User Guide - Fisher Sci
User GuideCalciumIon SelectiveElectrode
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Table of ContentsIntroduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1Required Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2Serial Dilutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3Electrode Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49720BNWP Calcium Combination Electrode Preparation . . . . . 49320BN Calcium Half-Cell Electrode Preparation . . . . . . . . . . . . 6900100 Single Junction Reference Electrode Preparation . . . . . . 6Checking Electrode Operation (Slope) . . . . . . . . . . . . . . . . . . . . . 7Measurement Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8Sample Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8Measuring Hints . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9Electrode Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10Electrode Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11Analytical Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13Direct Calibration Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . .Small Volume Direct Calibration Technique . . . . . . . . . . . . . . . .Low Level Calibration Technique . . . . . . . . . . . . . . . . . . . . . . . .Known Addition Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . .Calcium Titration Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . .1418222432Electrode Characteristics . . . . . . . . . . . . . . . . . . . . . . . . . 34Electrode Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34Reproducibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34Limits of Detection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35Electrode Life . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35Temperature Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36Complexation and Precipitation . . . . . . . . . . . . . . . . . . . . . . . . . 37Interferences . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38pH Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42Assistance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43Warranty . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43Troubleshooting Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44Ordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46Calcium Ion Selective Electrode User Guide
IICalcium Ion Selective Electrode User Guide
IntroductionThis user guide contains information on the preparation,operation and maintenance for the calcium ion selectiveelectrode (ISE). General analytical procedures, electrodecharacteristics and electrode theory are also included in this userguide. Calcium electrodes measure free calcium ions in aqueoussolutions quickly, simply, accurately and economically.Technical Support Chemists can be consulted for assistanceand troubleshooting advice. Within the United States call1.800.225.1480 and outside the United States call 978.232.6000or fax 978.232.6031. In Europe, the Middle East and Africa,contact your local authorized dealer. For the most currentcontact information, visit www.thermo.com/contactwater.For the latest application and technical resources for ThermoScientific Orion products, visit www.thermo.com/waterapps.Calcium ionplus Sure-Flow Plastic MembraneCombination ISE, Cat. No. 9720BNWPThe calcium combination electrode has the sensing andreference half-cells built into one electrode, which decreases theamount of required solutions and reduces waste. The built-inSure-Flow reference junction prevents electrode clogging andprovides fast and stabile readings. The calcium combinationelectrode is available with a waterproof BNC connector, Cat. No.9720BNWP. Electrodes with a waterproof BNC connector can beused on any ISE or mV meter with a BNC connection.Calcium Plastic Membrane Half-Cell ISE,Cat. No. 9320BNThe calcium half-cell electrode must be used with thesingle junction reference electrode, Cat. No. 900100. Thecalcium half-cell electrode is available with a BNC connector,Cat. No. 9320BN.Calcium Ion Selective Electrode User Guide
Required Equipment1.Thermo Scientific Orion ISE meter, such as the 4-Star pH/ISEmeter or 5-Star pH/ISE/DO/conductivity meter; equivalentISE meter; or mV meter with a 0.1 mV resolution.Calcium electrodes can be used on any ISE or mV meterwith a BNC connection. The electrodes can also be usedon meters with a variety of inputs when an adapter cable isused. Visit www.thermo.com/water for details.2. Thermo Scientific Orion calcium electrode.The 9320BN calcium half-cell electrode requires a separatereference electrode, Cat. No. 900100.3. Magnetic stirrer or Thermo Scientific Orion stirrer probe,Cat. No. 096019. The stirrer probe can be used with 3-Star,4-Star and 5-Star benchtop meters.4. Volumetric flasks, graduated cylinders and beakers. Plasticlabware is required for low level calcium analysis.5. Distilled or deionized water.6. Calcium electrode filling solution.Use Optimum Results A filling solution, Cat. No. 900061,for the 9720BNWP calcium combination electrode.Use 4 M KCl saturated with Ag/AgCl filling solution, Cat. No.900011, for the single junction reference electrode that isused with the 9320BN calcium half-cell electrode.7.0.1 M CaCl2 calcium calibration standard, Cat. No. 922006or 100 ppm calcium as CaCO3 calibration standard,Cat. No. 923206.1000 ppm calcium as Ca 2 solution – Add 25 mL of the 0.1M CaCl2 calcium standard to a 100 mL volumetric flask,dilute to the mark with distilled water and mix the solution.1000 ppm calcium as CaCO3 solution – Add 10 mL of the0.1 M CaCl2 calcium standard to a 100 mL volumetric flask,dilute to the mark with distilled water and mix the solution.8. Calcium ionic strength adjuster (ISA), Cat. No. 932011.ISA provides a constant background ionic strength forsamples and standards. Calcium Ion Selective Electrode User Guide
