CN101482506A - Mercury content measuring method and measuring device - Google Patents
Mercury content measuring method and measuring device Download PDFInfo
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- CN101482506A CN101482506A CNA2008100194618A CN200810019461A CN101482506A CN 101482506 A CN101482506 A CN 101482506A CN A2008100194618 A CNA2008100194618 A CN A2008100194618A CN 200810019461 A CN200810019461 A CN 200810019461A CN 101482506 A CN101482506 A CN 101482506A
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Abstract
The invention discloses a mercury content measuring method and a measuring device, wherein the measuring method comprises the steps of firstly using a reference blank colorimetric tube and a calibration measuring colorimetric tube to respectively carry out blank calibration and certain range value calibration on mercury-free air and standard mercury substances through ultraviolet light transmission, photoelectric converter conversion and circuit processing, then circulating an actually measured sample in the calibration measuring colorimetric tube after processing, and directly measuring the mercury content through conversion according to the calibration curve after the same operation; the two color comparison tubes in the measuring device are optical glass tubes with the same size, the two photoelectric converters are matched and screened, the parameters are the same, the related lenses are perpendicular to the axes of the color comparison tubes, and the calibration measuring color comparison tubes are detachably cleaned. The method is used for measuring the content of the toxic and harmful substance mercury in daily production and living environments, and has the advantages of simple and convenient operation, low investment cost, good measurement effect, high reliability and wide application range.
Description
Technical field
The present invention relates to a kind of is being used for detecting and producing or the measuring method and the measurement mechanism of the mercury content of living environment of principle development with the colourimetry.
Background technology
In the environment of our daily production or life, many poisonous and hazardous materials are arranged, wherein, mercury (Hg) and compound thereof belong to extremely toxic substance, can accumulate in vivo.Mercury is quiet to the harm of health, and the destruction result of generation is extremely serious, even the life security that is threatening people.Therefore, the mercury content that quick and precisely detects in production and the living environment is particularly important.
Cold-vapour atomic absorption method, Cold Atomic Fluorescent Mercury method are to measure the peculiar method of trace, Trace Hg in the water, and disturbing factor is few, and sensitivity is higher.The dithizone spectrophotometric method is to measure the universal method of multiple metallic ion, if can shelter interfering ion and the strict reaction conditions of grasping, and also can obtain satisfied result.During sampling, every collection 1L water sample should add 10mL sulfuric acid or 7mL nitric acid immediately, makes water sample pH value be less than or equal to 1, if can not measure immediately after the sampling, in every liter of sample, add 5% (m/V) liquor potassic permanganate 4mL, add in case of necessity, make it be lasting pale red.Sample is stored in the Pyrex bottle.All there are the requirement for experiment condition harshness in above method and used measurement mechanism, and experimental cost is uneconomical, operate cumbersomely, and the staff is required high defective.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of easy and simple to handle, input cost is few, measurement effect is good, the mercury content measuring method of applied range, and be provided for the measurement mechanism of this method.
Measuring method of the present invention is according to a conventional method the mercury ion in the sample to be reduced to mercury simple substance earlier, formation contains mercuryvapour, utilizing the ultraviolet light of wavelength 253.7nm will contain mercuryvapour again excites and produces resonance fluorescence, this fluorescence intensity is converted to electric signal by photoelectric commutator, measure the size of this electric signal and compare with calibration curve in advance and can calculate out mercury content in the test substance, specific operation process is as follows:
(1) the blank demarcation
Starter gear self-loopa sampling pump, to in the calibration measurements color comparison tube, circulate through the fresh air that no mercury deionized water filters, be full of inert gas in the blank color comparison tube of reference, the ultraviolet light that is taken place by the ultraviolet source generator sees through the blank color comparison tube of calibration measurements color comparison tube and reference simultaneously, and simultaneously convert electric signal to and be transported to processing of circuit through photoelectric commutator, as two signal unanimities, the display displayed value is zero on the device panel, as inconsistent, regulator potentiometer then, making the display displayed value is zero, finishes blank zeroing;
(2) certain range value is demarcated
Size according to the actual sample pump content of estimating, choose the slightly high known standard mercury material of mercury content, same by the self-loopa sampling pump, standard mercury material is circulated in the calibration measurements color comparison tube, produce resonance fluorescence by ultraviolet excitation, this fluorescence intensity is directly proportional with mercury concentration, the electric signal of being exported by the photoelectric commutator of this end of calibration measurements color comparison tube has just had obvious difference with the electric signal that the photoelectric commutator of blank this end of color comparison tube of reference is exported like this, regulator potentiometer makes the peak value of display demonstration identical with the known mercury content of standard mercury material again;
(3) detergent line
In general, measure the next mercury content for the treatment of test sample,, should carry out pipeline and clean if be lower than the content of previous sample, otherwise, then not detergent line;
(4) real standard specimen product are measured
After real standard specimen product processing, circulate in the calibration measurements color comparison tube by the self-loopa sampling pump, press above method by the photoelectric commutator output signal, according to the conversion by the calibration curve between determined null value of above-mentioned demarcation mode and a certain peak value, the displayed value of display is the mercury content value of real standard specimen product.
