CN101493384A - Half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus - Google Patents

Half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus Download PDF

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CN101493384A
CN101493384A CNA2009100784183A CN200910078418A CN101493384A CN 101493384 A CN101493384 A CN 101493384A CN A2009100784183 A CNA2009100784183 A CN A2009100784183A CN 200910078418 A CN200910078418 A CN 200910078418A CN 101493384 A CN101493384 A CN 101493384A
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sampling
sampling box
metal support
sampling apparatus
concentration
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CN101493384B (en
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曹军
陶澍
刘娅囡
邓蜀星
张羽中
王文涛
赵靖宇
王伟
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Peking University
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Peking University
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Abstract

The invention relates to a semi-volatile persistent organic pollutant ground concentration vertical section sampling device which comprises a metal support and a sampling box. The sampling device is characterized in that the metal support is vertically arranged on the ground and is provided with openings at different heights of different directions for arranging the sampling box. In the scheme, a passive sampling technology is adopted and passive sampling media are adopted at different heights from the ground, thus obtaining the ground gaseous semi-volatile persistent organic pollutant concentration vertical section information for earth-atmosphere exchange research, and avoiding the problem of disturbance to the air layer when an air pump in the active sampling technology extracts air, therefore, the sampling device is more applicable to obtaining the concentration section information of the pollutant in the vertical direction.

