WO2013019157A1 - Récipient à échantillon muni d'un bouchon et procédé de mesure utilisant ledit bouchon - Google Patents

Récipient à échantillon muni d'un bouchon et procédé de mesure utilisant ledit bouchon Download PDF

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Publication number
WO2013019157A1
WO2013019157A1 PCT/SE2012/050846 SE2012050846W WO2013019157A1 WO 2013019157 A1 WO2013019157 A1 WO 2013019157A1 SE 2012050846 W SE2012050846 W SE 2012050846W WO 2013019157 A1 WO2013019157 A1 WO 2013019157A1
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WO
WIPO (PCT)
Prior art keywords
stopper
sensor
section
sample
sample container
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
Application number
PCT/SE2012/050846
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English (en)
Inventor
Johan WIKNER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
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Individual
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Filing date
Publication date
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Publication of WO2013019157A1 publication Critical patent/WO2013019157A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/508—Rigid containers without fluid transport within
    • B01L3/5082—Test tubes per se
    • B01L3/50825—Closing or opening means, corks, bungs
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/04—Closures and closing means
    • B01L2300/041—Connecting closures to device or container
    • B01L2300/042—Caps; Plugs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/04—Closures and closing means
    • B01L2300/046—Function or devices integrated in the closure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/06—Auxiliary integrated devices, integrated components
    • B01L2300/0627—Sensor or part of a sensor is integrated
    • B01L2300/0663—Whole sensors
    • 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
    • G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
    • G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
    • G01N2001/2071—Removable sample bottle

