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Horiba Scientific 6561S-10C Instruction Manual

Combination type fluoride ion selective electrode
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Instruction Manual
Combination type Fluoride Ion
Selective Electrode
6561S-10C
ELECTRODE

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  • Page 1 Instruction Manual Combination type Fluoride Ion Selective Electrode 6561S-10C ELECTRODE...
  • Page 2 Preface This manual describes operation of the combination type fluoride ion selective electrode. Be sure to read this manual before using the product to ensure proper and safe operation of the product. Also safely store the manual so it is readily available whenever necessary. Please contact HORIBA Advanced Techno if any points regarding safety come to your attention during use.
  • Page 3  China regulation 标记的意义 Meaning of Marking 本标记适用在中华人民共和国销售电器电子产品， 标记中央的数字表示环 境保护使用期限的年数。 (不是表示产品质量保证期间。 ) 只要遵守这个产 品有关的安全和使用注意事项， 从制造日开始算起在这个年限内， 不会给环 境污染、 人体和财产带来严重的影响。 请不要随意废弃本电器电子产品。 This marking is applied to electric and electronic products sold in the People's Republic of China. The figure at the center of the marking indicates the environmental protection use period in years.
  • Page 4  For your safety  Hazard classification and warning symbols Warning messages are described in the following manner. Read the messages and follow the instructions carefully.  Hazard classification This indicates an imminently hazardous situation which, if not avoided, will result in death or serious injury.
  • Page 5  Safety precautions This section provides precautions for using the product safely and correctly and to prevent injury and damage. The terms of DANGER, WARNING, and CAUTION indicate the degree of imminency and hazardous situation. Read the precautions carefully as it contains important safety messages. Precautions for chemicals Solutions used for calibration and measurement must not come in contact with the skin, or consumed.
  • Page 6  Product handling information  Operational precautions Use of the product in a manner not specified by the manufacturer may impair the protection provided by the product. And it may also reduce product performance. Exercise the following precautions:  Use the supplied internal solution for the reference electrode. Using any other internal solutions may cause measurement errors.
  • Page 7  Manual information  Description in this manual The following explains the icons used in this manual. Icon Meaning This interprets the necessary points for correct operation and notifies the important points for handling the product. Note Note This indicates reference information. This indicates the part where to refer for information.

  • Page 9: Table Of Contents

    ontents Before Use Confirmation of the items included in the package ..2 About this product ....... . 3 Measurement procedure .
  • Page 10 How to clean the electrode ......44 Maintenance Storage ........50 Consumables .
  • Page 11 igures Fig. 1 Included items ......2 Fig. 2 System configuration..... . 3 Fig.
  • Page 12 ables Table 1 F concentration measurement unit conversion table ....... . . 35 Table 2 Check list .

  • Page 13: Before Use

    efore Use This chapter describes what you should know before using the product. Confirmation of the items included in the package ........2 About this product ......3 Product features............3 System configuration ...........3 Names of parts.............4 Measurement procedure ....5...

  • Page 14: Confirmation Of The Items Included In The Package

    onfirmation of the items included in the package Open the package and make sure that the following items are included. 1000 mg/L standard solution (50 mL) Main unit 100 mg/L standard solution (50 mL) of electrode Internal solution Ion electrode tip (50 mL) Instruction manual...

  • Page 15: About This Product

    bout this product  Product features The combination type fluoride ion selective electrode is an electrode that combines a tip type ion electrode with a reference electrode. This product has the following features.  Ion concentration can be measured with this one electrode. There is no need to use a pair of an ion selective electrode and reference electrode.

  • Page 16: Fig. 3 Names Of Parts

     Names of parts This product consists of the parts shown in the figure below. Cable Electrode cap Protective cap Internal solution fill port Internal solution chamber Electrode connector (BNC connector) Ion electrode tip Support pipe Ion selective membrane Liquid junction Rubber cap Protective pipe * When the ion electrode tip is...

  • Page 17: Measurement Procedure

    easurement procedure The following figure shows the procedure for measuring the F concentration. Measurement preparation Rinse with pure water. page 15) Fill with internal solution. page 12) Attach the ion electrode tip. page 10) Meter Connect the electrode to the meter. page 17)
  • Page 18 Calibration Measurement Prepare two types of Prepare the sample solution. solutions for calibration. page 36) page 23) Perform calibration. page 25) In the following cases, perform conditioning of the electrode before calibration. Perform measurement.  Before the first use page 37) ...
  • Page 19 After measurement Discharge the internal solution from the electrode. Rinse the electrode page 43) with pure water. page 44) When the electrode will not be used for two weeks or longer, store it as described on page 50. Note Note...

  • Page 21: Electrode Preparation

    lectrode Preparation This chapter describes the preparation that must be performed before using the product. Assembling the electrode (only when use for first time)......10 Filling with internal solution ..12 Rinsing the electrode..... 15 Connecting the electrode to the meter ..........

