CORDIS provides links to public deliverables and publications of HORIZON projects.
Links to deliverables and publications from FP7 projects, as well as links to some specific result types such as dataset and software, are dynamically retrieved from OpenAIRE .
Deliverables
Summary:
Continuous monitoring of organic compounds in both the influent and effluent of industrial waste water plants is required to detect any accidental discharge. A high input of organic chemicals could deteriorate the performance of the biological treatment step to such an extent that an additional load of pollutants is released into the environment.
As on-site monitoring system has been constructed which comprises a Solid-Phase Microextraction (SPME) unit coupled to a GC-FID. All steps including sampling, sample preparation, chromatographic separation and detection are fully automated. The extraction of organic compounds does not require solvents. Prior to extraction the sample is pumped into a 250 ml compounds does not require solvents. Prior to extraction the sample is pumped into a 250 ml vessel where parameters like pH, temperature and salt content can be adjusted automatically. Moreover, an internal standard is added here which can be used to quantify the organic compounds and to control the overall performance of the analytical system. Extraction id then performed in a heatable extraction vessel. It has an integrated magnetic stirrer and is suitable for both direct SPME and head space SPME. Since the sample flow into the vessel is stopped during extraction, methods developed by manual SPME can be transferred directly to the automated.
During the chromatographic separation, the next sample preparation step can be performed, resulting in high sample throughput. Analytic cycle times of less than 60 min can be achieved. The overall precision of the system is limited by the SPME technique. In general, RSD values in the range of 2%-6% can be obtained under optimized GC-conditions for direct and headspace SPME. The analytical data are automatically compared with critical limits and transmitted to a remote location so that appropriate safety measures can be carried out.
During the chromatographic separation, the next sample preparation step can be performed, resulting in high sample throughout. Analytical cycle times of less than 60 min can be achieved. The overall precision of the system is limited by the SPME technique. In general, RSD values in the range of 2%-6% can be obtained under optimized GC-conditions for direct and headspace SPME. The analytic data are automatically compared with critical limits and transmitted to a remote location so that appropriate safety measures can be carried out.
The system can also be applied for the analysis of ground, surface and drinking water.
Summary:
The determination of the AOX value (EN 1485) in water samples (adsorbable organic halogens) is a lengthy laboratory work which still requires one expensive employee doing nothing else than AOX determinations. A maximum of ten samples can be analysed per day provided that the minimum requirements of the Total Quality Management principles for the accuracy of the analytical results are filled.
The new developed automated AOX analyzer operates continuously in 20 minute periods and is able to monitor an effluent including the required TQM measures. If the AOX levels is determined to exceed a certain risk level, the AOX analyzer automatically carries out a calibration step pumping standards solutions through the charcoal columns.
Every waste water producer will now be able to monitor the AOX concentration of his effluent. Moreover, the new system distinguishes between the different halogens which together add up to the total AOX. And in contrast to the argentometric detection method of old AOX analyzers the new system is equipped with a Plasma Emission Detector which allows not only the differentiation between the AOX forming halogens but moreover the determination of adsorbable organic fluorine (AOF).
These features make the new element selective AOX analyzer very attractive for every company producing waste water with organic load. In Germany these companies have to pay penalties depending on the AOX concentrations in their effluent which motivates them to monitor the AOX value. The transfer of corresponding laws into European dimensions will surely create a great market for an automated AOX analyzer.
Summary:
TNO has developed an instrument which allows the semi-continuous determination of dissolved organic carbon in waste water. By coupling a liquid chromatograph (HPLC) with an organic-carbon (OC) detector the instrument is suited for the chromatographic characterization of organic compounds in waste water. The instrument consists of an automated injection/calibration system, a HPLC equipped with a GPC-type column, a DOC-detector based on on-line photo-oxidation of the dissolved organic compounds followed by infra-red detection of the produced CO2 and a data-logger that allows remote instrument control and data-acquisition. Furthermore, a UV-detector has been incorporated for the simultaneous detection of UV-sensitive organic compounds and a filter system has been incorporated allowing the monitoring of waste water. The complete instrument was built and validated in the laboratory. The linear concentration range is 1-1000 ppm with a detection limit of 0.6 ppm. The repeatability, stability and drift over a two week period ranged from 1 to 3%. The instrument is tested at the waste water facility of a chemical plant for a period of ten days and shows satisfactory results. The repeatability over this period was found to be within 10%. The drift of the signal over this period was found to be within 5%. A fingerprint of the composition of the DOC was obtained in the form of two chromatograms (DOC and UV). Changes in the DOC content and composition over the ten day period could be monitored.
Exploitable results
Within the joint project three instruments were developed for a quasi-continuous on-site monitoring of industrial effluents. While two instruments use sum parameters to characterize the waste water (sum of the organics with a given molecular weight, sum of organofluorine, organochlorine and organobromine compounds), the third instrument allows a quasi-continuous monitoring of individual organic compounds. Two of the three instruments have been extensively tested at the waste water plant. Negotiations with several companies for their production and commercial distribution have started. The instruments are considered as early warning systems which allow the detection of an accidental discharge of toxic compounds into the waste water treatment plant.
An automatic waste water analyzer has been developed based on the extraction of the organic waste water constituents by solid phase microextraction (SPME) and detection by gas chromatography (GC) with flame ionisation detection. It consists of three main parts all under computer control. Moreover, a remote control of the instrumental setup via modem is possible. The analyzer was extensively tested at the central waste water plant of a chemical company. The stability of the SPME fibre for the repeated extraction is at least several days. On-site testing revealed that the analyzer is sufficiently robust for an unattended operation of several weeks.
Within the project a quasi-continuously operating analyser for the determination of adsorbable organic halogenes (AOX) was developed. The monitor permits the differentiation between the elements fluorine, chlorine, bromine and iodine with use of an plasma emission spectroscopic detection system instead of conventionally used microcoulometry. For on-line measurements a new developed plasma excitation source was tested for its capability of exciting non-metals. The individual halogens are detected using different filters.
The instrument for on-site semi-continuous analyses, which does not monitor the individual compounds but rather their molecular weight, is ready. By coupling a liquid chromatograph (HPLC) with an organic-carbon detector this instrument is suited for the chromatographic characterization of organic compounds in waste water. The instrument consists of an automated injection/calibration system, a HPLC equipped with a GPC-type column, a DOC detector based on on-line photo-oxidation of the dissolved organic compounds followed by infra-red detection of the produced CO(2), and a data-logger that allows remote instrument control and data-acquisition. The complete instrument was build and validated in the laboratory. The linear concentration range is 1-50 ppm with a detection limit lower than 1 ppm. The repeatability, stability and drift over a two week period ranged from 1 to 3%. The oxidation efficiency was determined for several organic compounds using potassium hydrogenphthalates as a reference. With most compounds tested the oxidation efficiency was found to be close to 100%. For the field experiments a filter system is incorporated in the instrument allowing the monitoring of waste water. The instrument has been tested at the waste water facility of a chemical plant for a period of ten days and showed satisfactory results. During this on-site test the system has been operated by remote control from the laboratory.
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