DE20023183U1 - Passive collector for membrane-controlled extraction of dissolved organic substances in water - Google Patents
Passive collector for membrane-controlled extraction of dissolved organic substances in waterInfo
- Publication number
- DE20023183U1 DE20023183U1 DE20023183U DE20023183U DE20023183U1 DE 20023183 U1 DE20023183 U1 DE 20023183U1 DE 20023183 U DE20023183 U DE 20023183U DE 20023183 U DE20023183 U DE 20023183U DE 20023183 U1 DE20023183 U1 DE 20023183U1
- Authority
- DE
- Germany
- Prior art keywords
- collector according
- passive collector
- membrane
- passive
- extraction chamber
- 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.)
- Expired - Lifetime
Links
- 239000012528 membrane Substances 0.000 title claims description 32
- 238000000605 extraction Methods 0.000 title claims description 27
- 239000000126 substance Substances 0.000 title claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 20
- 239000002594 sorbent Substances 0.000 claims description 15
- -1 polysiloxanes Polymers 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 229920001684 low density polyethylene Polymers 0.000 claims description 7
- 239000004702 low-density polyethylene Substances 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 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
- 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
- 229920000592 inorganic polymer Polymers 0.000 claims description 4
- 229920000620 organic polymer Polymers 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002798 polar solvent Substances 0.000 claims description 3
- 239000004627 regenerated cellulose Substances 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000003795 desorption Methods 0.000 description 8
- 244000309464 bull Species 0.000 description 7
- 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
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000003993 organochlorine pesticide Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 3
- DXBHBZVCASKNBY-UHFFFAOYSA-N 1,2-Benz(a)anthracene Chemical compound C1=CC=C2C3=CC4=CC=CC=C4C=C3C=CC2=C1 DXBHBZVCASKNBY-UHFFFAOYSA-N 0.000 description 2
- 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 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000007613 environmental effect 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
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 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
- MINPZZUPSSVGJN-UHFFFAOYSA-N 1,1,1,4,4,4-hexachlorobutane Chemical compound ClC(Cl)(Cl)CCC(Cl)(Cl)Cl MINPZZUPSSVGJN-UHFFFAOYSA-N 0.000 description 1
- MVWHGTYKUMDIHL-UHFFFAOYSA-N 2,2',4,4',5,5'-hexachlorobiphenyl Chemical compound C1=C(Cl)C(Cl)=CC(Cl)=C1C1=CC(Cl)=C(Cl)C=C1Cl MVWHGTYKUMDIHL-UHFFFAOYSA-N 0.000 description 1
- 101150049492 DVR gene Proteins 0.000 description 1
- RPUMZMSNLZHIGZ-UHFFFAOYSA-N PCB138 Chemical compound C1=C(Cl)C(Cl)=CC(Cl)=C1C1=CC=C(Cl)C(Cl)=C1Cl RPUMZMSNLZHIGZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 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
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 231100000704 bioconcentration Toxicity 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
- 238000013461 design Methods 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
- 230000007717 exclusion Effects 0.000 description 1
- 229960002809 lindane Drugs 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 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
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012546 transfer 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
- 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
- B01D61/246—Membrane extraction
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Urology & Nephrology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Sampling And Sample Adjustment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Description
ANWALTSKANZLEILAW FIRM
Guide Hengelhaupt Ziebig & SchneiderGuide Hengelhaupt Ziebig & Schneider
Patente Marken Design LizenzenPatents Trademarks Design Licenses
1010
15 20 25 3015 20 25 30
Klaus W. Guide, Dipl.-Chem.* Jürgen D. Hengelhaupt, Dipl.-Ing.3" Dr. Marlene K. Ziebig, Dipl.-Chem.2" Henry Schneider, Dipl.-Ing.* Wilfried H. Goesch, Dipl.-Ing.1' Dieter K. Wicht, Dipl.-Ing. 1" Isolde U. Winkler, Dipl.-Ing.* Dorit Rasch, Dipl.-Chem.* Dr. Sven Lange, Dipl.-Biologe2 Stephan Mainitz, Dipl.-Chem.Klaus W. Guide, Dipl.-Chem.* Jürgen D. Hengelhaupt, Dipl.-Ing. 3 " Dr. Marlene K. Ziebig, Dipl.-Chem. 2 " Henry Schneider, Dipl.-Ing.* Wilfried H. Goesch, Dipl.-Ing. 1 ' Dieter K. Wicht, Dipl.-Ing. 1 " Isolde U. Winkler, Dipl.-Ing.* Dorit Rasch, Dipl.-Chem.* Dr. Sven Lange, Dipl.-Biologist 2 Stephan Mainitz, Dipl.-Chem.