  • Page 22: Assembling The Electrode (Only When Use For First Time)

    ssembling the electrode (only when use for first time) When using the product for the first time, assemble the View video View video electrode as described in the following procedure. Item to be prepared Ion electrode tip Remove the protective cap. Protective cap Remove the rubber cap.
  • Page 23 Attach the ion electrode tip by turning it clockwise. Ion electrode tip...

  • Page 24: Filling With Internal Solution

    illing with internal solution Be sure to fill the electrode with internal solution as View video View video described in the following procedure before use.  Be sure to fill with internal solution before use. If measurement is performed in the state in which there is not much internal solution, an inflow of sample solution into the electrode will result in accurate...
  • Page 25 Make sure that there is no internal solution remaining. If there is any internal solution remaining, remove it all. Steps 1 to 2 of “How to clean the electrode” (pages 44 to 45.)) Open the rubber stopper of the Rubber stopper internal solution fill port.
  • Page 26 Make sure that the inside of the electrode moves up and down and that internal solution oozes out from the liquid junction. View video View video The internal solution oozes out from the liquid junction. It is best that the internal solution oozes out slightly. If the outflow is extremely little, the potential of the reference electrode will become unstable and susceptible to stir.

  • Page 27: Rinsing The Electrode

    insing the electrode Make sure that no dirt and other foreign matters have View video View video adhered to the electrode before measurement. If dirt and other foreign matters have adhered to the electrode, rinse the electrode as described in the following procedure.
  • Page 28 Make sure that there are no dirt and crystals of internal solution adhered to the area around the liquid junction. Contamination If dirt and crystals of internal solution are adhered, they may affect the outflow of internal solution. Rinse the electrode with pure water again.

  • Page 29: Connecting The Electrode To The Meter

    onnecting the electrode to the meter Connect the electrode to the meter. View video View video For details on the connector of the meter to which the electrode will be connected, refer to the instruction manual of the meter. Connect the electrode connector to the meter. When disconnecting the electrode from the meter, disconnect it in the opposite direction from step 1.

  • Page 31: Calibration

    alibration This chapter describes calibration. Standard solutions......20 TISAB ..........21 Calibration operation ..... 23...

  • Page 32: Standard Solutions

    tandard solutions The following standard solutions are used for calibration and measurement.  1000 mg/L F standard solution Use the standard solution included in the package or available as consumables by HORIBA Advanced Techno.  100 mg/L F standard solution Use the standard solution included in the package or available as consumables by HORIBA Advanced Techno.

  • Page 33: Tisab

    ISAB The following TISAB (Total Ionic Strength Adjustment Buffer) is used for calibration and measurement.  When measuring a general sample solution Use the provided TISAB, or the TISAB sold separately by HORIBA Advanced Techno. Alternatively, prepare the sample solution as described in the following ASTM D1179 method B.
  • Page 34  When measuring a sample solution containing high- concentration steel and aluminum. Prepare the sample solution as described in the following ASTM D1179 method B. (1) Pour 500 mL of pure water in a 1 L beaker. (2) Add the following three to (1). ...

  • Page 35: Calibration Operation

    alibration operation Measure standard solutions in ascending order of ion concentration to create calibration curves in the meter ( “Measurement principle of ion selective electrode” (page 62)). Perform calibration once every day or before measurement as appropriate. Before operation  Be sure to fill with internal solution and rinse the electrode before the calibration operation.
  • Page 36 Set the meter as shown below. Set the valence as shown in the Setting item Setting value table on the right. Valence Prepare the standard solutions. Prepare the two types of standard solution to create F concentration ratio 1:10. For example, if the sample solution concentration is 250 mg/L, prepare standard solutions of 100 mg/L and 1000 mg/L.
  • Page 37 Additive amount of TISAB In the case using different volume from the example, note that the volume ratio shall be the standard solution: the Note Note TISAB = 1:1. Prepare the second solution for calibration. (1) Put 25 mL of standard solution (concentration of 1000 mg/L) in a 100 mL beaker.
  • Page 38 Wipe off the moisture. Wipe off the moisture using soft and clean lint-free paper or cloth. If the ion selective membrane is rubbed severely to remove the moisture, the ion selective membrane may tear or static electricity may be generated, resulting in a measurement errors.
  • Page 39 Soak the electrode in the first solution for calibration prepared in step 3. Place the electrode fully into the solution for calibration so that the solution comes up to the liquid junction.  Do not touch the stir bar with the electrode. It may damage the electrode.
  • Page 40 Shake the electrode to remove any air bubbles remaining on the ion selective membrane. Shake the electrode View video View video If air bubbles remain on the ion selective membrane, it may result in inaccurate measurement. Note Note Perform the first calibration. Wait for a stable reading and perform the first calibration as described in the Meter Instruction Manual.
  • Page 41 Wipe off the moisture. Wipe off the moisture using soft and clean lint-free paper or cloth. If the ion selective membrane is rubbed severely to remove the moisture, the ion selective membrane may tear or static electricity may be generated, resulting in a measurement errors.
  • Page 42 It is recommended to place the electrode in the electrode stand. Shake the electrode to remove any air bubbles remaining on the ion selective membrane. Shake the electrode View video View video If air bubbles remain on the ion selective membrane, it may result in inaccurate measurement.
  • Page 43 Check that slope is at least 80%. If the slope is less than 80%, the measurement may not be performed accurately. The possible causes of calibration failure are:  Dirt on the ion selective membrane or liquid junction  Change in the internal solution concentration ...
  • Page 44 Wipe off the moisture. Wipe off the moisture using soft and clean lint-free paper or cloth. If the ion selective membrane is rubbed severely to remove the moisture, the ion selective membrane may tear or static electricity may be generated, resulting in a measurement errors.

