CN105466737A - Passive sampler for gaseous polycyclic aromatic hydrocarbon in root box experiment and sample determining method thereof - Google Patents
Passive sampler for gaseous polycyclic aromatic hydrocarbon in root box experiment and sample determining method thereof Download PDFInfo
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- CN105466737A CN105466737A CN201511010215.2A CN201511010215A CN105466737A CN 105466737 A CN105466737 A CN 105466737A CN 201511010215 A CN201511010215 A CN 201511010215A CN 105466737 A CN105466737 A CN 105466737A
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- 238000002474 experimental method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 27
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- 230000004913 activation Effects 0.000 claims description 3
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- 230000008901 benefit Effects 0.000 description 2
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- 150000001875 compounds Chemical class 0.000 description 2
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- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 229920008128 Ameripol Polymers 0.000 description 1
- 241001589086 Bellapiscis medius Species 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
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- 238000013508 migration Methods 0.000 description 1
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- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/26—Devices for withdrawing samples in the gaseous state with provision for intake from several spaces
-
- G01N30/482—
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
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- Engineering & Computer Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a passive sampler for gaseous polycyclic aromatic hydrocarbon in a root box experiment. The passive sampler comprises a root box and a plurality of gas collectors, wherein the gas collectors are used for collecting the gases on different positions in the root box; SPE solid phase extraction column tubes with volume being 5-10ml are taken as the gas collectors; granular XAD-2 resins are contained in the gas collectors as the absorbents; the absorbents are characterized by having grain size of 20-60 meshes, superficial areas of more than or equal to 430m<2>/g and moisture content of 20%-45%; the dosage of the absorbents is 1.0g per gas collector. The invention also discloses a sample determining method for the passive sampler for the gaseous polycyclic aromatic hydrocarbon in the root box experiment. The passive sampler provided by the invention is simple in manufacturing and assembling and low in cost; the absorbents need not be separated from the gas collectors; the extraction for the polycyclic aromatic hydrocarbon can be finished by directly eluting, so that the usage of the organic solvent is greatly reduced and the analysis time is shortened, and meanwhile, the PAHs loss in the sample collection and transferring process is also reduced; the sampling rate is greatly increased; the passive sampler is fit for the passive sampling for the gaseous polycyclic aromatic hydrocarbon in the outdoor experimental root box or outdoor experiment.
Description
Technical field
The present invention relates to sampling and the determination techniques field of palycyclic aromatic, particularly gaseous PAHs Passive sampler and sampling determination method thereof in a kind of root case experiment.
Background technology
Palycyclic aromatic (PAHs) is a kind of important persistence organic pollutant (POPs) in air, be mainly derived from the human activities such as commercial production, organic matter pyrolysis or rough burning product to produce and discharge, such as incineration of waste, the flue gas of chemical fuel rough burning generation and the draw-off of vehicle exhaust, petrochemical industry and gasworks etc.Palycyclic aromatic (PAHs) is as a class combustion by-products, distribute in the environment quite extensive, wherein some have been proved to be has carcinogenic, the effect such as teratogenesis and mutagenesis, they not only cause very large pollution to environment, and suck this kind of hazardous contaminant for a long time and the food eaten by this kind of Substances Pollution, very large harm can be caused to health.This Chronic exposure palycyclic aromatic has carcinogenic effect.Therefore, accurately understand palycyclic aromatic levels in an atmosphere and seem most important.In research air, a fundamental of polycyclic aromatic hydrocarbon content is exactly the gas sampling assembly of palycyclic aromatic.Up to the present, a large amount of report has been shown in the research for the air PAHs of China's different cities point, but due to the restriction of Sampling techniques, these researchs are main pays close attention to single city point, region on a large scale in research also little.Current palycyclic aromatic (PAHs) although research comparative maturity, the PAHs research in air, water body, seashells, lake sediment and soil has report, and initiatively sampling and passiveness sampling method all have employing.Because initiatively sampling needs the supply of power, so in the place not having electricity supply, select passive sampling just relatively good.
Air is the main path of half volatile organic contaminant diffusion and migration, and along with becoming increasingly conspicuous of globalised environmental pollution problem, region on a large scale interior air pollution analysis research starts the great attention causing vast researcher.The monitoring of Atmospheric Organic Pollutants mainly comprises initiatively sampling and passive sampling technology.In air, POPs concentration changes along with pollutant source of release intensity, temperature and other environment meteorological factors.Such as rain, snowing to make pollutant levels in air reduce; Atmospheric air mass moves to sampling position from pollution source can make pollutant accumulate, and concentration improves.Initiatively sampling only can provide instantaneous sampling point pollutants in air concentration, and passive sampling can detect a period of time pollutants in air concentration.Accordingly, initiatively sampling can be used for evaluating the situation of pollutant levels with meteorological condition or source of release Strength Changes, and passive sampling can be used for the situation of change of detection of contamination concentration in a certain period.
