WO2000070339A1 - Water sampling with analyte extraction and integration - Google Patents
Water sampling with analyte extraction and integration Download PDFInfo
- Publication number
- WO2000070339A1 WO2000070339A1 PCT/US2000/013507 US0013507W WO0070339A1 WO 2000070339 A1 WO2000070339 A1 WO 2000070339A1 US 0013507 W US0013507 W US 0013507W WO 0070339 A1 WO0070339 A1 WO 0070339A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fluid
- water
- pump
- samples
- extraction device
- Prior art date
Links
Classifications
-
- 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
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
-
- 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
-
- 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
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
- Y10T436/25375—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.]
Definitions
- grab sampling is merely the collection of an instantaneous unit of water matrix in a sampling vessel such as a glass jar.
- a grab sample is often inadequate to characterize a dynamic water body such as a stream or river where flow patterns and content change rapidly and frequently.
- Still another disadvantage of some prior art is their need to use a high-pressure or high-capacity pump to generate the liquid flow demanded by the sampler cartridge. This requires generally higher voltage and ultimately higher power requirements not readily available by battery power alone. It is desirable to have a sampler capable of sampling in remote areas autonomously (i.e., without an external source of power).
- U.S. Patent No. 5,844,147 is directed to a water sampling apparatus in which a sample is collected at a relatively high flow rate and then is temporarily stored in a storage container under pressure before passing through a solid phase extraction device at a slower rate which corresponds to the flow tolerance of the extraction device. This enables a quantity of water to be sampled over a single limited time frame during which the storage container fills up.
- the apparatus does not include a backflush capability which would be necessary to keep the flow system clear for providing repetitive samples.
- a filter unit comprised of locking/unlocking male and female fittings, which conveniently allows the filter screen/membrane to be varied, and replaced after each use if desired.
- Fig. 1 shows an embodiment of the invention.
- Fig. 4 is an exploded cross-sectional view of a filter unit.
- Fig. 5 is a top view of the filter unit of Fig. 5.
- Fig. 6 is a plan view of the locking nut of Fig. 5.
- Fig. 7 is a flow diagram for operating a sampling apparatus in accordance with an embodiment of the invention.
- An inlet is formed in one side wall of the case in the form of a penetration 12 which may contain a PTFE fitting insert sealed to render it watertight.
- a pre-treatment filter unit 14 described in greater detail below, for removing interferences from the water matrix which is pumped through the apparatus.
- the pumping is accomplished by pump 18, which in the preferred embodiment is a peristaltic pump, capable of pumping in forward and reverse directions.
- An electric motor 40 drives the pump, while tubing 16 leads from the filter unit to the pump and tubing 20 is between the pump and three way electrically controlled valve 22.
- the valve is in fluid communication with liquid container 32 through tubing 28, which serves to backflush the apparatus through the pre-treatment unit.
- the valve also communicates through tubing 30 with solid phase extraction device 34.
- the device 34 extracts analyte of interest from the water matrix, while the discharge flows through tubing 35 to an outlet which is rendered watertight.
- the extraction device 34 may be comprised of a cartridge utilizing any desired solid phase media.
- the media may be selected to preferentially capture DNA, RNA and/or other biological or chemical molecules.
- Device 34 serves to concentrate and integrate the analyte over repetitive sampling cycles. It has enough capacity to capture the desired amount of analyte. The device is brought to the laboratory after the total sampling period and is eluted (emptied), after which the analyte is analyzed using chemical or biological laboratory procedures.
- the invention further has capability to be programmed for a specific sampling situation. For instance, if a particular contaminant/organism is known to proliferate at night, the sampler may be programmed to sample during that time.
- an aspect of the invention is to successively withdraw discrete samples of water from which analyte is extracted, while integrating the analyte which is extracted from successive samples. This allows samples to be taken over a relatively long period of time so that changing water conditions are represented in the integrated analyte.
- Fig. 2 depicts a block diagram for an embodiment of the programmable controller which is indicated by electronics 38 in Fig. 1.
- the controller is comprised of a clock 50 activated by a start/stop switch 52, and three counter circuits, 54, 56 and 58.
- Counter 54 is for the overall pump cycle
- counter 56 is for the time per cycle that the pump is operating in forward mode
- counter 58 is for how often the pump flushes.
- Two output displays 60 and 62 consist of 4-digit LCD readouts summarizing the total elapsed time the device has been in operation and elapsed time of pump operation, respectively.
