CN107271436A - A kind of preparation of quick detection agent for determining Determination of Trace Mercury In Water and application method - Google Patents
A kind of preparation of quick detection agent for determining Determination of Trace Mercury In Water and application method Download PDFInfo
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- CN107271436A CN107271436A CN201710411459.4A CN201710411459A CN107271436A CN 107271436 A CN107271436 A CN 107271436A CN 201710411459 A CN201710411459 A CN 201710411459A CN 107271436 A CN107271436 A CN 107271436A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
Abstract
The present invention relates to a kind of preparation of quick detection agent for determining Determination of Trace Mercury In Water and application method, the detection agent is made up of mercury detection agent I, mercury detection agent II and mercury detection agent III, and leading to X 100 etc. by cadion, stannous sulfate, sulfamic acid, Potassiumiodate, borax, Qula respectively is formulated.First pre-processed with multifunctional sample processing instrument and mercury detection agent I and II pair of water sample Trace Hg air lift, mercury detection agent III is then directly added into absorbing liquid after the pre-treatment and carries out chromogenic reaction, you can colorimeter or spectrophotometer measurement is utilized.Detecting instrument used in the present invention is simple, light, easy to operate, mercury detection pulvis steady quality, can preserve for a long time, and transport, it is easy to carry.Method detection limit of Hg 0.002mg/L, detection whole process was particularly suitable for surface water, the field of Industry Waste Determination of Trace Mercury In Water and field quick detection less than 20 minutes.
Description
Technical field
The present invention relates to a kind of preparation of quick detection agent for determining Determination of Trace Mercury In Water and application method, belong to environmental monitoring
Technical field.
Background technology
Mercury and its derivative organic mercury are the important poisonous and harmful environmental contaminants of a class, with persistence, easy migration,
The characteristic such as high bioconcentration and high bio-toxicity, can for a long time exist, and can migrate at a distance in air and food chain.It is
Global contaminant is classified as by United Nations Environment Programme, is that a kind of unique produced on global range influences in addition to greenhouse gases
Chemical substance, it has also become one of environmental contaminants of global extensive concern.Mercury is to the brain of human body, nerve, kidney and liver
Cause damage, or even stupor can be caused and dead.The discharge of mercury comes from two parts of natural source and artificial source, and discharge is related to neck
Domain is coal-burning power plant, coal-burning boiler, non-ferrous metal metallurgy, manufacture of cement, mercurous product etc..The Japan that 1950s occurs
Michigan, USA and Northeast China Song Hua River and Hebei province Ji canal basin that minamata disease and 1970s occur
The mercury pollution of generation is all because of pernicious Environment Pollution Event caused by the improper discharge of mercury, therefore the control of industrial mercury pollution
And monitor most important for whole world control mercury action.
At present, the conventional detection method of mercury mainly has cold-vapour atomic absorption method, Pressurized sample digestion, inductively coupled plasma
(ICP) method, atomic absorption spectrography (AAS), AAS etc..Zheng Aiting etc. develops the detecting system of mercury in water, fluorescence detector
It is connected with reactor, detects mercury vapor content, automaticity is high, but system and device complexity huge (Zheng Aiting, Li Yanli, pleasure
Literary will etc., a kind of system and method for being used to determine mercury concentration in water, Guangdong：CN103499558A, 2014).Zhao Changping is used
Hydride generation atomic fluorescence spectrometry is combined solution of potassium borohydride-mercury vapour generating means with atomic fluorescence spectrometry, behaviour
Make relative ease (Zhao Changping, hydride generation atomic fluorescence spectrometry determine water in mercury and mercury method, CN102706847A,
2012).Ma Zhongbin etc. produces mercury vapour using stannous chloride as reducing agent, enters under the condition determination of the fluorescence mercury vapourmeter of setting
Mercury in the water that row is determined, method sensitivity is higher, and test limit reaches 0.004mg/L, analyze speed is fast, stability it is good (Ma Zhongbin,
The detection method of mercury, CN104819971A, 2015 in Liu Yanni, bang English, a kind of water).Above-mentioned detection method is required for costliness
Detecting instrument, it is cumbersome, have higher requirement to the professional skill of operating personnel, can only be carried out in laboratory.It is double
