CN102721676A - Method for stably measuring arsenic and mercury in water by atomic fluorescence spectrometry - Google Patents
Method for stably measuring arsenic and mercury in water by atomic fluorescence spectrometry Download PDFInfo
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- CN102721676A CN102721676A CN2012102002271A CN201210200227A CN102721676A CN 102721676 A CN102721676 A CN 102721676A CN 2012102002271 A CN2012102002271 A CN 2012102002271A CN 201210200227 A CN201210200227 A CN 201210200227A CN 102721676 A CN102721676 A CN 102721676A
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Abstract
The invention belongs to the field of water environment monitoring methods, and particularly relates to a method for stably measuring arsenic and mercury in water by atomic fluorescence spectrometry. The method includes a), respectively preparing sample solution containing mercury and thiourea and sample solution containing arsenic and thiourea; b), mixing the sample solution containing the arsenic with potassium borohydride solution to generate arsine steam, and mixing the sample solution containing the mercury with stannous chloride solution to generate mercury steam; and c), guiding the arsine steam and the mercury steam into an atomizer by carrier gas, generating atomic fluorescence by an excitation effect of a special hollow cathode lamp which is a light source, and detecting the intensity of the atomic fluorescence. The content of the arsenic and the content of the mercury in the environmental water are measured by the atomic fluorescence spectrometry, operation is simple, convenient and speedy, labor, time and reagents are saved, and a measurement result is stable and reliable after the thiourea is additionally used in the method.
Description
Technical field
The invention belongs to monitoring water environment method field, be specifically related to the stable method of measuring arsenic and mercury in the water of a kind of atomic fluorescence spectrometry.
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; Cost plenty of time and manpower; Also consume more reagent, equipment, influence finding speed, and the mensuration result receives sample effect big; Stable inadequately, the method for the content of arsenic, mercury has outstanding realistic meaning in the therefore design mensuration water environment.
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; The arsenic in the ability fast measuring water sample and the content of mercury, easy and simple to handle quick, the tool saving of work and time is economized advantages such as reagent; Added thiocarbamide simultaneously, made measurement result reliable and stable.
Summary of the invention
The objective of the invention is to overcome the problems referred to above, provide arsenic and mercury content in a kind of AFS DETERMINATION Environmental Water, easy and simple to handle fast, saving of work and time economizes the stable method of measuring arsenic and mercury in the water of the reliable and stable atomic fluorescence spectrometry of reagent, measurement result.
For realizing above-mentioned purpose; The technical scheme that the present invention adopted is: the method for arsenic and mercury in the stable mensuration of the atomic fluorescence spectrometry water; It is characterized in that, comprise the steps: a) to prepare respectively mercurous with contain the arsenic sample solution, mercurous with contain the arsenic sample solution and contain thiocarbamide; B) mixing contains arsenic sample solution and solution of potassium borohydride generation arsenic hydride steam, mixes mercurous sample solution and stannous chloride solution and generates 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.
Aforesaid atomic fluorescence spectrometry is stable measures the method for arsenic and mercury in the water, and it is 5% that described thiocarbamide accounts for mass percent mercurous or that contain the arsenic sample solution.
The method of arsenic and mercury in the stable mensuration of the aforesaid atomic fluorescence spectrometry water, the concentration of described solution of potassium borohydride and stannous chloride solution 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 stable mensuration of the aforesaid atomic fluorescence spectrometry water, calculates the content of arsenic, mercury in the sample solution.
The method of arsenic and mercury in the stable mensuration of the aforesaid atomic fluorescence spectrometry 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 stannous chloride 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, easy and simple to handle fast, saving of work and time is economized reagent, has added thiocarbamide, makes measurement result reliable and stable.
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 stannous chloride 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 10gL
-1The potassium hydroxide solution dissolving also is settled to 100mL.
15gL
-1Stannous chloride solution: take by weighing the pure stannous chloride 1.5000g of top grade, use 10gL
-1Dissolving with hydrochloric acid also is settled to 100mL.
50gL
-1Thiourea solution: take by weighing top grade bright sulfur urea 5.000g, the water dissolving also is settled to 100mL (temperature can heat when low slightly).