Definitions

  • the following invention is directed towards a stopper according to claim 1 , a sample container according to claim 8, and a method according to claim 9.
  • Sensors are rapidly developed for continuous measurements of different dissolved quantities in aqueous samples. Placing and removing a sensor in a gas tight container may pose problems.
  • the sensor has to be attached to the container in a gas tight manner and sensors cables should be possible to connect from the outside.
  • a gastight seal between the container, the sensor, and the ambient environment has to be established when the sensor is placed in the container, and broken again when the sensor is removed.
  • air bubbles should not be trapped inside the container as they may interfere with the measurement.
  • the sensor should be easy to remove after measurement and not get stuck in the container. In sample containers which are filled with sample fluids and emptied with regular intervals the problem manifests itself regularly.
  • a stopper device for applying a sensor wherein said stopper comprises:
  • first section providing a first tapered section for fitting to a correspondingly tapered section of a sample container, said first section also comprises a second tapered section adjacent said first tapered section, said second tapered section has a more acute angle than the first tapered section for avoiding trapping of air bubbles during measurement, when said stopper is fitted to a sample container,
  • the first section is provided with a sealing means, preferably in the form of at least one o- ring, such that a gastight seal is provided between the stoppers first tapered section and the sample container,
  • the first section is provided with a void wherein at least part of the sensor can be fitted in an gas tight manner, said void runs through the first section,
  • a second section is provided with a channel for a sensor cable, said second section is also provided with removal means, arranged to raise the stopper from the sample container, thus facilitating removal of said stopper.
  • the stopper device may be used to close a container, specifically a sample container such as a sample bottle. Alternatively, the stopper device may be referred to as a stopper.
  • a container may be used for measuring water samples using a sensor. Water samples may be take e.g. from lakes and the sea, from process water used in various processing industries, from sewage, and water purification plants.
  • said void may be adapted for an optode sensor, preferably being capable of making online registration of respiration values from a sample of water from a coastal region.
  • respiration values may be measured in the form of oxygen content.
  • said sensor may be able to record any of the following parameters, pH, temperature, salinity, conductivity, or other parameters.
  • the removal means may be constituted by at least one screw, being arranged to raise said stopper by contacting the sample container when screwed, preferably the top of the sample container.
  • said sample container may be a sample bottle.
  • said stopper device may be arranged to fit a sample bottle of the size of at least 100 ml preferably at least 500 ml, more preferably of 1000 ml.
  • a sample container comprising a stopper device according to any one of aspect or embodiments described herein.
  • a method for measurement comprising the following steps:
  • the method may be used for measurement of pelagic respiration in aquatic samples, such as samples of coastal waters.
  • the registration of measurement values by said control unit may be a registration of respiration values.
  • the sample may be provided in the sample bottle.
  • said sample may have a size which is larger than 100 ml, preferably larger than 500 ml, more preferably a size of 1000 ml.
  • said control unit may be portable, preferably in the form of a portable computer such as a laptop, such that online measurement can be performed outside a normal laboratory environment.
  • measurement of the following parameters may be provided, H, temperature, salinity, conductivity, or others.
  • Fig. 1 Shows a stopper, release means and a seal, for an embodiment of the invention
  • Fig. 2 Shows a stopper according to an embodiment of the invention.
  • Fig. 3 Shows an experimental set-up for measurement with stopper, sample bottle and computer.
  • Fig. 4 Shows agreement of respiration measurement with established current method.
  • Fig. 5 Shows accuracy of respiration measurement.
  • Fig. 6 Shows detection limit and precision of respiration measurement.
  • a stopper 1 for providing a sensor in a gastight manner to a sample container is described.
  • the stopper 1 may also be referred to as a stopper device 1.
  • Said stopper has a first section 4 provided with two tapered sections 6 and 7.
  • the first tapered section 6 is arranged to be able to fit to a sample container's neck.
  • the second tapered section 7 is provided for avoiding trapping of gas bubbles during sampling.
  • the angle of the second tapered section 7 is more acute than that of the first tapered section 6.
  • a second section 5 is provided with non tapered sides.
  • the second section has through holes 8 for receiving release means 1 1.
  • Said release means can optionally be provided with an adjustment means 12.
  • the release means 1 1 is arranged to be able to contact the upper surface of a sample container.
  • the release means 11 is preferably constituted by at least one screw.
  • the adjustment means 12 is preferably constituted by at least one nut.
  • the stopper has a first void divided into two void sections 2 and 3. On of the void sections 3 is arranged to be able to receive the sensor discussed above. Preferably a section of the sensor is arranged to be fitted into said void section 3. Said void section 3 preferably has the form of a cylinder and is a through hole with a diameter that allows a sensor to be fitted thereto in a gas tight manner. The shape of the void section 3 can also be tapered. Adjacent and linked to said void section 3 is a larger void section 2 positioned. Said void section 2 is optimized for housing wiring and contacts to the said sensor. This void section 2 can be tapered or have cylinder shape.