Serial DilutionsSerial dilution is the best method for the preparation ofstandards. Serial dilution means that an initial standard is diluted,using volumetric glassware, to prepare a second standardsolution. The second standard is similarly diluted to prepare athird standard, and so on, until the desired range of standardshas been prepared.1.To prepare a 10-2 M standard (400.8 ppm as Ca 2 and1000.9 as CaCO3) – Pipet 10 mL of the 0.1 M standard intoa 100 mL volumetric flask. Dilute to the mark with deionizedwater and mix well.2.To prepare a 10-3 M standard (40.08 ppm as Ca 2 and100.09 as CaCO3) – Pipet 10 mL of the 10-2 M standard intoa 100 mL volumetric flask. Dilute to the mark with deionizedwater and mix well.3.To prepare a 10-4 M standard (4.008 ppm as Ca 2 and10.009 as CaCO3) – Pipet 10 mL of the 10-3 M standard intoa 100 mL volumetric flask. Dilute to the mark with deionizedwater and mix well.To prepare standards with a different concentration use thefollowing formula:C1 * V1 C2 * V2C1 concentration of original standardV1 volume of original standardC2 concentration of standard after dilutionV2 volume of standard after dilutionFor example, to prepare 100 mL of a 100 ppm calcium standardfrom a 4008 ppm calcium standard:C1 4008 ppm calciumV1 unknownC2 100 ppm calciumV2 100 mL4008 ppm * V1 100 ppm * 100 mLV1 (100 ppm * 100 mL) / 4008 ppm 2.5 mLCalcium Ion Selective Electrode User Guide
Electrode Setup9720BNWP Calcium CombinationElectrode PreparationNote: Do not to touch the sensing membrane or reference pelletduring the electrode assembly.1.Remove the sensing module from the vial and save the vialfor storage. Make sure that both O-rings are in place on themodule. Remove the electrode handle from the box.2. Unscrew the electrode cap. Slide the cap and spring downthe electrode cable.3. Hold the outer body sleeve and gently push the inner stemthrough the outer body. Slide the outer body sleeve downthe electrode cable until it is beyond the inner stem.4. Grasp the middle of the inner stem without touching thereference pellet. If a red storage tip is connected to theinner stem, unscrew it and save it for storage.5. Screw the sensing module into the stem until it stops andthe module is flush against the stem. Tighten the modulean additional one-quarter turn. The module should be firmlyattached to the stem. Do not overtighten the module.6. Hold the electrode cable and slide the outer body, spring andcap over the inner stem.7.Grasp the outer body sleeve, without touching the sensingmembrane, and gently screw the cap onto the inner stemwhile pulling on the cable. Stop when an opposite force isfelt. Do not overtighten or continue to turn the cap. The capwill not completely stop. If the inner body turns at all, thecap is too tight. Remove the cap and reassemble.8. Press on the top of the cap with your thumb to make surethat the electrode has a smooth flushing motion and theouter body sleeve returns to its original position.9. Install the flip spout cap onto the Optimum Results A fillingsolution bottle and lift the flip spout to a vertical position.Insert the spout into the electrode fill hole and add a smallamount of filling solution to the reference chamber.10. Hold the electrode body and use your thumb to push downon the electrode cap to allow a few drops of filling solutionto drain out of the electrode. Release the electrode cap. Calcium Ion Selective Electrode User Guide
11. If the sleeve does not return to its original position, addfilling solution and repeat step 10 until the sleeve returns toits original position.12. Add filling solution to the electrode up to the fill hole.13. Rinse the electrode with distilled water and soak it in a 100ppm or 10-2 M calcium standard for 1 to 2 hours prior to use.Note: Add filling solution each day before using the electrode.The filling solution level should be at least one inch above thelevel of sample in the beaker to ensure a proper flow rate. The fillhole should always be open when taking measurements.Figure 19720BNWP Calcium Combination Electrodecapspringfill holeouter body sleeveinner stemreference pelletO-ringssensing modulesensing membraneCalcium Ion Selective Electrode User Guide
9320BN Calcium Half-Cell ElectrodePreparationRemove the sensing module from the vial and save the vial forelectrode storage. Make sure that the rubber electrode washeron the sensing module is in place. See Figure 2. Screw thesensing module into the electrode body until the module isfinger-tight. To ensure electrical continuity, shake the electrodedown like a clinical thermometer. Rinse the calcium electrodewith distilled water and then soak it in a 100 ppm or 10-2 Mcalcium standard for 1 to 2 hours prior to use.Note: Do not immerse the electrode past the rubberelectrode washer.900100 Single Junction ReferenceElectrode PreparationPrepare the reference electrode according to the referenceelectrode user guide. Fill the reference electrode with 4 M KClsaturated with Ag/AgCl filling solution, Cat. No. 900011.Note: Do not use the filling solution that ships with the900100 single junction reference electrode because it containsinterferences for calcium measurements.Figure 29320BN Calcium Half-Cell ElectrodeElectrode BodyWasherSensing ModuleSensing Membrane Calcium Ion Selective Electrode User Guide