In air, the monitoring of organic contaminant has the method for initiatively sampling and passive sampling.What current active sampling application was more is volumes of air sampling instrument, and this sampling thief has history for many years for monitoring POPs in air.These systems make air by filter membrane collecting granules thing by sampling pump, collect gaseous substance by absorbing agent trap.Existing problem mainly comprises: volatile matter is from the surface particles volatilization collected by filter membrane, and gleanings is through absorbing agent trap, and in gas phase, compounds adsorb is in filter membrane.In addition, the cost that employing volumes of air sampling instrument carries out air active sampling is higher, needs the moment of power supply (power) and scientific research personnel to guard, is not suitable for field and samples for a long time on a large scale.The active sampling thief that another kind is used less is anemostat air sampler, it is a kind of low flow velocity sampling thief, it has the gaseous substance above an anemostat de-entrainment filter, recent research finds to adopt this sampling thief monitoring PAHs, large about 2 times of the result that in the particle obtained, PAHs concentration ratio traditional sampling method records.
Passive air sampling technology can make up the defect that tradition is initiatively sampled, have that sampler structure is simple, cheap, volume is little, lightweight, easy to carry, without the need to features such as power supply and special maintenances, the multi-point being applicable to very much POPs air sample gathers simultaneously, therefore this technology had both been adapted to the POPs air quality monitoring of small scale, microenvironment (as indoor environment, occupational exposure environment and community environment etc.), be applicable to large scale, regionality again, so the international co-operation study on monitoring of global air POPs.Totally see, the shortcoming of Passive sampler is that sample rate is relatively slow, needs the longer time to gather low concentration POPs in environment.But from other angle, this is its advantage just also, and it can reflect the time-weighted mean concentration of POPs.5 kinds of main passive air sampling devices (PAS:Passiveairsampler) of current application: semi-permeable diaphragm Passive sampler (SPMD-PAS:Semipermeablemembranedevice), isocyanurate foam video disc Passive sampler (PUF-PAS:Polyurethanefoamdisk), XAD-2 resin Passive sampler (XAD-2PAS:ResinXAD-2, styrene-divinylbenzenecopolymer), membrane closure absorbing coating Passive sampler (MESCOs-PAS:Membrane-enclosedsorptivecoatings), it comprises the stirring rod (stirbar of polymer-coated, " Twister ") and silication ameripol rod (siliconeelastomerrod) two type, and the PUF video disc Passive sampler (SIP-PAS:Sorbentimpregnatedpolyurethane) of up-to-date XAD-4 resin-dipping.
The passive sampling technology gathering organic contaminant in air in recent years obtains in the world shows great attention to.The research that passive sampling technology is used for Atmospheric Organic Pollutants has more than ten years history, and relevant patent and article also have a lot.In the passive sampling technology of external organic contaminant, patent KR20140010697A discloses the Passive sampler of a kind of organic contaminant or semi-volatile organic matter, and the filler of the inside is isocyanurate foam and glass fibre video disc; Patent JP2012026954 (A) discloses a kind of not by the stable passive air sampling device of the impact of wind speed; Patent JP2011169787 (A) disclose a kind of calibrate with active Sampling techniques combine be captured in the organic efficient passive gas samplers such as nicotine in tobacco smoke, the inside has used polystyrene and dimethyl silicone polymer as adsorbent; Patent CA2669901 (C) discloses a kind of multi-functional Passive sampler, and this sampling thief can collect multiple pollutant in air, as volatile organic contaminant (volatileorganiccompounds, VOC), aldehydes and ketone, NH
3, NO
2, H
2s, SO
2deng; Patent US2002148355 (A1) discloses a kind of Passive sampler can easily adsorbent transferred in detector tube, facilitates the carrying out of follow-up work.
Although domestic relevant report is less, but due to more and more higher for atmosphere polluting problem attention rate, the domestic existing patent about organic pollutant passiveness sampling method or adsorbent in air at present, as patent 201210172065.5, disclose the Passive sampler of persistent organism in a kind of air, this invention top cover is provided with low-density polyethylene film.Patent of invention 201210160706.5 discloses a kind of for gathering the sorbing material of persistence organic pollutant in ambient atmosphere (POPs), and this sorbing material is the isocyanurate foam of absorption XAD-2 resin; Patent CN2485644Y discloses a kind of passive atmospheric organic contaminant sampling thief for dry wet granular phase organic contaminant, relies on propagation in atmosphere and rainfall passive sampling; Patent 201110360613.2 discloses a kind of atmospheric detection system and the detection method that are suitable for onsite application, comprises the passive atmospheric sampling thief and portable spectrophotometer that split; Patent 201210554591.8 relate to a kind of can timing passive type air sampler; Patent 201310356702.9 discloses two kinds of passive type air samplers, two kinds of sampling thiefs are in gas transport, by the gap that adsorption cover is connected with main adsorption box, or the part pollutant that the gap be connected with base by adsorption cover enters into Passive sampler inside by additional adsorbent adsorption cleaning, thus can reduce the contaminated degree of passive sample devices to a great extent; Patent 201220118062.9 discloses a kind of passive air sampling rig gathering half volatile organic contaminant in air.