Jörg K. Grzam
Marco SchefflerJörg K. Grzam
Marco Scheffler
Tel.: 030/20623-0 / 030/26413 Fax: 030/20623-127 office@berlin-patent.net www.berlin-patent.net Tel.: 030/20623-0 / 030/26413 Fax: 030/20623-127 office@berlin-patent.net www.berlin-patent.net
35 Unser Zeich./our reference GM41902DE-Gu Datum/date35 Our reference GM41902DE-Gu Date
Berlin, 19.12.2002Berlin, 19.12.2002
4040
UFZ-UmweltforschungsZentrum Leipzig-Halle GmbH Permoserstraße 15 04318 LeipzigUFZ Environmental Research Centre Leipzig-Halle GmbH Permoserstrasse 15 04318 Leipzig
4545
Passivsammler zur membrankontrollxerten Extraktion gelöster organischer Substanzen im WasserPassive sampler for membrane-controlled extraction of dissolved organic substances in water
Passivsammler zur membrankontrollierten Extraktion gelöster organischer Substanzen im WasserPassive collector for membrane-controlled extraction of dissolved organic substances in water
Zur Bestimmung einer zeitlich gemittelten Konzentration gelöster organischer Verbindungen in Wässern werden u.a. integrative Passivsammler verwendet, die auf dem Prinzip der kinetischen Anreicherung basieren.To determine a time-averaged concentration of dissolved organic compounds in water, integrative passive samplers based on the principle of kinetic enrichment are used.
Zu diesen integrativen Passivsammlern gehören vor allem Semipermeable Membrane Devices (SPMDs) (Huckins,James N; Tubergen,Mark W; Manuweera,Gamini K (1990) : Semipermeable Membrane Devices Containing Model Lipid: A New Approach to Monitoring the Bioavailability of Lipophilic Contaminants andThese integrative passive samplers include mainly semipermeable membrane devices (SPMDs) (Huckins, James N; Tubergen, Mark W; Manuweera, Gamini K (1990) : Semipermeable Membrane Devices Containing Model Lipid: A New Approach to Monitoring the Bioavailability of Lipophilic Contaminants and
.20 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 water. Environ. Sei. Technol. 27, 2489-2496; U.S. Patent (5098 573), die aus einer schlauchförmigen Polyethylenmembran geringer Dichte (LDPE) bestehen, die in der Regel mit neutra lern 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 kostenaufwendige Probenaufarbeitung mit hohem Ver-brauch von Lösemitteln bei der dialytischen Rückgewinnung von akkumulierten 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-.20 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 water. Environ. Sei. Technol. 27, 2489-2496; U.S. Patent (5098 573), which consist of a tubular low-density polyethylene membrane (LDPE) that is usually filled with neutral lipid (triolein) as a reference phase. SPMD technology enables the determination of a time-averaged concentration of dissolved organic substances in water. The disadvantage of this technique is the time-consuming and costly sample preparation with high consumption of solvents during the dialytic recovery of accumulated substances from the 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, 2 90-293; U.S. Patent 5 395 426) und Notwendigkeit eines Clean-up der Proben vor der chromatographischen Analyse.nants. J. Assoc. Off. Anal. Chem. 73, 2 90-293; 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 (Blanchard, 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): Determination of phenolic pollutants in water using permeation sampling. J. Environ. Sei. Health A 24, 279-295) und monocyclischen 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 Wässern beschäftigt. Sie entwickelten Passivsammler, die aus einem Glasröhrchen bestehen, das auf der einen Seite mit einer Silikon-Polykarbonat-Membran, die für die zu untersuchenden Substanzen durchlässig ist, und auf der anderen Seite 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 Glasröhrchen 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 geeigneten Gerätekombination (Thermodesorptionssystem-GC) analysiert. Der Vorteil dieser Vorrichtung besteht in der Variabilität, die durch die verschiedenen Adsorbentien gegeben ist und in der Anwendung der Thermodesorption. Nachteile liegen in der im Vergleich zu SPMDs geringeren aktiven Fläche (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-Independently of this work, Hardy et al. have investigated the use of permeation samplers for the determination of volatile organic substances (Blanchard, 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): Determination 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 samplers consisting of a glass tube sealed on one side with a silicone-polycarbonate membrane permeable to the substances to be studied 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) that is placed in 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 provided by the different adsorbents and the application of thermal desorption. Disadvantages are the smaller active area (approx. 25 cm 2 ) compared to SPMDs and the transfer processes, which are time-consuming and can cause fine-grained material to be lost. In addition, these adsorbents only enrich volatile substances. The absorption rate of 1,2,4-trichlorobenzene, for example, is lower than that of dichloro-
benzene schon erheblich geringer (Intern. J. Environ.Anal.
