CN103499558A - System and method for determining mercury concentration in water - Google Patents
System and method for determining mercury concentration in water Download PDFInfo
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- CN103499558A CN103499558A CN201310403760.2A CN201310403760A CN103499558A CN 103499558 A CN103499558 A CN 103499558A CN 201310403760 A CN201310403760 A CN 201310403760A CN 103499558 A CN103499558 A CN 103499558A
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Abstract
A system for determining mercury concentration in water comprises a peristaltic pump sample introduction system, reagent storage tanks, a control valve set, a reactor, a fluorescent detector and a data acquisition processing system; the peristaltic pump sample introduction system, which is used to control on-off of electric signals for realizing on-off of the control valve set, is electrically connected with the control valve set; the control valve set is connected with the reagent storage tanks and the reactor via pipelines, and is communicated with the reagent storage tanks and a water sample, so that the water sample and corresponding reagents in the reagent storage tanks are taken out and conveyed to the reactor for chemical reactions; the fluorescent detector is connected with the reactor via pipelines, and is used to receive mercury-containing steam and detect the content of mercury in the steam; and the data acquisition processing system is electrically connected with the fluorescent detector, and is used to receive the mercury content value detected by the fluorescent detector and process the data for acquisition of the mercury concentration of a detected sample.
Description
Technical field
The present invention relates to the mensuration system and method for mercury concentration, refer in particular to a kind of mercury concentration determination system and method that adopts atomic fluorescence detection technique and cold steam technology to combine.
Background technology
Mercury (Hg) and compound thereof belong to extremely toxic substance, can in human body, accumulate.Mercury can enter people's respiratory tract by contaminated air, enter after human body and strong interactions occur for protein, enzyme etc., and they are lost activity, and also can in some organs of human body, accumulate and enrichment, endangers people's health.The inorganic mercury ion that enters water body can change the organic mercury that toxicity is larger into, through food chain, enters human body, causes poisoning.All extremely pay close attention to prevention and the improvement of mercury pollution both at home and abroad, promulgated a lot of detection methods and standard.Mercury is one of index of China's enforcement total emission volumn control.
At present, the detection technique in Mercury in Water Body concentration mainly contains electrochemical methods, sampling Graphite Furnace Atomic emission spectrometry, NITRATE BY FLAME ATOMIC spectroscopic methodology, cold atomic absorption spectrometry, inductively coupled plasma emission spectrometry and Cold Atomic Fluorescent Mercury spectroscopic methodology etc.Although electrochemical methods sensitivity is very high, owing to can only using the noble metal solid electrode, therefore the ageing of electrode phenomenon is serious.Must use the reason such as noble metal to be difficult to obtain reliable data precision, it is very large that electrode expends simultaneously, and cost is very high.Atomic emission spectrometry, though have good repeatability and reliability, accuracy and measurement data degree of confidence are very high, but its sensitivity is difficult to the mercury content in the Measurement accuracy potable water in the ppm magnitude.
Summary of the invention
Based on the deficiencies in the prior art, fundamental purpose of the present invention is to provide a kind of highly sensitive cold steam atomic fluorescence spectrometry to measure the system and method for mercury concentration in water, to solve the lower or unsettled problem of test data of existing detecting instrument sensitivity.
The invention provides a kind of for measuring the system of water mercury concentration, it comprises: peristaltic pump sampling system, reagent hold-up vessel, operation valve group, reactor, fluorescence detector and data acquisition processing system, described peristaltic pump sampling system is electrically connected to the operation valve group, realizes the switch of described operation valve group for the break-make of controlling respectively electric signal; Described operation valve group is connected with reactor with the reagent hold-up vessel respectively by pipeline, connects respectively each required reagent hold-up vessel and water sample, extracts and transfers to reactor with the corresponding reagent by water sample and reagent hold-up vessel and carry out chemical reaction; Described fluorescence detector, be connected by pipeline with reactor, contains mercuryvapour for receiving through reacted, and detect the wherein content of mercury; Described data acquisition processing system, be electrically connected to fluorescence detector, receives the mercury content value of its detection, and, after data are processed, obtain the mercury concentration of sample.