Description

The half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus
Technical field
The present invention relates to the atmospheric surveillance technical field, relate in particular to a kind of concentration vertical section passive sampling apparatus near the ground of gaseous state half-volatilization persistency organic contaminant thing.
Background technology
The half-volatilization persistency organic contaminant thing mainly is present in soil and atmospheric medium in environment, and acts between soil-aerosphere face by sedimentation, volatilization, diffusion etc. and to exchange.By means of the information of concentration profile near the ground, the migratory direction of deducibility half-volatilization persistency organic contaminant thing between rustic interface, and estimate two alternate diffusion fluxs indirectly.
The general at present concentration information collection near the ground of adopting the active Sampling techniques to finish the half-volatilization persistency organic contaminant thing.For example, (Perihan Binnur Kurt-Karakus such as Kurt-Karakus, Terry F.Bidleman, Ralf M.Staebler, and Kevin C.Jones, Measurement of DDT Fluxes from a Historically Treated AgriculturalSoil in Canada, Environ.Sci.Technol., 2006,40 (15), pp 4578-4585) adopt the concentration of initiatively Sampling techniques monitoring DDT in the face of land differing heights place air under study for action, finding that DDT concentration increases with vertical height reduces, prove DDT in this area by soil to aerial migration.Its mode that obtains concentration vertical section information is carried out the active sampling for the sampling head with air sampler is separately fixed at apart from the position of ground 5,20,72 and 200cm, and the microclimate conditional information of synchronous recording sampling point height.
Yet utilize conventional initiatively Sampling techniques to need power resources in the above-mentioned existing scheme, sampling point is selected to have relatively high expectations; In addition, can produce disturbance to the surface air layer when air pump is bled, be difficult to collect under the high-resolution gaseous sample apart from the ground differing heights.
Summary of the invention
The purpose of this invention is to provide a kind of half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus, to solve the above-mentioned defective that existing initiatively Sampling techniques exist.
In order to achieve the above object, technical scheme of the present invention proposes a kind of half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus, comprise metal support and sampling box, described metal support is perpendicular to floor mounted, and, install for described sampling box in the differing heights place perforate of different directions.
In the above-mentioned sampling apparatus, described sampling box upper end closed, lower ending opening, the inner polyurethane foamed material PUF that places is as absorbing medium.
In the above-mentioned sampling apparatus, the xsect of described metal support is a square, the side is evenly distributed with the rectangle hole, and described sampling box utilizes rectangle hole helical arrangement to be fixed in the side differing heights of described metal support, is blocked with the lower ending opening of avoiding sampling box.
In the above-mentioned sampling apparatus, described sampling box is the stainless steel right cylinder, and adopts the rectangle hole secure fit of screw and described metal support.
In the above-mentioned sampling apparatus, the lower ending opening place of described sampling box is provided with the filtration copper mesh, causes interference to avoid particle to enter sampling box.
The solution of the present invention adopts the passive sampling technology, places the passive sampling medium at distance ground differing heights, thereby obtains gaseous state half-volatilization persistency organic contaminant substrate concentration vertical section information near the ground, is used for ground vapour exchange research; In the time of can avoiding simultaneously initiatively that air pump is bled in the Sampling techniques air layer is produced the problem of disturbance, therefore more be applicable to the pollutant information of concentration profile in vertical direction that obtains.
Description of drawings
Fig. 1 is a half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus structural drawing of the present invention;
Fig. 2 is the sampling box three-dimensional cross-section diagram in the device shown in Figure 1;
Fig. 3 is for using in the embodiments of the invention one three kinds of absorbing medium sampling efficiencies and the blank comparison of background synoptic diagram;
Two kinds of absorbing medium sample effect compare synoptic diagram to Fig. 4 in the embodiments of the invention one in order to use;
Fig. 5 is for using the PAH of each sampling point in the embodiments of the invention two 9Average daily sampling quantity vertical cross section;
Fig. 6 is the average daily sampling quantity vertical section of the sampling point C ACE of place, FLA and PYR in the application embodiments of the invention two.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Fig. 1 is a half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus structural drawing of the present invention, as shown in the figure, sampling apparatus of the present invention comprises: metal support 11 and sampling box 12, wherein, metal support 11 is installed perpendicular to ground 13, and, install for sampling box 12 in the differing heights place perforate of different directions.Wherein, sampling box 12 upper end closeds, lower ending opening, the inner polyurethane foamed material PUF that places is as absorbing medium.
Specifically in the present embodiment, the height of metal support 11 is 1 meter, and xsect is the square of 5cm * 5cm, and the side evenly distributes, and (2cm * 1cm) is used for the fixing of sampling box 12 to the rectangle hole.