As can be seen from above data, passive air sampling technology is applied a lot really, but also there are a lot of report and research to show, passive air sampling device particularly result not all satisfactory after long-time running a period of time in actual operating state, occurred a lot of problems, these problems all have to be solved.Wherein mainly comprise: no matter be domestic or external technology, no matter the function whether expanded, passive air sampling device has complex structure, make, complex operation expensive with transportation cost and the deficiency grown analysis time.
Summary of the invention
Technical matters to be solved by this invention overcomes the deficiencies in the prior art and provides gaseous PAHs Passive sampler and sampling determination method thereof in the experiment of a kind of root case, the actual needs that the present invention be directed to gaseous PAHs concentration determination in palycyclic aromatic in current air or the experiment of root case designs, and has light, easy to operate and cheap advantage.
The present invention is for solving the problems of the technologies described above by the following technical solutions:
According to gaseous PAHs Passive sampler in a kind of root case experiment of the present invention, comprise root case and some gas collector, described gas collector is suspended on the diverse location in root case and the gas for gathering diverse location place in root case, the SPE Solid-Phase Extraction column jecket of described gas collector to be volume be 5 ~ 10mL, described gas collector built with graininess XAD-2 resin as adsorbent, the particle diameter of adsorbent is 20 ~ 60 orders, surface area>=430m
2/ g, water percentage is 20% ~ 45%, and in each gas collector, adsorbent is 1.0g, and described case is provided with lid, and lid is provided with the circular hole being used for fixing gas collector.
As the further prioritization scheme of gaseous PAHs Passive sampler in a kind of root case experiment of the present invention, described gas collector is colourless SPE Solid-Phase Extraction column jecket, and its diameter is 1 ~ 2cm, is highly 6 ~ 7cm, when gas collector hangs in root case, column jecket osculum upwards.
As the further prioritization scheme of gaseous PAHs Passive sampler in a kind of root case experiment of the present invention, described gas collector comprises adsorbent, two panels porous Teflon pad; Wherein, adsorbent is arranged between two panels porous Teflon pad, a slice porous Teflon pad is arranged on 2cm place bottom distance SPE Solid-Phase Extraction column jecket, and another sheet porous Teflon pad is arranged on the sorbent, and adsorbent is arranged on the centre of SPE Solid-Phase Extraction column jecket.
As the further prioritization scheme of gaseous PAHs Passive sampler in a kind of root case experiment of the present invention, the height of described case is 90 ~ 100cm.
A sampling determination method for gaseous PAHs Passive sampler in the experiment of piece case, comprises the following steps:
I) pre-service of adsorbent:
Before sampling starts, adsorbent is used methylene chloride and the normal hexane mixed liquor static rinse 15min at 150 DEG C that chromatographically pure volume ratio is 1:1, circulate 3 times; Then at 150 DEG C, clean 15min with acetonitrile, circulate 3 times; Dry up rear masking foil with nitrogen again to package rear sealing and be stored in the baking oven of 50 DEG C stand-by; First after 1 ~ 2 hour with alcohol immersion activation, after nitrogen dries up, add high performance liquid chromatography water, make its water cut reach 20% before using;
Ii) sampling process:
Step I being housed) adsorbent after cleaning takes 1g and moves into SPE teflon gasket being housed one end and extract in void column pipe, then another sheet teflon gasket is adopted adsorbent to be fixed on the centre of SPE extraction void column pipe, obtain gas collector, gas collector is connected with the circular hole on the lid of root case by cord, and hang in root case, the adsorbent surface in each gas collector is kept to flush, start to carry out collection timing to the palycyclic aromatic in gas phase in root case simultaneously, the sample duration of Passive sampler is t, after sampling terminates, gas collector two ends are sealed, stand-by at being stored in-20 DEG C,
Iii) in adsorbent, the wash-out of palycyclic aromatic extracts:
By step I i) sampled after gas collector in adsorbent 15mL methylene chloride and acetone by volume 1:1 carry out SPE wash-out, elution speed controls at 1mL/ minute, recycling elution 3 times, eluent concentrates through rotary evaporation in vacuo, it is 40 DEG C that temperature controls, after nitrogen blows and is concentrated into 0.6 ~ 1.0mL, concentrate is moved into decontaminating column, the upper strata of decontaminating column is 1g anhydrous sodium sulfate, the lower floor of decontaminating column is 0.5g silica gel, be that the normal hexane of 1:1 and methylene chloride mixed liquor carry out wash-out by the volume ratio of 15mL again, eluent is collected in pear shape bottle, finally concentrate with Rotary Evaporators, be settled to 1mL with acetonitrile and be placed in 2mL analysis bottle, to be determined at being stored in-20 DEG C,
