Thermo Products REDOX/ORP 9678BNWP User's Manual
Contents
1. 9778BNWP and 9778SC The glass body enables the electrode to be used in solutions that contain organic solvents Use the electrode in water wastewater metal plating and organic solvent samples Epoxy Refillable ORP ATC Triode Cat No 9180BNMD and 9180BN The electrode includes a built in temperature probe for measuring ORP and temperature with one electrode The refillable design allows the electrode filling solution to be changed in case of contamination or clogging Epoxy Low Maintenance ORP ATC Triode Cat No 9179BNMD and 9179BN The electrodes include a built in temperature probe for measuring ORP and temperature with one electrode The electrodes contain a gel reference solution so no filling solution is required Note Redox ORP electrodes are not designed for constant current or amperometric titrations such as Karl Fischer moisture analysis Redox ORP Electrode User Guide 1 Required Equipment 1 Thermo Scientific Orion pH mV meter such as the 3 Star pH meter 4 Star pH ISE meter 4 Star pH DO meter 4 Star pH conductivity meter or 5 Star pH ISE DO conductivity meter ORP electrodes can be used on any pH mV meter with a BNC or U S standard connection The electrodes can also be used on meters with a variety of inputs when an adapter cable is used Visit www thermo com water for details Refillable ORP Triodes have temperature connectors that are compatible with specific meters refer to the list below2. 166 Cummings Center Beverly MA 01915 USA Tel 978 232 6000 Toll Free 800 225 1480 Dom Fax 978 232 6015 Int l Fax 978 232 6031 254794 001 Rev A www thermo com water
3. Thermo Scientific Orion ORP electrode The 9180BNMD and 9179BNMD ORP ATC Triode electrodes have a temperature connector that is compatible with the Star Series meters The 9180BN 9179BN ORP ATC Triode electrode have a temperature connector that is compatible with the A Series meters ORP electrode filling solution Use Cat No 900011 filling solution for samples that have a total ionic strength greater than 0 2 M Use Cat No 900001 filling solution for samples that have a total ionic strength less than 0 2 M ORP electrode filling solution is not required if using a 9179BNMD or 9179BN low maintenance ORP ATC Triode ORP standard Cat No 967901 or 967961 ORP standard is highly recommended to ensure accurate ORP measurements Beakers plastic or glass Magnetic stirrer or Orion stirrer probe Cat No 096019 The stirrer probe can be used with 3 Star 4 Star and 5 Star benchtop meters Distilled or deionized water Redox ORP Electrode User Guide Sample Requirements Electrodes with an epoxy body should only be used in aqueous solutions Electrodes with a glass body may be used in non aqueous solutions and solutions that contain organic solvents The ORP electrodes contain a silver silver chloride Ag AgCl reference that may become clogged in solutions that contain silver complexing or binding agents such as TRIS proteins and sulfides Frequent cleaning may be required when measuring solutions tha
4. distilled water 1 Hold the electrode body with one hand and use your thumb to push down on the electrode cap to drain the chamber Push down on the cap until all the filling solution is drained from the chamber 2 Fill the electrode with distilled water and then push down on the cap until all the water is drained from the chamber 3 Fill the electrode with fresh filling solution up to the fill hole Push down on the cap to allow a few drops of filling solution to drain out of the electrode and then refill any lost filling solution Disassembling the Sure Flow Electrode Note Disassembly is usually not required and should not be done unless a thorough cleaning is required 1 Tip the electrode so the filling solution moistens the O ring on the electrode body Hold the electrode body with one hand and use your thumb to push down on the electrode cap to drain the chamber 2 Unscrew the cap counter clock wise and then slide the cap and the spring up the cable 3 Hold the outer sleeve with one hand and firmly push down on the threaded portion with the thumb and forefinger to separate the inner body from the sleeve 4 Grasp the cone with a clean lint free tissue and withdraw the body from the sleeve using a gentle twisting motion Do not touch the pellet above the cone it will damage to the pellet Rinse the outside of the electrode body and the entire sleeve with distilled water Allow it to air dry 16 Redox ORP Electrode
