CN106644994A - Method for detecting inorganic mercury and organic mercury in water by solid-phase extraction-mercury analyzer - Google Patents
Method for detecting inorganic mercury and organic mercury in water by solid-phase extraction-mercury analyzer Download PDFInfo
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- CN106644994A CN106644994A CN201611192721.2A CN201611192721A CN106644994A CN 106644994 A CN106644994 A CN 106644994A CN 201611192721 A CN201611192721 A CN 201611192721A CN 106644994 A CN106644994 A CN 106644994A
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007790 solid phase Substances 0.000 title claims abstract description 10
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 21
- 239000000523 sample Substances 0.000 claims description 19
- 229910000497 Amalgam Inorganic materials 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 239000012086 standard solution Substances 0.000 claims description 9
- 239000012224 working solution Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 239000010931 gold Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 229960002523 mercuric chloride Drugs 0.000 claims description 6
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 claims description 6
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000002835 absorbance Methods 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- 238000007233 catalytic pyrolysis Methods 0.000 claims description 3
- 238000007405 data analysis Methods 0.000 claims description 3
- 238000010812 external standard method Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 230000008033 biological extinction Effects 0.000 claims 1
- 239000003643 water by type Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 230000000877 morphologic effect Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000003786 sclera Anatomy 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for detecting inorganic mercury and organic mercury in water by a solid-phase extraction-mercury analyzer and belongs to the technical field of environment detection. The method comprises the following steps: 1) regulating the pH (Potential of Hydrogen) of a water sample; 2) after adjusting the pH, carrying out solid-phase extraction and enrichment on the water sample; 3) detecting by utilizing a mercury analyzer; and 4) analyzing a result. The method for detecting inorganic mercury and organic mercury in water by the solid-phase extraction-mercury analyzer is simple, convenient and rapid to operate, high in sensitivity and good in selectivity; the use amount of an organic solvent is less, and a toxic reagent is not used; and the sensitivity and the selectivity on mercury with different shapes can still keep a relatively good level. The quality accuracy of inorganic mercury and organic mercury is smaller than 0.1ppb, the detection limit is 0.01mu g/L-10mu g/L, and the fortified recovery is 90%-100%.
Description
Technical field
The present invention relates to technical field of environmental detection, the inorganic mercury being specifically related in Solid-Phase Extraction-mercury vapourmeter detection water
With organomercurial method.
Background technology
The whole world is every year because human production activity gives off to obtain the most of burning from coal and other fuel of hydrargyrum.Hydrargyrum is with more
Plant form to be distributed widely in nature, including organic mercury and inorganic mercury.Organic mercury because with lipotropy and biological amplification,
Toxicity is more than inorganic mercury.Only hydrargyrum total concentration is inadequate in determination sample, in addition it is also necessary to distinguish organic mercury and inorganic mercury, therefore hydrargyrum
Morphological analyses it is significant in environmental science.
For assay method, the morphological analyses of hydrargyrum determine much more difficult than the total amount of hydrargyrum, need to be rich by high efficiency separation
Collection technology is in combination with high-sensitivity detecting method.At present, mercury morphological analysis be mostly first with the methods such as chromatograph separation after use again
It is measured with the selective detection meanss of element.Such as by gas chromatogram, the separation means such as liquid chromatograph, capillary electrophoresis with
The determination techniques such as atomic absorption spectrum, atomic emission spectrum, atomic fluorescence spectrophotometry, inductivity coupled plasma mass spectrometry combine.
These methods have good selectivity and higher sensitivity to the hydrargyrum of different shape, but need to consume in continuous mode and have in a large number
Machine solvent and poisonous chemical reagent, and under normal circumstances instrument of the separation means in combination with detection technique costly, greatly
It is big to increase testing cost.
Inorganic mercury and organic mercury method are that have choosing to organic mercury using adsorption stuffing in Solid-Phase Extraction-mercury vapourmeter detection water
Selecting property is adsorbed, and the separation for realizing organic mercury and inorganic mercury is not adsorbed to inorganic mercury, then again by the organic mercury and nothing after separation
Mercury content is determined in machine hydrargyrum injection mercury vapourmeter, the method is easy to operate, and organic reagent usage amount is few, and avoids toxic reagent
Use, and sensitivity and to preferable level still can be preserved on the selectivity of mercury species.At present the country there is no to solid phase
The research of extraction-mercury vapourmeter method.
The content of the invention
For the problem that prior art is present, it is an object of the invention to provide a kind of quick, easy, sensitivity height, choosing
Inorganic mercury and organomercurial method in the good Solid-Phase Extraction of selecting property-mercury vapourmeter detection water.