The measurement mechanism that is used for above-mentioned measuring method is: blank color comparison tube of reference and calibration measurements color comparison tube that coaxial cable is installed on the strip base plate, be provided with the ultraviolet source generator between the relative end of two kinds of color comparison tubes, the other end is respectively equipped with the identical photoelectric commutator of parameter, the reception minute surface of the convex lens of the both sides of described ultraviolet source generator and photoelectric commutator is all perpendicular to the axis of color comparison tube, two kinds of optical glass pipes that color comparison tube is a consistent size, its two ends are sealed by the optical glass plano lens respectively, wherein be full of inert gas in the blank color comparison tube of reference, import and outlet are arranged on the calibration measurements color comparison tube.
The optical glass plano lens at described calibration measurements color comparison tube two ends is compressed by end cap, but becomes the sealing construct for handling.
Adopt measuring method provided by the invention and measurement mechanism, as long as circulate with sending into after the sample preparation in the calibration measurements color comparison tube, conversion by photosignal is measured and the calculation of specific calibration curve in advance, can directly read mercury content in the sample, easy and simple to handle, do not need harsh experiment condition, do not need special instrument and reagent, input cost is few; The structure energy strict guarantee Photoelectric Detection performance of used measurement mechanism, particularly two photoelectric commutators are through strictness pairing screening, and parameter is identical, has improved measurement effect; End cap is established at calibration measurements color comparison tube two ends, is convenient to disassembly, cleaning, guarantees to measure reliability.The present invention can be used for the measurement of mercury content in the poisonous and harmful substance in daily production and the living environment, applied range.
Description of drawings
Accompanying drawing is measurement mechanism structural representation among the present invention.
Embodiment
Further specify embodiments of the invention in conjunction with the accompanying drawings.Measuring process is as follows:
(1) the blank demarcation
Starter gear self-loopa sampling pump, to in calibration measurements color comparison tube 4, circulate through the fresh air that no mercury deionized water filters, be full of the inert gas helium in the blank color comparison tube 2 of reference, the ultraviolet light that is sent by ultraviolet source generator 3 is tranmittance colour tube 2 and 4 simultaneously, and simultaneously convert electric signal to and be transported to processing of circuit through the identical photoelectric commutator 1 and 10 of parameter, as two signal unanimities, the display displayed value is zero on the device panel, as inconsistent, regulator potentiometer then, making the display displayed value is zero, finishes blank zeroing;
(2) certain range value is demarcated
Size according to the actual sample mercury content of estimating, choose the slightly high known standard mercury material of mercury content, by the self-loopa sampling pump, it is circulated in calibration measurements color comparison tube 4, produce resonance fluorescence through ultraviolet excitation, like this, obvious difference is arranged through the transmission of color comparison tube 2 and 4 and the electric signal of exporting by the conversion of photoelectric commutator 1 and 10, regulator potentiometer makes the peak value of display demonstration identical with the known mercury content of standard mercury material again;
(3) detergent line
After more than demarcation is finished, carry out the measurement that first treats test sample, answer detergent line, when cleaning the calibration measurements color comparison tube, unload color comparison tube 4 from base plate 6, pull out the flexible pipe on the import and export, pull down the end cap 7 and the plano lens at two ends, carrying out conventional method cleans, when the measurement next one is treated test sample,, answer detergent line if its mercury content is lower than the content of previous sample, otherwise, then not detergent line;
(4) real standard specimen product are measured
Actual sample is handled routinely, formation contains mercuryvapour, circulate in the calibration measurements color comparison tube by the self-loopa sampling pump, press above method by the photoelectric commutator output signal, according to the conversion by the determined calibration curve of above-mentioned demarcation mode, the displayed value of display is the mercury content value of actual sample.