Iv) hplc determination process:
Testing tool is high performance liquid chromatograph HPLC, HPLC condition: chromatographic column is AgilentZORBAXEclipseXDB-C18,4.6*250mm, thickness of liquid film 5 μm, fluorescence detector FLD, mobile phase is acetonitrile and water, and starting condition is be the acetonitrile of 6:4 by volume: water, then in 60min with 0.75mL/min linear elution to 100% acetonitrile; Determined wavelength: carry out time programming with FLD signal, 0 ~ 9 minute: Ex λ=260nm, Em λ=380nm; 9 ~ 16 minutes: Ex λ=260nm, Em λ=340nm; 16 ~ 18 minutes: Ex λ=260nm, Em λ=380nm; 18 ~ 21 minutes: Ex λ=260nm, Em λ=380nm; 21 ~ 23 minutes: Ex λ=289nm, Em λ=462nm; 23 ~ 30 minutes: Ex λ=320nm, Em λ=380nm; 30 ~ 36 minutes: Ex λ=266nm, Em λ=403nm; 36 ~ 52 minutes: Ex λ=294nm, Em λ=430nm; 52 minutes: Ex λ=290nm, Em λ=500nm; In the eluent recorded, PAHs concentration is changed and is set as mass M
g,i;
V) the determination of Passive sampler sampling rate R:
The concentration adopting initiatively sampling thief to record each palycyclic aromatic in the outdoor root case experiment in same place is C
a,i, the mass M of PAHs in the eluent obtained v) is analyzed according to step I
g,i, calculate Passive sampler by formula (1) and to sample the equivalent air volume Veq obtained:
Veq=M
g,i/C
a,i（1）
Wherein: Veq is that Passive sampler is sampled the equivalent air volume obtained, and unit is m
3;
M
g,ifor Passive sampler is sampled the quality of the i-th kind of PAHs obtained, unit is ng;
C
a,ifor the concentration of i-th kind of PAHs that active sampler samples obtains, unit is ng/m
3;
According to the drafting Veq value that the different sampling stages calculated obtains, draw Veq-t scatter diagram, line linearity matching of going forward side by side, according to the sampling rate R of fit line slope determination Passive sampler, unit is m
3/ day;
Vi) the concentration of palycyclic aromatic is calculated:
The mean concentration C of each palycyclic aromatic in root case gas
g,icalculated by formula (2):
C
g,i=24×M
g,i/（R×t）（2）
Wherein: C
g,ifor Passive sampler is sampled the mean concentration of the i-th kind of PAHs obtained, unit is ng/m
3;
M
g,ifor Passive sampler is sampled the quality of the i-th kind of PAHs obtained, unit is ng;
R is the sampling rate of Passive sampler, by v) initiatively sampling thief correct and determine, unit is m
3/ day;
T is the sampling time of Passive sampler, and unit is h.
As the further prioritization scheme of sampling determination method of palycyclic aromatic Passive sampler in a kind of case experiment of the present invention, the described step I ii) temperature of middle evaporimeter controls to be 40 DEG C.
The present invention adopts above technical scheme compared with prior art, has following technique effect:
(1) compared with the present invention is the Passive sampler of adsorbing medium with PUF conventional at present, the graininess XAD-2 resin adopting specific surface area larger is adsorbent, its volume is little, cleaning is simple, have result of study to show, XAD-2PAS is little by air speed influence, all more stable in larger temperature range, for more than 1 year sampling period, POPs class material is still in the linear absorption stage; And the extraction of palycyclic aromatic in adsorbent only need by wash-out, purified, greatly reduce the use of organic solvent and shorten analysis time;
(2) the present invention and at present conventional complex structure, makes with transportation cost more expensive, the XAD-2PAS of trivial operations compares, Passive sampler making of the present invention and operate easier, and price is more cheap;
(3) the present invention is compared with traditional XAD-2PAS, and adsorbent need not shift from sampling thief by the extraction process of PAHs, directly can carry out Solid-Phase Extraction, simplify leaching process and decrease this process PAHs loss, there is novelty; And resin of the present invention does not fill up sampling thief completely, with two panels porous Teflon pad for supporting, adsorbent is placed between two parties in SPE Solid-Phase Extraction column jecket, gas area of passage is large, sample rate is fast, substantially increase sampling rate, calibrate with active sampling thief and combine, be suitable for the sampling of palycyclic aromatic in outdoor root case experiment root case;
(4) Passive sampler of the present invention makes, assembles simply, and sampling thief (comprising sampling bottle and root case) general assembly (TW) is no more than 500g, only need be suspended in the root case of certain altitude, be suitable for the passive sampling of the palycyclic aromatic of differing heights in root case;
(5) the present invention is by the passive sampling of 30 days test, and result of calculation shows that this novel Passive sampler can be suitable for the monitoring of gaseous state PAHs in air, and along with the prolongation in sampling time, test result is more stable, has good application prospect.
Accompanying drawing explanation
Fig. 1 is palycyclic aromatic passive sampling system schematic in of the present invention case experiment.
Fig. 2 is the structural representation of gas collector in Passive sampler of the present invention.
Fig. 3 palycyclic aromatic mixed sample goes out peak figure on HPLC.