Checking Electrode Operation (Slope)These are general instructions that can be used with mostmeters to check the electrode operation. Refer to the meter userguide for more specific information.This procedure measures electrode slope. Slope is definedas the change in millivolts observed with every tenfold changein concentration. Obtaining the slope value provides the bestmeans for checking electrode operation.1.If the electrode has been stored dry, prepare the electrodeas described in the Electrode Preparation section.2. Connect the electrode to a meter with a mV mode. Set themeter to the mV mode.3. Add 100 mL of distilled water and 2 mL of ISA into a 150 mLbeaker. Stir the solution thoroughly.4. Rinse the electrode with distilled water and place theelectrode into the solution prepared in step 3.5. Select either a 0.1 M or 1000 ppm calcium standard. Pipet1 mL of the standard into the beaker and stir the solutionthoroughly. When a stable reading is displayed, record theelectrode potential in millivolts.6. Pipet 10 mL of the same standard into the same beakerand stir the solution thoroughly. When a stable reading isdisplayed, record the electrode potential in millivolts.7.There should be a 25 to 30 mV difference between the twomillivolt readings when the solution temperature is between20 to 25 C. If the millivolt potential is not within this range,refer to the Troubleshooting section.Calcium Ion Selective Electrode User Guide
Measurement UnitsCalcium concentration can be measured in moles per liter (M),parts per million (ppm) or any convenient concentration unit.Table 1Concentration Unit Conversion FactorsMoles/Liter (M)ppm as Ca 2ppm as 10-340.1100.08910-44.010.0089Sample RequirementsAll samples must be aqueous and must not contain organicsolvents. Contact Technical Support for information on using theelectrode for specific applications.The solution temperature must be less than 40 C.Samples and standards should be at the same temperature. A1 C difference in temperature for a 10-3 M calcium solution willgive rise to about a 4% error when using the 9320BN calciumhalf-cell electrode and about a 1.2% error when using the9720BNWP calcium combination electrode.Interferences should be absent from all samples. See theInterferences section for a list of possible interferences.In all analytical procedures, ISA must be added to all samples andstandards before measurements are taken. Calcium Ion Selective Electrode User Guide
Measuring Hints Stir all standards and samples at a uniform, moderate rate.Place a piece of insulating material, such as Styrofoam orcardboard, between the magnetic stir plate and beaker toprevent measurement errors from the transfer of heat tothe sample. Always use freshly prepared standards for calibration. Always rinse the electrode with distilled water betweenmeasurements and shake the electrode to remove thewater and prevent sample carryover. Do not wipe or rub theelectrode sensing module. Store the calcium electrode in a 10-2 M or 100 ppm calciumstandard between measurements. The 9320BN calcium half-cell electrode should be immersedin standards and samples to approximately half the length ofthe calcium module. Do not immerse the calcium electrodepast the electrode washer. Immerse the referenceelectrode to the same depth as the calcium electrode. Allow all standards and samples to reach the sametemperature for precise measurements. Verify the electrode calibration every two hours by placingthe electrode in a fresh aliquot of the least concentratedstandard used for calibration. If the value has changed bymore than 2%, recalibrate the electrode. After immersing the electrode in a solution, check theelectrode sensing surface for air bubbles and remove airbubbles by reimmersing the electrode in the solution andgently tapping it. For high ionic strength samples, prepare standards with abackground composition similar to the sample. The fill hole cover must be open during measurements toensure a uniform flow of filling solution. If the combination electrode is used and the electrode isused in dirty or viscous samples or the electrode responsebecomes sluggish, empty the electrode completely, holdthe junction open and flush the junction with distilled water.Empty any water from the electrode and refill it with freshfilling solution. Press down on the electrode cap to let a fewdrops of the filling solution flow out of the electrode andthen replenish any lost solution.Calcium Ion Selective Electrode User Guide
Electrode StorageCalcium Combination Electrode Storage,Cat. No. 9720BNWPFor storage between measurements and up to three days, storethe electrode in a 10-2 M or 100 ppm calcium standard. The fillingsolution inside the electrode should not be allowed to evaporate,as crystallization will result.For storage longer than one week, drain the electrode, flushthe reference chamber with distilled water, disassemble theelectrode and store the sensing module in the glass vial.1.Grasp the outer body sleeve and unscrew the electrode cap.Slide the cap and spring assembly down the electrode cable.2. Push the inner stem of the electrode handle out through theouter electrode sleeve, exposing the sensing module.3. Rinse the inner stem and module well with distilled water.Gently blot dry to prevent damaging the sensing module.4. Carefully unscrew the sensing module from the inner stem,taking care not to touch the sensing membrane.5. Place the calci
Prepare the reference electrode according to the reference electrode user guide . Fill the reference electrode with 4 M KCl saturated with Ag/AgCl filling solution, Cat . No . 900011 . Note: Do not use the filling solution that ships with the 900100 single junction reference electrode because it contains interferences for calcium measurements .
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