  • the stopper can be provided with a notch 14 for receiving a sealing means 10, preferably in the form of an O-ring. Said notch can be suspended with if another type of seal is provided.
  • the main application of said stopper is for an Optode sensor.
  • Said sensor is preferably used in an online measurement of respiration in coastal waters. However adjustments of the stopper would allow it to be used with other sensors as well.
  • stopper 1 In a method of measurement of respiration of coastal waters said stopper 1 may be utilized, the method comprises the following steps:
  • the sample size can be larger than 100 m!, preferably larger than 500 ml. However should a smaller sensor be used a smaller sample size could be allowed.
  • Said control unit is preferably provided with a computer program product able to store the sensors measurement values, and evaluate the said values, such that an online
  • stopper and method also are applicable for fresh water, sewage water, and process water application. It has been shown to be possible to record oxygen content in fresh water as well.
  • the invention is further described in the following:
  • Respiration is one of the most important processes in the biosphere, from the ievel of metabolism in individual organisms to regulation of C0 2 and O2 levels in the atmosphere. Respiration is also fundamental to understand occurrence of hypoxic waters and the balance between auto- and heterotrophic processes in the sea and its influence of the downward transport of biomass through sedimentation (i.e. the marine biological pump). Measurement of biological oxygen demand (BOD) is also a standard method in controlling the quality of waste waters.
  • BOD biological oxygen demand
  • estimates of respiration are important to understand mechanisms behind current societal concerns like the increasing levels of C0 2 in the atmosphere (i.e., the Greenhouse effect) and oxygen deficiency in coastal water bodies (hypoxia). Understanding the Ievel and control of respiration is, therefore, an important issue for natural science.
  • respiration studies currently are scarce, compared with C0 2 fixation measurements, partly due to methodological reasons.
  • sample volumes are typically 60-120 ml, excluding sufficient numbers of larger zoop!ankton to determine their contribution to the measured respiration rate.
  • the in vitro dark bottle incubation measuring change in oxygen concentration with the Winkier technique is the most commonly used method, comprising more than 90 % of the values reported in marine pelagic environments.
  • a sensor technique to measure oxygen is based on the Clark electrode. It has a reported precision of 0.1 ⁇ when measuring oxygen concentration. However, the electrode has an inherent oxygen consumption corresponding to 0.3 mmol m "3 d "1 , which is higher than the detection limit of the high-precision Winkler technique. Lower inherent oxygen consumption is reported at the Unisense® web page, however, no published reference or calculation is provided. In the original reference to the method a precision of 2.4 mmol m "3 d "1 or higher is reported for respiration measurement. This is a more than 10 times higher uncertainty than the results of the high precision Winkler technique.
  • DLQ Dynamic luminescence quenching
  • Oxygen concentration in the respiration experiments were measured with four commercially available Optodes with an integrated temperature sensor (Optode 3835, Aanderaa Data Instruments AS, www.aadi.no). This type of sensor has been frequently used. As with most other oxygen sensors Optodes measure the partial pressure of oxygen dissolved in water. By tuning the sensor to the salinity of the water sample, data were automatically converted to the absolute oxygen concentration ⁇ [0 2 j, pmol dm "3 ) using reported formulas. Sensor readings were plotted and logged in real-time using the software package Oxyview by Aanderaa Data Instruments AS (www ; aadi, no).
  • FIG. 3 shows a schematic diagram of the respiration measurement unit: 21 , Immersion cooler; 22, Water bath with thermostat; 23, Sample bottles with cables connected to the sensor plug in the stopper; 24, Magnetic stirrers; 25, Serial Hub; 26, USB Hub for 5 V power to sensors; 27, Portable computer.
  • a sample container such as an analysis bottle, and mounting of the Optode may be utilized as follows: A 1 dm 3 dear g!ass bottle (Cat. No. HAVA23231607, VWR) with a NS60 grounded neck, (inner 0 60 mm) was selected as the incubation vessel. This provides a sample volume about 10 times larger than is typically used in Winkler titrations.
  • An important advantage of the present technique is that, at least in coastal areas (5-10 individuals dm "3 ), large zooplankton may a!so be sampled in a statistically acceptable number to be included in the respiration estimate.
  • a stopper device 1 may be constructed from acrylic plastic (po!y(methylmethacry!ate)) to mount the Optode in, forming an air-tight seai by an o-ring, e.g.Nitrile 50.52 x 1.78 mm, while still allowing easy removal of the stopper after incubations. The latter is further aided by release means 1 1 , such as three screws placed in the upper part of the stopper device 1 . The air-tight seal ensures that minimum gas exchange between the sample and the surrounding air.
  • the stopper device 1 has a conical shape, similar to the design of typical Winkler bottles (Biochemical Oxygen Demand bottles), to allow air bubbles to readily escape.
  • the stopper device 1 allows simple mounting and dismounting of the Optode onto the sample bottle, without the trapping of air bubbles.