Reference numeral in figure is interpreted as: 1-circular hole, 2-root case, 3-gas collector, 4-bucket, 5-SPE extractor, 6-pear shape bottle, 7-SPE Solid-Phase Extraction column jecket, 8-XAD-2 resin, 9-porous Teflon pad.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described in further detail:
Shown in composition graphs 1, a kind of Passive sampler for palycyclic aromatic in the experiment of root case in the present embodiment, it comprises gas collector 3 and root case 2, the colourless SPE solid-phase extraction column void column pipe of gas collector 3 to be volumes be 5 ~ 10mL in the present embodiment, its diameter is 1 ~ 2cm, be highly 6 ~ 7cm, this gas collector 3 built with graininess XAD-2 as adsorbent, adsorbent according to actual needs, also other materials can be selected as adsorbent, the particle diameter of adsorbent is 20 ~ 60 orders, in each gas collector, the consumption of adsorbent is 1.0g, gas collector 3 can arrange multiple according to actual needs, root case 2 is the good rectangular shaped post with cover of organic glass sealing, long: 20 ~ 25cm, wide: 20 ~ 25cm, high: 90 ~ 100cm, lid is provided with the circular hole 1 that 1 diameter is 1 ~ 5mm, can circular hole 1 be passed to make cord and tie up on the waddy of long 5cm, spacing 6 ~ the 7cm of this circular hole 1, and be suspended on root case 2 lid circular hole 3 place, what deserves to be explained is, before sampling, the teflon gasket with micropore in gas collector 3 will cover tightly, and the height of gas collector in root case is different.When gas collector hangs in root case, column jecket osculum upwards, effectively can reduce dried wet deposition impact.Bucket 4 is back cut diameters is 30cm, and base diameter is the Plastic Drum of 20cm, and SPE extractor 5 is the solid extractors in 12 holes, and pear shape bottle 6 capacity is 50mL glass pear shape bottle, concentrates for rotary evaporation in vacuo.Fig. 2 is the structural representation of gas collector in Passive sampler of the present invention, 7 is SPE Solid-Phase Extraction column jecket, 8 is XAD-2 resin, also can select other adsorbent according to actual needs, and 9 is adsorbent two ends 1mm thickness for fixing and have the teflon gasket of micropore.In gas collector, the type of feed of adsorbent is, with two panels porous Teflon pad for supporting, adsorbent is placed between two parties in SPE Solid-Phase Extraction column jecket, under adsorbent, teflon gasket is 1cm apart from the distance bottom SPE extracting tube, this design can make gas area of passage increase, sample rate is fast, substantially increases sampling rate.
Embodiment 1:
Gaseous PAHs Passive sampler in a kind of root case experiment,: comprise root case and some gas collector, described gas collector is suspended on the diverse location in root case and the gas for gathering diverse location place in root case, the SPE Solid-Phase Extraction column jecket of described gas collector to be volume be 5mL, described gas collector built with graininess XAD-2 resin as adsorbent, the particle diameter of adsorbent is 20 orders, and surface area is 430m
2/ g, water percentage is 20%, and in each collector, adsorbent is 1.0g, and described case is provided with lid, and lid is provided with the circular hole being used for fixing gas collector.
Described gas collector is colourless SPE Solid-Phase Extraction column jecket, and its diameter is 1cm, is highly 6cm, and when gas collector hangs in root case, column jecket osculum upwards.
Described gas collector comprises adsorbent, two panels porous Teflon pad; Wherein, adsorbent is arranged between two panels porous Teflon pad, a slice porous Teflon pad is arranged on 2cm place bottom distance SPE Solid-Phase Extraction column jecket, and another sheet porous Teflon pad is arranged on the sorbent, and adsorbent is arranged on the centre of SPE Solid-Phase Extraction column jecket.The height of described case is 90cm.
Embodiment 2:
Gaseous PAHs Passive sampler in a kind of root case experiment,: comprise root case and some gas collector, described gas collector is suspended on the diverse location in root case and the gas for gathering diverse location place in root case, the SPE Solid-Phase Extraction column jecket of described gas collector to be volume be 10mL, described gas collector built with graininess XAD-2 resin as adsorbent, the particle diameter of adsorbent is 60 orders, surface area 460m
2/ g, water percentage is 45%, and in each collector, adsorbent is 1.0g, and described case is provided with lid, and lid is provided with the circular hole being used for fixing gas collector.
Described gas collector is colourless SPE Solid-Phase Extraction column jecket, and its diameter is 2cm, is highly 7cm, and when gas collector hangs in root case, column jecket osculum upwards.
Described gas collector comprises adsorbent, two panels porous Teflon pad; Wherein, adsorbent is arranged between two panels porous Teflon pad, a slice porous Teflon pad is arranged on 2cm place bottom distance SPE Solid-Phase Extraction column jecket, and another sheet porous Teflon pad is arranged on the sorbent, and adsorbent is arranged on the centre of SPE Solid-Phase Extraction column jecket.The height of described case is 100cm.
Embodiment 3:
Gaseous PAHs Passive sampler in a kind of root case experiment,: comprise root case and some gas collector, described gas collector is suspended on the diverse location in root case and the gas for gathering diverse location place in root case, the SPE Solid-Phase Extraction column jecket of described gas collector to be volume be 8mL, described gas collector built with graininess XAD-2 resin as adsorbent, the particle diameter of adsorbent is 40 orders, surface area 470m
2/ g, water percentage is 35%, and in each collector, adsorbent is 1.0g, and described case is provided with lid, and lid is provided with the circular hole being used for fixing gas collector.
