CN101358924A - Morphological analysis apparatus for mercury element and analysis method thereof - Google Patents

Morphological analysis apparatus for mercury element and analysis method thereof Download PDF

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Publication number
CN101358924A
CN101358924A CNA2007101199258A CN200710119925A CN101358924A CN 101358924 A CN101358924 A CN 101358924A CN A2007101199258 A CNA2007101199258 A CN A2007101199258A CN 200710119925 A CN200710119925 A CN 200710119925A CN 101358924 A CN101358924 A CN 101358924A
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mercury
gas
photoinduction
steam generator
atomizer
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CN101358924B (en
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魏文元
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Beijing Bo Hui innovative biotechnology Limited by Share Ltd
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BEIJING LWL INSTRUMENT Co Ltd
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Abstract

The invention discloses a hydrargyrum form analyzing instrument applied in the field of analytical chemistry and as well as a method thereof. The analyzing instrument comprises a sample-feeding unit, a medium selective entrance control unit, a photoinduction steam generator, a gas-liquid separator and a detector; the sample-feeding unit, the medium selective entrance control unit are connected with one end of the photoinduction steam generator; the other end of the photoinduction steam generator is connected with the gas-liquid separator; and the gas which passes through the gas-liquid separator is imported into the detector (11) for testing. The advantages of the invention include: the sequence of injection-photoinduction-selective hydrargyrum steam generation and sample feeding system is adopted to make different hydrargyrum forms take place, and thereby, effective separation of hydrargyrum in different forms is realized. In addition, the detector adopts an atomizer (absorption cell), fluorescence excitation and fluorescence testing integrated design, the fluorescence testing area is increased, the distance between the detector and the atomizer is reduced, and the measurement sensitivity is improved.