5. 7 399 220 68 48 398 220 168 49 397 220 168 50 396 220 67 Redox ORP Electrode User Guide Measurement Techniques e Always use fresh ORP standard for calibration e fthe electrode is refillable remove the filling hole cover during measurements to ensure a uniform flow of filling solution e Between measurements thoroughly rinse the electrode with distilled water Gently shake the electrode after rinsing to prevent solution carryover and then blot the electrode dry with a lint free tissue e Stir all standards and samples at a uniform rate e Place a piece of insulating material such as Styrofoam or cardboard between the magnetic stirrer and beaker to prevent measurement errors from the transfer of heat to the sample e Allow all standards and samples to come to room temperature for precise measurements e fthe electrode is used in dirty or viscous samples or the electrode response becomes sluggish empty the electrode completely and hold the junction under running water Empty any water from the electrode and refill it with fresh electrode filling solution e If a Sure Flow electrode is used in dirty or viscous samples or the electrode response becomes sluggish empty the electrode completely and hold the junction open under running water Empty any water from the electrode and refill it with fresh electrode filling solution Press down on he electrode cap to let a few drops of the filling solution low out of the elec
6. 900011 filling solution for this testing procedure 1 Prepare solution A 0 1 M potassium ferrocyanide 0 05 M potassium ferricyanide weigh out 4 22 g reagent grade K4Fe CN se3H50 and 1 65 g reagent grade KsFe CN s Place in a 100 mL volumetric flask Add about 50 mL distilled water and swirl to dissolve solids Dilute to volume with distilled water 2 Prepare solution B 0 01 M potassium ferrocyanide 0 05 M potassium ferricyanide and 0 36 M potassium fluoride weigh out 0 42 g reagent grade K4Fe CN g 3H20 1 65 g reagent grade and 3 39 g reagent grade KFe2H5 O Place in a 100 mL volumetric flask Add 50 mL distilled water and swirl to dissolve solids Dilute to volume with distilled water 3 Transfer solution A to a 150 mL beaker Place the electrode in the solution and wait until the reading stabilizes The potential should be about 234 mV 4 Transfer solution to a 150 mL beaker Rinse the electrode and then place it in the solution and wait until the reading stabilizes The potential should be about 66 mV greater in solution B than in solution A Assistance After troubleshooting all components of your measurement system contact Technical Support Within the United States call 1 800 225 1480 and outside the United States call 978 232 6000 or fax 978 232 6031 In Europe the Middle East and Africa contact your local authorized dealer For the most current contact information visit www thermo co
7. K2Cr207 sodium iodate NalO3 or samples containing Titration Reaction 5Sb 2 16H gt 5Sb 2Mn 8H O 3As 6H Br 3As 5H5 05 t 2MnO 4 6 2Mn 8H20 in acid solution Cl 217 gt 15 2 In basic solution 2CIO 2L o 1 2Cl 20H 21 103 BHCN H gt 5ICN l2 2S203 22 54062 Fe Ce 2 Fe Cr205 2 6Fe 14H gt 2Cr 6Fe 7H2O MnO 5Fet 8 gt Mn 5Fet 4H O 3Mn 2MnO 7H20 gt 5MnO3 H20 AH Sn 2Ce a Sn 2Ce SO l2 2H20 gt 5042 21 4H 3Ti 6H gt Br Tit l2 2S203 227 5406 3UO 2 8H 2Cr 4 ZnHg SCN 6103 6 8H gt 2 2 Hg 6ICI 4HCN 4S0 Redox ORP Electrode User Guide Ref 13 Electrode Maintenance 14 Inspect the electrode for scratches cracks salt crystal buildup or membrane junction deposits Rinse off any salt buildup with distilled water Remove any membrane junction deposits as directed in the General Cleaning section If the electrode is refillable drain the reference chamber flush it with fresh filling solution and refill the chamber with fresh filling solution If the electrode is refillable make sure that the filling solution does not crystallize or dry out Remove any crystals by rinsing the electrode with distill