Sampling box 12 then in the shape of a spiral shape be arranged in the position of differing heights around the metal support 11, be blocked to avoid lower ending opening.Fig. 2 is the three-dimensional cross-section diagram of sampling box, and as shown in the figure, sampling box shell 121 is the right cylinder of stainless steel, cross section internal diameter 3.8cm, high 2cm, upper end closed, lower ending opening; Absorbing medium 122 be polyurethane foamed material (PolyurethaneFoam, PUF), radius 2cm, thick 1cm; The opening shape of bottom 123 is circular, diameter 3cm; 124 of 400 order copper mesh are used for preventing that particle from entering into sampling box.
Below further specify effect of the present invention by instantiation.
Embodiment one
Obviously be not inconsistent in the plant bulk that uses in following examples and the above-mentioned Fig. 1 explanation, the test material size that adopts with present embodiment is as the criterion.This example is selected PUF (22mm OD * 3.8cm) as absorbing medium for use, choose semipermeable membrane device (Semipermeablemembrane devices simultaneously, SPMD, 5.5cm * 3.2cm) with SDEB styrene diethylenebenzene polymkeric substance (styrene-divinylbenzene polymer, XAD-2, the 2.5g/ device) test for relatively reference; And sampling box is individually fixed in apart from ground 0.5,2,3,4,5,8,12,15,17,20,25,30,40, the height of 45cm.Reclaim whole device exposes 42 days in outdoor environment after, measure, analyze, 16 kinds of palycyclic aromatics (naphthalene NAP, acenaphthylene ACY, acenaphthene ACE, fluorenes FLO, luxuriant and rich with fragrance PHE, anthracene ANT, fluoranthene FLA, pyrene PYR, benzanthrene BaA, CHR, benzo [b] fluoranthene BbF in the wrong, benzo [k] fluoranthene BkF, benzo [a] pyrene BaP, indeno 1 with the preferential control of USEPA, 2,3-cd pyrene IcdP, dibenzo [a, h] and anthracene DahA and benzo [ghi] perylene BghiP) be example, to absorption efficiency, background is blank and index such as recall rate detects.
After sampling finishes, with fatty extractor absorbing medium is carried out Soxhlet and extract (100ml methylene chloride, 50 ℃, 24 hours), extract revolves and steams to the 1ml, as the extract clear after concentrating, impurity is less, can add continue to be concentrated into behind about 10ml normal hexane mark in the back adds about 1ml (inner mark method ration, interior mark is selected 2-fluoro-1,1 '-biphenyl and p-terphenyl-d14, J﹠amp for use; K Chemical, USA) the direct GC-MS instrument of going up in back is analyzed.More as extract impurity, need to purify the back and go up the machine analysis.Purify and adopt the chromatographic column purification method, neutral silica gel (4g from the bottom to top successively packs into, 80～100 orders, 3% deactivation)+neutral alumina (4.75g, 3% deactivation)+anhydrous sodium sulfate (height 1cm), 50ml methylene chloride and normal hexane mixed solution (1: 1) dash with the speed of 2.0ml/min and drench back collection leacheate, are concentrated into about 1ml, and mark is to be measured in adding.
Sample analysis adopts GC-MSD (Agilent 6890N/5973I automatic sampler, HP-5 capillary column, 30.0m * 0.25mm * 0.25 μ m), presses 0.003MPa before the carrier gas He, post, and 250 ℃ of injector temperatures adopt to be regardless of to flow to sample loading mode; Heating schedule: 60 ℃ of initial temperatures, be warming up to 300 ℃ with 5 ℃/min, keep 15min and flow out chromatographic column fully to sample; Mass spectrum condition: EI ionization source 70Ev, mass range 45-400aum, photomultiplier cell voltage 950V, 230 ℃ of ion source temperatures, sweep velocity 0.82sec/scan, solvent delay 5min.Utilize PAHs to mix the GC retention time of 16 kinds of PAHs in the mark (US Chem Service, PAH-Mixture 610/525/550) and mass spectrometric data storehouse (NIST) and the PAHs in the sample is carried out qualitative, carry out quantitatively with external standard method according to the molecular ion peak of each PAHs.
As for the quality control of analytical approach, the method detection limit and the method recovery are as shown in table 1.All monitoring results all (are about to sampling media and place the sampling apparatus identical with sample through the over-sampling blank, transport with sample, use with quadrat method after sampling finishes and extract, measure), the correction of experiment blank (adopt to use the same method extract synchronously and step such as purification with sample) and the recovery.
Table 1
NAP ACE ACY FLO PHE ANT FLA PYR
Detection limit ng/ml 1.02 0.76 0.79 0.87 1.80 0.64 0.85 0.80
The recovery 51％ 67％ 75％ 83％ 77％ 98％ 124％ 51％
BaA CHR BbF BkF BaP DahA IcdP BghiP
Detection limit ng/ml 0.90 1.20 1.85 1.10 0.85 1.52 1.80 1.38
The recovery 92％ 121％ 90％ 108％ 102％ 127％ 65％ 92％
As shown in Figure 3, above-mentioned three kinds of absorbing medium sampling efficiencies choosing and flow process blank have certain difference, wherein P16, P9 represent 16 kinds of palycyclic aromatics and 9 kinds of representative palycyclic aromatics (ACE, ACY, FLO, PHE, ANT, FLA, PYR, BaA and CHR) concentration summation respectively, result of study shows, the XAD sampling efficiency is higher than PUF and SPMD, but the flow process blank will cause the recall rate of sample and degree of accuracy to reduce also far above PUF and SPMD simultaneously.
The recall rate that compares palycyclic aromatic in three kinds of absorbing mediums again according to table 2, except that DahA does not detect fully, the BaP recall rate is 0.85, every other compound recall rate is 100% in its demonstration PUF sample, and the recall rate of XAD and SPMD sample is relatively low.
Table 2
NAP ACE ACY FLO PHE ANT FLA PYR
PUF 100％ 100％ 100％ 100％ 100％ 100％ 100％ 100％
SPMD 89％ 96％ 100％ 100％ 100％ 100％ 100％ 100％
XAD 100％ 100％ 100％ 100％ 92％ 88％ 88％ 83％
BaA CHR BbF BkF BaP DahA IcdP BghiP
PUF 100％ 100％ 100％ 100％ 85％ 0％ 100％ 100％
SPMD 89％ 50％ 68％ 46％ 36％ 0％ 25％ 39％
XAD 33％ 75％ 29％ 29％ 75％ 88％ 50％ 50％