Description

A kind of mercury element morphological analysis means and analytical approach thereof
Technical field
The invention belongs to light, mechanical, electrical integrated analysis instrument, be mercury element morphological analysis instrument and the analytical approach of using in a kind of analytical chemistry field thereof, especially relate to instrument and under not by means of the situation of any pre-separation technology, can carry out the while method for measuring the different shape of mercury in institute's specimen.
Background technology
Mercury is as a kind of hypertoxicity element, and its toxicity and its occurrence status in sample is closely related, and for example methyl mercury is more a lot of greatly than inorganic mercury toxicity.At present; all very pay close attention to the morphological analysis of mercury both at home and abroad; the sample that relates to fields such as food security, environmental protection not only will carry out the mensuration of total mercury; also to measure, for example require total mercury in the food and organic mercury are measured (GB/T 5009.17-2003) in the state food examination criteria of China's promulgation in 2003 form of mercury.But morphological analysis is mainly some coupling techniques about mercury element both at home and abroad at present, and these technology at first make the different shape pre-separation of mercury with isolation technics commonly used, use atomic spectrum (mass spectrum) to measure as testing tool then.Mainly comprise: high performance liquid chromatography-plasma mass coupling (HPLC-ICP-MS), high performance liquid chromatography-atomic absorption coupling (HPLC-AAS), high performance liquid chromatography-atomic fluorescence coupling (HPLC-AFS) and gas chromatography combined with mass spectrometry (GC-MS).These coupling techniques exist apparatus expensive, the high deficiency of operating cost.Particularly the general requirement of HPLC and GC technology sampling amount is very little, usually in micro updating (μ L) level, and ICP-MS, FAAS, AFS need milliliter level (mL) sample usually, because sampling amount very little causes the detection lower limit deficiency of these coupling techniques, can not satisfy the test request of many actual samples usually like this.
Summary of the invention
In order to overcome the existing mercury morphological analysis technology that is used in the deficiency aspect equipment/operating cost and the detection lower limit, invention provides a kind of high-sensitive mercury morphological analysis instrumentation.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of mercury element morphological analysis means comprises that sample introduction parts 2, medium selection enter control assembly, photoinduction steam generator 6, gas-liquid separator 9 and detecting device 11; Described sample introduction parts 2 are selected to enter control assembly with medium and are connected with described photoinduction steam generator 6 one ends, and the other end of described photoinduction steam generator 6 is connected with gas-liquid separator 9, detects through the gas input detector 11 behind the gas-liquid separator 9.
In concrete application, described medium is selected to enter control assembly and is comprised three solution inlet port and a four-way valve 1; Described four-way valve 1 described three solution inlet port of control and a liquid outlet are selected into/fluid; Described three solution inlet port comprise acetate import, formic acid import and cleaning fluid mouth.
In concrete application, described sample introduction parts 2 are selected to enter control assembly with medium and are connected with photoinduction steam generator 6 with first threeway 5 by peristaltic pump 4, promptly by peristaltic pump 4 and first threeway 5 sample and medium solution are delivered in the photoinduction steam generator 6;
In the middle of described photoinduction steam generator 6 and described gas-liquid separator 9, also comprise second threeway 7, and inject argon gas by an inlet 8 of described second threeway 7; The mercuryvapour that promptly passes through described photoinduction steam generator 6 and produce and the argon gas of injection together enter gas-liquid separator 9 and carry out gas-liquid separation;
In the middle of described gas-liquid separator 9 and detecting device 11, also comprise a mercury enrichment pipe 10; Promptly carry out the gas enrichment through the mercury vapour input mercury enrichment pipe 10 after separating.
In concrete application, described detecting device 11 is taked atomizer 115, fluorescence excitation 113 and fluoroscopic examination 116 integrated apparatus; Comprise detection system shell 111, detection system inner casing 112, fluorescence excitation 113, entrance slit 114, atomizer 115, fluoroscopic examination 116, mercury vapour inlet 117 and mercury vapour outlet 118.
Described fluorescence excitation 113 is the pen type mercury lamp, and described fluoroscopic examination 116 is a photomultiplier, and described atomizer 115 is an absorption cell; And atomizer 115 adopts the thin flat structure, adopts the quartzy material of hollow; Distance between described pen type mercury lamp 113 and the atomizer 115 is 1-10cm, and the distance between described atomizer 115 and the photomultiplier 116 is 1-10cm.
Distance between preferably described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
A kind of method of utilizing the mercury element morphological analysis means to carry out the mercury element morphological analysis
Described method comprises:
A formic acid medium analysis step: operation four-way valve 1 rotates, and o, a position are communicated, and pumps into formic acid, and pumps into sample from sample pipe 2; Described sample and formic acid converge and enter described photoinduction steam generator 6 in first threeway 5, this moment comprises organic in the test solution and total mercury solution inorganic mercury can produce mercury vapour under UV light-induced, after described gas-liquid separator 9 separated, described mercury vapour was brought into described enrichment pipe 10 by argon gas;
B cleans and testing procedure a: operation four-way valve 1 rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe 10 simultaneously after, enter described detecting device 11 and detect, record the content of total mercury;
C acetic acid medium analytical procedure: operation four-way valve 1 rotates, and o, c position are communicated, and pumps into acetate, and pumps into sample from sample pipe 2; Sample and acetate converge and enter described photoinduction steam generator 6 in first threeway 5, organic mercury optionally produces mercury vapour in the test solution under UV light-induced at this moment, after described gas-liquid separator 9 separated, described mercury vapour was brought into described enrichment pipe 10 by argon gas;
D cleans and testing procedure b: operation four-way valve 1 rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe 10 simultaneously after, enter described detecting device 11 and detect, record organomercurial content.
In the application of reality,
The concentration of described formic acid medium solution is: 0.05-40% (v/v)
The concentration of described acetic acid medium solution is: 0.05-20% (v/v)
Carry out ultraviolet at described photoinduction steam generator and produce in the process of mercury vapour, the time of ultraviolet irradiation is: 5-1200s.
The technical scheme that technical solution problem of the present invention is adopted is to utilize in the formic acid medium, and the mercury of different shapes such as inorganic mercury ion, organic mercury can be at the UV light-induced mercury vapour that generates down; And in acetic acid medium, have only organic mercury can be induced the generation mercury vapour, so the selective chemical steam that can reach different shape mercury by the change reaction medium takes place.The cold steam that produces is by after the enrichment of one-level amalgam, and the heating of the mercury vapour of enrichment discharges into detection system, detects with the principle of atomic fluorescence.
Beneficial effect of the present invention is: (1) adopts sequential injection-photoinduction-selectivity mercury vapour generation sampling system, and the different shape selectivity of mercury element is taken place, and has realized effective separation of different shape mercury; (2) detector design is taked atomizer (absorption cell), fluorescence excitation, fluoroscopic examination integrated design, has increased the fluoroscopic examination area, has shortened the distance between detecting device and the atomizer, has improved mensuration sensitivity.