  • the Optode adaptor foot is inserted into the stopper tube and sealed by 2 o-rings towards the tube wall.
  • the cable attachment screw will lock the Optode in the stopper device 1 from the outside.
  • a magnetic stirrer Ikamag RET, www.ika.com
  • 2 cm magnetic rods were used for each analysis bottle. The magnetic stirrer was set at 80 rpm to mix the water in the analysis bottle.
  • a stand may be provided to keep bottles in position during rough seas and maintain proper stirring and temperature control of the samples.
  • the thermostat heated water bath may have inner dimensions of 32.5 cm (length), 30 cm (width) and 14.5 cm (depth) (Julabo 12 B, www.vwr.com), allowing the sample bottle to be covered by liquid up to the lower part of the neck.
  • the bath was used in conjunction with an immersion cooler (Julabo FT 200, www.vwr.com) to control the incubator bath e.g. in a range of 0-30 °C with a precision of ⁇ 0.05 °C.
  • 30 % polypropylene glycol may be used as the bath liquid.
  • the bottles and immersion cooler probe may be placed in a specially designed plastic holder to keep them in a fixed position and promote stable temperatures.
  • Samples may be protected from light with a cardboard box and black plastic bag.
  • the level of light irradiation inside the cardboard box may be below the detection limit ( ⁇ 0.04 ⁇ m "2 s "1 ) at an ambient room light of 17.6 pmol m "2 s "1 .
  • Light inside the incubators may be measured with a Li-Cor data logger (L!-1000) and a spherical quantum sensor for photosynthetic active radiation (Biosperical Instruments, QSPL 2101 , www.biospherical.com) immersed in the water bath.
  • drift-corrected Optode calibrated with Winkler measurements may be performed as follows:
  • the Optode measurements that were corrected for drift showed good agreement with respiration rates determined by the Winkler titration method, Fig. 4.
  • the Optode-based rates were 105 % and 101 % that of the Winkler-based values at the in situ and + 3°
  • the detection limit of the Optode in the field was about 3 times higher than the best reported high-precision Winkler titrations from two field studies, while being comparable to other studies using Winkler titrations.
  • the Optode sensor showed the best precision for sensor-based techniques that have been reported in the literature. Pre-treatment of the stopper and Optode in low oxygen also show a potential to approach the best precision reported (i.e. 0.15 mmol m "3 d "1 ).
  • the primary advantage of the Optode method is that it provides a simple and operator- independent protocol to measure respiration in natural waters without inherent oxygen consumption.
  • the Optod can run for several years with annual calibration and the sensor foil alone can be renewed to extend the life-time of the Optode, promoting good economy. This may promote the incorporation of respiration measurements in field studies and make the use of respiration data in environmental monitoring programs feasible. Due to the ability to easily perform many measurements, the Optode technique could lead to new insights about factors that affect respiration rates. Additionally, with a higher rate of data collection in time and space, a better basis for establishing regional and g!obal carbon budgets may be gained.
  • the developed analytical unit and protocol was able to be used aboard research vessels, even during rough seas.
  • the time from sampling to the start of 4 incubations was typically less than 20 minutes.
  • the working time was limited to emptying, rinsing and filling sample bottles, followed by setting up the measurements in the Optode software.
  • the avoidance of wet chemistry minimized operator influence on the results, resources, waste, and improved safety for technical staff.
  • the Optode method required stringent temperature control and evaluation of time series.
  • the stable temperature ( ⁇ 0.05 °C) that was routinely achieved minimized the temperature influence on oxygen measurements.
  • One further advantage of the presented Optode method is the 3-20 times larger sample volume (1 dm '3 ) obtained compared to Winkler titrations (0.05-0.3 dm "3 ).
  • a larger sample includes more organisms. This is advantageous if a general estimate of plankton oxygen consumption. A larger sample also may reduce other containment effects and allows extended incubation time.
  • the current setup of present technique would, therefore, give an accurate estimate of microbial plankton respiration comprising, on average, 99 % of aquatic respiration.
  • the online continuous monitoring of the oxygen concentration by computer software precluded assumptions of linearity of oxygen change. This also enabled a correct mathematical model to be applied for rate determination. However, approximately linear development with time was typically observed at most sites investigated.
  • the present Optode method is appiicab!e to other aquatic environments where respiration rates are above 0.3 mmol m "3 d " ⁇ Fig. 6.
  • the detection limit must be lowered.
  • Pre-incubating the stopper and Optode in low oxygen water 24 hours prior to measurements, to remove oxygen bound to the plastic material may be performed. This improved the detection limit to 0.19 mmol m "3 d ⁇ 1 .
  • the stopper device 1 and Optode may be without plastic material.
  • Fig. 6 shows performance of the dynamic luminescence technique as measured with the Optode sensor.
  • Accuracy shows the relative deviation from Winkler titrations when the drift correction is applied.
  • Precision shows the combined 95 % confidence intervals for field incubations and the drift subtraction.
  • the detection limit is defined as one 95 % confidence interval.
  • the system drift is the mean of 37 measurements in autociaved sea water samples.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Clinical Laboratory Science (AREA)
  • Hematology (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

