BA 114C/07/en/04.95 No. 50074196 CCS 240 / 241 Chlorine Dioxide Measuring Cell Operating Instructions Endress + Hauser Nothing beats know-how Table of contents CCS 240 / 241 BE1CS240.CHP Table of contents 1. 1.1 1.2 1.3 1.4 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Areas of application . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Unpacking . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Ordering system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 2 2 2 2 2. Measuring system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 3. 3.1 3.2 3.3 Design and function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Construction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Operating principle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Influences on the measuring signal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4. 4.1 4.2 Installation in flow assemblies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Flow assembly CCA 250 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Other flow assemblies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 5. 5.1 5.2 5.3 5.4 Start-up and calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Connection to the measuring transmitter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Polarisation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Reference measurement according to the DPD method. . . . . . . . . . . . . . . . . . . . . . . . . . . Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 6 6 7 7 6. 6.1 6.2 6.3 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Checks and membrane change. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Filling with electrolyte . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 8 8 8 7. Regeneration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 8. Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 9. Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 10. Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 4 4 5 5 1 1. General CCS 240 / 241 1. General 1.1 Areas of application 1.3 Scope of delivery Drinking, service and pool water must be disinfected by means of suitable disinfectants, such as chlorine dioxide. The amount of disinfectant added must be constantly adapted to continuously fluctuating operating conditions. Disinfectant concentrations that are too low compromise disinfection; excessively high concentrations drive up costs and may cause corrosion and have a negative effect on taste. The delivery comprises: • 1 chlorine dioxide measuring cell CCS 240 or CCS 241 • 1 cap for membrane protection or for storage • 50 ml of spare electrolyte in a squeeze bottle • 1 spare cartridge with pretensioned membrane • 1 copy of installation and operating instructions The chlorine dioxide measuring cell CCS 240 or CCS 241 has been developed specifically for this purpose and is used for continuous acquisition of the chlorine dioxide concentration. In conjunction with a measuring and control instrument, it maintains the desired optimal operating conditions for disinfection. Areas of application of the chlorine dioxide measuring cell: CCS 240: 0.05 – 20.00 mg ClO2/l CCS 241: 0.01 – 5.00 mg ClO2/l (trace range) 1.2 Unpacking • Inspect for any damaged packaging! The post office or freight carrier must be informed of any damage. Keep damaged packaging until the matter has been settled! • Verify that the contents are undamaged! Inform the post office or freight carrier as well as the supplier of any damage. • Check that the delivery is complete (see section 1.3) and agrees with the shipping documents and your order: – Quantity delivered – Unit type and version according to nameplate – Operating instructions To facilitate distinction, the measuring cell types are equipped with a rating plate and a colour-coded ring on the cable gland: • Chlorine dioxide measuring cell CCS 240: green ring • Chlorine dioxide measuring cell CCS 241: yellow ring 1.4 Ordering system Chlorine dioxide sensor CCS 240 Version N with NTC thermistor detector Y special version CCS 240- Trace chlorine dioxide sensor CCS 241 If you have any questions, consult your supplier or the Endress+Hauser sales office in your area (see back cover of these operating instructions for addresses). Version N with NTC thermistor detector Y special version CCS 241- 2 ⇐ complete order code ⇐ complete order code 2. CCS 240 / 241 Measuring system BE1CS240.CHP 2. Measuring system The complete measuring system comprises: • Chlorine dioxide measuring cell CCS 240 or CCS 241 • Measuring transmitter Mycom CCM 121/151 • Measuring cable CMK (order no. 50005374) for