DE10042074A1 - Passive collector for extraction of dissolved organic compounds, useful for monitoring pesticides, comprises sorbent body placed inside membrane chamber - Google Patents
Passive collector for extraction of dissolved organic compounds, useful for monitoring pesticides, comprises sorbent body placed inside membrane chamberInfo
- Publication number
- DE10042074A1 DE10042074A1 DE10042074A DE10042074A DE10042074A1 DE 10042074 A1 DE10042074 A1 DE 10042074A1 DE 10042074 A DE10042074 A DE 10042074A DE 10042074 A DE10042074 A DE 10042074A DE 10042074 A1 DE10042074 A1 DE 10042074A1
- Authority
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- Germany
- Prior art keywords
- passive collector
- collector according
- extraction chamber
- membrane
- passive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 32
- 238000000605 extraction Methods 0.000 title claims abstract description 26
- 239000002594 sorbent Substances 0.000 title claims abstract description 17
- 238000012544 monitoring process Methods 0.000 title description 4
- 150000002894 organic compounds Chemical class 0.000 title description 2
- 239000000575 pesticide Substances 0.000 title 1
- 239000000126 substance Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012530 fluid Substances 0.000 claims abstract description 13
- -1 polysiloxanes Polymers 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 5
- 229920001684 low density polyethylene Polymers 0.000 claims description 5
- 239000004702 low-density polyethylene Substances 0.000 claims description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920000620 organic polymer Polymers 0.000 claims description 3
- 239000002798 polar solvent Substances 0.000 claims description 3
- 239000004627 regenerated cellulose Substances 0.000 claims description 3
- 235000005505 Ziziphus oenoplia Nutrition 0.000 claims description 2
- 244000104547 Ziziphus oenoplia Species 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- BHMLFPOTZYRDKA-IRXDYDNUSA-N (2s)-2-[(s)-(2-iodophenoxy)-phenylmethyl]morpholine Chemical compound IC1=CC=CC=C1O[C@@H](C=1C=CC=CC=1)[C@H]1OCCNC1 BHMLFPOTZYRDKA-IRXDYDNUSA-N 0.000 claims 1
- 239000012153 distilled water Substances 0.000 claims 1
- 229920000592 inorganic polymer Polymers 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 210000004379 membrane Anatomy 0.000 description 19
- 238000003795 desorption Methods 0.000 description 6
- 241001589086 Bellapiscis medius Species 0.000 description 5
- 238000000502 dialysis Methods 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000003673 groundwater Substances 0.000 description 2
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- CEOCDNVZRAIOQZ-UHFFFAOYSA-N pentachlorobenzene Chemical compound ClC1=CC(Cl)=C(Cl)C(Cl)=C1Cl CEOCDNVZRAIOQZ-UHFFFAOYSA-N 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BGPVFRJUHWVFKM-UHFFFAOYSA-N N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] Chemical compound N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] BGPVFRJUHWVFKM-UHFFFAOYSA-N 0.000 description 1
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 description 1
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 description 1
- 231100000704 bioconcentration Toxicity 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 150000004074 biphenyls Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229940117389 dichlorobenzene Drugs 0.000 description 1
- 239000012154 double-distilled water Substances 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000036651 mood Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000003993 organochlorine pesticide Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 1
- 229940117972 triolein Drugs 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/24—Dialysis ; Membrane extraction
- B01D61/246—Membrane extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/24—Dialysis ; Membrane extraction
- B01D61/28—Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/2805—Sorbents inside a permeable or porous casing, e.g. inside a container, bag or membrane
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
-
- 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
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
-
- 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
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
- G01N2001/4016—Concentrating samples by transferring a selected component through a membrane being a selective membrane, e.g. dialysis or osmosis
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
Abstract
Description
Zur Bestimmung einer zeitlich gemittelten Konzentration ge löster organischer Verbindungen in Wässern werden u. a. inte grative Passivsammler verwendet, die auf dem Prinzip der ki netischen Anreicherung basieren.To determine a concentration averaged over time Solved organic compounds in water are u. a. inte grative passive collectors based on the principle of ki based on netic enrichment.
