Classifications

• • 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
  • G01N1/02—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
• • 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
  • G01N2001/2064—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 using a by-pass loop
• • 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
  • Y10T436/11—Automated chemical analysis
• • 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
  • Y10T436/11—Automated chemical analysis
  • Y10T436/117497—Automated chemical analysis with a continuously flowing sample or carrier stream
• • 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
• • 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
  • Y10T436/2575—Volumetric liquid transfer

Definitions

• the invention relates to a device designed to carry out the continuous sampling and analysis of a liquid effluent, for example from an industrial installation.
• these waters are subjected to a flocculation treatment using iron sulphate and lime, then to the decantation of the sludge, all of these operations being carried out under
• the purpose of this treatment is to remove heavy metals.
• the water is collected in a secondary basin where it is analyzed, before being discharged into the environment. This analysis is most often carried out manually, on the basis of one or two daily samples from the said secondary basin. Each sample is analyzed, for example using a plasma torch coupled to a mass spectrometer.
• the devices used for the analysis of industrial effluents such as ion chromatography or capillary electrophoresis devices do not allow working on a continuous sample of said effluent.
• These devices are, on the contrary, designed to work from samples.
• these samples are collected in test tubes and these are placed on a carousel making it possible to take these samples in turn in front of the sampling means of these devices. This results in extremely long manual handling and is incompatible with continuous monitoring of effluents.
• the invention aims to solve this problem.
• the invention relates to a device for the continuous sampling and analysis of a liquid effluent.
• this device comprises:
• This device allows samples to be taken continuously and, therefore, no information concerning possible pollution of the liquid effluent is lost.
• the various temporary storage containers are successively filled, then emptied inside the collection cell where a sample collection representing a tiny part of this volume is carried out, to then be treated by the analysis device (s).
• the rest of the volume of liquid that has circulated in the sample cell is evacuated to the outside or is stored for later analyzes. Thus, if pollution is noted, it is possible to carry out more precise or larger analyzes. number of chemical elements.
• the device according to the invention also comprises:
• second distribution means connected to the outlet of the sampling cell and making it possible to empty the liquid contained in this cell in the temporary storage container from which this liquid originates, before this storage container is refilled,
• the evacuation pipe can be connected to a sampling device for the storage and preservation of samples, so as not to lose information. This is the case, for example, when the measurement carried out exceeds a threshold value.
• the discharge pipe can also be connected to a pipe in which the initial liquid effluent to be analyzed circulates, downstream of the aforementioned diversion means. This is possible since only the very small fraction of liquid sampled and then taken to the measuring device is possibly contaminated with chemical reagents while almost all of the diverted effluent is absolutely not polluted.
• the means for diverting into consist of a solenoid valve or a proportional pump, these means being controlled by a flow meter measuring the flow rate of the liquid effluent, so as to take a constant proportion of the latter.
• a flow meter measuring the flow rate of the liquid effluent
• the first and second dispensing means are constituted by a dispensing valve.
• the temporary storage containers are fixed and the dispensing valve makes it possible to direct the flow of diverted liquid effluent in turn, in the direction of the temporary storage containers.
• the distribution means could be constituted by mobile temporary storage containers moving successively in front of the outlet orifice of a pipe connected to the diversion means.
• the measuring device is a capillary electrophoresis device which makes it possible to carry out a rapid measurement, in approximately 10 minutes.
• FIG. 1 is a diagram illustrating the device for the continuous sampling and analysis of a liquid effluent according to the invention.
• the device according to the invention comprises a main pipe 2 in which the liquid effluent to be analyzed flows.
• This main pipe 2 is provided with a flow meter 4 and means 6 for permanently diverting part of the flow of the liquid effluent to be analyzed, in the direction of a diversion pipe 8.
• the means 6 are constituted by a solenoid valve or a proportional pump and are slaved to the flow meter 4, as shown by an arrow in FIG. 1.
• these means 6 make it possible to take a constant proportion of the flow rate of the liquid effluent circulating in the main pipe 2.
• the device according to the invention comprises at least two temporary storage containers 10.
• each storage container 10 is provided with an agitator 11 (magnetic or propeller).
• the diversion pipe 8 is connected, via first distribution means 12 and distribution pipes 14, to each of these temporary storage containers.
• Each temporary storage container 10 is provided with first and second emptying means, referenced respectively 16 and 18 and generally constituted by a valve.
• the valve 16 is placed on an inlet pipe 20 with several branches, connecting each temporary storage container 10 to a sampling cell 22.