The blank color comparison tube 2 of the reference of used measurement mechanism, calibration measurements color comparison tube 4 coaxial cables are installed on the strip base plate 6 in more than measuring, be provided with ultraviolet source generator 3 between the two color comparison tube opposite ends, the two color comparison tube other ends are respectively equipped with through pairing screening, photoelectric commutator 1 and 10 that parameter is identical, the convex lens of ultraviolet source generator both sides and two photoelectric commutators accept minute surface all perpendicular to the color comparison tube axis.Two color comparison tubes are the optical glass pipe of consistent size, wherein the blank color comparison tube of reference 2 two ends are shut by the optical glass plano lens, be full of the inert gas helium in the pipe, the optical glass plano lens at calibration measurements color comparison tube 4 two ends is compressed by end cap 7 and joint 5, but become the sealing construct for handling, import 8, outlet 9 are arranged on the pipe.
Claims (3)
1, a kind of mercury content measuring method, mercury ion in the sample is reduced to simple substance mercury, formation contains mercuryvapour, it is characterized in that utilizing wavelength to excite and produce resonance fluorescence for the ultraviolet light of 253.7nm will contain mercuryvapour, this fluorescence intensity is converted to electric signal by photoelectric commutator, measure the size of this electric signal and compare with calibration curve in advance and can calculate out mercury content in the test substance, specific operation process is as follows:
(1) the blank demarcation
Starter gear self-loopa sampling pump, to in the calibration measurements color comparison tube, circulate through the fresh air that no mercury deionized water filters, be full of inert gas in the blank color comparison tube of reference, the ultraviolet light that is taken place by the ultraviolet source generator sees through the blank color comparison tube of calibration measurements color comparison tube and reference simultaneously, and simultaneously convert electric signal to and be transported to processing of circuit through photoelectric commutator, as two signal unanimities, the display displayed value is zero on the device panel, as inconsistent, regulator potentiometer then, making the display displayed value is zero, finishes blank zeroing;
(2) certain range value is demarcated
Size according to the actual sample mercury content of estimating, choose the slightly high known standard mercury material of mercury content, same by the self-loopa sampling pump, standard mercury material is circulated in the calibration measurements color comparison tube, produce resonance fluorescence by ultraviolet excitation, this fluorescence intensity is directly proportional with mercury concentration, the electric signal of being exported by the photoelectric commutator of this end of calibration measurements color comparison tube has just had obvious difference with the electric signal that the photoelectric commutator of blank this end of color comparison tube of reference is exported like this, regulator potentiometer makes the peak value of display demonstration identical with the known mercury content of standard mercury material again;
(3) detergent line
In general, measure the next mercury content for the treatment of test sample,, should carry out pipeline and clean if be lower than the content of previous sample, otherwise, then not detergent line;
(4) real standard specimen product are measured
After real standard specimen product processing, circulate in the calibration measurements color comparison tube by the self-loopa sampling pump, press above method by the photoelectric commutator output signal, according to the conversion by the calibration curve between determined null value of above-mentioned demarcation mode and a certain peak value, the displayed value of display is the mercury content value of real standard specimen product.
2, a kind of mercury content measurement mechanism that is used for the described measuring method of claim 1, it is characterized in that on the strip base plate, installing the blank color comparison tube of reference and the calibration measurements color comparison tube of coaxial cable, be provided with the ultraviolet source generator between the relative end of two kinds of color comparison tubes, the other end is respectively equipped with the identical photoelectric commutator of parameter, the reception minute surface of the convex lens of the both sides of described ultraviolet source generator and photoelectric commutator is all perpendicular to the axis of color comparison tube, two kinds of optical glass pipes that color comparison tube is a consistent size, its two ends are sealed by the optical glass plano lens respectively, wherein be full of inert gas in the blank color comparison tube of reference, import and outlet are arranged on the calibration measurements color comparison tube.
