride generating system, and mercury and potassium borohydride reaction generate the atomic state mercury vapour.
Arsenic hydride and mercury vapour are directly imported in the quartz atomizer by carrier gas (argon gas), so in argon-hydrogen flame atomization.Ground state atom receives exciting of extraordinary hollow cathode lamp source, produces atomic fluorescence, through detecting the intensity of atomic fluorescence, utilizes the proportional relation of arsenic, mercury content in fluorescence intensity and the solution, calculates the content of corresponding composition in the sample solution.
1.2 instrument and reagent
AFS-830 type two pass AFS, arsenic, the mercury extraordinary atomic spectrum lamp of encoding.
Arsenic, mercury standard inventory solution: 1.000gL
-1Stepwise dilution becomes arsenic, mercury standard to mix use solution, As1.000mgL
-1, Hg0.100mgL
-1Can dilute according to demand and to be variable concentrations solution.
15gL
-1Solution of potassium borohydride: take by weighing the pure potassium borohydride 1.5000g of top grade, use 10 gL
-1The potassium hydroxide solution dissolving also is settled to 100mL.
Above reagent is all existing with join at present, and test water is a secondary deionized water.
1.3 instrument condition of work
Lamp current arsenic is 60mA, and mercury is 30mA; All the other conditions are all identical, and the photomultiplier negative high voltage is 270V, and the atomizer height is 8mm, and argon gas is carrier gas, and flow is 400mLmin
-1, the shield gas flow amount is 800 Lmin
-1(purity of argon is 99.999%), 200 ℃ of atomization temperatures, sampling volume 1.0 mL, the reading mode peak area, time delay 1s, reading duration 12s.
1.4 test method
1.4.1 water sample is handled
The underground water and the surface water of cleaning, direct sample is measured.
1.4.2 the preparation of hybrid standard series solution
Stepwise dilution arsenic, mercury standard are mixed use solution, and wherein standard solution is As1.000mgL
-1, Hg0.100mgL
-1, place 15min, pour the dilution of arsenic and mercury into the 25mL color comparison tube respectively, insert automatic sampler, measure by two pass AFS condition of work.
2 results and discussion
2.1 solution of potassium borohydride concentration is selected
Borane reducing agent hydrofining solution concentration is more obvious to the influence of the mensuration of arsenic and mercury, and potassium borohydride concentration is too high, and it is too much to produce amounts of hydrogen during reaction, and transmission solution is diluted and cause sensitivity to reduce; If potassium borohydride concentration is too low, reducing power weakens, and sensitivity reduces equally.Experiment selected 15gL
-1Solution of potassium borohydride, the result who measures in the time of to arsenic, mercury is all satisfied.
2.2 working curve and detection limit
By test method arsenic, mercury standard solution are measured working curve and solution concentration optimum range, arsenic, mercury are respectively 0.50 ~ 50.0 μ gL
-1With 0.05～5.00 μ gL
-1Linear in the scope with its fluorescence intensity, equation of linear regression I
As=28.9C (μ gL
-1)+5.12, I
Hg=59.8C (μ gL
-1)+0.061.Related coefficient C is all greater than 0.9990.Reagent blank is METHOD FOR CONTINUOUS DETERMINATION 11 times then, and with the detection limit (3S) of 3 times of standard deviation computing method, arsenic is 0.045 μ gL
-1, mercury 0.011 μ gL
-1
2.3 precision
Arsenic, mercury in every kind of water sample are distinguished METHOD FOR CONTINUOUS DETERMINATION 6 times, and gained relative standard deviation RSD is all less than 6.0%.
The foregoing description does not limit the present invention in any form, and all employings are equal to the technical scheme that mode obtained of replacement or equivalent transformation, all drop in protection scope of the present invention.
Claims (4)
1. the method for arsenic and mercury in the hydride generation atomic fluorescence spectrometry mensuration water is characterized in that, comprises the steps: that a) preparation is mercurous and contains arsenic recombined sample solution; B) recombined sample solution and solution of potassium borohydride generate arsenic hydride steam and mercury vapour; C) arsenic hydride and mercury vapour import atomizer by carrier gas, via exciting of extraordinary hollow cathode lamp source, produce atomic fluorescence, detect the intensity of atomic fluorescence.
2. the method for arsenic and mercury in the hydride generation atomic fluorescence spectrometry mensuration water according to claim 1, it is characterized in that: the concentration of described solution of potassium borohydride is 15gL
-1
3. the method for arsenic and mercury is characterized in that: utilize the proportional relation that arsenic, mercury content were in fluorescence intensity and the solution, calculate the content of arsenic, mercury in the sample solution in the hydride generation atomic fluorescence spectrometry mensuration water according to claim 1.
4. the method for arsenic and mercury in the hydride generation atomic fluorescence spectrometry mensuration water according to claim 1, it is characterized in that: in the described sample solution, the content range of mercury is 0.05～5.00 μ gL
-1, the content range of arsenic is 0.50 ~ 50.0 μ gL
-1
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| CN108844927A (en) * | 2018-04-20 | 2018-11-20 | 中国地质大学（武汉） | A kind of sample introduction system and its Atomic Fluorescence Spectrometer |
| CN111103270A (en) * | 2018-10-29 | 2020-05-05 | 谱焰实业(上海)有限公司 | Method for synchronously measuring mercury and arsenic by using atomic fluorescence analysis with water as carrier |
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Application publication date: 20121003 |