Zu diesen integrativen Passivsammlern gehören vor allem Se mipermeable Membrane Devices (SPMDs) (Huckins, James N; Tu bergen, Mark W; Manuweera,Gamini K (1990): Semipermeable Mem brane Devices Containing Model Lipid: A New Approach to Mo nitoring the Bioavailability of Lipophilic Contaminants and Estimating Their Bioconcentration Potential. Chemosphere 20 (5), 533-552; Huckins, JN; Manuweera, GK; Petty, JD; Mackay, D; Lebo, JA (1993): Lipid-containing semipermeable membrane devices for monitoring organic contaminants in wa ter. Environ. Sci. Technol. 27, 2489-2496; U.S. Patent (5 098 573), die aus einer schlauchförmigen Polyethylenmembran ge ringer Dichte (LDPE) bestehen, die in der Regel mit neutra lem Lipid (Triolein) als Referenzphase gefüllt ist. Die SPMD-Technologie ermöglicht die Bestimmung einer zeitlich gemittelten Konzentration gelöster organischer Stoffe im Wasser. Nachteilig bei dieser Technik ist eine Zeit- und ko stenaufwendige Probenaufarbeitung mit hohem Verbrauch von Lösemitteln bei der dialytischen Rückgewinnung von akkumu lierten Substanzen aus den SPMDs (Huckins, JM; Tubergen, MW; Lebo, JA; Gale, W; Schwartz, TR (1990): Polymeric film dialysis in organic solvent media for cleanup of organic contami nants. J. Assoc. Off. Anal. Chem. 73, 290-293; U.S. Patent 5 395 426) und Notwendigkeit eines Clean-up der Proben vor der chromatographischen Analyse.These integrative passive collectors primarily include Se mipermeable Membrane Devices (SPMDs) (Huckins, James N; Tu bergen, Mark W; Manuweera, Gamini K (1990): Semipermeable Mem brane Devices Containing Model Lipid: A New Approach to Mo monitoring the bioavailability of lipophilic contaminants and Estimating Their Bioconcentration Potential. Chemosphere 20 (5), 533-552; Huckins, JN; Manuweera, GK; Petty, JD; Mackay, D; Lebo, JA (1993): Lipid-containing semipermeable membrane devices for monitoring organic contaminants in wa ter. Environ. Sci. Technol. 27, 2489-2496; U.S. patent (5 098 573), which consists of a tubular polyethylene membrane low density (LDPE), usually with neutra lem lipid (triolein) is filled as a reference phase. The SPMD technology enables the determination of a time averaged concentration of dissolved organic substances in the Water. The disadvantage of this technique is a time and knockout most expensive sample preparation with high consumption of Solvents in the dialytic recovery of accumulators gated substances from the SPMDs (Huckins, JM; Tubergen, MW; Lebo, YES; Gale, W; Schwartz, TR (1990): Polymeric film dialysis in organic solvent media for cleanup of organic contami nants. J. Assoc. Off. Anal. Chem. 73, 290-293; U.S. patent 5 395 426) and the need to clean up the samples before chromatographic analysis.