- the controller sends signals via relays 64 and 66 to a control unit for motor 40 for forward and reverse operation for the sampling and flushing cycles respectively.
- programming the apparatus includes first setting the total cycle time from 1 to 99 minutes (pulses). The pump on time is then set from 1 minute to the total cycle time. Then, the cycle to flush on is set. If the settings are 5, 3, and 2, then the pump will run for 3 minutes every 5 minutes with a flush cycle after the completion of every 2 main cycles.
- the system may be configured so that no pump activity happens on the initial cycle, when time is provided to place the apparatus.
- a feature of invention is that the total time of operation of the pump is indicated by display 62. From this, with a means of calculating the number of pump rotations, the total volume of water sampled can be easily calculated. This obviates the need for more complicated equipment to measure sample volume. Other methods of flow measurement are also possible.
- an aspect of the invention is that the need for storage containers for the water matrix is obviated by matching the fluid transport system with the flow characteristics of the extraction device so that a continuous flow without fluid storage is achieved through the device over successive sampling cycles.
- a graph or relationship of flow velocity in cm/hr vs. pressure for the extraction device used may be derived or obtained from the manufacturer. Pressure losses vary with flow and include frictional losses through the tubing as well as pressure drop due to the filtration and the collecting apparatus. It was estimated that, at the operating flow rates, the system pressure losses are minor for most components except the extraction device itself unless severe plugging of the filtration system occurs. The pressure drop across the extraction device depends on the size of the column and the packing.
- the illustrative extraction device is the DEAE 650S resin by Toyopearl which uses a methacrylic polymer phase material.
- the particular device (also called a "column") used had a 7.5 mm diameter and a 8.5 cm length.
- the pump chosen, capable of attaining such pressures was a peristaltic pump having an integral variable frequency drive controller for controlling speed and direction of rotation.
- the flow rate is altered by changing rotational speed as well as by changing the diameter of tubing running through the pump.
- a specific pump for purposes of illustration, is the ProflexTM Series 710 Mini-Peristaltic Pump having a maximum flow capacity of up to 58 ml/min depending on the diameter (ID) of internal tubing, corresponding to a rated top speed of 93 RPM.
- fluid is drawn in through the intake 76 of the female fitting. Flow enters through the top recessed aperture, wherein the recessed portion serves to lessen dead volume in the device. As flow enters the device it immediately passes a series of successively finer filter membranes starting with a screen 80 for removing large debris such as stones and plant material. Successively finer mesh and membrane filters (82, 84, 86 and 88) remove finer and finer particulate matter without removing the analyte from the matrix. The flow rate through the surface area is such that an excessive pressure drop across the filter media is not encountered. Silver wool may be placed between the screen 80 and the membrane filter 82 for the control of bacterial growth.
- a ferrule 110 and compression fitting 104 are threaded and inserted into the female end of the male connector fitting 94.
- the (e.g. TFE) Tubing enters and is held securely by the ferrule and compression fitting combination. Flow continues through the tubing to the rest of the sampler.
- the overall flow system may be configured to allow backflushing through the filter to clear it of debris.
- taper 78 of the female fitting minimizes dead space and promotes the flow of fresh rather than stale water matrix into the sampler.
- Taper 98 of the male fitting ensures that flow emanates from the entire surface area of the frit 90.
- a flow chart depicted in Fig. 8 illustrates the use of the water sampling apparatus.
- the procedure is begun (block 120) by connecting the circuit to battery 36 (block 122).
- the cycle time, pump time, and flush time are then programmed in the respective counters (block 124) after which the start switch 52 is activated (block 126).
- the sampler is then positioned and anchored in the stream or other body of water (block 128) and is left alone to allow the sampling events to elapse (block 130).
- the sampler is then retrieved, the analyte extraction device is removed and sent to the laboratory for being analyzed (block 132), whereupon the procedure is ended (block 134).