8. User Guide Reassembling the Sure Flow Electrode 1 Moisten the O ring on the electrode body with a drop of filling solution Insert the screw thread end of the electrode body into the tapered ground end of the sleeve 2 Push the body into the sleeve using a gentle twisting motion until the bottom surface of the inner cone is flush with the tapered end of the sleeve 3 Place the spring onto the electrode body and screw on the cap Refill the electrode with filling solution Electrode Storage Short term Storage up to one day To ensure a quick response and free flowing junction the reference junction must not dry out It is recommended that the electrode be soaked in a 4 M potassium chloride KCI solution Electrodes may also be stored in water Long term Storage over one day For gel filled electrodes rinse the electrode with distilled water dry the electrode with a lint free tissue and cover the measuring surface with the protective cap For refillable electrodes rinse the electrode with distilled water drain all of the filling solution from the electrode flush out the electrode with distilled water cover the measuring surface with the protective cap and store the electrode dry Redox ORP Electrode User Guide 17 Troubleshooting Follow a systematic procedure to isolate the problem The measuring system can be divided into four components for ease in troubleshooting meter electrode sample application and te
9. User Guide Redox ORP Electrodes ROSS and the COIL trade dress are trademarks of Thermo Fisher Scientific Inc AQUAfast Cahn ionplus KNIpHE No Cal ORION perpHect PerpHecT PerpHecTion pHISA pHuture Pure Water Sage Sensing the Future SensorLink ROSS ROSS Ultra Sure Flow Titrator PLUS and TURBO2 are registered trademarks of Thermo Fisher 1 888 pHAX ION A All in One Aplus AQUAsnap AssuredAccuracy AUTO BAR AUTO CAL AUTO DISPENSER Auto ID AUTO LOG AUTO READ AUTO STIR Auto Test BOD AutoEZ Cable Free CERTI CAL CISA DataCOLLECT DataPLUS digital LogR DirectCal DuraProbe Environmental Product Authority Extra Easy Extra Value FAST QC GAP GLPcal GLPcheck GLPdoc ISEasy KAP LabConnect LogR Low Maintenance Triode Minimum Stir Requirement MSR NISS One Touch One Touch Calibration One Touch Measurement Optimum Results Orion Star Pentrode pHuture MMS pHuture Pentrode pHuture Quatrode pHuture Triode Quatrode QuiKcheK rf link ROSS Resolution SAOB SMART AVERAGING Smart CheK SMART STABILITY Stacked Star Navigator 21 Stat Face The Enhanced Lab ThermaSense riode TRIUMpH Unbreakable pH Universal Access are trademarks of hermo Fisher Guaranteed Success and The Technical Edge are service marks of Thermo Fisher PerpHecT meters are protected by U S patent 6 168 707 PerpHecT ROSS are protected by U S patent 6 168 707 ORION Series A meters and 900A printer are pro
10. chnique Meter The meter is the easiest component to eliminate as a possible cause of error Thermo Scientific Orion meters include an instrument checkout procedure and shorting cap for convenience in troubleshooting Consult the pH meter user guide for directions Electrode 1 Thoroughly rinse the electrode with distilled water 2 Place electrode in the Orion ORP standard and wait until the reading stabilizes 3 The mV potential should be 220 mV 60 mV If the mV reading is out of range repeat the measurement with fresh ORP standard If the electrode fails this procedure clean the electrode thoroughly as directed in the Electrode Maintenance section If the electrode response is slow or drifting and the electrode is refillable drain and refill the electrode with fresh filling solution Replace the electrode if cleaning and maintenance fail to rejuvenate it Sample Application The electrode and meter may operate with standards but not with the sample In this case check the sample composition for interferences incompatibilities or temperature effects Technique If trouble persists review operating procedures Review calibration and measurement sections to be sure proper technique has been followed 18 Redox ORP Electrode User Guide Checking Electrode Operation Checking the electrode is necessary only when there is evidence of malfunction that cannot be traced to other causes Fill the electrode with Cat No