Unabhängig von diesen Arbeiten haben sich Hardy u. a. mit der Verwendung von Permeationssammlern für die Bestimmung von flüchtigen organischen Substanzen (Bianchard, R. D., Hardy, J. K. (1985): Use of permeation sampler in the collection of 23 volatile Organic priority pollutants. Anal. Chem. 57, 2349-2351), Phenolen (Zhang, G. Z., Hardy, J. K. (1989): De termination of phenolic pollutants in water using permeation sampling. J. Environ. Sci. Health A 24, 279-295) und monocy clischen aromatischen Verbindungen (Lee, HL; Hardy, JK (1998): Passive sampling of monocyclic aromatic priority pollutants in water. Intern. J. Environ. Anal. Chem. 72, 83-97) in Wäs sern beschäftigt. Sie entwickelten Passivsammler, die aus einem Glasröhrchen bestehen, das auf der einen Seite mit ei ner Silikon-Polykarbonat-Membran, die für die zu untersu chenden Substanzen durchlässig ist, und auf der anderen Sei te mit einem Gummistopfen verschlossen ist. Die Substanzen werden dann auf einem festen Adsorbens (Tenax-TA, XAD-7, Chromosorb 103 oder Porapak Q) gesammelt, das in das Glas röhrchen eingefüllt wird. Nach der Exposition des Röhrchens wird das Adsorbens in ein mit einem Septum verschlossenes Vial umgefüllt und später mit Lösemittel extrahiert oder in ein Thermodesorptionsröhrchen eingebracht und in einer ge eigneten Gerätekombination (Thermodesorptionssystem-GC) ana lysiert. Der Vorteil dieser Vorrichtung besteht in der Va riabilität, die durch die verschiedenen Adsorbentien gegeben ist und in der Anwendung der Thermodesorption. Nachteile liegen in der im Vergleich zu SPMDs geringeren aktiven Flä che (ca. 25 cm2) und den Umfüllprozessen, die zeitaufwendig sind und bei denen feinkörniges Material verloren gehen kann. Darüber hinaus werden mit diesen Adsorbentien nur leichtflüchtige Substanzen angereichert. Die Aufnahmerate von 1,2,4-Trichlorbenzen ist z. B. gegenüber der der Dichlor benzene schon erheblich geringer (Intern. J. Environ. Anal. Chem. 72, 83-97).Regardless of this work, Hardy has, among other things, dealt with the use of permeation collectors for the determination of volatile organic substances (Bianchard, RD, Hardy, JK (1985): Use of permeation sampler in the collection of 23 volatile organic priority pollutants. Anal. Chem. 57, 2349-2351), phenols (Zhang, GZ, Hardy, JK (1989): De termination of phenolic pollutants in water using permeation sampling. J. Environ. Sci. Health A 24, 279-295) and monocyclic aromatic compounds (Lee, HL; Hardy, JK (1998): Passive sampling of monocyclic aromatic priority pollutants in water. Intern. J. Environ. Anal. Chem. 72, 83-97) in water. They developed passive collectors that consist of a glass tube that is sealed on one side with a silicone polycarbonate membrane that is permeable to the substances to be examined, and on the other side with a rubber stopper. The substances are then collected on a solid adsorbent (Tenax-TA, XAD-7, Chromosorb 103 or Porapak Q), which is filled into the glass tube. After exposure of the tube, the adsorbent is transferred to a vial sealed with a septum and later extracted with solvent or placed in a thermal desorption tube and analyzed in a suitable device combination (thermal desorption system GC). The advantage of this device is the variability that is given by the various adsorbents and the use of thermal desorption. Disadvantages lie in the smaller active area (approx. 25 cm 2 ) compared to SPMDs and the refilling processes, which are time-consuming and in which fine-grained material can be lost. In addition, only highly volatile substances are enriched with these adsorbents. The uptake rate of 1,2,4-trichlorobenzene is e.g. B. compared to that of the dichlorobenzene already considerably lower (Intern. J. Environ. Anal. Chem. 72, 83-97).
Aufgabe der Erfindung ist es, einen Passivsammler zur Be stimmung zeitlich gemittelter Konzentrationen organischer Substanzen mit geringer Polarität (z. B. Organochlorpestizi de, polycyclische aromatische Kohlenwasserstoffe, polychlo rierte Biphenyle usw.) in Wässern anzubieten, der einfach manipulierbar und thermisch desorbierbar ist und auch die Anreicherung und Desorption mittel- und schwerflüchtiger Substanzen ermöglicht.The object of the invention is to provide a passive collector for loading mood of temporally averaged concentrations of organic Low polarity substances (e.g. Organochlorpestizi de, polycyclic aromatic hydrocarbons, polychlo biphenyls etc.) in water, which is easy is manipulable and thermally desorbable and also the Enrichment and desorption of medium and low volatility Substances.