connecting the chlorine measuring cell to the measuring transmitter (only if cable extension is required) • The maximum line length is 30 m • Flow assembly CCA 250 • Measuring instrument to determine the reference value according to the DPD method, e.g. microprocessor photometer CCM 181 Chlorine dioxide meas. cell Measuring cable CMK Mounting positions for pH and redox electrodes Meas. transmitter Mycom CCM 121 Inductive proximity switch for flow monitoring Outlet hose connector MYCOM-C mg/l °C pHComp % HOLD pH1 CAL pH2 DPD 1 H0 Flow monitoring float for 30 l/h min. flow detection V0 mg/l V1 pH V2 1 V3 2 2 H1 °C H2 HOLD CAL Cl pH ON/OFF ON/OFF Inlet hose connector Closure and calibration solution cap Fig. 2.1: Example of complete measuring system 3 3. Design and function 3. CCS 240 / 241 Design and function 3.1 Construction The chlorine dioxide measuring cell CCS 240 or CCS 241 has been designed for easy handling and can be dismantled for filling, membrane changes and regeneration (see fig. 3.1). The measuring electrodes are located in a measuring chamber that is separated from the medium by a PTFE membrane highly resistant to chemicals and mechanical stress. The plastic-embedded gold cathode and the silver/silver chloride anode are arranged in the lower end of the shaft with the connecting cable. A special support grid between the gold cathode and the PTFE membrane maintains a defined distance und therefore also a uniform electrolyte film with the advantage of a relatively stable display with fluctuating pressures and flow rates. The large electrolyte volume combined with a large anode and a small cathode area assures long life. The membrane cap can be changed after removal of the screw cap. An NTC thermistor resistor is embedded in the lower third of the shaft. Thanks to this sensor, the measuring signal can be automatically temperature-compensated, and the temperature of the medium can be displayed on the measuring transmitter. 1 2 Fig. 3.1: Chlorine meas. cell CCS 240 or CCS 241: Ready to operate and dismantled 1 2 3 4 5 6 4 Permanently attached 3 m cable Measuring chamber Membrane cap with robust dirt-repelling membrane in “sandwich” design Screw cap to hold the membrane cap in place Large-area anode silver/silver chloride Gold cathode 5 6 3 4 CCS 240 / 241 3. Design and function BE1CS240.CHP 3.2 Operating principle 3.3 Influences on the measuring signal When a measuring cell is connected to the corresponding measuring transmitter, a fixed external voltage is applied to the electrodes. Due to the difference in electrode area, this results in a polarisation at the gold cathode. The polarisation current generated during polarisation is visible on the measuring transmitter by very high display values which decrease over time and eventually stabilise. Polarisation must be complete before the measuring cell can be calibrated. Flow rate The membrane-covered measuring cell requires a minimum flow velocity of 15 cm/s in order to function. When using the flow assembly CCA 250, this value corresponds to a flow rate of 30 litres per hour (upper edge of float at level of red bar mark). The measuring signal is virtually flow-independent at more elevated flow rates while a flow dependence exists for flow velocities lower than the value mentioned above. When an INS proximity switch is installed in the assembly, insufficient flow rates can be reliably detected, and an alarm signal can be issued, e.g. to disable chlorine dioxide proportioning. Chlorine dioxide is present in the medium as a physically dissolved gas and is transported towards the membrane by the medium flow which is required for measurement. The membrane materials assure that only dissolved gases but no liquid-phase constituents can pass through the membrane. Dissolved salts and ionic substances are also held back. This is the reason why - contrary to the open measuring principle - the conductivity of the medium does not influence the measuring signal. The chlorine dioxide diffusing through the membrane is reduced to chloride ions at the gold cathode while silver is oxidised to silver chloride at the anode. The related electron release at the cathode and electron acceptance at the anode cause a current flow which - under constant conditions - is proportional to the external concentration of chlorine dioxide in the medium. Due to this measuring principle, the chlorine dioxide measuring cells described here are termed to be amperometric. The current flow is converted in the measuring transmitter and shown on the display as the dissolved chlorine dioxide concentration in mg/l. Temperature Changes in the medium