11. d water 3 Shake the electrode downward similar to a clinical thermometer to remove air bubbles 4 Connect the electrode to the meter 4 Redox ORP Electrode User Guide filling hole filling lution Ag AgCl 50 internal chamber reference ceramic reference sensing junction element Figure 1 Refillable ORP Electrode fill hole reference AgAgCI filling solution internal chamber reference sensing Sure Flow element junction Figure 2 Sure Flow Refillable ORP Electrode Redox ORP Electrode User Guide Electrode Calibration ORP readings can be reported using the absolute mV values or the Ey mV values mV values give the corresponding mV values that would be obtained using a Standard Hydrogen Electrode SHE also known as the Normal Hydrogen Electrode NHE Orion ORP standard Cat No 967901 or 967961 allows operators to correlate measurements to the Ey mV value with an Orion ORP electrode The relative mV mode can be used to calibrate the ORP electrode so the electrode reads the Ey mV values in samples When an ORP electrode is calibrated to read Ey mV values the resulting sample readings can be compared among multiple meter and electrode systems Note the meter can perform an automatic calibration using an E mode refer to the meter user guide for detailed instructions on the meter calibration procedure 1 Setthe meter to the relative millivolt mode Refer to the meter user guide fo
12. ed water or wiping with a damp lint free tissue To prevent crystallization of the filling solution cover the fill hole whenever the electrode is being stored and open the fill hole when calibrating and measuring Redox ORP Electrode User Guide Electrode Cleaning Procedures General Cleaning 1 Soak the electrode in 0 1 or HNO for half an hour The electrode can also be soaked for 15 minutes in a 1 10 dilution of household laundry bleach or a 0 1 to 0 5 liquid detergent solution mixed with hot water The solution should be stirred at a moderate to fast rate If the electrode is refillable drain the reference chamber and refill it with fresh filling solution Cleaning Solutions Cat No 900021 pH clean contaminants Cat No 900022 pH clean contaminants Cat No 900023 pH clean Cat No 900024 pH clean grease contaminants Cat No 900020 pH clean solutions A B C and D Redox ORP Electrode User ing so ing so ing so ing so ing so Guide u u u u u Thoroughly rinse the electrode with distilled water ion A for removing protein ion B for removing bacterial ion C for general cleaning ion D for removing oil and ion kit includes cleaning 15 Sure Flow Electrode Cleaning Cat No 9678BNWP and 967800 If the area between the electrode sleeve and inner cone becomes clogged with sample or precipitate flush the area with filling solution or
13. m water Warranty For the most current warranty information visit www thermo com water Redox ORP Electrode User Guide 19 Ordering Information Cat No 9179BNMD 9179BN 9180BNMD 9180BN 9678BNWP 967800 9778BNWP 9778SC 900011 900001 967901 967961 910001 20 Description Low maintenance gel ORP ATC Triode with epoxy body and waterproof BNC and 8 pin MiniDIN connectors Low maintenance gel ORP ATC Triode with epoxy body and BNC and 8 pin DIN connectors Refillable ORP ATC Triode with epoxy body and waterproof BNC and 8 pin MiniDIN connectors Refillable ORP ATC Triode with epoxy body and BNC and 8 pin DIN connectors Sure Flow refillable ORP redox electrode with epoxy body and waterproof BNC connector Sure Flow refillable ORP redox electrode with epoxy body and U S standard connector Refillable ORP redox electrode with glass body and waterproof BNC connector Refillable ORP redox electrode with glass body and screw cap connector ORP electrode filling solution for samples that have a total ionic strength greater than 0 2 M 5 x 60 mL bottles ORP electrode filling solution for samples that have a total ionic strength less than 0 2 M 5 x 60 mL bottles ORP standard 475 mL bottle ORP standard 5 x 60 mL bottles 4 M KCI storage solution 475 mL bottle Redox ORP Electrode User Guide Thermo Fisher Scientific Environmental Instruments Water Analysis Instruments
14. r add increments of 0 1 to 0 2 mL Continue the titration 3 to 4 mL past the endpoint 5 Plot the electrode potential versus volume of added titrant on linear graph paper and draw a smooth curve through the points The endpoint is the point of inflection the point of greatest slope 10 Redox ORP Electrode User Guide 6 Calculate the normality of the sample N in equivalents per liter Ve Vx where normality of titrant Eg 1 volume of titrant at end point mL Ss ll volume of sample mL Table 2 References 1 Furman ed Scott s Standard Methods of Chemical Analysis 5th Ed Van Nostrand Princeton N J 1938 2 Hillebrand Lundell Bright and Hoffman Applied Inorganic Analysis 2nd Ed Wiley New York 1953 3 Kolthoff and Sandell Testbook of Quantitative Inorganic Analysis 3rd Ed MacMillan New York 1952 4 Newer Methods of Volumetric Chemical Analysis Van Nostrand Princeton N J 1938 5 Treadwell and Hall Analytical Chemistry vol 2 Quantitative Analysis 8th Ed Wiley New York 1935 Redox ORP Electrode User Guide 11 Table 2 Typical Redox Titration Methods Unknown antimony Sb 3 arsenic Ast hydrogen peroxide H202 hypochlorite ion CIO or chlorine Cl iodine l5 iodine l5 iron as Fe Fe or in steel iron as Fe Fe or in steel manganese as permanganate Mn0 manganese as Mn s