And the instrumentation that the present invention developed need be by means of pre-separation technology such as HPLC and GC, reaches selective determination to the mercury different shape according to mercury selective chemical steam in the differential responses medium of different shape.But because large volume sampling (2-10ml), and taked incorporate detection system, made this special use instrument can finish mensuration in proper order, measured lower limit and can reach pieck stage (pg) level, low 2-3 the order of magnitude of conventional at present coupling technique different shape mercury.
Description of drawings
Fig. 1 is the principle schematic of mercury element morphological analysis means of the present invention;
Fig. 2 is the integrated detecting device in the mercury element morphological analysis means of the present invention;
Fig. 3 carries out sequential injection selectivity mercury vapour generation sampling system synoptic diagram in the analytical approach for the present invention utilizes the mercury element morphological analysis means.
More than each width of cloth accompanying drawing will specifically describe in detail in conjunction with following embodiment.
Embodiment
Fig. 1 is the principle schematic of mercury element morphological analysis means of the present invention.
A kind of mercury element morphological analysis means shown in Figure 1 comprises that sample introduction parts 2, medium selection enter control assembly, photoinduction steam generator 6, gas-liquid separator 9 and detecting device 11; Described sample introduction parts 2 are selected to enter control assembly with medium and are connected with described photoinduction steam generator 6 one ends, and the other end of described photoinduction steam generator 6 is connected with gas-liquid separator 9, detects through the gas input detector 11 behind the gas-liquid separator 9.3 is waste liquid outlet
Described medium is selected to enter control assembly and is comprised three solution inlet port and a four-way valve 1; Described four-way valve 1 described three solution inlet port of control and a liquid outlet are selected into/fluid (concrete selection course please refer to Fig. 3); Described three solution inlet port comprise acetate import, formic acid import and cleaning fluid mouth.
Described sample introduction parts 2 are selected to enter control assembly with medium and are connected with photoinduction steam generator 6 with first threeway 5 by peristaltic pump 4, promptly by peristaltic pump 4 and first threeway 5 sample and medium solution are delivered in the photoinduction steam generator 6;
In the middle of described photoinduction steam generator 6 and described gas-liquid separator 9, also comprise second threeway 7, and inject argon gas by an inlet 8 of described second threeway 7; The mercuryvapour that promptly passes through described photoinduction steam generator 6 and produce and the argon gas of injection together enter gas-liquid separator 9 and carry out gas-liquid separation;
In the middle of described gas-liquid separator 9 and detecting device 11, also comprise a mercury enrichment pipe 10; Promptly carry out the gas enrichment through the mercury vapour input mercury enrichment pipe 10 after separating.
Described detecting device 11 is taked atomizer 115, fluorescence excitation 113 and fluoroscopic examination 116 integrated apparatus; Detecting device 11 comprises detection system shell 111, detection system inner casing 112, fluorescence excitation 113, entrance slit 114, atomizer 115, fluoroscopic examination 116, mercury vapour inlet 117 and mercury vapour outlet 118.
Described fluorescence excitation 113 is the pen type mercury lamp, and described fluoroscopic examination 116 is a photomultiplier, and described atomizer 115 is an absorption cell; And atomizer 115 adopts the thin flat structure, adopts the quartzy material of hollow; Distance between described pen type mercury lamp 113 and the atomizer 115 is 1-10cm, and the distance between described atomizer 115 and the photomultiplier 116 is 1-10cm.
Distance between preferably described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
Fig. 2 is the integrated detecting device in the mercury element morphological analysis means of the present invention
Described detecting device 11 is taked atomizer 115, fluorescence excitation 113 and fluoroscopic examination 116 integrated apparatus; Detecting device 11 comprises detection system shell 111, detection system inner casing 112, fluorescence excitation 113, entrance slit 114, atomizer 115, fluoroscopic examination 116, mercury vapour inlet 117 and mercury vapour outlet 118.
Described fluorescence excitation 113 is the pen type mercury lamp, and described fluoroscopic examination 116 is a photomultiplier, and described atomizer 115 is an absorption cell; And the distance between described pen type mercury lamp 113 and the atomizer 115 is 1-10cm, and the distance between described atomizer 115 and the photomultiplier 116 is 1-10cm.Distance between preferred described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
Wherein, pen type mercury lamp 113 sends the radiant light with specific wavelength and enters atomizer 115 by entrance slit 114, mercury atom in the excited atom device 115 (absorption cell) makes it transit to high-energy state, the mercury atom of high-energy state gives off its feature when getting back to ground state or low-energy state fluorescent line carries out measuring after the opto-electronic conversion after being accepted by photomultiplier 116.Carried out the integrated design of atomizer 115, fluoroscopic examination 116 and fluorescence excitation 113 in the present invention.Distance between fluorescence excitation 113 and the atomizer 115 is 1-10cm, and the distance between atomizer 115 and the fluoroscopic examination 116 is 1-10cm.Ultrashort light path has reduced the loss of light, helps to improve the sensitivity of mensuration.In addition, atomizer 115 adopts ultra-thin dull and stereotyped hollow quartz material to make, and helps the area of detection that concentrates and increase fluorescence in the mercury element part, helps to improve the sensitivity of mensuration.
Fig. 3 carries out sequential injection selectivity mercury vapour generation sampling system synoptic diagram in the analytical approach for the present invention utilizes the mercury element morphological analysis means.
A kind of method of utilizing the mercury element morphological analysis means to carry out the mercury element morphological analysis
Described method comprises:
Fig. 3 (A) formic acid medium analysis step: operation four-way valve 1 rotates, and o, a position are communicated, and pumps into formic acid, and pumps into sample from sample pipe 2; Described sample and formic acid converge and enter described photoinduction steam generator 6 in first threeway 5, this moment comprises organic in the test solution and total mercury solution inorganic mercury can produce mercury vapour under UV light-induced, after described gas-liquid separator 9 separated, described mercury vapour was brought into described enrichment pipe 10 by argon gas;
Fig. 3 (B) cleans and testing procedure a: operation four-way valve 1 rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe 10 simultaneously after, enter described detecting device 11 and detect, record the content of total mercury;
Fig. 3 (C) acetic acid medium analytical procedure: operation four-way valve 1 rotates, and o, c position are communicated, and pumps into acetate, and pumps into sample from sample pipe 2; Sample and acetate converge and enter described photoinduction steam generator 6 in first threeway 5, organic mercury optionally produces mercury vapour in the test solution under UV light-induced at this moment, after described gas-liquid separator 9 separated, described mercury vapour was brought into described enrichment pipe 10 by argon gas;
Fig. 3 (D) cleans and testing procedure b: operation four-way valve 1 rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe 10 simultaneously after, enter described detecting device 11 and detect, record organomercurial content.
1 is four-way valve among the figure, a-formic acid inlet, b-filter washing water inlet, c-acetate inlet, o-outlet; The 2nd, sample inlet; The 4th, peristaltic pump; The 5th, first threeway; The 6th, the photoinduction steam generator.
The concentration of described formic acid medium solution is: 0.05-40% (v/v)
The concentration of described acetic acid medium solution is: 0.05-20% (v/v)
Carry out ultraviolet at described photoinduction steam generator and produce in the process of mercury vapour, the time of ultraviolet irradiation is: 5-1200s.