temperature affect the measuring signal. An increase in temperature increases the measured value and lower temperatures result in lower measured values. The temperature sensor built into the measuring cell measures the medium temperature, permitting the measuring transmitter to perform a temperature compensation of the measured value display within the permissible temperature range. Free chlorine Since chlorine dioxide is explosive when mixed with air, it must be produced directly at the place of intended use. It can be obtained by means of two different methods: The sodium chlorite-hydrochloric acid process which results in solutions which are practically free of chlorine, and the sodium chlorite-chlorine gas method which may also produce free chlorine besides chlorine dioxide, depending on the system parameters. In the second case, the cross-sensitivity of the chlorine dioxide measuring cells to free chlorine is approx. 5 % of the DPD 1 value for free chlorine alone at 25 °C and pH 7.2. 5 4. Installation in flow assemblies 4. Installation in flow assemblies CCS 240 / 241 5. Start-up and calibration 4.1 Flow assembly CCA 250 5.1 Connection to the measuring transmitter The flow assembly CCA 250 is intended for installation of the measuring cell in the field. This assembly will hold a pH and a redox electrode in addition to the chlorine dioxide measuring cell. A needle valve regulates the flow rate in the range from 30 to 120 l/h. Flow rates below 30 l/h or total loss of flow can be detected by installing an inductive proximity switch (-INS option, order no. 50005179). The resulting signal can be used to issue an alarm and disable chlorine dioxide metering if necessary. The chlorine dioxide measuring cell is installed in the flow assembly by means of the union nut (refer to the operating instructions supplied with the flow assembly for detailed notes on installation). Note the following cable assignments when connecting the measuring cell: Warning: When the assembly is operated under pressure, the counterpressure on the measuring cell generated on the outlet side must not exceed 1 bar and must remain constant. 4.2 Other flow assemblies When other assemblies are to be used, a minimum flow velocity of 15 cm/s at the membrane must be guaranteed at all times. The measuring cell is to be installed such that the medium flows from the bottom to the top in order to assure removal of air bubbles contained in the medium, preventing them from collecting at the membrane. The medium flow should be directed directly towards the membrane. • Transparent wire, designation on sleeve „K“: gold cathode • Red wire, designation on sleeve „A“: silver/silver chloride anode • Green wire / brown wire: NTC thermistor detector (polarity does not matter) • Wire mesh: outer cable screen For connection to the measuring transmitter Mycom CCM 121 (panel-mounted 96 x 96 mm unit), a right-angle BNC connector must be installed for the gold cathode and silver/ silver chloride anode. The coaxial cable must be wired as follows: • Wire inside coaxial cable: gold cathode • Screen of coaxial cable (not external cable screen): silver/silver chloride anode Also refer to the Mycom CCM 121/151 installation and operating instructions within this context. 5.2 Polarisation The voltage applied between the cathode and anode by the measuring transmitter polarises the cathode surface. Times required for polarisation: • First start-up: 30 minutes (CCS 240) 90 minutes (CCS 241) • Subsequent start-up: 10 minutes (CCS 240) 45 minutes (CCS 241) Note: Calibration can only be performed upon expiration of the periods listed above. 6 5. CCS 240 / 241 Start-up and calibration BE1CS240.CHP 5.3 Reference measurement according to the DPD method 5.4 Calibration The measuring system is calibrated by performing a colorimetric reference measurement according to the DPD method. Chlorine dioxide reacts with diethyl-p-phenylendiamine by producing a red colorant, with the intensity of the red colour being proportional to the chlorine dioxide concentration. Simple visual methods employing comparators are inaccurate and subject to the wide variation introduced by subjective evaluation by different persons. Today, the chlorine dioxide concentration can be determined objectively and accurately using economical microprocessor photometers (order no. CCM 181-1). Zero adjustments are unnecessary due to the zero stability of the membrane-covered measuring cell. Proceed as follows to adjust the slope (sensitivity): An important fact which must be kept in mind for the DPD method is that this is not a selective measuring method for chlorine