15. r detailed instructions 2 Place the ORP electrode in ORP standard Cat No 967901 or 967961 3 Set the meter to the Ey mV value of the standard at the measured temperature using the information in Table 1 Table 1 ORP Standard Values Absolute mV values may vary by x 60 mV Temperature Value Absolute Value Absolute Value C mV with Cat No with Cat No 900011 Filling 900001 Filling Solution mV Solution mV 0 438 218 76 1 437 218 76 2 437 218 76 3 436 218 76 4 435 218 76 5 435 218 76 6 434 218 76 7 433 218 76 8 433 218 75 9 432 219 75 6 Redox ORP Electrode User Guide Temperature Eu Value Absolute Value Absolute Value C mV with Cat No with Cat No 900011 Filling 900001 Filling Solution mV Solution mV 10 431 219 175 11 430 219 75 12 430 219 75 13 429 219 175 14 428 219 175 15 428 219 75 16 427 219 174 17 426 219 174 18 425 219 74 19 424 219 174 20 424 219 174 21 423 219 74 22 422 219 74 23 421 219 173 24 420 220 73 25 420 220 73 26 419 220 173 27 418 220 73 28 417 220 72 29 416 220 172 30 415 220 172 31 414 220 72 32 413 220 172 33 412 220 171 34 412 220 71 35 411 220 171 36 410 220 171 37 409 220 71 38 408 220 70 39 407 220 170 40 406 220 70 41 405 220 70 42 404 220 169 43 403 220 69 44 402 220 69 45 401 220 169 46 400 220 168 4
16. t contain these agents Proteins cause the additional problem of coating the electrode so extra care should be taken to keep the electrode clean while measuring samples that contain proteins Redox ORP Electrode User Guide 3 Electrode Preparation Electrode Preparation for Refillable Electrodes 1 Remove the protective shipping cap from the sensing element and save the cap for storage 2 Clean any salt deposits from the exterior of the electrode by rinsing with distilled water 3 Uncover the filling hole by removing the tape and then add electrode filling solution Cat No 900011 to the electrode To maintain an adequate flow rate the level of filling solution must always be above the reference junction and at least one inch above the sample level The filling hole should be open whenever the electrode is in use 4 For Sure Flow electrode only wet the junction by pressing down on the electrode cap to let a few drops of the filling solution flow out of the electrode and then replenish any lost solution 5 Shake the electrode downward similar to a clinical thermometer to remove air bubbles 6 Connect the electrode to the meter Note The fill hole must be open when the electrode is in use Electrode Preparation for Gel Filled Electrodes 1 Remove the protective shipping cap from the sensing element and save the cap for storage 2 Clean any salt deposits from the exterior of the electrode by rinsing with distille
17. tannous tin Sn sulfur as sulfur dioxide SO thallium Ti thiosulfate ion S203 2 uranium as uranyl ion UO Zinc Zn 12 Interferences As Fe SO V and organic substances other reducing agents preservatives present in commercial H203 may interfere Br and other oxidizing agents interfere by liberating 12 other reducing agents direct sunlight high acidity copper salts and other catalysts promote air oxidation and cause false high results high levels of organic acids such as acetic oxalic tartaric and alcohols F if present in more than trace amounts PO4 remove by adding acid other reducing agents other oxidizing agents other reducing agents other reducing agents S and SO remove by shaking with CdCO3 and filtering other reducing agents S 50 2 remove by shaking with CdCO3 and filtering other reducing agents other reducing agents Redox ORP Electrode User Guide Suitable Titrants potassium permanganate sodium bromate potassium permanganate KMnO sodium iodide Nal sodium iodate NalO3 sodium thiosulfate Na2S203 ceric sulfate Ce S04 2 not recommended for samples containing potassium dichromate KzCr3O7 recommended errous sulfate FeSO potassium permanganate KMnQ ceric sulfate Ce SO 2 iodine l2 sodium bromate NaBrOs lodine l2 potassium dichromate