Described gas collector is colourless SPE Solid-Phase Extraction column jecket, and its diameter is 1.5cm, is highly 6.5cm, and when gas collector hangs in root case, column jecket osculum upwards.
Described gas collector comprises adsorbent, two panels porous Teflon pad; Wherein, adsorbent is arranged between two panels porous Teflon pad, a slice porous Teflon pad is arranged on 2cm place bottom distance SPE Solid-Phase Extraction column jecket, and another sheet porous Teflon pad is arranged on the sorbent, and adsorbent is arranged on the centre of SPE Solid-Phase Extraction column jecket.The height of described case is 95cm.
What the present embodiment was implemented is, and a kind of to measure the concrete sampling determination method of palycyclic aromatic for the Passive sampler of palycyclic aromatic in the experiment of root case as described below:
I) pre-service of adsorbent:
Before sampling starts, adsorbent is used methylene chloride and the normal hexane mixed liquor static rinse 15min at 150 DEG C that chromatographically pure volume ratio is 1:1, circulate 3 times; Then at 150 DEG C, clean 15min with acetonitrile, circulate 3 times; Dry up rear masking foil with nitrogen again to package rear sealing and be stored in the baking oven of 50 DEG C stand-by; First after 1 ~ 2 hour (can be 1 hour, 1.5 hours, 2 hours) with alcohol immersion activation, after nitrogen dries up, add high performance liquid chromatography water, make its water cut reach 20% before using.
Ii) sampling process:
Step I being housed) adsorbent after cleaning takes 1g and moves into SPE teflon gasket 9 being housed one end and extract in void column pipe 7, then another sheet teflon gasket 9 is used adsorbent 8 to be fixed on the centre of SPE void column pipe 7, obtain gas collector 3, it is fastened with cord, cord through root box cover circular hole 1, hang in root case 2, the adsorbent surface in each gas collector 3 is kept to flush, start to carry out collection timing to the palycyclic aromatic in gas phase in root case simultaneously, the sample duration of Passive sampler is the t(this patent actual sample checking sampling period select 30 days), after sampling terminates, gas collector two ends are sealed, stand-by at being stored in-20 DEG C,
Iii) the wash-out of palycyclic aromatic in adsorbent:
By step I i) sampled after gas collector in adsorbent 15mL methylene chloride and acetone by volume 1:1 carry out SPE wash-out, elution speed controls at 1mL/ minute, recycling elution 3 times, eluent is through rotary evaporation in vacuo concentrated (40 DEG C), nitrogen blows and is concentrated into 0.6 ~ 1.0mL(0.6mL, 0.7mL, 1.0mL all can) after, concentrate is moved into decontaminating column (upper strata 1g anhydrous sodium sulfate+lower floor 0.5g silica gel), the normal hexane of 15ml and methylene chloride (1:1) mixed liquor is used to carry out wash-out again, eluent is collected in pear shape bottle, finally with Rotary Evaporators concentrated (40 DEG C), be settled to 1mL with acetonitrile and be placed in 2mL analysis bottle, to be determined at being stored in-20 DEG C,
Iv) liquid chromatogram measuring process:
Testing tool is the high performance liquid chromatograph (HPLC) of Agilent company of the U.S., and chromatographic column is AgilentZORBAXEclipseXDB-C18(4.6*250mm, thickness of liquid film 5 μm), fluorescence detector (FLD).HPLC condition: mobile phase is acetonitrile and water, starting condition is the acetonitrile of 6:4: water (V:V), then in 60min with 0.75mL/min linear elution to 100% acetonitrile.Determined wavelength: carry out time programming with FLD signal, 0 ~ 9 minute: Ex λ=260nm, Em λ=380nm; 9 ~ 16 minutes: Ex λ=260nm, Em λ=340nm; 16 ~ 18 minutes: Ex λ=260nm, Em λ=380nm; 18 ~ 21 minutes: Ex λ=260nm, Em λ=380nm; 21 ~ 23 minutes: Ex λ=289nm, Em λ=462nm; 23 ~ 30 minutes: Ex λ=320nm, Em λ=380nm; 30 ~ 36 minutes: Ex λ=266nm, Em λ=403nm; 36 ~ 52 minutes: Ex λ=294nm, Em λ=430nm; 52 minutes: Ex λ=290nm, Em λ=500nm.In the eluent recorded, PAHs concentration is changed and is set as mass M
g,i.Fig. 3 is that palycyclic aromatic mixed sample goes out peak figure on HPLC, can find, each material goes out peak and is separated better, illustrates that existing method of testing is feasible.