dioxide alone but that other oxidizing agents present in the medium can also be registered (see DIN 38408, part 5, section 4). Moreover, the lower measuring range of the photometers is limited and does not permit measurement in the very low trace range. For purposes of verification, a sample of the medium without added chlorine dioxide should be subjected to the DPD measurement if this is possible. This measurement should produce a measured value near zero and should differ significantly from the value obtained for the sample containing chlorine dioxide. • Make sure the medium temperature is constant. • Take a medium sample from the sampling cock and read the actual chlorine dioxide value on the measuring transmitter display. • Use the photometer to determine the chlorine dioxide concentration according to the DPD method. • Set the measuring transmitter to the DPD value determined (when there is a difference from previously read actual value). On the Mycom CCM 121/151 measuring transmitters, the measured value is entered in matrix position V1 / H1 (also refer to Mycom installation and operating instructions). • Check calibration after several hours or the next day and repeat if necessary. Refer to the installation and operating instructions for the photometer CCM 181-1 with regard to chlorine dioxide content measurement in the presence of free chlorine. 7 6. Maintenance CCS 240 / 241 6. Maintenance 6.1 Checks and membrane change 6.3 Storage The following maintenance work and checks are to be performed when the measuring cell is in operation: When not in use, the measuring cell should be stored as follows: • Regular checks of the measurement should be performed at intervals that depend on operating conditions but at least once a month. Recalibrate as necessary. In the case of visible membrane soiling, remove the measuring cell from the flow assembly. Clean the membrane only mechanically under a light jet of water or chemically by placing it in 1 – 10 % hydrochloric acid for a few minutes without adding any other chemicals. Chemicals that lower the surface tension are not permissible. • The electrolyte in the measuring cell should be replaced or refilled once per season or every 12 months. This interval may be longer or shorter depending on the chlorine dioxide content in the field (procedure as per section 6.2). • The membrane must be replaced when strongly soiled or leaky. For replacement, first unscrew the measuring chamber and then the front screw cap (see fig. 3.1). Replace the membrane cap with spare cartridge CCY 14-WP and refill the measuring chamber with electrolyte CCY 24-F as described in section 6.2. • In the case of short-term interruptions in operation, the measuring cell can remain in the flow assembly. In order to prevent the membrane from drying out, the assembly must never be empty of medium. If this cannot be guaranteed, the measuring cell must be removed from the assembly. To keep the membrane moist, moisten the sponge inside the protection cap with electrolyte and insert the protection cap on the measuring chamber. • If the measuring cell will not be in use for an extended period, in particular if it is likely to dry out, the measuring cell must be emptied. To clean, rinse the measuring chamber and electrode shaft with cold water and allow to dry. Then screw the measuring cell closed only loosely (not all the way to the stop) to leave the membrane relaxed. Proceed according to section 6.2 to return the measuring cell to use. 6.2 Filling with electrolyte The electrolyte filling in the chlorine dioxide measuring cell is used up slowly during measurement due to chemical reactions. The silver chloride coating on the anode applied at the factory continues to grow during the operation of the measuring cell. This has no influence on the reaction taking place at the cathode. Proceed as described below to replace the electrolyte CCY 24-F (see fig. 3.1): • Unscrew the measuring chamber from the shaft. • Hold the measuring chamber at an angle and fill in electrolyte close to the upper rim. • Knock the electrolyte-filled chamber against a plane surface several times to loosen small air bubbles adhering on the inside and make them rise. • Screw the electrode shaft into the measuring chamber from vertically above, making sure all the air on the inside is displaced. • When the O-ring starts to seal, screw in the shaft slowly all the way to the stop. The measuring cell is now ready to operate. 