Chem. 72, 83 - 97).benzene is 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. Organochlorpestizide, polycyclische aromatische Kohlenwasserstoffe, polychlorierte 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 determining time-averaged concentrations of organic substances with low polarity (e.g. organochlorine pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, etc.) in water, which is easy to manipulate and thermally desorbable and also enables the enrichment and desorption of medium and low volatile 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 characterizing part of patent claim 1. Advantageous further developments are 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 the membrane-controlled extraction of dissolved organic substances in water is advantageously suitable for the simple and robust determination of a concentration of dissolved organic trace substances in surface and groundwater averaged over longer time intervals, which is to be used in environmental monitoring.
Der erfindungsgemäße Passivsammler besteht aus einer Extraktionskammer deren Wandung mindestens teilweise durch eine Membran gebildet wird. Die Extraktionskammer ist nach außen dicht und ermöglicht nur einen Stofftransport durch die Membran. 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 extraction chamber whose wall is at least partially formed by a membrane. The extraction chamber is sealed to the outside and only allows material to be transported through the membrane. According to the invention, the interior of the extraction chamber is filled with sorbents that are 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 is formed by a tubular membrane closed on both sides.
In einer weiteren Ausführungsform ist eine zylinderförmig angeordnete Membran beidseitig mit einem Verschluss dicht verschlossen. Hierzu eignet sich beispielsweise sehr vorteilhaft der Einsatz einer Dialysemembran, die an den beiden 5 offenen Enden mit Verschlüssen aus Polypropylen geschlossen ist.In another embodiment, a cylindrically arranged membrane is tightly closed on both sides with a closure. For example, it is very advantageous to use a dialysis membrane that is closed at the two open ends with closures made of polypropylene.
Als Fluide werden vorteilhafterweise Luft, Wasser und/oder polare Lösungsmittel eingebracht, in denen die Sorbentien verteilt sind. Als Sorbentien eignen sich insbesondere anorganische und organische Polymere und inerte Festkörper, die sorptionsfähige Beschichtungen aus anorganischen und organischen Polymeren aufweisen. Als besonders vorteilhaft hat sich der Einsatz von Silikonstücken bzw. eine Beschichtung der inerten Festkörper aus Polydimethylsxloxan herausgestellt. Die Wahl des jeweiligen Sorbens und des Fluids wird durch die zu untersuchenden und zu analysierenden organischen Spurensubstanzen aus den Oberflächen- und Grundwässern bestimmt.Air, water and/or polar solvents are advantageously introduced as fluids in which the sorbents are distributed. Inorganic and organic polymers and inert solids with sorption-capable coatings made of inorganic and organic polymers are particularly suitable as sorbents. The use of silicone pieces or a coating of the inert solids made of polydimethylsxloxane has proven to be particularly advantageous. The choice of the respective sorbent and fluid is determined by the organic trace substances from the surface and groundwater to be examined and analyzed.