Claims (8)

1 one kinds of mercury element morphological analysis means is characterized in that: comprise that sample introduction parts (2), medium selection enter control assembly, photoinduction steam generator (6), gas-liquid separator (9) and detecting device (11); Described sample introduction parts (2) are selected to enter control assembly with medium and are connected with described photoinduction steam generator (6) one ends, the other end of described photoinduction steam generator (6) is connected with gas-liquid separator (9), detects through the gas input detector (11) behind the gas-liquid separator (9).
2 a kind of mercury element morphological analysis means according to claim 1 is characterized in that: described medium is selected to enter control assembly and is comprised three solution inlet port and a four-way valve (1); Described four-way valve (1) described three solution inlet port of control and a liquid outlet; Described three solution inlet port comprise acetate import, formic acid import and cleaning fluid mouth.
3 a kind of mercury element morphological analysis means according to claim 1, it is characterized in that: described sample introduction parts are selected to enter control assembly with medium and are connected with photoinduction steam generator (6) with first threeway (5) by peristaltic pump (4), promptly by peristaltic pump (4) and first threeway (5) sample and medium solution are delivered in the photoinduction steam generator (6);
In the middle of described photoinduction steam generator (6) and described gas-liquid separator (9), also comprise second threeway (7), and inject argon gas by an inlet (8) of described second threeway (7); The mercuryvapour that promptly passes through described photoinduction steam generator (6) and produce and the argon gas of injection together enter gas-liquid separator (9) and carry out gas-liquid separation;
In the middle of described gas-liquid separator (9) and detecting device (11), also comprise a mercury enrichment pipe (10); Promptly carry out the gas enrichment through the mercury vapour input mercury enrichment pipe (10) after separating.
4 a kind of mercury element morphological analysis means according to claim 1 is characterized in that: described detecting device (11) is taked atomizer (115), fluorescence excitation (113) and fluoroscopic examination (116) integrated apparatus; Comprise detection system shell (111), detection system inner casing (112), fluorescence excitation (113), entrance slit (114), atomizer (115), fluoroscopic examination (116), mercury vapour inlet (117) and mercury vapour outlet (118).
5 a kind of mercury element morphological analysis means according to claim 4, it is characterized in that: described fluorescence excitation (113) is the pen type mercury lamp, and described fluoroscopic examination (116) is a photomultiplier, and described atomizer (115) is an absorption cell; And atomizer (115) adopts the thin flat structure, adopts the quartzy material of hollow; Distance between described pen type mercury lamp (113) and the atomizer (115) is 1-10cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1-10cm.
6 a kind of mercury element morphological analysis means according to claim 5 is characterized in that: the distance between described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
7 analytical approachs as the described mercury element morphological analysis means of one of claim 1-6 is characterized in that:
Described method comprises:
A formic acid medium analysis step: operation four-way valve (1) rotates, and o, a position are communicated, and pumps into formic acid, and pumps into sample from sample pipe (2); Described sample and formic acid converge and enter described photoinduction steam generator (6) in first threeway (5), this moment comprises organic in the test solution and total mercury solution inorganic mercury can produce mercury vapour under UV light-induced, after described gas-liquid separator (9) separated, described mercury vapour was brought into described enrichment pipe (10) by argon gas;
B cleans and testing procedure a: operation four-way valve (1) rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe (10) simultaneously after, enter described detecting device (11) and detect, record the content of total mercury;
C acetic acid medium analytical procedure: operation four-way valve (1) rotates, and o, c position are communicated, and pumps into acetate, and pumps into sample from sample pipe (2); Sample and acetate converge and enter described photoinduction steam generator (6) in first threeway (5), organic mercury optionally produces mercury vapour in the test solution under UV light-induced at this moment, after described gas-liquid separator (9) separated, described mercury vapour was brought into described enrichment pipe (10) by argon gas;
D cleans and testing procedure b: operation four-way valve (1) rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe (10) simultaneously after, enter described detecting device (11) and detect, record organomercurial content.
The analytical approach of 8 mercury element morphological analysis means according to claim 7 is characterized in that:
The concentration of described formic acid medium solution is: 0.05-40% (v/v);
The concentration of described acetic acid medium solution is: 0.05-20% (v/v).
Carry out ultraviolet at described photoinduction steam generator and produce in the process of mercury vapour, the time of ultraviolet irradiation is: 5-1200s.
CN2007101199258A 2007-08-03 2007-08-03 Morphological analysis apparatus for mercury element and analysis method thereof Active CN101358924B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101995439A (en) * 2009-08-12 2011-03-30 中国科学院生态环境研究中心 Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms
CN102445442A (en) * 2010-10-15 2012-05-09 西北有色地质研究院 Intelligent general type mercury measuring device and detection method thereof
CN103499558A (en) * 2013-09-06 2014-01-08 深圳市中兴环境仪器有限公司 System and method for determining mercury concentration in water
CN104769417A (en) * 2012-09-28 2015-07-08 布鲁克斯·兰德公司 Mercury monitoring systems and methods
CN108896519A (en) * 2018-05-21 2018-11-27 南京工程学院 Double spectrum gas mercury analytical equipments and corresponding method