3, by the described mercury content measurement mechanism of claim 2, it is characterized in that the optical glass plano lens at described calibration measurements color comparison tube two ends is compressed by end cap, but become the sealing construct for handling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100194618A CN101482506B (en) | 2008-01-10 | 2008-01-10 | Mercury content measuring method and device |
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| CN2008100194618A CN101482506B (en) | 2008-01-10 | 2008-01-10 | Mercury content measuring method and device |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253168A (en) * | 2011-04-21 | 2011-11-23 | 上海理工大学 | Method and apparatus for producing mercury vapor with standard concentration |
| CN102435549A (en) * | 2011-09-16 | 2012-05-02 | 北京雪迪龙科技股份有限公司 | Flue gas mercury analyzer |
| CN102621082A (en) * | 2012-03-07 | 2012-08-01 | 中国科学院安徽光学精密机械研究所 | Constant-magnetic-field transverse Zeeman effect atmospheric mercury detection method |
| CN102998268A (en) * | 2012-11-22 | 2013-03-27 | 中科天融(北京)科技有限公司 | A flue gas mercury online monitoring instrument |
| RU2493553C1 (en) * | 2011-01-27 | 2013-09-20 | Зик Аг | Gas analyser to measure mercury content in gas |
| CN104819971A (en) * | 2015-05-21 | 2015-08-05 | 山东格林检测股份有限公司 | Detection method for mercury in water |
| CN113155812A (en) * | 2021-03-13 | 2021-07-23 | 竑迈环境科技(上海)有限公司 | Mercury detection and analysis device |
| CN115931808A (en) * | 2023-02-09 | 2023-04-07 | 北京鹏宇昌亚环保科技有限公司 | Totally-enclosed light path device of mercury detector |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6690462B2 (en) * | 2001-12-05 | 2004-02-10 | The United States Of America As Represented By The Secretary Of The Navy | Calibration scheme for continuous monitoring of mercury emissions from stationary sources by plasma emission spectrometry |
| CN2599579Y (en) * | 2003-01-21 | 2004-01-14 | 南开大学 | On-line interface for capillary electrophoresis hydride generation atomic fluorescence spectrometry |
| CN100529739C (en) * | 2005-07-22 | 2009-08-19 | 四川大学 | Method for measuring trace amount hydrargyrum in alcoholic and acetic sample by photo-induced cold steam generation |
| CN201000434Y (en) * | 2007-01-12 | 2008-01-02 | 北京瑞利分析仪器公司 | Ultra trace mercury measuring apparatus in water sample for atomic fluorescence optical spectrometer |
| CN100543461C (en) * | 2007-05-31 | 2009-09-23 | 中国铝业股份有限公司 | The assay method of Trace Mercury in a kind of aluminium ingot |
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2008
- 2008-01-10 CN CN2008100194618A patent/CN101482506B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2493553C1 (en) * | 2011-01-27 | 2013-09-20 | Зик Аг | Gas analyser to measure mercury content in gas |
| CN102253168A (en) * | 2011-04-21 | 2011-11-23 | 上海理工大学 | Method and apparatus for producing mercury vapor with standard concentration |
| CN102253168B (en) * | 2011-04-21 | 2014-01-22 | 上海理工大学 | Method and apparatus for producing mercury vapor with standard concentration |
| CN102435549A (en) * | 2011-09-16 | 2012-05-02 | 北京雪迪龙科技股份有限公司 | Flue gas mercury analyzer |
| CN102621082A (en) * | 2012-03-07 | 2012-08-01 | 中国科学院安徽光学精密机械研究所 | Constant-magnetic-field transverse Zeeman effect atmospheric mercury detection method |
| CN102998268A (en) * | 2012-11-22 | 2013-03-27 | 中科天融(北京)科技有限公司 | A flue gas mercury online monitoring instrument |
| CN104819971A (en) * | 2015-05-21 | 2015-08-05 | 山东格林检测股份有限公司 | Detection method for mercury in water |
| CN113155812A (en) * | 2021-03-13 | 2021-07-23 | 竑迈环境科技(上海)有限公司 | Mercury detection and analysis device |
| CN115931808A (en) * | 2023-02-09 | 2023-04-07 | 北京鹏宇昌亚环保科技有限公司 | Totally-enclosed light path device of mercury detector |
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| CN101482506B (en) | 2012-03-28 |
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Granted publication date: 20120328 Termination date: 20180110 |