• the inlet pipe 20 is advantageously provided with a pump 24.
• this pump n is not mandatory.
• a capillary 28 capable of plunging into said sampling cell 22 makes it possible to take the samples at regular intervals and to route the minute quantities taken towards at least
• the collection cell 22 is emptied as soon as the sample or samples are taken. It is then refilled.
• this sampling cell 22 is filled in its upper part and emptied in its lower part by means of an outlet pipe 32.
• other embodiments of said cell are possible and one of them is described later.
• the outlet pipe 32 is connected to the second distribution means 36.
• the latter generally consist of a distribution valve which makes it possible to drain the liquid contained in the sampling cell 22 in a pipe dispenser 37 and then into the temporary storage container 10 from which this liquid comes.
• the inlet pipe 20, the sampling cell 22, the outlet pipe 32, the second distribution means 36 and the distribution pipe 37 thus form a circulation loop for the diverted liquid.
• each temporary storage container 10 is mounted on an evacuation pipe 38.
• This evacuation pipe 38 can be connected at its end 40, for example to a sampling device (not shown) which allows store representative samples of the circulating liquid flow for later analysis.
• the evacuation pipe 38 comprises a valve 42 placed at the intersection between said pipe 38 and a return pipe 44.
• This return pipe 44 connects the main 2, downstream of the diversion valve 6.
• the outlet pipe 32 can also include a branch branch 46 allowing it to be connected to the discharge pipe 38.
• the latter is controlled so as to direct the effluent to one of the distribution pipes 14 and a first corresponding storage container 10.
• a detector (not shown) acts on the dispensing valve 12 so as to modify the position of the latter to authorize the filling of a second temporary storage container 10.
• the valve 16 is open so as to fill the sampling cell 22.
• the sampling cell 22 is then emptied and its content is directed either directly to the main line 2, via lines 32, 46 and 44, either towards the end 40 of the evacuation line 38, or again towards the first storage container 10 from which it comes.
• this second container is emptied into the sampling cell 22 where the operations mentioned above take place.
• a third or nth provisional storage container 10 is filled. These containers are emptied in the order of their filling in the sampling cell 22.
• a When the content of the sampling cell 22 is not discharged directly but is returned a second time to the storage container 10 from which it comes, it is led again into the sampling cell 22 for a new intake of sample, before the contents of another storage container 10 is emptied into this cell. This makes it possible to entrain the few droplets of liquid which could have remained in the inlet pipe 20. The measurements carried out are therefore more reliable.
• the measuring device 30 is a capillary electrophoresis device which has the advantage of carrying out an analysis in approximately 10 minutes.
• the sampling cell 22 has the structure illustrated in FIG. 2. This cell has a cubic or cylindrical shape delimited by walls 50. It has in its upper part an opening 52, intended for the passage of the capillary 28 (not shown ).
• the cell 22 internally comprises an "overflow" bowl 54, for example in the form of a truncated cone, the base of which is connected to an inlet pipe 20 '.
• this bowl 54 is less than the height of the cell 22, so that the liquid entering the line 20 'progressively rises in said bowl and overflows inside the cell 22 as shown by the arrows 56
• the sampling cell 22 has at its base means 58 (for example an inclined plane) allowing the collection of the liquid having overflowed from the bowl 54 and its conduct in the direction of an outlet pipe 32 '.
• the diversion valve 6 makes it possible to take 1/2000 of the flow of the effluent to be analyzed circulating in the main pipeline 2.
• the device comprises two temporary storage tanks 10 of a volume adapted to the maximum flows treated by the power plant ( ⁇ of 300 ml at 15 1) in flared shape.
• the flow rate of circulation of the liquid inside the device is 160 ml / min.
• the volume of the sampling cell 22 is 4 ml.
• the first measuring device 30 is a capillary electrophoresis device applied to the analysis of anions such as Cl “ , SC * 4 2 ⁇ , Br ⁇ , CIO.] -, HC0 3 " , N ⁇ 2 ⁇ , ⁇ 3 ⁇ , F -, Cr0 4 2 " , HP0 4 2 ⁇ , SCN-. •
• the second measuring device 30 is an ion cation chromatography device.
• the sampling cell 22 is advantageously mounted on a lifting device, so that it can be raised by about ten centimeters for a few seconds.
• the capillary 28 then acts as a siphoning pipe. This allows very simple injection into the capillary electrophoresis device, a liquid volume representative of the diverted effluent.

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• Life Sciences & Earth Sciences (AREA)
• Health & Medical Sciences (AREA)
• Chemical & Material Sciences (AREA)
• Biochemistry (AREA)
• Physics & Mathematics (AREA)
• Analytical Chemistry (AREA)
• General Health & Medical Sciences (AREA)
• General Physics & Mathematics (AREA)
• Immunology (AREA)
• Pathology (AREA)
• Hydrology & Water Resources (AREA)
• Engineering & Computer Science (AREA)
• Food Science & Technology (AREA)
• Medicinal Chemistry (AREA)
• Sampling And Sample Adjustment (AREA)

Applications Claiming Priority (3)

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• 1994
  • 1994-07-19 FR FR9408909A patent/FR2722879B1/fr not_active Expired - Fee Related
• 1995
  • 1995-07-18 WO PCT/FR1995/000963 patent/WO1996002818A1/fr not_active Application Discontinuation
  • 1995-07-18 US US08/617,786 patent/US5723093A/en not_active Expired - Fee Related
  • 1995-07-18 EP EP95943536A patent/EP0719407A1/de not_active Withdrawn

Non-Patent Citations (1)

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