Die Lösung der Aufgabe erfolgt mit dem kennzeichnenden Teil des Patentanspruches 1. Vorteilhafte Weiterbildungen sind in den Unteransprüchen angegeben.The problem is solved with the characteristic part of claim 1. Advantageous further developments are in specified in the subclaims.
Der erfindungsgemäße Passivsammler zur membrankontrollierten Extraktion gelöster organischer Substanzen in Wasser ist vorteilhafter Weise zur einfachen und robusten Bestimmung einer über längere Zeitintervalle gemittelten Konzentration von gelösten organischen Spurensubstanzen in Oberflächen- und Grundwässern, die im Umweltmonitoring ihre Anwendung finden soll, geeignet.The passive collector according to the invention for membrane-controlled Extraction of dissolved organic substances in water advantageous for simple and robust determination a concentration averaged over longer time intervals of dissolved organic trace substances in surface and groundwater used in environmental monitoring should find suitable.
Der erfindungsgemäße Passivsammler besteht aus einer Extrak tionskammer deren Wandung mindestens teilweise durch eine Membran gebildet wird. Die Extraktionskammer ist nach außen dicht und ermöglicht nur einen Stofftransport durch die Mem bran. Das Innere der Extraktionskammer ist erfindungsgemäß mit Sorbentien gefüllt, die in einem Fluid eingebettet sind.The passive collector according to the invention consists of an extract tion chamber whose wall is at least partially by a Membrane is formed. The extraction chamber is on the outside tight and only allows mass transport through the membrane bran. The interior of the extraction chamber is according to the invention filled with sorbents embedded in a fluid.
In einer vorteilhaften Weiterbildung der Erfindung wird die Extraktionskammer durch eine beidseitig verschlossene, schlauchförmige Membran gebildet. In an advantageous development of the invention, the Extraction chamber by a closed on both sides, tubular membrane formed.
In einer weiteren Ausführungsform ist eine zylinderförmig angeordnete Membran beidseitig mit einem Verschluss dicht verschlossen. Hierzu eignet sich beispielsweise sehr vor teilhaft der Einsatz einer Dialysemembran, die an den beiden offenen Enden mit Verschlüssen aus Polypropylen geschlossen ist.In another embodiment, one is cylindrical arranged membrane sealed on both sides with a closure locked. This is very useful, for example partial use of a dialysis membrane attached to the two open ends closed with closures made of polypropylene is.
Als Fluide werden vorteilhafterweise Luft, Wasser und/oder polare Lösungsmittel eingebracht, in denen die Sorbentien verteilt sind. Als Sorbentien eignen sich insbesondere anor ganische und organische Polymere und inerte Festkörper, die sorptionsfähige Beschichtungen aus anorganischen und organi schen Polymeren aufweisen. Als besonders vorteilhaft hat sich der Einsatz von Silikonstücken bzw. eine Beschichtung der inerten Festkörper aus Polydimethylsiloxan heraus gestellt. Die Wahl des jeweiligen Sorbens und des Fluids wird durch die zu untersuchenden und zu analysierenden orga nischen Spurensubstanzen aus den Oberflächen- und Grundwäs sern bestimmt.Air, water and / or are advantageously used as fluids introduced polar solvents in which the sorbents are distributed. Anor are particularly suitable as sorbents ganic and organic polymers and inert solids, the sorbable coatings made of inorganic and organic have polymers. Has been particularly advantageous the use of silicone pieces or a coating the inert solid out of polydimethylsiloxane posed. The choice of the respective sorbent and the fluid is determined by the organization to be examined and analyzed African trace substances from the surface and groundwater determined.