Sulphur hydrazone development process is the National Standard Method for determining Trace Mercury in water, studies and is most widely used in the chromogenic assay of mercury.Chloroform,
In carbon tetrachloride or benzole soln, mercury and dithizone reaction generation yellow complex salt by organic extractant phase so as to determine mercury, but operate step
Rapid cumbersome, selectivity and sensitivity is not high, and organic solvent is harmful.Paraffin phase spectrophotometry is by separation, enrichment
It is combined together with chromogenic assay, with Solid-phase Photometry sensitivity height, good selective.Li Manxiu etc. establishes double sulphur
Method (Li Manxiu, Lv Yanhua, metallurgical analysis, 2006, (5) of mercury in hydrazone-Paraffin Phase Spectrophotometric Determination sewage：87-88),
Mercury-dithizone complex compound can be by paraffin quantified extract in ammoniacal liquor-ammonium chloride medium, and mercury meets more fixed than ear in 0-20 μ g ranges
Rule, the μ g/mL of detection limit 0.0017, lead, bismuth, zinc ion must extract removing in advance.Sun Xuhui etc. is using triton x-100 as solubilizer
Establish Trace Hg in aqueous phase dithizone directly determine photometry (Sun Xuhui, Ma Jun, Li little Hua etc., Treatment of Industrial Water,
2008, (12)：73-76), molar absorption coefficient is 4.7 × 104L·mol-1·cm-1, 5~60 μ g/L mercury meet law of Beer,
This method preci-sion and accuracy has comparativity with National Standard Method.Flood all etc. have studied cadion and cadion 2B colour developing light splitting
Photometry detection mercury (flood all, Wu Shuisheng, environmental science, 1981, (3)：20-24), with arsenic acid in the presence of triton x-100
Salt shelters the interfering ions such as zinc, cadmium, and molar absorption coefficient is 1.20 × 105L·mol-1·cm-1, available for directly measure industry
Mercury in Wastewater.Zhu Youyu etc. have studied in borax-hydrochloride buffer medium, in the presence of anion surfactant, with 5-Br-
PADAP detects method (Zhu Youyu, Li Shunyong, Hangzhou University's journal-natural science edition, 1988, (1) of mercury as developer：
74-80), apparent molar absorption coefficient 1.12 × 105L·mol-1·cm-1, range of linearity 0-3 5 μ g/25ml are easy to operate, are
Determine one of mercury photometry in higher sensitivity.Electrochemical process is also widely used in mercury detection, and analogy roc is using on dithizone
The characteristic of sulfydryl and azo group and heavy metal ion formation chelate, by modified glassy carbon electrode, have studied Anodic stripping survey
Determine Trace Hg method (analogy roc, the research for detecting heavy metal ion electrochemical sensor, Central South University's Master's thesis,
2011), range of linearity 2.0-20.0 μ g/L, the μ g/L of minimal detectable concentration 2.0.Pay quiet based on Differential Pulse Anodic Stripping Voltammetry
Selection gold electrode measure mercury (pair quiet, the research of the electrochemical sensor of water environment heavy metal analysis, Zhejiang University's Master's thesis,
2007) micro- spun gold electrode, is prepared for, the measure of mercury can be realized using the fibril electrode, the range of linearity is 0.5-50 μ g/L mercury,
The μ g/L mercury of detection limit 0.06.Be present big interference, poor selectivity, sensitivity in chromogenic reaction method, can not often meet
The requirement of the quick detection Trace Mercury in scene or field, and electrochemical process is usually present coexistent metallic ion serious interference, data
Poor reproducibility, electrode be unstable and the problems such as troublesome maintenance.
On field and Site Detection, Wei Yongge etc. develops mercury ion kit (Wei Yongge, Chen Kun, Zhang Haochen etc., one
Plant the kit and its detection method of mercury ion in colorimetric determination sewage, CN105548152A, 2016), sewage sample is first
Cleared up and neutralized again by acid permanganate soln, then the methanol solution with vacant six molybdic acid of the list of organic decoration is mixed
It is even, specificity interaction then occurs with mercury ion, causes solution colour to change, color is carried out with mercury colorimetric card in kit
Compare, to detect mercury content in sample, the method is easy, specificity is high, detection speed is fast, sensitive height, but quantitative effect is poor, the back of the body
Scape serious interference, testing cost are high.Therefore, a kind of convenient, quick, accurate, sensitive mercury detection method is designed and develops with suitable
Close the quick detection demand of field or live water sample Trace Hg.
The content of the invention
High, cheap suitable of easy to use, steady quality, sensitivity is carried it is an object of the invention to provide a kind of
Together in surface water, the quick detection agent of Industry Waste Determination of Trace Mercury In Water and detection method.