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CN100507570C (en) * 2005-05-27 2009-07-01 清华大学 High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface
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
CN201075087Y (en) * 2007-08-03 2008-06-18 北京路捷仪器有限公司 Device for analyzing quicksilver element form

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101995439A (en) * 2009-08-12 2011-03-30 中国科学院生态环境研究中心 Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms
CN102445442A (en) * 2010-10-15 2012-05-09 西北有色地质研究院 Intelligent general type mercury measuring device and detection method thereof
CN102445442B (en) * 2010-10-15 2013-07-03 西北有色地质研究院 Intelligent general type mercury measuring device and detection method thereof
CN104769417A (en) * 2012-09-28 2015-07-08 布鲁克斯·兰德公司 Mercury monitoring systems and methods
CN104769417B (en) * 2012-09-28 2019-04-09 布鲁克斯·兰德公司 Mercury monitoring system and method
CN103499558A (en) * 2013-09-06 2014-01-08 深圳市中兴环境仪器有限公司 System and method for determining mercury concentration in water
CN108896519A (en) * 2018-05-21 2018-11-27 南京工程学院 Double spectrum gas mercury analytical equipments and corresponding method
CN108896519B (en) * 2018-05-21 2021-04-27 南京工程学院 Double-spectrum flue gas mercury analysis device and corresponding method

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