Wesentlich für die effektive Funktion des Passivsammlers ist die Auswahl der Sorbentien nach ihren thermodesorbierbaren Eigenschaften. Die Abgabe der sorbierten organischen Sub stanzen soll quantitativ erfolgen. Besonders vorteilhaft einsetzbare Membranmaterialien sind die, die aus Polyethylen geringer Dichte, Polypropylen geringer Dichte, Silikon, Po lydimethylsiloxan oder regenerierter Zellulose bestehen.It is essential for the passive collector to function effectively the selection of sorbents according to their thermodesorbable Characteristics. The release of the sorbed organic sub punching should be quantitative. Particularly advantageous membrane materials that can be used are those made of polyethylene low density, low density polypropylene, silicone, butt lydimethylsiloxane or regenerated cellulose.
Wird als Fluid Wasser eingesetzt, sollte es vorteilhafter weise mehrfach destilliert sein. Organische Lösungsmittel, die auch im Gemisch mit Wasser eingesetzt werden, sind ins besondere Ethanol, Aceton und DMSO.If water is used as the fluid, it should be more advantageous be distilled several times. Organic solvents, which are also used in a mixture with water are ins special ethanol, acetone and DMSO.
Inerte Festkörper, die insbesondere vorteilhaft eingesetzt werden können, sind magnetische Materialien aber auch Glas und keramische Materialien. Durch entsprechende Auswahl der Sorbentien und der Fluide ist es auch möglich, weniger flüchtige Substanzen mit, dem Passivsammler aufzunehmen und thermisch wieder abzugeben.Inert solids, which are used particularly advantageously magnetic materials are also glass and ceramic materials. By appropriate selection of the Sorbents and the fluids are also possible less volatile substances with the passive collector and to be released thermally.
Die Erfindung wird anhand von Ausführungsbeispielen und ei ner Zeichnung näher erläutert. Es zeigenThe invention is based on exemplary embodiments and egg ner drawing explained in more detail. Show it
Fig. 1 eine schematische Darstellung eines Passivsammlers mit einer Extraktionskammer, die aus einer schlauch förmigen Membran gebildet ist und Fig. 1 is a schematic representation of a passive collector with an extraction chamber, which is formed from a tubular membrane and
Fig. 2 eine schematische Darstellung eines Passivsammlers, dessen Extraktionskammer durch eine beidseitig ver schlossene Dialysemembran gebildet ist. Fig. 2 is a schematic representation of a passive collector, the extraction chamber is formed by a closed dialysis membrane on both sides ver.
Der beispielhaft dargestellte Passivsammler gemäß Fig. 1 be steht aus einer Extraktionskammer 1, in der ein Fluid 2 ent halten ist, in dem Sorbentien 3 eingebettet sind. Die Wan dung 6 besteht aus einer Membran, die aus einer schlauchför migen Polyethylen geringen Dichte gebildet ist.The passive collector shown by way of example according to FIG. 1 be consists of an extraction chamber 1 , in which a fluid 2 is contained, in which sorbents 3 are embedded. The wall 6 consists of a membrane which is formed from a hose-shaped low density polyethylene.
Die Extraktionskammer 1 gemäß Fig. 2 enthält ein Sorbens 3, das aus einem inerten Festkörper, hier ein Magnet 4, und ei ner sorptionsfähigen Beschichtung 5 aus Polydimethylsiloxan besteht. Das Sorbens ist in bidestilliertes Wasser als Fluid 2 eingebettet. Eine Wandung 6 der Extraktionskammer 1 wird durch die Membran 7 gebildet, die hier eine Dialysemembran ist, die beidseitig mit einem Verschluss 8 aus Polypropylen abgedichtet ist.The extraction chamber 1 shown in FIG. 2 contains a sorbent 3 , which consists of an inert solid, here a magnet 4 , and egg ner sorbable coating 5 made of polydimethylsiloxane. The sorbent is embedded in bidistilled water as fluid 2 . A wall 6 of the extraction chamber 1 is formed by the membrane 7 , which here is a dialysis membrane, which is sealed on both sides with a closure 8 made of polypropylene.