La présente invention concerne un dispositif de type bouchon permettant la mise en œuvre d'un capteur, ledit bouchon comprenant une première partie constituée d'une première partie conique pouvant être introduite dans une partie pareillement conique d'un récipient à échantillon, ladite première partie comprenant également une seconde partie conique adjacente à ladite première partie conique. La première partie est équipée d'un moyen d'étanchéité assurant une étanchéité aux gaz entre la première partie conique du bouchon et le récipient à échantillon. La première partie comporte un espace vide dans lequel au moins une partie du capteur peut être introduite d'une manière étanche aux gaz. La seconde partie comporte une gouttière pour câble de capteur. L'invention concerne également un récipient à échantillon et un procédé de mesure.
PCT/SE2012/050846 2011-07-29 2012-07-20 Récipient à échantillon muni d'un bouchon et procédé de mesure utilisant ledit bouchon Ceased WO2013019157A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201161512947P 2011-07-29 2011-07-29
US61/512,947 2011-07-29

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WO2013019157A1 true WO2013019157A1 (fr) 2013-02-07

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3136440A (en) * 1963-06-25 1964-06-09 Becton Dickinson Co Self sealing pierceable stopper for sealed containers
US3958572A (en) * 1974-12-16 1976-05-25 Corning Glass Works Blood collecting and separating assembly stopper
US3974930A (en) * 1975-04-09 1976-08-17 Becton, Dickinson And Company Stopper for specimen container
EP0208949A2 (fr) * 1985-07-08 1987-01-21 Plischke & Buhr KG Dispositif de mesure de pression, en particulier pour détecter des variations de quantités de gaz dans une enceinte de réaction fermée
US5085759A (en) * 1989-11-13 1992-02-04 Duncan Instrument Company Apparatus for rapid biological oxidation demand of liquids
US5447374A (en) * 1994-01-03 1995-09-05 Fts Systems, Inc. Positioning device for temperature sensor in freeze drying
US5770153A (en) * 1994-07-07 1998-06-23 Wtw Wissenschaftlich-Technische Werkstatten Gmbh Integrated analytical device for determining the gas consumption of matter

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3136440A (en) * 1963-06-25 1964-06-09 Becton Dickinson Co Self sealing pierceable stopper for sealed containers
US3958572A (en) * 1974-12-16 1976-05-25 Corning Glass Works Blood collecting and separating assembly stopper
US3974930A (en) * 1975-04-09 1976-08-17 Becton, Dickinson And Company Stopper for specimen container
EP0208949A2 (fr) * 1985-07-08 1987-01-21 Plischke & Buhr KG Dispositif de mesure de pression, en particulier pour détecter des variations de quantités de gaz dans une enceinte de réaction fermée
US5085759A (en) * 1989-11-13 1992-02-04 Duncan Instrument Company Apparatus for rapid biological oxidation demand of liquids
US5447374A (en) * 1994-01-03 1995-09-05 Fts Systems, Inc. Positioning device for temperature sensor in freeze drying
US5770153A (en) * 1994-07-07 1998-06-23 Wtw Wissenschaftlich-Technische Werkstatten Gmbh Integrated analytical device for determining the gas consumption of matter

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