Preferably, described reagent hold-up vessel comprises oxygenant tank and reductive agent tank, respectively the Oxidizing and Reducing Agents of storage is delivered in reactor, in reactor successively, the reagent passed into carries out oxidation reaction and reduction reaction successively with water sample respectively, obtains the Elemental Mercury atom vapor.
Preferably, described system further comprises inert gas control gas sheath, the one end is connected with the inert gas compressed tanks, the other end is connected with reactor pipeline, at inert gas, control under the driving control of gas sheath, pass into inert gas to reactor, make it to mix with the Elemental Mercury atom vapor that reacts acquisition, obtain mixed gas.Described inert gas is high-purity argon gas.
Preferably, described system further comprises gas-liquid separator, and it is connected with described reactor pipeline, the mixed gas of reactor output carries out gas-liquid separation through gas-liquid separator, acquisition includes the mixed vapour of mercuryvapour and inert gas, in detection, has avoided the interference of matrix to mercuryvapour.
Preferably, described system also further comprises exsiccator, and it is connected with gas-liquid separator, carries out drying for the mixed vapour to after gas-liquid separation and processes.
The present invention also provides a kind of method of measuring mercury concentration in water, and it adopts cold steam atomic fluorescence spectrometry, and it comprises the following steps:
Step 1) sample and clear up, quantitatively extracting mercurous water sample and oxygenant, and passing into respectively in reactor, being cleared up reaction, the mercury oxidation that makes the various valence states in water sample is Hg
2+;
Step 2) reduction passes into reductive agent, with the Hg by after clearing up in reactor
2+be reduced to the Elemental Mercury atom vapor;
Step 3) separate, pass into inert gas to reactor, described Elemental Mercury atom vapor is written into to gas-liquid separator, so that mercuryvapour is carried out to gas-liquid separation, obtain the mixed gas of Elemental Mercury atomic gas and inert gas;
Step 4) detect, mixed gas is passed into to fluorescence detector and detect analysis, obtain the mercury content of detected water sample.
Preferably, in step 1) further comprise: step is preliminary rinse a), and water sample is introduced to reactor, with the former ducted old liquid of new liquid displacement, reactor and pipeline thereof is carried out to rinse, and the water sample gathered to guarantee is fresh, avoids mixing with old liquid.
Preferably, in step 3) and step 4) between further comprise: step b) drying, the mixed gas after gas-liquid separation is passed into to exsiccator, it is carried out to drying and processes, remove water vapour, improve the precision detected;
Preferably, in step 4) afterwards, further comprise step c) reclaim, the mixed gas after detecting is passed into to active carbon filter and absorb processing.
Compared with prior art, in the present invention, measure in the method for mercury concentration in water, successively through rinse, sample and clear up, reduce, separate, dry, detection and recycling, adopt atom fluorimetry technology and cold steam technology to combine, by oxygenant, the mercury oxidation of various valence states in water sample is become to Hg
2+, extract dimercurion, then, pass into reductive agent and will clear up the Hg that reaction generates
2+be reduced into Elemental Mercury steam, after passing into the inert gas argon gas mercuryvapour being brought into to gas-liquid separator and carried out gas-liquid separation, through super-dry, remove the water vapour in steam, dried mercuryvapour, pass into the mensuration that fluorescence detector carries out mercury atom concentration, obtain thus the content of mercury in water.In the present invention, adopt high-precision peristaltic pump sampling system, utilize Single-chip Controlling peristaltic pump sample introduction, improve the accuracy rate of each sample size, reproducible.Utilizing the Single-chip Controlling solenoid valve to automatically switch, is the closed loop gas circuit during measuring state, while cleaning state, is the open loop gas circuit, data stabilization while making to measure like this, and pipeline is easy to clean.Adopt high purity argon as carrier gas, realize gas-liquid separation, by the infiltration type dry technology, make mercuryvapour and matrix realize thoroughly separating, improve measurement sensitivity.Employing is cleared up, atomization is carried out in same reactor, has reduced loss and pollution, guarantees the accuracy of measuring.Adopt the high-precision pressure control system, can strictly control and pass into carrier gas flux, because carrier gas flux is excessive, can rush the concentration of rare determined composition, too smallly can not bring tested composition into detecting device rapidly, can improve accuracy and the sensitivity of test.