Die Erfindung soll am Beispiel der kinetischen Anreicherung von Pentachlorbenzen und Hexachlorbenzen und der nachfolgen den thermischen Desorption dieser Substanzen näher erläutert werden. Silikonschlauch (2,0 mm, innen, × 2,4 mm, außen, Fa. Reichelt) wird in Stücke zu 0,4-0,6 mm Länge zerschnitten. Zur Herstellung des erfindungsgemäßen Passivsammlers werden 500 mg dieser Schlauchstücke in eine schlauchförmige Membran (100 µm dicke) aus LDPE (Polyethylen mit geringer Dichte, Polymer-Synthesewerk GmbH Rheinberg, Germany), die die Ex traktionskammer 1 bildet, gefüllt und die Membran anschlie ßend verschweißt. Die Außenseite der Extraktionskammer 1, die mit Wasser in Kontakt kommt, hat eine Oberfläche von 66 cm2 (Fig. 1).The invention will be explained using the example of the kinetic enrichment of pentachlorobenzene and hexachlorobenzene and the subsequent thermal desorption of these substances. Silicone tube (2.0 mm, inside, × 2.4 mm, outside, from Reichelt) is cut into pieces with a length of 0.4-0.6 mm. To produce the passive collector according to the invention, 500 mg of these tube pieces are filled into a tubular membrane (100 μm thick) made of LDPE (low-density polyethylene, Polymer-Synthesewerk GmbH Rheinberg, Germany), which forms the extraction chamber 1 , and the membrane is then welded , The outside of the extraction chamber 1 , which comes into contact with water, has a surface area of 66 cm 2 ( FIG. 1).
Der Passivsammler wird in einem Durchflusssystem (Durchfluss 36 l/h) in einer wäßrigen Lösung (50 ng/l) der getesteten Stoffe bei 19°C exponiert. Die Stoffkonzentration in der wäßrigen Lösung wird in Abständen von 48 Stunden überprüft. Nach einer bestimmten Expositionszeit wird der Passivsammler aus dem Durchflusssystem entnommen, die Polyethylenmembran wird aufgeschnitten und die Silikonstücke werden entnommen, in ein Thermodesorptionsröhrchen (Fa. Gerstel) gefüllt, das in einer an sich bekannten Gerätekombination, bestehend aus Thermodesorber, Kaltausgabesystem, GC und MSD (Fa. Gerstel), analysiert wird. Die Chromatogramme zeigen ein kontinuierli ches Anwachsen der Peakflächen mit der Expositionszeit, die zu 2, 6, 8, 9 und 14 Tagen gewählt war. Die lineare Anreiche rungsgeschwindigkeit beträgt 0,9 ng/h für Pentachlorbenzen und 1,3 ng/h für Hexachlorbenzen.The passive collector is in a flow system (flow 36 l / h) in an aqueous solution (50 ng / l) of the tested Substances exposed at 19 ° C. The substance concentration in the aqueous solution is checked at 48 hour intervals. After a certain exposure time, the passive collector taken from the flow system, the polyethylene membrane is cut open and the silicone pieces are removed, filled into a thermodesorption tube (Gerstel), the in a device combination known per se, consisting of Thermal desorber, cold dispensing system, GC and MSD (Gerstel), is analyzed. The chromatograms show a continuous growth of the peak areas with the exposure time, the for 2, 6, 8, 9 and 14 days. The linear range speed is 0.9 ng / h for pentachlorobenzene and 1.3 ng / h for hexachlorobenzene.