V) the mensuration of Passive sampler sampling rate R:
The sampling rate of Passive sampler is the key parameter of sampling thief performance, sampling rate reflects the mean value of surveyed compound in whole linear absorption stage, the present embodiment adopts initiatively sampling thief to correct sampling rate, initiatively sampling pipe is also SPE Solid-Phase Extraction column jecket, its length is 6 ~ 7cm, internal diameter is 1 ~ 2cm, initiatively fill XAD-2 in sampling pipe, two ends are the glass wool cleaned up in advance, initiatively sampling pipe Connexon amasss sampling pump, flow rate set is 40mL/min, and correct through soap film flowmeter, in the present embodiment, initiatively sampling thief is placed on the other synchronized sampling of Passive sampler of the present invention, and air intake is in sustained height, sampling terminates at rear aluminium-foil paper wraps and be stored in-20 DEG C, the concentration obtaining adopting initiatively sampling thief to record each palycyclic aromatic in the rice root case of same place is by analysis C
a,i, the mass M of extract China and Philippines and the pyrene obtained v) is analyzed according to step I
g,i, calculate Passive sampler by formula one and to sample the equivalent air volume Veq obtained:
Veq=M
g,i/ C
a,i(formula one)
Wherein: Veq is that Passive sampler is sampled the equivalent air volume obtained, and unit is m
3;
M
g,ifor Passive sampler is sampled the quality of the i-th kind of PAHs obtained, unit is ng;
C
a,ifor the concentration of i-th kind of PAHs that active sampler samples obtains, unit is ng/m
3;
According to the drafting Veq value that the different sampling stages calculated obtains, draw Veq-t scatter diagram, line linearity matching of going forward side by side, according to the sampling rate R of fit line slope determination Passive sampler, unit is m
3/ day.
Vi) the concentration of palycyclic aromatic is calculated:
The mean concentration C of each palycyclic aromatic in root case experiment gas phase
g,icalculated by formula two, the concentration levels of phenanthrene and pyrene:
C
g,i=24 × M
g,i/ (R × t) (formula two)
Wherein: C
g,ifor Passive sampler is sampled the mean concentration of the i-th kind of PAHs obtained, unit is ng/m
3;
M
g,ifor Passive sampler is sampled the quality of the i-th kind of PAHs obtained, unit is ng;
R is the sampling rate of Passive sampler, and corrected by active sampling thief and determine, unit is m
3/ day;
T is the sampling time of Passive sampler, and unit is h.
Above-described specific embodiments; further detailed description has been carried out to object of the present invention, technical scheme and beneficial effect; be understood that; the foregoing is only specific embodiment of the invention scheme; and be not used to limit scope of the present invention; any those skilled in the art, the equivalent variations made under the prerequisite not departing from design of the present invention and principle and amendment, all should belong to the scope of protection of the invention.
Claims (6)
1. gaseous PAHs Passive sampler in a root case experiment, it is characterized in that, comprise root case and some gas collector, described gas collector is suspended on the diverse location in root case and the gas for gathering diverse location place in root case, the SPE Solid-Phase Extraction column jecket of described gas collector to be volume be 5 ~ 10mL, described gas collector is built with graininess XAD-2 resin as adsorbent, and the particle diameter of adsorbent is 20 ~ 60 orders, surface area>=430m
2/ g, water percentage is 20% ~ 45%, and in each gas collector, adsorbent is 1.0g, and described case is provided with lid, and lid is provided with the circular hole being used for fixing gas collector.
2. gaseous PAHs Passive sampler in a kind of root case experiment according to claim 1, it is characterized in that, described gas collector is colourless SPE Solid-Phase Extraction column jecket, its diameter is 1 ~ 2cm, be highly 6 ~ 7cm, when gas collector hangs in root case, column jecket osculum upwards.
3. gaseous PAHs Passive sampler in a kind of root case experiment according to claim 1, it is characterized in that, described gas collector comprises adsorbent, two panels porous Teflon pad; Wherein, adsorbent is arranged between two panels porous Teflon pad, a slice porous Teflon pad is arranged on 2cm place bottom distance SPE Solid-Phase Extraction column jecket, and another sheet porous Teflon pad is arranged on the sorbent, and adsorbent is arranged on the centre of SPE Solid-Phase Extraction column jecket.
4. gaseous PAHs Passive sampler in a kind of root case experiment according to claim 1, it is characterized in that, the height of described case is 90 ~ 100cm.