To solve above-mentioned technical problem, the technical solution adopted in the present invention is：
Inorganic mercury and organomercurial method in Solid-Phase Extraction-mercury vapourmeter method detection water, comprise the following steps：
1) pH regulator of water sample：50mL water samples are measured, nitric acid adjustment pH to 2-5 is added；
2) the solid phase extraction concentration concentration of water sample after pH is adjusted：Respectively with 5mL methanol and 10mL deionized water activated solids
Extraction column, flow velocity is 5-10mL/min, and the water sample that pH is adjusted to 2-5 after activation passes through solid-phase extraction column with 3-5mL/min flow velocitys,
Collect effluent A to be measured；Then solid-phase extraction column 30min is dried, finally with 5m methanol-eluted fractions solid-phase extraction columns, flow velocity is 3mL/
Min, collects eluent B to be measured；
3) detected using mercury vapourmeter：
A. the preparation of standard solution：Mercuric chloride is accurately weighed, using deionized water dissolving, the standard storage of 0.2mg/mL is made into
Standby solution or directly buy it is commercially available have card standard solution, deionized water is diluted to standard working solution when using；
B. using mercury vapourmeter examination criteria working solution and sample solution：The standard solution of 200uL or sample solution are added
Quartz specimen boat, sample enters catalytic pyrolysis furnace, and each identical hydrargyrum is reduced to Elemental Mercury, by gold amalgam selective absorption, blender
Fast heating, the hydrargyrum desorbing that amalgam is adsorbed forms mercury vapour, into Clod Vapour Atomic Absorption spectrogrph, under 253.7nm it is determined
Absorbance；
4) data analysiss：As abscissa, sample absorbance is vertical coordinate to mass concentration X with standard working solution, draws mark
Quasi- working curve, quantified by external standard method is carried out with standard working curve to sample.
Further, in such scheme, nitric acid used is electronic pure nitric acid in the step 1.
Further, in such scheme, solid-phase extraction column used is sulfydryl SPE pillars in the step 2, and specification is
6cc/500mg。
Further, in such scheme, the mercuric chloride in the step 3 is top pure grade.
Further, in such scheme, mercury vapourmeter analysis condition in the step 3：Baking temperature：200 DEG C, when being dried
Between：10s, decomposition temperature：700 DEG C, the resolving time：140s, catalytic temperature：600 DEG C, gold amalgam Hybrid Heating temperature：900 DEG C,
The gold amalgam Hybrid Heating time：12s.
The invention has the beneficial effects as follows：
Inorganic mercury and organomercurial method in the Solid-Phase Extraction of the present invention-mercury vapourmeter detection water, easy to operate, quick, spirit
Sensitivity is high, selectivity is good, and organic reagent usage amount is few, and avoids the use of toxic reagent, and sensitivity and to different shape
But preferable level still can be preserved on the selectivity of hydrargyrum.The present invention is less than to inorganic mercury and organomercurial mass accuracy
0.1ppb, detection is limited to 0.01-10ug/L, and TIANZHU XINGNAO Capsul is 90%-100%.
Description of the drawings
Fig. 1 is sclera remodeling standard curve；
Fig. 2 is mercury vapourmeter Elevated Temperature Conditions.
Specific embodiment
Inorganic mercury and organomercurial method in Solid-Phase Extraction-mercury vapourmeter method detection water, comprise the following steps：
1) pH regulator of water sample：50mL water samples are measured, nitric acid adjustment pH to 2-5 is added, nitric acid used is electronic pure nitric acid；
2) the solid phase extraction concentration concentration of water sample after pH is adjusted：Respectively with 5mL methanol and 10mL deionized water activated solids
Extraction column, flow velocity is 5mL/min, and solid-phase extraction column used is sulfydryl SPE pillars, and specification is 6cc/500mg；By pH after activation
The water sample for being adjusted to 5 passes through solid-phase extraction column with 3mL/min flow velocitys, collects effluent A to be measured；Then it is dried solid-phase extraction column
30min, finally with 5m methanol-eluted fractions solid-phase extraction columns, flow velocity is 3mL/min, collects eluent B to be measured；
3) detected using mercury vapourmeter：
A. the preparation of standard solution：Mercuric chloride is accurately weighed, the mercuric chloride is top pure grade, using deionized water dissolving, is matched somebody with somebody
Into 0.2mg/mL Standard Stock solutions or directly buy it is commercially available have card standard solution, deionized water is diluted to mark when using
Quasi- working solution；
B. using mercury vapourmeter examination criteria working solution and sample solution：The standard solution of 200uL or sample solution are added
Quartz specimen boat, sample enters catalytic pyrolysis furnace, and each identical hydrargyrum is reduced to Elemental Mercury, by gold amalgam selective absorption, blender
Fast heating, the hydrargyrum desorbing that amalgam is adsorbed forms mercury vapour, into Clod Vapour Atomic Absorption spectrogrph, under 253.7nm it is determined
Absorbance；Wherein, mercury vapourmeter analysis condition is：Baking temperature：200 DEG C, drying time：10s, decomposition temperature：700 DEG C, decompose
Time：140s, catalytic temperature：600 DEG C, gold amalgam Hybrid Heating temperature：900 DEG C, the gold amalgam Hybrid Heating time：12s, specifically
See Fig. 2；
4) data analysiss：As abscissa, sample absorbance is vertical coordinate to mass concentration X with standard working solution, draws mark
Quasi- working curve, with standard working curve quantified by external standard method is carried out to sample, and specific standards curve is shown in Fig. 1.In wherein effluent A
Hydrargyrum concentration is inorganic mercury concentration, and hydrargyrum concentration is organic mercury concentration by multiple correction in eluent B.