Adopt high-purity argon gas as carrier gas, can effectively reduce the content of impurity in carrier gas, improve sensitivity and the precision of test.Because the mercury atom excited gives off fluorescence except spontaneously returning to ground state, also can bump with background particle and energy be changed into to the thermal motion of particle, thereby produced non-blooming transition, reduced fluorescence intensity, the phenomenon of atomic fluorescence quencher that Here it is.Owing to being excited, mercury atom is more much smaller than airborne nitrogen, oxygen, carbon dioxide etc. with the probability of argon gas collision, and while therefore adopting argon gas to use nitrogen as the source of the gas ratio, sensitivity is much higher.
Simultaneously, the Cold Atomic Fluorescent Mercury spectroscopic methodology is surveyed mercury and is had very low detection limit, is better than additive method and has obtained using widely.The Cold Atomic Fluorescent Mercury method is surveyed the principle of mercury: the mercury ion in water sample is reduced agent and is reduced to Elemental Mercury steam.Its ground state mercury atom is subject to the ultraviolet excitation of wavelength 253.7nm, when excited state mercury atom deexcitation, just gives off fluorescence, and under given condition and in lower concentration range, fluorescence intensity is directly proportional to the concentration of mercury.
The accompanying drawing explanation
Fig. 1 is the present invention for the structural representation of the system of measuring water mercury concentration.
Embodiment
Shown in Fig. 1, for mercury concentration is accurately measured, the invention provides a kind of for measuring the system of water mercury concentration, having adopted atomic fluorescence and cold steam technology to combine is measured, it comprises: peristaltic pump sampling system 1, operation valve group 2, reagent hold-up vessel 3, reactor 4, fluorescence detector 5 and data acquisition processing system 6, wherein, described peristaltic pump sampling system 1 is electrically connected to operation valve group 2, realizes the switch of described operation valve group 2 for the break-make of controlling respectively electric signal; Described operation valve group 2 is connected with reactor 4 with reagent hold-up vessel 3 respectively by pipeline, connects respectively each required reagent hold-up vessel 3 and water sample, extracts and transfers to reactor 4 with the corresponding reagent by water sample and reagent hold-up vessel 3 and carry out chemical reaction; Described fluorescence detector 5, be connected by pipeline with reactor 4, contains mercuryvapour for receiving through reacted, and detect the wherein content of mercury; Described data acquisition processing system 6, be electrically connected to fluorescence detector 5, receives the mercury content value of its detection, and, after data are processed, obtain the mercury concentration of sample.
Wherein, described peristaltic pump sampling system 1, as the control driver element of sample and various reagent, is electrically connected to operation valve group 2, according to the programming requirement, to the break-make of each operation valve, extracts according to the order of sequence each reagent respectively, makes the reaction substep carry out.Operation valve group 2 comprises several operation valves 20, and described operation valve 20 is connected respectively each reagent hold-up vessel 3, to drive it, carries corresponding reagent or water sample to reactor respectively.Wherein, described reagent is respectively reductive agent and oxygenant, and preferably, described reductive agent is SnCl
2, described oxygenant is potassium bromate-potassium bromide intermixture.Described water sample is mercurous solution water sample to be determined.
Described reagent hold-up vessel 3 at least comprises oxygenant tank 30 and reductive agent tank 32, respectively the Oxidizing and Reducing Agents of storage is delivered in reactor 4 successively, in reactor 4, the reagent passed into carries out oxidation reaction and reduction reaction successively with water sample 34 respectively, obtains the Elemental Mercury atom vapor.Respectively required reagent is extracted in each reagent hold-up vessel 3 by reagent pump, through pipeline, be delivered in reactor 4 and carry out oxidation or reduction reaction.