Wesentlich für die effektive Funktion des Passivsammlers ist die Auswahl der Sorbentien nach ihren thermodesorbierbaren Eigenschaften. Die Abgabe der sorbierten organischen Substanzen soll quantitativ erfolgen. Besonders vorteilhaft einsetzbare Membranmaterialien sind die, die aus Polyethylen geringer Dichte, Polypropylen geringer Dichte, Silikon, Polydimethylsiloxan oder regenerierter Zellulose bestehen.The selection of sorbents according to their thermodesorbable properties is essential for the effective functioning of the passive collector. The release of the sorbed organic substances should be quantitative. Membrane materials that are particularly advantageous are those made of low-density polyethylene, low-density polypropylene, silicone, polydimethylsiloxane or regenerated cellulose.
Wird als Fluid Wasser eingesetzt, sollte es vorteilhafterweise mehrfach destilliert sein. Organische Lösungsmittel, die auch im Gemisch mit Wasser eingesetzt werden, sind insbesondere Ethanol, Aceton und DMSO.If water is used as a fluid, it should preferably be distilled several times. Organic solvents that are also used in a mixture with water are in particular ethanol, acetone and DMSO.
Inerte Festkörper, die insbesondere vorteilhaft eingesetzt werden können, sind magnetische Materialien aber auch Glas und keramische Materialien. Durch entsprechende Auswahl derInert solids that can be used particularly advantageously are magnetic materials, but also glass and ceramic materials. By selecting the appropriate
Sorbentien und der Fluide ist es auch möglich, weniger flüchtige Substanzen mit dem Passivsammler aufzunehmen und thermisch wieder abzugeben.In addition to the sorbents and fluids, it is also possible to absorb less volatile substances with the passive collector and release them again thermally.
Die Erfindung wird anhand von Ausfuhrungsbeispielen und einer Zeichnung näher erläutert. Es zeigenThe invention is explained in more detail using exemplary embodiments and a drawing.
Fig. 1 eine schematische Darstellung eines Passivsammlers mit einer Extraktionskammer, die aus einer schlauchförmigen Membran gebildet ist undFig. 1 is a schematic representation of a passive sampler with an extraction chamber formed from a tubular membrane and
Fig. 2 eine schematische Darstellung eines Passivsammlers, dessen Extraktionskammer durch eine beidseitig verschlossene Dialysemembran gebildet ist.Fig. 2 is a schematic representation of a passive sampler whose extraction chamber is formed by a dialysis membrane closed on both sides.
Der beispielhaft dargestellte Passivsammler gemäß Fig. 1 besteht aus einer Extrakt ions kammer 1, in der ein Fluid 2 enthalten ist, in dem Sorbentien 3 eingebettet sind. Die Wandung 6 besteht aus einer Membran, die aus einer schlauchförmigen Polyethylen geringen Dichte gebildet ist.The passive collector shown as an example in Fig. 1 consists of an extraction chamber 1 containing a fluid 2 in which sorbents 3 are embedded. The wall 6 consists of a membrane made of tubular low-density polyethylene.
Die Extraktionskammer 1 gemäß Fig. 2 enthält ein Sorbens 3, das aus einem inerten Festkörper, hier ein Magnet 4, und einer sorptionsfähigen Beschichtung 5 aus Polydimethylsiloxan besteht. Das Sorbens ist in bidestilliertes Wasser als Fluid 2 eingebettet. Eine Wandung 6 der Extraktions-kammer 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 according to Fig. 2 contains a sorbent 3, which consists of an inert solid, here a magnet 4, and a sorption-capable coating 5 made of polydimethylsiloxane. The sorbent is embedded in double-distilled water as fluid 2. A wall 6 of the extraction chamber 1 is formed by the membrane 7, which here is a dialysis membrane that 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 nachfolgenden thermischen Desorption dieser Substanzen näher erläutert werden. Silikonschlauch (2,Omm,innen, &khgr; 2,4mm,außen, Fa.The invention will be explained in more detail using the example of the kinetic enrichment of pentachlorobenzene and hexachlorobenzene and the subsequent thermal desorption of these substances. Silicone hose (2.0mm, inside, Ø 2.4mm, outside, from Fa.