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 800Lmin
-1(purity of argon is 99.999%), 200 ℃ of atomization temperatures, sampling volume 1.0mL, 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 standard serial solution
Stepwise dilution arsenic, mercury standard are used solution, and wherein standard solution is As1.000mgL
-1, Hg0.100mgL
-1, place 15min.It is 5% that thiocarbamide accounts for mass percent mercurous or that contain the arsenic sample solution, pours the sample solution of arsenic or mercury into the 25mL color comparison tube respectively, inserts automatic sampler, measures by two pass AFS condition of work.Wherein sample solution is meant and directly is used for the solution that the two pass AFS is measured.
2 results and discussion
2.1 working curve and detection limit
By test method arsenic, mercury 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
2.2 interference test
Having in the presence of the thiocarbamide that to eliminate interference, measuring arsenic 10.0 μ gL
-1, mercury 1.00 μ gL
-1And when requiring error at measurment in 5%, 10.0mgL
-1Ca
2+, Zn
2+, Mg
2+, Fe
2+, Mn
2+, Pb
2+, Cd and K, Na all do not have obvious interference.And in the environmental water sample these coexisting ion content far below this experimental amount.
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 5.0%.
2.4 the water sample analysis and the recovery
As stated above mineral water, surface water, underground water and landscape water are measured, and done the mark-on recovery test, test findings is seen table 1, and the sample recovery of standard addition is all between 96.8%～100.4%.
Table 1 sample analysis and recovery test result
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 (5)
1. the stable method of measuring arsenic and mercury in the water of atomic fluorescence spectrometry is characterized in that, comprise the steps: a) to prepare respectively mercurous with contain the arsenic sample solution, mercurous and contain the arsenic sample solution and contain thiocarbamide; B) mixing contains arsenic sample solution and solution of potassium borohydride generation arsenic hydride steam, mixes mercurous sample solution and stannous chloride solution and generates 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. atomic fluorescence spectrometry according to claim 1 is stable measures the method for arsenic and mercury in the water, it is characterized in that: it is 5% that described thiocarbamide accounts for mass percent mercurous or that contain the arsenic sample solution.
3. the method for arsenic and mercury in the stable mensuration of the atomic fluorescence spectrometry according to claim 1 water, it is characterized in that: the concentration of described solution of potassium borohydride and stannous chloride solution is 15gL
-1
4. the method for arsenic and mercury in the stable mensuration of the atomic fluorescence spectrometry according to claim 1 water 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.
5. the method for arsenic and mercury in the stable mensuration of the atomic fluorescence spectrometry according to claim 1 water, 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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Cited By (5)
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| CN102879372A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for determining arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry |
| CN103063641A (en) * | 2012-12-28 | 2013-04-24 | 张海珍 | Method for determining arsenic content of plants |
| CN107957412A (en) * | 2017-12-21 | 2018-04-24 | 酒泉钢铁(集团)有限责任公司 | A kind of heating board digestion of arsenic and mercury-atom fluorimetry method in soil |
| CN109425595A (en) * | 2017-08-24 | 2019-03-05 | 上海利元环保检测技术有限公司 | A kind of Mercury in Soil detection technique improved method |
| CN109781684A (en) * | 2019-01-23 | 2019-05-21 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of detection method of Mercury in Marine Sediment and arsenic |
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| CN103063641A (en) * | 2012-12-28 | 2013-04-24 | 张海珍 | Method for determining arsenic content of plants |
| CN109425595A (en) * | 2017-08-24 | 2019-03-05 | 上海利元环保检测技术有限公司 | A kind of Mercury in Soil detection technique improved method |
| CN107957412A (en) * | 2017-12-21 | 2018-04-24 | 酒泉钢铁(集团)有限责任公司 | A kind of heating board digestion of arsenic and mercury-atom fluorimetry method in soil |
| CN109781684A (en) * | 2019-01-23 | 2019-05-21 | 广东省测试分析研究所（中国广州分析测试中心） | A kind of detection method of Mercury in Marine Sediment and arsenic |
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Application publication date: 20121010 |