In a preferred embodiment of the invention, described system further comprises inert gas control gas sheath 7, the one end is connected with inert gas compressed tanks 11, the other end is connected with the air inlet pipeline of reactor 4, at inert gas, control under the driving control of gas sheath 7, pass into inert gas to reactor 4, make it to mix with the Elemental Mercury atom vapor that reacts acquisition, obtain mixed gas.Wherein, described inert gas be high-purity argon gas as carrier gas, high-purity argon gas can effectively reduce the impurity content in carrier gas, improves sensitivity and the precision of test.
In another preferred embodiment of the present invention, described system further comprises gas-liquid separator 8, its outlet pipe with described reactor 4 is connected, the mixed gas of reactor 4 output by high-purity argon gas as carrier gas, mercuryvapour is conveyed into to gas-liquid separator 8 and carries out gas-liquid separation, by the infiltration type dry technology, acquisition includes the mixed vapour of mercury atom steam and inertia steam, realize separating of mercury atom steam and matrix, described matrix is reacted solution, comprises the solution after former water sample and the reagent reacting that adds.
In another preferred embodiment of the present invention, described system also further comprises exsiccator 9, and its input end is connected with gas-liquid separator 8, and its output terminal is connected with fluorescence detector 5, carries out drying for the mixed vapour to after gas-liquid separation and processes.Mercury atom steam after separation enters exsiccator 9 under the promotion of high-purity argon gas, enters after drying the mensuration that fluorescence detector 5 carries out mercury content, and data transmission to the data acquisition system (DAS) after measuring is carried out to analyzing and processing, obtains the mercury content of detected water sample.
Preferably, described system also further comprises waste liquid recovery apparatus, with fluorescence detector 5, be connected, and several waste treatments after the mercury atom steam after detecting with recovery.Described waste liquid recovery apparatus can be active carbon filter 10.
The invention provides a kind of method of measuring mercury concentration in water, adopt cold steam atomic fluorescence spectrometry, comprise the following steps:
Step 1) sampling, quantitatively extract the water sample that contains the mercury molecule, and by the reagent pump of peristaltic pump sampling system 1 startup oxygenant, drive it to derive from oxygenant tank 30, and be delivered in reactor, in reactor, water sample is mixed mutually with oxygenant, cleared up reaction, the mercury oxidation that makes the various valence states in water sample is Hg
2+; Wherein, the preferred potassium bromate of described oxygenant-potassium bromide intermixture.
Step 2) reduction, the reagent pump by peristaltic pump sampling system 1 startup reductive agent, drive it to import from reductive agent tank 32, and be delivered in reactor, in reactor, will clear up reacted containing Hg
2+aqueous solution and reductive agent carry out reduction reaction, with the Hg2+ by after clearing up, are reduced to the Elemental Mercury atom vapor, make original mercury element be reduced into simple substance steam; Described reductive agent is SnCl2.Elemental Mercury in solution can be evaporated to mercuryvapour at normal temperatures, passes into argon gas, can take mercuryvapour out of.
Step 3) separate, control the gas sheath by inert gas by inert gas, as high-purity argon gas is delivered in reactor by pipeline, by described argon gas, described Elemental Mercury atom vapor is written in gas-liquid separator, so that mercuryvapour is carried out to gas-liquid separation, obtain the mixed gas of Elemental Mercury atomic gas and inert gas;
Step 4) detect, mixed gas is passed into to fluorescence detector and detect analysis, obtain the mercury content of detected water sample.Ground state gaseous mercury atom is subject to wavelength 253.7nm ultraviolet excitation, absorbed certain energy and by ground state transition the excited state to high energy, when excited state mercury atom deexcitation, be accompanied by the release of energy, give off fluorescence.This fluorescence is transformed into electric signal through the photomultiplier reception and is received by data acquisition system (DAS).When the mercury atom vapour concentration is very low, the fluorescence intensity recorded is directly proportional to the mercury atom vapour concentration, can record thus the concentration of mercury.The advantage of atomic fluorescence method mainly contains: the impact of matrix is easily eliminated, measurement sensitivity is high, detection limit is low and the range of linearity is wide.