18. tate After each addition of titrant the platinum redox electrode develops a potential proportional to the logarithm of the ratio of the activities of the two oxidation states At the inflection point or endpoint the titrant has completely oxidized or reduced the unknown causing a sharp change in the logarithm of the ratio of the activities of the two oxidation states A corresponding sharp change in the potential is developed by the platinum electrode Often several oxidizing or reducing species can be precisely determined in the same solution by a single titration with several inflection points Table 2 lists suitable titrants for different unknowns the equation for the titration reaction interferences and a reference where information about preparing the sample and running the titration can be found For similar information about unknowns not listed in the table consult the standard texts listed as references The following is a general procedure for performing a redox titration once the sample is prepared 1 Filla 10 mL buret with a standard titrant solution whose normality is 5 10 times that of the sample 2 Connect the electrode to the meter and set the meter to the mV mode 3 Pipet 50 mL of sample into a 150 mL beaker Stir the solution thoroughly throughout the titration 4 At first add titrant in 0 5 to 1 mL increments recording the potential after each addition Near the endpoint when large potential changes appea
19. tected by U S patents 5 198 093 D334 208 and D346 753 ionplus electrodes and Optimum Results solutions are protected by US Patent 5 830 338 ROSS Ultra electrodes are protected by US patents 6 793 787 Orion ORP Standard is protected by US Patent 6 350 367 Orion NoCal electrodes with stabilized potential patent pending 2007 Thermo Fisher Scientific Inc All rights reserved All trademarks are the property of Thermo Fisher Scientific Inc and its subsidiaries The specifications descriptions drawings ordering information and part numbers within this document are subject to change without notice This publication supersedes all previous publications on this subject Introduction This user guide contains information on the preparation operation and maintenance of the Thermo Scientific Orion ORP electrodes These ORP electrodes combine a platinum redox sensing electrode and a silver silver chloride reference electrode in one body The redox ORP electrodes can be used to make direct measurements of redox potentials or perform potentiometric titrations The ORP Triode electrodes have a built in thermistor for measuring temperature Epoxy Sure Flow Combination Redox ORP Electrodes Cat No 9678BNWP and 967800 The Sure Flow junction prevents the electrode from clogging in dirty viscous or wastewater samples The epoxy body is break resistant for rugged environments Glass Combination Redox ORP Electrodes Cat No
20. trode and then replenish any lost solution e ake sure the electrode filling solution is appropriate or the sample Use Cat No 900011 filling solution for samples that have a total ionic strength greater than 0 2 M Use Cat No 900001 filling solution for samples that have a otal ionic strength less than 0 2 M 8 Redox ORP Electrode User Guide Electrode Measurements Direct Measurements Direct oxidation reduction potential ORP measurements can be used to determine the oxidizing or reducing capability of a solution and are commonly made in polluted streams chlorinated waters industrial wastewaters and other water samples 1 Prepare the electrode according to the Electrode Preparation section 2 Set the meter to the millivolt relative millivolt or Ey measurement mode 3 Place the electrode into the sample solution 4 When the reading stabilizes record the displayed mV potential and temperature Note Platinum redox electrodes may give unstable readings in solutions that contain chromous vanadous and titanous ions or other ions that are stronger reducing agents than hydrogen or platinum Redox ORP Electrode User Guide Oxidation Reduction Titrations Oxidation reduction or redox titrations provide a simple reliable method for determining many substances in solution A redox titration consists of adding to an unknown sample small increments of a titrant that converts the unknown to a different oxidation s
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