• ··
• ··
9 ·9 ·
• ··
•ff ····•ff ····
Reichelt) wird in Stücke zu O,4-0,6mm Länge zerschnitten. Zur Herstellung des erfindungsgemäßen Passivsammlers werden 500mg dieser Schlauchstücke in eine schlauchförmige Membran (&Igr;&Ogr;&Ogr;&mgr;&tgr;&eegr; dicke) aus LDPE (Polyethylen mit geringer Dichte, Polymer-Synthesewerk GmbH Rheinberg, Germany), die die Extraktionskammer 1 bildet, gefüllt und die Membran anschließend verschweißt. Die Außenseite der Extraktionskammer 1, die mit Wasser in Kontakt kommt, hat eine Oberfläche von 66 cm2 (Fig. 1).Reichelt) is cut into pieces of 0.4-0.6 mm length. To produce the passive collector according to the invention, 500 mg of these tube pieces are filled into a tubular membrane (100 mm 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/1) der getesteten Stoffe bei 19°C exponiert. Die Stoffkonzentration in der wäßrigen Lösung wird in Abständen von 4 8 Stunden überprüft.The passive sampler is exposed in a flow system (flow 36 l/h) in an aqueous solution (50 ng/l) of the tested substances at 19°C. The substance concentration in the aqueous solution is checked at intervals of 4 to 8 hours.
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 kontinuierliches Anwachsen der Peakflachen mit der Expositionszeit, die zu 2,6,8,9 und 14 Tagen gewählt war. Die lineare Anreicherungsgeschwindigkeit beträgt 0,9 ng/h für Pentachlorbenzen und 1,3 ng/h für Hexachlorbenzen.After a certain exposure time, the passive collector is removed from the flow system, the polyethylene membrane is cut open and the silicone pieces are removed and filled into a thermal desorption tube (Gerstel), which is analyzed in a known device combination consisting of a thermal desorber, cold dispensing system, GC and MSD (Gerstel). The chromatograms show a continuous increase in the peak areas with the exposure time, which was chosen to be 2, 6, 8, 9 and 14 days. The linear enrichment rate is 0.9 ng/h for pentachlorobenzene and 1.3 ng/h for hexachlorobenzene.
Ausführungsbeispiel 2Example 2
Die Erfindung soll am Beispiel der kinetischen Anreicherung von Organochlorpestiziden, polycyclischen aromatischen Kohlenwasserstoffen und polychlorierten Biphenylen und der nachfolgenden thermischen Desorption dieser Substanzen mit einer weiteren beispielhaften Ausführungsform der Erfindung näher erläutert werden.
35The invention will be explained in more detail using the example of the kinetic enrichment of organochlorine pesticides, polycyclic aromatic hydrocarbons and polychlorinated biphenyls and the subsequent thermal desorption of these substances with a further exemplary embodiment of the invention.
35
ViYViY
::
Ein mit Polydimethylsiloxan beschichteter magnetischer Rührer TWISTER (15 mm lang; Fa. Gerstel GmbH, Mühlheim a.d. Ruhr) wird in eine Spektra/Por 6 Dialysemembran (Extraktionskammer 1) aus regenerierter Zellulose (18 mm breit, 3 0 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 TWISTER magnetic stirrer coated with polydimethylsiloxane (15 mm long; Gerstel GmbH, Mühlheim a.d. Ruhr) is filled into a Spektra/Por 6 dialysis membrane (extraction chamber 1) made of regenerated cellulose (18 mm wide, 30 mm long; pore size corresponds to an exclusion limit with respect to the molecular weight of 1000 Daltons). The membrane is filled with 5 ml of bidistilled 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 getesteten Stoffe unter gleichen Bedingungen wie im Beispiel 1 exponiert. The passive sampler according to the invention thus prepared is exposed in a flow system in an aqueous solution of the tested substances under the same conditions as in Example 1 .