5., based on the sampling determination method of gaseous PAHs Passive sampler in a kind of case experiment according to claim 1, it is characterized in that, comprise the following steps:
I) pre-service of adsorbent:
Before sampling starts, adsorbent is used methylene chloride and the normal hexane mixed liquor static rinse 15min at 150 DEG C that chromatographically pure volume ratio is 1:1, circulate 3 times; Then at 150 DEG C, clean 15min with acetonitrile, circulate 3 times; Dry up rear masking foil with nitrogen again to package rear sealing and be stored in the baking oven of 50 DEG C stand-by; First after 1 ~ 2 hour with alcohol immersion activation, after nitrogen dries up, add high performance liquid chromatography water, make its water cut reach 20% before using;
Ii) sampling process:
Step I being housed) adsorbent after cleaning takes 1g and moves into SPE teflon gasket being housed one end and extract in void column pipe, then another sheet teflon gasket is adopted adsorbent to be fixed on the centre of SPE extraction void column pipe, obtain gas collector, gas collector is connected with the circular hole on the lid of root case by cord, and hang in root case, the adsorbent surface in each gas collector is kept to flush, start to carry out collection timing to the palycyclic aromatic in gas phase in root case simultaneously, the sample duration of Passive sampler is t, after sampling terminates, gas collector two ends are sealed, stand-by at being stored in-20 DEG C,
Iii) in adsorbent, the wash-out of palycyclic aromatic extracts:
By step I i) sampled after gas collector in adsorbent 15mL methylene chloride and acetone by volume 1:1 carry out SPE wash-out, elution speed controls at 1mL/ minute, recycling elution 3 times, eluent concentrates through rotary evaporation in vacuo, it is 40 DEG C that temperature controls, after nitrogen blows and is concentrated into 0.6 ~ 1.0mL, concentrate is moved into decontaminating column, the upper strata of decontaminating column is 1g anhydrous sodium sulfate, the lower floor of decontaminating column is 0.5g silica gel, be that the normal hexane of 1:1 and methylene chloride mixed liquor carry out wash-out by the volume ratio of 15mL again, eluent is collected in pear shape bottle, finally concentrate with Rotary Evaporators, be settled to 1mL with acetonitrile and be placed in 2mL analysis bottle, to be determined at being stored in-20 DEG C,
Iv) hplc determination process:
Testing tool is high performance liquid chromatograph HPLC, HPLC condition: chromatographic column is AgilentZORBAXEclipseXDB-C18,4.6*250mm, thickness of liquid film 5 μm, fluorescence detector FLD, mobile phase is acetonitrile and water, and starting condition is be the acetonitrile of 6:4 by volume: water, then in 60min with 0.75mL/min linear elution to 100% acetonitrile; Determined wavelength: carry out time programming with FLD signal, 0 ~ 9 minute: Ex λ=260nm, Em λ=380nm; 9 ~ 16 minutes: Ex λ=260nm, Em λ=340nm; 16 ~ 18 minutes: Ex λ=260nm, Em λ=380nm; 18 ~ 21 minutes: Ex λ=260nm, Em λ=380nm; 21 ~ 23 minutes: Ex λ=289nm, Em λ=462nm; 23 ~ 30 minutes: Ex λ=320nm, Em λ=380nm; 30 ~ 36 minutes: Ex λ=266nm, Em λ=403nm; 36 ~ 52 minutes: Ex λ=294nm, Em λ=430nm; 52 minutes: Ex λ=290nm, Em λ=500nm; In the eluent recorded, PAHs concentration is changed and is set as mass M
g,i;
V) the determination of Passive sampler sampling rate R:
The concentration adopting initiatively sampling thief to record each palycyclic aromatic in the outdoor root case experiment in same place is C
a,i, the mass M of PAHs in the eluent obtained v) is analyzed according to step I
g,i, calculate Passive sampler by formula (1) and to sample the equivalent air volume Veq obtained:
Veq=M
g,i/C
a,i（1）
Wherein: Veq is that Passive sampler is sampled the equivalent air volume obtained, and unit is m
3;
M
g,ifor Passive sampler is sampled the quality of the i-th kind of PAHs obtained, unit is ng;
C
a,ifor the concentration of i-th kind of PAHs that active sampler samples obtains, unit is ng/m
3;
According to the drafting Veq value that the different sampling stages calculated obtains, draw Veq-t scatter diagram, line linearity matching of going forward side by side, according to the sampling rate R of fit line slope determination Passive sampler, unit is m
3/ day;
Vi) the concentration of palycyclic aromatic is calculated:
The mean concentration C of each palycyclic aromatic in root case gas
g,icalculated by formula (2):
C
g,i=24×M
g,i/（R×t）（2）
Wherein: C
g,ifor Passive sampler is sampled the mean concentration of the i-th kind of PAHs obtained, unit is ng/m
3;
M
g,ifor Passive sampler is sampled the quality of the i-th kind of PAHs obtained, unit is ng;
R is the sampling rate of Passive sampler, by v) initiatively sampling thief correct and determine, unit is m
3/ day;
T is the sampling time of Passive sampler, and unit is h.
6. the sampling determination method of gaseous PAHs Passive sampler in a kind of case experiment according to claim 5, is characterized in that, described step I ii) in the temperature of evaporimeter control to be 40 DEG C.
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| CN113310770A (en) * | 2021-06-23 | 2021-08-27 | 生态环境部华南环境科学研究所 | Preservation method for monitoring and analyzing persistent organic pollutant sample in environment |
| CN114459831A (en) * | 2021-12-31 | 2022-05-10 | 天津津普利环保科技股份有限公司 | Multi-channel gas sampling and measuring method with flow control function |
| CN114459831B (en) * | 2021-12-31 | 2023-08-08 | 天津津普利环保科技股份有限公司 | Multichannel gas sampling measurement method with flow control |
| CN115508475A (en) * | 2022-11-01 | 2022-12-23 | 未名环境分子诊断(广东)有限公司 | Method for detecting content of diphenoxylate in sewage |
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