Preferably, in step 1) further comprise: step is preliminary rinse a), and water sample is introduced to reactor, with the former ducted old liquid of new liquid displacement, reactor and pipeline thereof is carried out to rinse, is disposed to waste liquid barrel after rinse and is processed.Through preliminary rinse, replace original ducted old liquid, the liquid that guarantees every sub-sampling gained of take is fresh water sample, the accuracy of sample thief mercury content to guarantee.
Preferably, in step 3) and step 4) between further comprise: step b) drying, mixed gas after gas-liquid separation is passed into to exsiccator, it is carried out to drying processes, by the infiltration type dry technology, make mercuryvapour and matrix realize separating, remove the water vapour of carrying secretly in mixed gas, detected by fluorescence detector again, improved the purity of mercury atom steam.
Preferably, in step 4) afterwards, further comprise step c) reclaim, the mixed gas after fluorescence detector detects is passed in active carbon filter 10 and absorbs and process, last, enter castoff processing system.
In mensuration water of the present invention in the method for mercury concentration, pass through successively rinse, sampling, reduction, separation, drying, detection and recycling, adopt atom fluorimetry technology and cold steam technology to combine, by cold steam technology, with oxygenant, the mercury oxidation of various valence states in water sample is become to Hg
2+, extract dimercurion, then, pass into reductive agent and will clear up the Hg that reaction generates
2+be reduced into mercury atom simple substance, after passing into the inert gas argon gas mercuryvapour being brought into to gas-liquid separator and carried out gas-liquid separation, remove the water vapour in steam through super-dry, after removing moisture, pass into the mensuration that fluorescence detector carries out mercury atom concentration, obtain thus the content of mercury concentration in water.In the present invention, adopt high-precision peristaltic pump sampling system, utilize Single-chip Controlling peristaltic pump sample introduction, improve the accuracy rate of each sample size, reproducible.Utilizing the Single-chip Controlling solenoid valve to automatically switch, is the closed loop gas circuit during measuring state, while cleaning state, is the open loop gas circuit, data stabilization while making to measure like this, and pipeline is easy to clean.Adopt high purity argon as carrier gas, realize gas-liquid separation, by the infiltration type dry technology, make mercuryvapour and matrix realize thoroughly separating, improve measurement sensitivity.Employing is cleared up, atomization is carried out in same reactor, has reduced loss and pollution, guarantees the accuracy of measuring.Adopt high-purity argon gas as carrier gas, can effectively reduce the content of impurity in carrier gas, improve sensitivity and the precision of test.
With traditional method of testing, compare, the advantage of cold steam atomic fluorescence method mainly contains:
The impact of l, matrix is easily eliminated, and low-down background interference is arranged;
2, adopt high-purity argon gas as carrier gas, reduce the impact of impurity, measurement sensitivity is high;
3, detection limit is low, can survey the mercury of trace;
4, adopt high-precision peristaltic pump sampling system, improve the accuracy rate of each sample size, reproducible.
Claims (10)
1. one kind for measuring the system of water mercury concentration, it is characterized in that comprising: peristaltic pump sampling system, reagent hold-up vessel, operation valve group, reactor, fluorescence detector and data acquisition processing system, described peristaltic pump sampling system is electrically connected to the operation valve group, realizes the switch of described operation valve group for the break-make of controlling respectively electric signal; Described operation valve group is connected with reactor with the reagent hold-up vessel respectively by pipeline, connects respectively each required reagent hold-up vessel and water sample, extracts and transfers to reactor with the corresponding reagent by water sample and reagent hold-up vessel and carry out chemical reaction; Described fluorescence detector, be connected by pipeline with reactor, contains mercuryvapour for receiving through reacted, and detect the wherein content of mercury; Described data acquisition processing system, be electrically connected to fluorescence detector, receives the mercury content value of its detection, and, after data are processed, obtain the mercury concentration of sample.