8 7. Regeneration Indications for regeneration are sluggish measured value display and slope adjustments that can only be performed with difficulty or not at all. The time intervals between regeneration depend on the chlorine dioxide concentration in the medium, where higher concentrations require more frequent regeneration. When the measuring cell is used in water with an average chlorine dioxide concentration, the measuring cell will operate properly for many years. If the measuring cell requires regeneration, it must be returned to the manufacturer. 8. CCS 240 / 241 Troubleshooting BE1CS240.CHP 8. Troubleshooting Problems are basically possible in three areas of the measuring system: • Measuring transmitter • Cables and connections • Chlorine dioxide measuring cell and medium Measuring transmitter, cable and connection problems should always be eliminated first. Problem No display Measuring cell does not respond Display value too high In this case, refer to the installation and operating instructions of the measuring transmitter for troubleshooting. If the problem cannot be eliminated, proceed with the following troubleshooting chart. Possible cause Measuring transmitter is not supplied with power Remedy Establish mains connection. Break in line from the measuring cell to the measuring transmitter Establish cable connection. No electrolyte in measuring chamber Fill measuring chamber (see section 6. 2). No medium flow Establish medium flow, clean filter. Measuring cell not completely polarised Wait for polarisation to complete (section 5.2). Membrane defective Replace membrane cap. Shunt (e.g., moisture bridge) in the Open measuring chamber. Rub measuring cell, at the connections gold cathode dry. A shunt or in the connecting cable exists if the transmitter display does not return to zero. Display value too low Interference by foreign oxidizing agents Check medium, check chemicals. Measuring chamber not screwed all the way tight Screw on measuring chamber or screw cap completely. Membrane soiled Clean membrane. Air bubble on outside of membrane Eliminate air bubble. Display value fluctuates considerably Temperature display too high too low Air bubble inside between cathode and membrane Open measuring chamber, fill in some electrolyte, knock. Medium flow insufficient Establish required flow rate. DPD measurement is rendered inaccurate by foreign oxidizing agents Check medium, check chemicals. Hole in membrane Replace membrane cap External voltage in medium Disconnect wire from PMC pin on CCA 250 assembly. Measure voltage between PMC pin and protective ground (AC and DC ranges). Locate external voltage source and eliminate if values exceeding a few volts are measured. NTC thermistor line: break short circuit Test wires (green/brown) and measure resistance (NTC), replace measuring cell if necessary 9 9. Technical data CCS 240 / 241 9. Technical data Measuring system Shaft material Membrane material Membrane cap Cable connection passively operated measuring cell with gold cathode and silver/silver chloride anode PVC PTFE exchangeable low-noise, four-wire cable, length 3 m, dual screen transparent, „K“: gold cathode red, „A“: silver/silver chloride anode green/brown: NTC thermistor detector wire mesh: outer screen Measuring range Polarisation period (first polarisation): Subsequent polarisation Response time after sudden change in measured value Minimum flow for CCA 250 assembly Minimum flow velocity Permissible temperature range Maximum counterpressure Drift Average life of filling electrolyte Temperature sensor CCS 240 CCS 241 0.05 – 20 mg ClO2/l 0.01 – 5.00 mg/l up to 30 min up to 90 min up to 10 min up to 45 min 90 % < 2 min. 99 % < 5 min. 30 l/h 15 cm/s 2 ... 45 °C 1 bar < 1.5 % per month typ. 12 months NTC 10 kohm at 25 °C 10. Accessories CCY 14-WP 2 ready-made spare cartridges for cells CCS 140/141/240/241 Order no. 50005255 CCY 24-F 50 ml filling electrolyte for cells CCS 240/241 Order no. 50064294 Supplementary documentation Operating instructions for CCA 250 Flow assembly for chlorine measurement BA 062/07/en Operating instructions for Mycom CCM 121/151 Chlorine measuring transmitter/controller BA 108C/07/en 10 Europe Austria ❑ Endress+Hauser Ges.m.b.H. Wien Tel. (01) 8 80 56-0, Fax (01) 8 80 56-35 Belarus Belorgsintez Minsk Tel. (01 72) 26 31 66, Fax (01 72) 26 31 11 Belgium / Luxembourg ❑ Endress+Hauser S.A./N.V. Brussels Tel. (02) 2 48 06 00, Fax (02) 2 48 05 53 Bulgaria INTERTECH-AUTOMATION Sofia Tel. (02) 65 28 09, Fax (02) 65 28 09 Croatia ❑ Endress+Hauser GmbH+Co. Zagreb Tel. (01) 6 60 14 18, Fax (01) 6 60 14 18 Cyprus I+G Electrical Services Co. Ltd. Nicosia Tel. (02) 48 47 88, Fax (02) 48 46 90 Czech Republic ❑ Endress+Hauser GmbH+Co. Praha Tel. 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