Die Erfindung soll am Beispiel der kinetischen Anreicherung von Organochlorpestiziden, polycyclischen aromatischen Koh lenwasserstoffen und polychlorierten Biphenylen und der nachfolgenden thermischen Desorption dieser Substanzen mit einer weiteren beispielhaften Ausführungsform der Erfindung näher erläutert werden. The invention is based on the example of kinetic enrichment of organochlorine pesticides, polycyclic aromatic Koh hydrogen and polychlorinated biphenyls and the subsequent thermal desorption of these substances a further exemplary embodiment of the invention are explained in more detail.
Ein mit Polydimethylsiloxan beschichteter magnetischer Rüh rer TWISTER (15 mm lang; Fa. Gerstel GmbH, Mühlheim a. d. Ruhr) wird in eine Spektra/Por 6 Dialysemembran (Extrakti onskammer 1) aus regenerierter Zellulose (18 mm breit, 30 mm lang; Porengröße entspricht einer Ausschlußgrenze bezüglich des Molekulargewichts von 1000 Dalton) gefüllt, die Membran wird mit 5 ml bidestiliertem Wasser gefüllt und an beiden offenen Enden mit Spectra/Por Verschlüssen aus Polypropylen geschlossen (Fig. 2).A magnetic stirrer TWISTER (15 mm long; Fa. Gerstel GmbH, Mühlheim ad Ruhr) coated with polydimethylsiloxane is placed in a Spektra / Por 6 dialysis membrane (extraction chamber 1 ) made of regenerated cellulose (18 mm wide, 30 mm long; pore size corresponds to one Exclusion limit with respect to the molecular weight of 1000 daltons), the membrane is filled with 5 ml of double-distilled water and closed at both open ends with Spectra / Por closures made of polypropylene ( FIG. 2).
Der so hergestellte erfindungsgemäße Passivsammler wird in einem Durchflußsystem in einer wässrigen Lösung der geteste ten Stoffe unter gleichen Bedingungen wie im Beispiel 1 ex poniert.The passive collector according to the invention thus produced is shown in a flow system in an aqueous solution ten substances under the same conditions as in Example 1 ex posited.
Nach einer bestimmten Expositionszeit wird der Passivsammler aus dem Durchflußsystem entnommen, der TWISTER-Rührer wird von der Zellulosemembran getrennt und in ein Thermodesorpti onsröhrchen übertragen. Die auf dem TWISTER absorbierte Stoffmenge wird in einer an sich bekannten Gerätekombinati on, bestehend aus Thermodesorber, Kryofokusierung, GC und MSD (Fa. Gerstel), analysiert.After a certain exposure time, the passive collector taken from the flow system, the TWISTER stirrer becomes separated from the cellulose membrane and into a thermodesorpti transferred onsröhrchen. The absorbed on the TWISTER The amount of substance is in a device combination known per se on, consisting of thermal desorber, cryofocusing, GC and MSD (from Gerstel), analyzed.
Unter diesen Bedingungen bleibt das Prinzip der kinetischen Anreicherung für alle untersuchte organische Stoffe (Tabelle 1) mindestens bis zur 96-ten Expositionsstunde erhalten. Die lineare Anreicherungsgeschwindigkeiten an dem TWISTER-Rührer für die untersuchten organischen Stoffe sind in der Tabelle 1 gezeigt. Under these conditions, the principle of kinetic remains Enrichment for all examined organic substances (table 1) received at least until the 96th hour of exposure. The linear enrichment speeds on the TWISTER stirrer for the examined organic substances are in the table 1 shown.
Lineare Anreicherungsgeschwindigkeiten organischer Schad
stoffe an dem TWISTER-Rührer aus der Vorrichtung beschrieben
im Ausführungsbeispiel 2 während der Exposition in wäßriger
Lösung (50 ng/L) im Durchfluss bei 19°C. Details sind im
Ausführungsbeispiel 2 beschrieben.
Linear enrichment rates of organic pollutants on the TWISTER stirrer from the device described in embodiment 2 during exposure in aqueous solution (50 ng / L) in flow at 19 ° C. Details are described in embodiment 2.