Comprehensive relatively sampling efficiency, background blank and palycyclic aromatic recall rate, though the sampling efficiency of XAD is the highest, because the influence of high background, 16 kinds of PAHs recall rates are lower.In addition, the fine particle shape of the physical aspect of XAD for disperseing is not easy to transport, the sample in preservation and the field trial installs and reclaim, under the humidity condition with higher, the moisture absorption caking phenomenon may appear in XAD, may cause certain influence to sampled result, therefore at first XAD is got rid of.
The sampling efficiency of the sample effect of comprehensive reference Fig. 4 and Fig. 3 as can be known again, PUF has higher sampling efficiency, and the PAHs detected level and the SPMD of its flow process blank are suitable, and recall rate is higher than SPMD, transportation is relative simple and easy to do with preservation, so the present invention selects the absorbing medium of PUF as sampling apparatus for use.In addition, the concentration profile by Fig. 4 gained shows PAH 9Total concentration increase with vertical range by the face of land and in rising trend, reach stable in about 18cm position, PAH is described 9Migratory direction between the rustic interface of this sampled point is for to be moved to soil by atmosphere.
Embodiment two
This example in autumn in 2007 in Mentougou, Beijing, 3 sampled points of Miyun and Tianjin Environmental Protection Agency install half-volatilization persistency organic contaminant near groundlevel concentration vertical profile passive sampling apparatus of the present invention respectively, in order to check field sample effect on the spot, the sampled point relevant information sees Table 3.
Table 3
The sampling point position Type Date collected
A Mentougou, Beijing: small arc shaped forest systematic study station Background 9/20-11/16
B Beijing Miyun: west of a river village, Gu Beikou town The rural area 9/22-11/14
C Urban district, Tianjin: Environmental Protection Agency The city 9/25-11/15
Average daily sampling quantity with each layer of sampling point sampling box comes secondary indication surface air PAHs concentration vertical section, thereby judges the migratory direction of PAHs between rustic interface near the ground.Fig. 5 is the concentration profile of the monitoring result of each sampling point surface air vertical section passive sampling device, and the result shows, the PAH of sampling point A and B 9Concentration raises to be similar to the distance floor level and is linear increase trend, and sampling point C concentration (PAH 9) with highly there not being marked change.Infer thus, in A, B spot area scope, PAH 9Mainly move mutually to soil, i.e. the PAH that discharges in the adsorption by soil atmosphere by atmosphere 9, in view of the influence of the degree of stability of surface air layer, rustic exchange boundary layer is greater than 45cm.C sampling point concentration of profile total amount is with highly there not being significant change, but observe (with ACE from the profile morphology of each component of palycyclic aromatic, FLA, PYR is an example, see Fig. 6), still there is concentration gradient in this sampling point PAHs between rustic, wherein be that the low cyclic compound concentration of representative descends with highly raising with ACE, from ground to aerial migration; FLA and PYR then with highly raising, move to soil from atmosphere.PAH in this sampling point 9The concentration profile of total amount is horizontal linear substantially, is because the vertical section of various ingredients superposes mutually and offsets and cause.May there be different emission sources in each component of PAHs in the different migratory direction explanations this area of compound.
Above-mentioned result of study shows, half-volatilization persistency organic contaminant near groundlevel concentration vertical profile passive sampling apparatus of the present invention has sample effect preferably, can under undisturbed situation, collect the concentration profile that to discern, thereby judge rustic exchange migration direction ground air.PAH from sampling point 9Total amount and each component be divided by other concentration profile, and PAHs concentration increases with rising highly, illustrates that PAHs is mainly by atmosphere to spread to soil in the sampling point scope.
More than be preferred forms of the present invention, according to content disclosed by the invention, those of ordinary skill in the art can expect some identical, replacement schemes apparently, all should fall into the scope of protection of the invention.

Claims (5)

1, a kind of half-volatilization persistency organic contaminant near groundlevel concentration vertical profile sampling apparatus, comprise metal support and sampling box, it is characterized in that described metal support is perpendicular to floor mounted, and, install for described sampling box in the differing heights place perforate of different directions.
2, sampling apparatus as claimed in claim 1 is characterized in that, described sampling box upper end closed, lower ending opening, and the inner polyurethane foamed material PUF that places is as absorbing medium.
3, sampling apparatus as claimed in claim 2, it is characterized in that, the xsect of described metal support is a square, the side is evenly distributed with the rectangle hole, described sampling box utilizes rectangle hole helical arrangement to be fixed in the side differing heights of described metal support, is blocked with the lower ending opening of avoiding sampling box.
4, sampling apparatus as claimed in claim 3 is characterized in that, described sampling box is the stainless steel right cylinder, and has the screw that is used for the rectangle hole secure fit of described metal support.
As each described sampling apparatus of claim 2～4, it is characterized in that 5, the lower ending opening place of described sampling box is provided with the filtration copper mesh, cause interference to avoid particle to enter sampling box.
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