CN101358924B - Morphological analysis apparatus for mercury element and analysis method thereof - Google Patents
Morphological analysis apparatus for mercury element and analysis method thereof Download PDFInfo
- Publication number
- CN101358924B CN101358924B CN2007101199258A CN200710119925A CN101358924B CN 101358924 B CN101358924 B CN 101358924B CN 2007101199258 A CN2007101199258 A CN 2007101199258A CN 200710119925 A CN200710119925 A CN 200710119925A CN 101358924 B CN101358924 B CN 101358924B
- Authority
- CN
- China
- Prior art keywords
- mercury
- gas
- photoinduction
- atomizer
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 238000004458 analytical method Methods 0.000 title claims description 30
- 230000000877 morphologic effect Effects 0.000 title claims description 23
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 230000005284 excitation Effects 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 229910052753 mercury Inorganic materials 0.000 claims description 90
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 18
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 16
- 235000019253 formic acid Nutrition 0.000 claims description 16
- 238000001514 detection method Methods 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 9
- 230000002572 peristaltic effect Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- 230000008676 import Effects 0.000 claims description 6
- 239000012085 test solution Substances 0.000 claims description 6
- 238000012956 testing procedure Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 238000013459 approach Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- 238000012351 Integrated analysis Methods 0.000 description 1
- JJWSNOOGIUMOEE-UHFFFAOYSA-N Monomethylmercury Chemical compound [Hg]C JJWSNOOGIUMOEE-UHFFFAOYSA-N 0.000 description 1
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 1
- 238000001675 atomic spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001927 high performance liquid chromatography-inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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
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/T5009.17-2003) 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 (4)
1. the method for a mercury element morphological analysis is characterized in that:
The analytical equipment of using in the described method, its structure comprise,
Sample introduction parts, medium select to enter control assembly, photoinduction steam generator (6), gas-liquid separator (9) and detecting device (11);
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;
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 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; Detect through the gas input detector (11) behind the gas-liquid separator (9);
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 method comprises the steps:
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 in first threeway (5) goes forward side by side into photoinduction steam generator (6), this moment comprises organic in the test solution and total mercury solution inorganic mercury can produce mercury vapour under UV light-induced, after gas-liquid separator (9) separated, described mercury vapour was brought into 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 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.
2. the method for mercury element morphological analysis according to claim 1 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.
3. a kind of mercury element morphological analysis method according to claim 1 is characterized in that: described fluorescence excitation (113) is the pen type mercury lamp, and described fluoroscopic examination 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.
4. a kind of mercury element morphological analysis method according to claim 3 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101199258A CN101358924B (en) | 2007-08-03 | 2007-08-03 | Morphological analysis apparatus for mercury element and analysis method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101199258A CN101358924B (en) | 2007-08-03 | 2007-08-03 | Morphological analysis apparatus for mercury element and analysis method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101358924A CN101358924A (en) | 2009-02-04 |
| CN101358924B true CN101358924B (en) | 2011-05-04 |
Family
ID=40331432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101199258A Active CN101358924B (en) | 2007-08-03 | 2007-08-03 | Morphological analysis apparatus for mercury element and analysis method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101358924B (en) |
Families Citing this family (5)
| 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 |
| 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 |
| 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 |
| CN108896519B (en) * | 2018-05-21 | 2021-04-27 | 南京工程学院 | Double-spectrum flue gas mercury analysis device and corresponding method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1700012A (en) * | 2005-05-27 | 2005-11-23 | 清华大学 | High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface |
| CN1737537A (en) * | 2005-07-22 | 2006-02-22 | 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 |
-
2007
- 2007-08-03 CN CN2007101199258A patent/CN101358924B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1700012A (en) * | 2005-05-27 | 2005-11-23 | 清华大学 | High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface |
| CN1737537A (en) * | 2005-07-22 | 2006-02-22 | 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 |
Non-Patent Citations (4)
| Title |
|---|
| JP特开平6-241990A 1994.09.02 |
| Mariana A et al.Determinatino of total mercury and methylmercury in biological samples by photochemical vapor generation.《Annal Bioanal Chem》.2007,第388卷(第4期),837-847. * |
| 梁立娜 等.冷蒸气发生-原子荧光光谱法测定化工废水中的无机汞和总有机汞.《分析化学研究简报》.2001,第29卷(第4期),403-405. |
| 梁立娜等.冷蒸气发生-原子荧光光谱法测定化工废水中的无机汞和总有机汞.《分析化学研究简报》.2001,第29卷(第4期),403-405. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101358924A (en) | 2009-02-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102445442B (en) | Intelligent general type mercury measuring device and detection method thereof | |
| CN101128728B (en) | Apparatus and method for mobile collection of atmospheric sample for chemical analysis | |
| Kallithrakas-Kontos et al. | Recent advances in the analysis of mercury in water-review | |
| Guo et al. | Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches | |
| CN101358924B (en) | Morphological analysis apparatus for mercury element and analysis method thereof | |
| Boring et al. | Field measurement of acid gases and soluble anions in atmospheric particulate matter using a parallel plate wet denuder and an alternating filter-based automated analysis system | |
| Alexovič et al. | An automatic, vigorous-injection assisted dispersive liquid–liquid microextraction technique for stopped-flow spectrophotometric detection of boron | |
| Yang et al. | Sensitive determination of mercury by a miniaturized spectrophotometer after in situ single-drop microextraction | |
| CN101762653B (en) | Method for determining main phenolic compounds in main stream smoke of cigarette | |
| Li et al. | Atomic spectrometric detectors for gas chromatography | |
| CN105590827A (en) | Mass spectrum low-temperature enrichment high-temperature thermal analysis sweeping type membrane sample feeding apparatus and application | |
| Nascimento et al. | Spectrofluorimetric determination of bisphenol A in tap waters by exploiting liquid-liquid microextraction in a sequential injection system | |
| Borowska et al. | Sensitive determination of bioaccessible mercury in complex matrix samples by combined photochemical vapor generation and solid phase microextraction coupled with microwave induced plasma optical emission spectrometry | |
| Yu et al. | Development of a miniature analytical system in a lab-on-valve for determination of trace copper by bead injection spectroscopy | |
| CN102749411A (en) | Determination method for acrylamide in main stream smoke of cigarette | |
| CN104977420B (en) | A kind of water quality analytical system | |
| CN100538354C (en) | A kind of method that detects estrogen active contribution in the sewage | |
| CN201141856Y (en) | Coupling system for detecting organo-tin compound | |
| CN201075087Y (en) | Device for analyzing quicksilver element form | |
| CN101482545A (en) | Measuring method for OH free radical in low-temperature plasma degradation organic waste gas | |
| CN101995439A (en) | Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms | |
| CN105136931A (en) | Method for determining polyaromatic hydrocarbons in smokeless tobacco product by utilization of on-line solid phase extraction high performance liquid chromatography | |
| CN101650350A (en) | Instrument coupled speciation measuring method of gaseous arsenic compound | |
| CN202599841U (en) | Sampling device of atomic fluorescence instrument | |
| CN203216848U (en) | Sample injection device of atomic fluorescence spectrometer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: BEIJING RUIGUANG INSTRUMENT CO., LTD. Free format text: FORMER NAME: BEIJING LWL INSTRUMENT CO., LTD. |
|
| CP03 | Change of name, title or address |
Address after: 100015, M5 building, 5 floors, workshop of Seven Star Huadian Industrial Park, No. 1, Jiuxianqiao East Road, Beijing, Chaoyang District Patentee after: Beijing Ruiguang Instrument Co.,Ltd. Address before: 100016, M5 building, No. 1 East Jiuxianqiao Road, Beijing, Chaoyang District Patentee before: BEIJING LWL INSTRUMENT Co.,Ltd. |
|
| ASS | Succession or assignment of patent right |
Owner name: BEIJING BOHUI INNOVATION TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: BEIJING RUIGUANG INSTRUMENT CO., LTD. Effective date: 20141021 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100015 CHAOYANG, BEIJING TO: 102206 CHANGPING, BEIJING |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20141021 Address after: 102206 No. 9 middle road, Changping District life science and Technology Park, Beijing Patentee after: BEIJING BOHUI INNOVATION TECHNOLOGY Co.,Ltd. Address before: 100015, M5 building, 5 floors, workshop of Seven Star Huadian Industrial Park, No. 1, Jiuxianqiao East Road, Beijing, Chaoyang District Patentee before: Beijing Ruiguang Instrument Co.,Ltd. |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 102206 9 life Garden Road, Changping District, Beijing Patentee after: BEIJING BOHUI INNOVATION BIOTECHNOLOGY Co.,Ltd. Address before: 102206 No. 9 middle road, life science and Technology Park, Changping District, Beijing Patentee before: BEIJING BOHUI INNOVATION TECHNOLOGY Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 102206 9 life Garden Road, Changping District, Beijing Patentee after: Beijing Bohui innovative biotechnology group Co.,Ltd. Address before: 102206 9 life Garden Road, Changping District, Beijing Patentee before: BEIJING BOHUI INNOVATION BIOTECHNOLOGY Co.,Ltd. |