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU48543/00A AU4854300A (en) | 1999-05-19 | 2000-05-18 | Water sampling with analyte extraction and integration |
CA002372702A CA2372702C (en) | 1999-05-19 | 2000-05-18 | Water sampling with analyte extraction and integration |
JP2000618724A JP2002544519A (en) | 1999-05-19 | 2000-05-18 | Water sampling with analyte extraction and accumulation |
EP00930783A EP1194774A4 (en) | 1999-05-19 | 2000-05-18 | Water sampling with analyte extraction and integration |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/314,004 US6306350B1 (en) | 1999-05-19 | 1999-05-19 | Water sampling method and apparatus with analyte integration |
US09/314,004 | 1999-05-19 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2000070339A1 true WO2000070339A1 (en) | 2000-11-23 |
Family
ID=23218118
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2000/013507 WO2000070339A1 (en) | 1999-05-19 | 2000-05-18 | Water sampling with analyte extraction and integration |
Country Status (6)
Country | Link |
---|---|
US (1) | US6306350B1 (en) |
EP (1) | EP1194774A4 (en) |
JP (1) | JP2002544519A (en) |
AU (1) | AU4854300A (en) |
CA (1) | CA2372702C (en) |
WO (1) | WO2000070339A1 (en) |
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WO2009001142A1 (en) * | 2007-06-26 | 2008-12-31 | Balvinder Singh Nagi | Filtering system with means for purging the system |
CN103033397A (en) * | 2012-12-12 | 2013-04-10 | 山东省农业科学院农业资源与环境研究所 | Field portable sampling device and using method thereof |
CN103424283A (en) * | 2013-09-10 | 2013-12-04 | 中国环境科学研究院 | Portable underground water sampler |
CN105758675A (en) * | 2016-04-26 | 2016-07-13 | 天津市环境保护科学研究院 | Active sampler for water persistent organic pollutants based on suction filtration and preconcentration |
CN108152464A (en) * | 2017-12-11 | 2018-06-12 | 百奥森(江苏)食品安全科技有限公司 | A kind of continuous type water quality detecting device |
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GB0611254D0 (en) * | 2006-06-07 | 2006-07-19 | Selsdon Leslie D | Portable filtration apparatus with a remote monitoring facility |
US7691602B1 (en) | 2007-03-02 | 2010-04-06 | Hanson Technologies, Inc. | Agricultural screening system and method for detection of infectious microorganisms |
US8857279B2 (en) * | 2008-03-03 | 2014-10-14 | William P. Hanson | Analyte screening and detection systems and methods |
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US9341609B2 (en) * | 2010-02-08 | 2016-05-17 | Arizona Board Of Regents Acting For And On Behalf Of Arizona State University | Methods and systems for ultra-trace analysis of liquids |
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US9921139B1 (en) | 2010-10-06 | 2018-03-20 | The United States Of America As Represented By The Secretary Of The Department Of The Interior | Handheld, underwater suction sampler |
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- 1999-05-19 US US09/314,004 patent/US6306350B1/en not_active Expired - Lifetime
-
2000
- 2000-05-18 JP JP2000618724A patent/JP2002544519A/en active Pending
- 2000-05-18 WO PCT/US2000/013507 patent/WO2000070339A1/en active Application Filing
- 2000-05-18 EP EP00930783A patent/EP1194774A4/en not_active Ceased
- 2000-05-18 AU AU48543/00A patent/AU4854300A/en not_active Abandoned
- 2000-05-18 CA CA002372702A patent/CA2372702C/en not_active Expired - Fee Related
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US4554826A (en) * | 1982-01-28 | 1985-11-26 | Barry Judith A | Automatic depth-determining aquatic sampling device |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2009001142A1 (en) * | 2007-06-26 | 2008-12-31 | Balvinder Singh Nagi | Filtering system with means for purging the system |
CN103033397A (en) * | 2012-12-12 | 2013-04-10 | 山东省农业科学院农业资源与环境研究所 | Field portable sampling device and using method thereof |
CN103424283A (en) * | 2013-09-10 | 2013-12-04 | 中国环境科学研究院 | Portable underground water sampler |
CN105758675A (en) * | 2016-04-26 | 2016-07-13 | 天津市环境保护科学研究院 | Active sampler for water persistent organic pollutants based on suction filtration and preconcentration |
CN108152464A (en) * | 2017-12-11 | 2018-06-12 | 百奥森(江苏)食品安全科技有限公司 | A kind of continuous type water quality detecting device |
CN108152464B (en) * | 2017-12-11 | 2020-10-27 | 绿桥(泰州)生态修复有限公司 | Continuous type water quality testing device |
Also Published As
Publication number | Publication date |
---|---|
JP2002544519A (en) | 2002-12-24 |
EP1194774A1 (en) | 2002-04-10 |
US6306350B1 (en) | 2001-10-23 |
AU4854300A (en) | 2000-12-05 |
EP1194774A4 (en) | 2009-03-11 |
CA2372702C (en) | 2004-11-02 |
CA2372702A1 (en) | 2000-11-23 |
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