CN101482506B - Mercury content measuring method and device - Google Patents
Mercury content measuring method and device Download PDFInfo
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- CN101482506B CN101482506B CN2008100194618A CN200810019461A CN101482506B CN 101482506 B CN101482506 B CN 101482506B CN 2008100194618 A CN2008100194618 A CN 2008100194618A CN 200810019461 A CN200810019461 A CN 200810019461A CN 101482506 B CN101482506 B CN 101482506B
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Abstract
The invention discloses a mercury content measurement method and device, wherein the measurement method comprises: respectively performing the blank calibration and a some range calibration of the no-mercury air and standard mercury material subjected to ultraviolet light transmission, optical-electrical converter change-over and circuit treatment using a reference blank color comparison tube and a calibration measurement color comparison tube; processing the actual-measurement sampler and circulating the sampler in the calibration measurement color comparison tube, and directly measuring the mercury content based on the said calibration curve. The two color comparison tubes are the optical glass tubes of the same size and the two optical-electrical converters are matched and screened with the same parameters, each relative lens is perpendicular to the color-tube axle and the calibration measurement color comparison tube can be dismounted and cleaned. The mercury content measurement method and device can be used for measuring the content of the poisonous and harmful substance mercury in day-to-day production and living environment with features of simple operation, less input 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 AAS is a universal method of measuring 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.Above method and used measurement mechanism all exist requirement for experiment condition harsh, and experimental cost is uneconomical, operate cumbersomely, and the staff is required high defective.
Summary of the invention
The technical matters that the present invention will solve 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 by 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; Convert this fluorescence intensity into 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 following:
(1) the blank demarcation
Starter gear self-loopa sampling pump, the fresh air that will pass through no mercury deionized water filtration circulates in the calibration measurements color comparison tube, is 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 through photoelectric commutator and be transported to processing of circuit, consistent like two signals, the display displayed value is zero on the device panel; As inconsistent; Regulator potentiometer then, making the display displayed value is zero, accomplishes blank zeroing;
(2) certain range value is demarcated
Size based on the actual sample pump content of estimating; Choose the slightly high known standard mercury material of mercury content; Through the self-loopa sampling pump, standard mercury material is circulated in the calibration measurements colorimetric cylinder equally, produce resonance fluorescence by ultraviolet excitation; This fluorescence intensity is directly proportional with mercury concentration; The signal of telecommunication of being exported by the optical-electrical converter of this end of calibration measurements colorimetric cylinder has just had obvious difference with the signal of telecommunication that the optical-electrical converter of blank this end of colorimetric cylinder of reference is exported like this, and regulator potentiometer makes the peak value of display demonstration identical with the known mercury content of standard mercury material again;
(3) detergent line
Generally speaking, measure the next mercury content of treating 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 article are measured
After real standard specimen article processing; Circulate in the calibration measurements color comparison tube through the self-loopa sampling pump; Export signal by above method by photoelectric commutator; 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 article.
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 said 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, and 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 said 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, measure and the calculation of specific calibration curve in advance through the conversion of photosignal, 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 ability 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 reliable measurement property.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 accompanying drawing.Measuring process is following:
(1) the blank demarcation
Starter gear self-loopa sampling pump, the fresh air that will pass through no mercury deionized water filtration circulates in calibration measurements color comparison tube 4, is 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 through the identical photoelectric commutator 1 and 10 of parameter and be transported to processing of circuit, consistent like two signals, the display displayed value is zero on the device panel; As inconsistent; Regulator potentiometer then, making the display displayed value is zero, accomplishes blank zeroing;
(2) certain range value is demarcated
Based on the size of the actual sample mercury content of estimating, choose the slightly high known standard mercury material of mercury content, through the self-loopa sampling pump; It is circulated in calibration measurements colorimetric cylinder 4; Produce resonance fluorescence through ultraviolet excitation, like this, obvious difference is arranged through the transmission of colorimetric cylinder 2 and 4 and the signal of telecommunication of exporting by the conversion of optical-electrical converter 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 demarcating completion, 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; Carry out conventional method and clean, when the measurement next one is treated test sample, if its mercury content is lower than the content of previous sample; Answer detergent line, otherwise, then not detergent line;
(4) real standard specimen article are measured
Actual sample is pressed conventional processing; Formation contains mercuryvapour; Circulate in the calibration measurements color comparison tube through the self-loopa sampling pump; Export signal by above method by photoelectric commutator, 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 becomes the sealing construct for handling, and import 8, outlet 9 are arranged on the pipe.
Claims (3)
1. 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, converts this fluorescence intensity into 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 following:
(1) the blank demarcation
Starter gear self-loopa sampling pump, the fresh air that will pass through no mercury deionized water filtration circulates in the calibration measurements color comparison tube, is 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 through photoelectric commutator and be transported to processing of circuit, consistent like two signals, the display displayed value is zero on the device panel; As inconsistent; Regulator potentiometer then, making the display displayed value is zero, accomplishes blank zeroing;
(2) certain range value is demarcated
Numerical range according to the actual sample mercury content; Choose a kind of known slightly high standard mercury material of mercury content; Through the self-loopa sampling pump, standard mercury material is circulated in the calibration measurements color comparison tube equally, 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 so just had obvious difference with the electric signal that the photoelectric commutator of blank this end of color comparison tube of reference is exported, and regulator potentiometer makes the peak value of display demonstration identical with the known mercury content of standard mercury material again;
(3) detergent line
Measure the next mercury content of treating 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 article are measured
After real standard specimen article processing; Circulate in the calibration measurements color comparison tube through the self-loopa sampling pump; Export signal by above method by photoelectric commutator; 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 article.
2. mercury content measurement mechanism that is used for the said 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, and the reception minute surface of the convex lens of the both sides of said 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 are full of inert gas in the blank color comparison tube of reference, and 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 said calibration measurements color comparison tube two ends is compressed by end cap, but become the sealing construct for handling.
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CN2008100194618A CN101482506B (en) | 2008-01-10 | 2008-01-10 | Mercury content measuring method and device |
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CN101482506B true CN101482506B (en) | 2012-03-28 |
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EP2482057B1 (en) * | 2011-01-27 | 2013-03-20 | Sick Ag | Gas analyser for measuring the mercury content of a gas and calibration method |
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 | Smoke mercury online monitoring instrument |
CN104819971B (en) * | 2015-05-21 | 2018-05-18 | 山东格林检测股份有限公司 | The detection method of mercury in a kind of 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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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 |
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