Nach einer bestimmten Expositionszeit wird der Passivsammler aus dem Durchflußsystem entnommen, der TWISTER-Rührer wird von der Zellulosemembran getrennt und in ein Thermodesorptionsröhrchen übertragen. Die auf dem TWISTER absorbierte Stoffmenge wird in einer an sich bekannten Gerätekombination, bestehend aus Thermodesorber, Kryofokusierung, GC und MSD (Fa. Gerstel), analysiert.After a certain exposure time, the passive collector is removed from the flow system, the TWISTER stirrer is separated from the cellulose membrane and transferred to a thermal desorption tube. The amount of substance absorbed on the TWISTER is analyzed in a known device combination consisting of a thermal desorber, cryofocusing, GC and MSD (Gerstel).
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 enrichment is maintained for all organic substances investigated (Table 1) at least until the 96th hour of exposure. The linear enrichment rates on the TWISTER stirrer for the organic substances investigated are shown in Table 1.
• f ·• f ·
• f• f
Lineare Anreicherungsgeschwindigkeiten organischer Schadstoffe 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 accumulation rates of organic pollutants on the TWISTER stirrer from the device described in Example 2 during exposure to aqueous solution (50 ng/L) in flow at 19°C. Details are described in Example 2.
« ♦ t« ♦ t
9999 999999 99
9999 999999 99
99 99 9 999 99 9 9
1 Extraktionskammer 2 Fluid 3 Sorbens 4 Magnet 5 Beschichtung S Wandung 7 Membran 8 Verschluss1 Extraction chamber 2 Fluid 3 Sorbent 4 Magnet 5 Coating S Wall 7 Membrane 8 Closure
Claims (15)
Priority Applications (1)
| 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 |
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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 |
| DE20023183U 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 |
| 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 |
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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 |
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| FR2878333B1 (en) * | 2004-11-25 | 2007-04-27 | 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 |
| DE102013015522B4 (en) * | 2013-09-18 | 2023-04-13 | Pharma Test Apparatebau AG | Dialysis cell for in vitro dissolution test apparatus, Use of the dialysis cell and in vitro dissolution test apparatus |
| CN104730177B (en) * | 2015-04-01 | 2017-01-25 | 东南大学 | Concentrator for collection of multiple pollutants in high vacuum environment and method of use |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3924219A (en) * | 1971-12-22 | 1975-12-02 | Minnesota Mining & Mfg | Gas detection device |
| GB1556050A (en) * | 1975-08-13 | 1979-11-21 | Inveresk Res Int | Device for monitoring the metal content of aqueous systems and monitoring method |
| GB2064765B (en) * | 1979-07-12 | 1983-06-22 | Perkin Elmer Ltd | Personal gas monitors |
| GB2152407A (en) * | 1984-01-06 | 1985-08-07 | Gen Electric | Grooving insert |
| IL76275A (en) * | 1985-09-02 | 1989-02-28 | Yeda Res & Dev | Water sampling system |
| US4942135A (en) * | 1986-08-04 | 1990-07-17 | The United States Of America As Represented By The United States Department Of Energy | Method for preconcentrating a sample for subsequent analysis |
| DE3735307A1 (en) * | 1987-10-17 | 1989-04-27 | Draegerwerk Ag | DIFFUSION COLLECTOR |
| US5106759A (en) * | 1988-06-28 | 1992-04-21 | Addison Clark D | Method for collecting radon and testing therefor |
| US5437979A (en) * | 1989-07-24 | 1995-08-01 | Beckman Instruments, Inc. | Solid phase system for sequential reactions |
| DE4345211C2 (en) * | 1992-03-04 | 1996-08-08 | Fujitsu Ltd | Measuring equipment for simplified measurement of the ambient atmosphere |
| GB9316945D0 (en) * | 1993-08-14 | 1993-09-29 | Univ Lancaster | Probe device |
| DE19648131A1 (en) * | 1996-11-21 | 1998-05-28 | Wolfgang Prof Dr Dr Herrmann | Determination of components of low density lipoprotein |
| DE19710525C2 (en) * | 1997-03-14 | 1999-11-11 | Cammann Karl | Passive diffusion collector for analytes contained in gases as well as methods for passive sampling and analysis |
| IT1302323B1 (en) * | 1998-09-11 | 2000-09-05 | Consiglio Nazionale Ricerche | DEVICE FOR DIFFUSIONAL VAPOR SAMPLING ORGANIC IN THE ENVIRONMENT. |
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2000
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