Finally it should be noted that：Above example only to illustrate technical scheme, rather than a limitation；Although
The present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To modify to the technical scheme described in previous embodiment, or equivalent is carried out to which part technical characteristic；And
These modifications are replaced, and do not make the spirit and model of the essence disengaging embodiment of the present invention technical scheme of appropriate technical solution
Enclose.
Claims (4)
1. Solid-Phase Extraction-mercury vapourmeter method detects inorganic mercury and organomercurial method in water, it is characterised in that comprise the following steps：
1) pH regulator of water sample：50mL water samples are measured, nitric acid adjustment pH to 2-5 is added.
2) the solid phase extraction concentration concentration of water sample after pH is adjusted：Extracted with 5mL methanol and 10mL deionized waters activated solid respectively
Post, flow velocity is 5-10mL/mi, and the water sample that pH is adjusted to 2-5 after activation passes through solid-phase extraction column with 3-5mL/min flow velocitys, collects
Effluent A is to be measured；Then solid-phase extraction column 30min is dried, finally with 5m methanol-eluted fractions solid-phase extraction columns, flow velocity is 3mL/min,
Collect eluent B to be measured.
3) detected using mercury vapourmeter：
A. the preparation of standard solution：Mercuric chloride is accurately weighed, using deionized water dissolving, the standard inventory for being made into 0.2mg/mL is molten
Liquid or directly buy it is commercially available have card standard solution, deionized water is diluted to mark standard working solution when using.
B. using mercury vapourmeter examination criteria working solution and sample solution：The standard solution of 200uL or sample solution are added into quartz
Example boat, sample enters catalytic pyrolysis furnace, and each identical hydrargyrum is reduced to Elemental Mercury, and by gold amalgam selective absorption, blender is quick
Heating, the hydrargyrum desorbing that amalgam is adsorbed forms mercury vapour, into Clod Vapour Atomic Absorption spectrogrph, its extinction is determined under 253.7nm
Degree.
4) data analysiss：As abscissa, sample absorbance is vertical mark to mass concentration X with standard working solution, draws standard work
Curve, quantified by external standard method is carried out with standard working curve to sample.
2. Solid-Phase Extraction according to claim 1-mercury vapourmeter detects the inorganic mercury and organomercurial method in water, its feature
It is that nitric acid used is electronic pure nitric acid in the step 1.
3. Solid-Phase Extraction according to claim 1-mercury vapourmeter detects the inorganic mercury and organomercurial method in water, its feature
It is that solid-phase extraction column used is sulfydryl SPE pillars in the step 3, and specification is 6cc/500mg.
4. Solid-Phase Extraction according to claim 1-mercury vapourmeter detects the inorganic mercury and organomercurial method in water, its feature
It is that the mercuric chloride in the step 3 is top pure grade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611192721.2A CN106644994A (en) | 2016-12-21 | 2016-12-21 | Method for detecting inorganic mercury and organic mercury in water by solid-phase extraction-mercury analyzer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611192721.2A CN106644994A (en) | 2016-12-21 | 2016-12-21 | Method for detecting inorganic mercury and organic mercury in water by solid-phase extraction-mercury analyzer |
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Family
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| CN201611192721.2A Pending CN106644994A (en) | 2016-12-21 | 2016-12-21 | Method for detecting inorganic mercury and organic mercury in water by solid-phase extraction-mercury analyzer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107505308A (en) * | 2017-08-11 | 2017-12-22 | 深圳市九五至尊珠宝有限公司 | A kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium |
| CN108181445A (en) * | 2018-01-02 | 2018-06-19 | 江苏中宜金大分析检测有限公司 | A kind of method for measuring mercury in soils content |
| CN112665933A (en) * | 2020-12-04 | 2021-04-16 | 安徽大学 | Pretreatment method for mercury isotope determination of environmental sample |
| CN114236072A (en) * | 2021-12-06 | 2022-03-25 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Method for rapidly determining mercury form in water |
| CN114236072B (en) * | 2021-12-06 | 2024-06-11 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Method for rapidly determining mercury form in water |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107505308A (en) * | 2017-08-11 | 2017-12-22 | 深圳市九五至尊珠宝有限公司 | A kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium |
| CN108181445A (en) * | 2018-01-02 | 2018-06-19 | 江苏中宜金大分析检测有限公司 | A kind of method for measuring mercury in soils content |
| CN112665933A (en) * | 2020-12-04 | 2021-04-16 | 安徽大学 | Pretreatment method for mercury isotope determination of environmental sample |
| CN114236072A (en) * | 2021-12-06 | 2022-03-25 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Method for rapidly determining mercury form in water |
| CN114236072B (en) * | 2021-12-06 | 2024-06-11 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Method for rapidly determining mercury form in water |
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