11
Extraktionskammer
extraction chamber
22
Fluid
fluid
33
Sorbens
sorbent
44
Magnet
magnet
55
Beschichtung
coating
66
Wandung
wall
77
Membran
membrane
88th
Verschluss
shutter
Claims (15)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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DE20023183U DE20023183U1 (en) | 2000-08-16 | 2000-08-16 | Passive collector for membrane-controlled extraction of dissolved organic substances in water |
DE10042074A DE10042074A1 (en) | 2000-08-16 | 2000-08-16 | Passive collector for extraction of dissolved organic compounds, useful for monitoring pesticides, comprises sorbent body placed inside membrane chamber |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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DE10042074A DE10042074A1 (en) | 2000-08-16 | 2000-08-16 | Passive collector for extraction of dissolved organic compounds, useful for monitoring pesticides, comprises sorbent body placed inside membrane chamber |
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DE10042074A1 true DE10042074A1 (en) | 2002-03-07 |
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DE10042074A Ceased DE10042074A1 (en) | 2000-08-16 | 2000-08-16 | Passive collector for extraction of dissolved organic compounds, useful for monitoring pesticides, comprises sorbent body placed inside membrane chamber |
DE20023183U Expired - Lifetime DE20023183U1 (en) | 2000-08-16 | 2000-08-16 | Passive collector for membrane-controlled extraction of dissolved organic substances in water |
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DE20023183U Expired - Lifetime DE20023183U1 (en) | 2000-08-16 | 2000-08-16 | Passive collector for membrane-controlled extraction of dissolved organic substances in water |
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Cited By (5)
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FR2878333A1 (en) * | 2004-11-25 | 2006-05-26 | Cie Gen De S Eaux Soc En Comma | CASE FOR COLLECTING WATER AND CAPTURING ODOR-PRODUCING SUBSTANCES AND / OR GOUTS IN THE WATER |
CN101126751B (en) * | 2007-09-11 | 2011-05-04 | 南京大学 | Gas phase chromatogram- ion trap tandem mass spectrometry method for detecting organochlorine pesticide |
DE102013015522A1 (en) * | 2013-09-18 | 2015-03-19 | Johann-Wolfgang-Goethe Universität Frankfurt am Main | Dialysis cell for in vitro release test apparatus, use of dialysis cell and in vitro release test apparatus |
CN104730177A (en) * | 2015-04-01 | 2015-06-24 | 东南大学 | Enrichment apparatus used for collecting a variety of pollutants in high vacuum environment and use method thereof |
CN105181393A (en) * | 2015-10-21 | 2015-12-23 | 核工业北京化工冶金研究院 | Water sample collection system and water sample collection method for taking sample from water drained from pump pipe |
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---|---|---|---|---|
FR2878333A1 (en) * | 2004-11-25 | 2006-05-26 | Cie Gen De S Eaux Soc En Comma | CASE FOR COLLECTING WATER AND CAPTURING ODOR-PRODUCING SUBSTANCES AND / OR GOUTS IN THE WATER |
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DE102013015522A1 (en) * | 2013-09-18 | 2015-03-19 | Johann-Wolfgang-Goethe Universität Frankfurt am Main | Dialysis cell for in vitro release test apparatus, use of dialysis cell and in vitro release test apparatus |
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CN104730177A (en) * | 2015-04-01 | 2015-06-24 | 东南大学 | Enrichment apparatus used for collecting a variety of pollutants in high vacuum environment and use method thereof |
CN105181393A (en) * | 2015-10-21 | 2015-12-23 | 核工业北京化工冶金研究院 | Water sample collection system and water sample collection method for taking sample from water drained from pump pipe |
CN105181393B (en) * | 2015-10-21 | 2017-08-25 | 核工业北京化工冶金研究院 | The water sampling system and water sampling method sampled from pump line draining |
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