Present invention discover that Determination of Trace Mercury In Water be chlorinated stannous be reduced to Elemental Mercury can air stream extract and it is molten by Potassiumiodate
Liquid enrichment absorbs, and Quick Oxidation is dimercurion, then with cadion reaction generation red complex, takes this principle preparation
Mercury quick detection agent.The detection agent is made up of mercury detection agent I, mercury detection agent II and mercury detection agent III, and specific preparation method is as follows：
A, weighs 5~10g Potassiumiodates and 10~60g ammonium hydrogen sulfates respectively, and mixing, grinding is uniform, obtains mercury detection agent I；
B, weighs 5~10g stannous sulfates and 1~5g sulfamic acids respectively, and mixing, grinding is uniform, obtains mercury detection agent II；
C, weighs 0.02~0.1g cadions, is dissolved in 2~5ml absolute ethyl alcohols, adds 1~5ml triton x-100s, mixes
Close uniform, then mixed with 20~30g beta cyclodextrins, 5~20g boraxs and 1~10g sodium hydroxides, in 60 DEG C of heating, dryings 1 hour,
Grinding, obtains mercury detection agent III；
Above-mentioned Potassiumiodate, ammonium hydrogen sulfate, stannous sulfate, sulfamic acid, cadion, borax, beta cyclodextrin, absolute ethyl alcohol, song
It is commercially available analysis pure chemicals to draw logical X-100 and sodium hydroxide.
The application method of mercury detection agent：Take 5ml distilled water in the absorption tube of multifunctional sample processing instrument, plus 0.1~0.4g
Mercury detection agent I, shakes up dissolving, is connected appropriate with airway tube.25ml water samples to be measured are taken in reaction tube, plus 0.1~detection of 0.5g mercury
Agent II, inserts heater, is installed to original position, and couple with airway tube.Power-on, 0.2~0.5L/min of setting gas flow
With 10~20 minutes working times, be absorbed liquid after being pre-processed, and is then directly added into absorbing liquid after the pre-treatment
0.1~0.3g mercury detection agent III, shakes up dissolving, stands 2~10 minutes, using colorimeter or spectrophotometer measurement, produces and treat
Survey mercury content in water sample.
Above-mentioned multifunctional sample processing instrument is commercial instruments, by gas production pump, gas flowmeter, reaction tube, airway tube, absorption
Pipe, heater, time controller and lithium battery group into.
Above-mentioned water sample to be measured refers to ground water and industrial effluents.
Advantages of the present invention and effect are as follows：
1, the present invention uses the sample pretreating method of potassium iodate solution rich absorbent mercury vapour first, and passes through cadion
Develop the color colorimetric determination Trace Hg, substitutes the operation of the large-scale instruments such as traditional atomic fluorescence, and instrument is simple light, easy to operate, inspection
Whole process is surveyed less than 20 minutes, method detection is limited to 0.002mg/L Hg, is suitable for the open country of Trace Hg in ground water and industrial effluents
Outer or field quick detection.
2, the present invention prepares detection pulvis and substitutes a variety of aqueous solution that laboratory is prepared, easy quantitative sealed packaging, matter first
Amount stationary phase is long, and transports, carries, using more convenient, both avoids hydrolysis and illumination effect, has also prevented plurality of reagents
Waste.
Embodiment
The preparation of the mercury detection agent of embodiment 1
10g Potassiumiodates, 60g ammonium hydrogen sulfates are weighed, is mixed, grinding obtains mercury detection agent I；Weigh 5g stannous sulfates, 5g amino
Sulfonic acid, is mixed, and grinding obtains mercury detection agent II；0.02g cadions are weighed, 2ml absolute ethyl alcohols are dissolved in, 1ml Qulas is added and leads to X-
100, it is well mixed, mix with 20g beta cyclodextrins, 5g boraxs and 8g sodium hydroxides, in 60 DEG C of heating, dryings 1 hour, grinds, obtain
Mercury detection agent III.