2. according to claim 1 for measuring the system of water mercury concentration, it is characterized in that: described reagent hold-up vessel comprises oxygenant tank and reductive agent tank, to be delivered to successively in reactor by the Oxidizing and Reducing Agents of storage respectively, in reactor, the reagent passed into carries out oxidation reaction and reduction reaction successively with water sample to be determined respectively, obtains the Elemental Mercury atom vapor.
3. according to claim 2 for measuring the system of water mercury concentration, it is characterized in that: described system further comprises inert gas control gas sheath, the one end is connected with the inert gas compressed tanks, the other end is connected with reactor pipeline, at inert gas, control under the driving control of gas sheath, pass into inert gas to reactor, make it to mix with the Elemental Mercury atom vapor that reacts acquisition, obtain mixed gas.
4. according to claim 3 for measuring the system of water mercury concentration, it is characterized in that: described system further comprises gas-liquid separator, it is connected with the output terminal pipeline of described reactor, the mixed gas of reactor output carries out gas-liquid separation through gas-liquid separator, obtains the mixed vapour that includes mercuryvapour and inertia steam.
5. according to claim 4 for measuring the system of water mercury concentration, it is characterized in that: described system also further comprises exsiccator, and it is connected with the output terminal of gas-liquid separator, carries out drying for the mixed vapour to after gas-liquid separation and processes.
6. a method of measuring mercury concentration in water, it adopts cold steam atomic fluorescence spectrometry, it is characterized in that comprising the following steps:
Step 1) sample and clear up, quantitatively extracting mercurous water sample and oxygenant, and passing into respectively in reactor, being cleared up reaction, the mercury oxidation that makes the various valence states in water sample is Hg
2+;
Step 2) reduction passes into reductive agent, with the Hg by after clearing up in reactor
2+be reduced to the Elemental Mercury atom vapor;
Step 3) separate, pass into inert gas to reactor, described Elemental Mercury atom vapor is written into to gas-liquid separator, so that mercuryvapour is carried out to gas-liquid separation, obtain the mixed gas of Elemental Mercury atomic gas and inert gas;
Step 4) detect, mixed gas is passed into to fluorescence detector and detect analysis, obtain the mercury content of detected water sample.
7. the method for mercury concentration in mensuration water according to claim 6, it is characterized in that: in step 1) further comprise: step is preliminary rinse a), water sample is introduced to reactor, with the former ducted old liquid of new liquid displacement, reactor and pipeline thereof are carried out to rinse.
8. the method for mercury concentration in mensuration water according to claim 7, is characterized in that: in step 3) and step 4) between further comprise: step b) drying, the mixed gas after gas-liquid separation is passed into to exsiccator, it is carried out to drying and processes.
9. the method for mercury concentration in mensuration water according to claim 8, is characterized in that: in step 4) afterwards, further comprise step c) reclaim, the mixed gas after detecting is passed into to active carbon filter and absorb processing.
10. the method for mercury concentration in mensuration water according to claim 6, it is characterized in that: described inert gas is high-purity argon gas.
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| CN103926206A (en) * | 2014-05-09 | 2014-07-16 | 天津师范大学 | Device for detecting carbonate in water solution rapidly |
| CN103954609A (en) * | 2014-05-09 | 2014-07-30 | 天津师范大学 | Rapid detection device for inorganic carbon and form thereof |
| 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 |
| CN106198914A (en) * | 2016-07-07 | 2016-12-07 | 深圳市朗石科学仪器有限公司 | A kind of measure the system and method for mercury content in water sample |
| CN108107029A (en) * | 2017-12-14 | 2018-06-01 | 浙江微兰环境科技有限公司 | A kind of detection method of water quality total mercury |
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Application publication date: 20140108 |