The application method for the mercury detection agent that embodiment 2 is obtained using embodiments of the invention 1-Mercury in Wastewater detection
Take 5ml distilled water in the absorption tube of multifunctional sample processing instrument, plus 0.2g mercury detection agent I, shake up dissolving, connection is led
Tracheae.Take 25ml waste water in reaction tube, plus 0.4g mercury detection agent II, insert heater, be installed to original position, and join with airway tube
Connect.Power-on, setting gas velocity 0.3L/min and 10 minutes working times.After pretreatment, 0.1g is directly added into absorbing liquid
Mercury detection agent III, shakes up dissolving, stands 5 minutes, is transferred to colorimetric pool, suction is determined at wavelength 480nm using spectrophotometer
Luminosity, substitutes into standard curve and calculates, waste water mercury 0.068 ± 0.012mg/L of concentration of three parallel determinations, and detection is whole only every time
20 minutes, and testing result is consistent with ICP detection method results 0.076mg/L, and therefore, this method detection Mercury in Wastewater is accurate
It is really feasible.
Mercury is detected in application method-certain lake water for the mercury detection agent that embodiment 3 is obtained using embodiments of the invention 1
Take 5ml distilled water in the absorption tube of multifunctional sample processing instrument, plus 0.2g mercury detection agent I, shake up dissolving, connection is led
Tracheae.Take 25ml lake water in reaction tube, plus 0.4g mercury detection agent II, insert heater, be installed to original position, and join with airway tube
Connect, power-on, setting gas velocity 0.3L/min；Be absorbed liquid after after pretreatment 10 minutes, then after the pre-treatment
0.1g mercury detection agent III is directly added into absorbing liquid, dissolving is shaken up, 5 minutes is stood, is transferred to colorimetric pool, utilizes spectrophotometer
Absorbance is determined at wavelength 480nm, standard curve is substituted into and calculates lake water mercury concentration less than 0.002mg/L, whole detection process
Only 17 minutes, mark-on 0.020mg/L mercury, measure the mercury rate of recovery be 80%-90%.
Above-mentioned multifunctional sample processing instrument is GE STD01 types, by gas production pump, gas flowmeter, reaction tube, airway tube, suction
Closed tube, heater, time controller and lithium battery group are into, maximum airflow 1L/min, by the scientific and technological limited public affairs of upper sea green Supreme Being's environmental protection
Department's production.
Claims (2)
1. a kind of preparation method for the quick detection agent for determining Determination of Trace Mercury In Water, it is characterised in that：The detection agent is by mercury detection agent
Ith, mercury detection agent II and mercury detection agent III are constituted, and specific preparation method is as follows：
A, weighs 5~10g Potassiumiodates and 10~60g ammonium hydrogen sulfates respectively, and mixing, grinding is uniform, obtains mercury detection agent I；
B, weighs 5~10g stannous sulfates and 1~5g sulfamic acids respectively, and mixing, grinding is uniform, obtains mercury detection agent II；
C, weighs 0.02~0.1g cadions, is dissolved in 2~5ml absolute ethyl alcohols, adds 1~5ml triton x-100s, and mixing is equal
It is even, then mixed with 20~30g beta cyclodextrins, 5~20g boraxs and 1~10g sodium hydroxides, heating, drying 1 hour, grinds at 60 DEG C
Mill, obtains mercury detection agent III；
Above-mentioned Potassiumiodate, ammonium hydrogen sulfate, stannous sulfate, sulfamic acid, cadion, borax, beta cyclodextrin, absolute ethyl alcohol, Qula are led to
X-100 and sodium hydroxide are commercially available analysis pure chemicals.
2. a kind of application method for the quick detection agent for determining Determination of Trace Mercury In Water, it is characterised in that：5ml distilled water is taken in multi-functional
The absorption tube of sample treatment instrument, plus 0.1~0.4g mercury detection agent I, shakes up dissolving, be connected appropriate with airway tube, take 25ml to be measured
Water sample plus 0.1~0.5g mercury detection agent II in reaction tube, inserts heater, is installed to original position, and couples with airway tube, opens
Power supply, setting 0.2~0.5L/min of gas flow and 10~20 minutes working times, be absorbed liquid after being pre-processed, so
0.1~0.3g mercury detection agent III is directly added into absorbing liquid after the pre-treatment afterwards, dissolving is shaken up, 2~10 minutes are stood, utilized
Colorimeter or spectrophotometer measurement, produce mercury content in water sample to be measured；
Above-mentioned multifunctional sample processing instrument be commercial instruments, by gas production pump, gas flowmeter, reaction tube, airway tube, absorption tube,
Heater, time controller and lithium battery group into；
Above-mentioned water sample to be measured refers to ground water and industrial effluents.
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Cited By (1)
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| CN109211819A (en) * | 2018-11-08 | 2019-01-15 | 闫宏涛 | Measure the combine detection agent of Soil Available potassium content |
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Application publication date: 20171020 |