  • Page 45: Measurement

    easurement This chapter describes measurement. Requirements for sample and standard solutions ......34 Measurement hints ......35 Measurement units ......35 Measurement operation....36...

  • Page 46: Requirements For Sample And Standard Solutions

    equirements for sample and standard solutions The requirements for sample solutions and standard solutions are as follows:  Sample solutions shall not contain organic substances. It may cause electrode deterioration.  The temperatures of sample solution and standard solution shall be kept at 50°C or less.

  • Page 47: Measurement Hints

    easurement hints  A gradual rise in solution temperature due to the magnetic stirrer generating heat may cause an apparent potential drift. When it happens, reduce the influence of the temperature changes by covering the magnetic stirrer with heat insulation such as polystyrene foam or using a thermostatic bath.

  • Page 48: Measurement Operation

    easurement operation Before operation The calibration characteristics vary depending on the temperature. The standard solution in calibration and the sample solution in measurement shall have almost the same temperature. Match the temperature as close as possible by, for Note Note example, using a thermostatic bath.
  • Page 49 (1) Put 25 mL of sample solution (concentration of 250 mg/L) in a 100 TISAB: 25 mL mL beaker. Sample solution (2) Add 25 mL of TISAB. (250 mg/L): (3) Stir the solution slowly with a magnetic 25 mL Beaker: 100 mL stirrer.
  • Page 50 Wipe off the moisture. Wipe off the moisture using soft and clean lint-free paper or cloth. If the ion selective membrane is rubbed severely to remove the moisture, the ion selective membrane may tear or static electricity may be generated, resulting in a measurement errors.
  • Page 51  Do not touch the stir bar with the electrode. It may damage the electrode.  Make sure that the rubber stopper of the internal solution fill port is open during measurement. If it is closed, the internal Note Note solution does not ooze out very much from the liquid junction.
  • Page 52 View video View video If air bubbles remain on the ion selective membrane, it may result in inaccurate measurement. Note Note Perform the measurement. Wait for a stable reading and measure the ion concentration as described in the Meter Instruction Manual. When the measurement of the ion concentration is finished, take out the electrode from the sample solution.
  • Page 53 Wipe off the moisture. Wipe off the moisture using soft and clean lint-free paper or cloth. If the ion selective membrane is rubbed severely to remove the moisture, the ion selective membrane may tear or static electricity may be generated, resulting in a measurement errors.

  • Page 55: After Measurement

    fter Measurement This chapter describes cleaning of the electrode after measurement. How to clean the electrode.... 44...

  • Page 56: How To Clean The Electrode

    ow to clean the electrode Clean the electrode after use as described in the following View video View video procedure. Item to be prepared Dropper Open the rubber stopper of the Rubber stopper internal solution fill port.
  • Page 57 Remove the internal solution in one of the following ways. <Discharging from the liquid junction> Spread soft and clean lint-free paper or cloth beneath the electrode and then press the electrode against it from above. The inside of the electrode moves up and The internal solution down.
  • Page 58 Close the rubber stopper of the internal solution fill port. Rinse the electrode with pure water. Wipe off the moisture. Wipe off the moisture using soft and clean lint-free paper or cloth. If the ion selective membrane is rubbed severely to remove the moisture, the ion selective membrane may tear or static electricity may be generated, resulting in a measurement errors.
  • Page 59 Make sure there are no dirt and crystals of internal solution adhered to the area around the liquid junction. If dirt remains, repeat steps 4 and 5. Contamination Attach the protective cap. Do not get water and foreign matters inside of the protective cap when attaching it to the electrode.

  • Page 61: Maintenance

    aintenance This chapter describes the storage procedure of the electrode as well as the lifespan and replacement procedure of each part. Storage..........50 Main unit of electrode..........50 Consumables........51 Consumables and replacement periods ....51...

  • Page 62: Storage

    torage When the electrode will not be used for two weeks or longer, store it as described in the following procedure.  Main unit of electrode Clean the electrode and discharge the internal solution. “After Measurement” (page 43)) Attach the protective cap. ...

  • Page 63: Consumables

    onsumables  Consumables and replacement periods The consumables that need to be replaced and the replacement periods are as follows. Replace each part at the appropriate timing to ensure accurate measurement. approx. 1 year approx. 1 year approx. 1 year Replace Service life Ion electrode tip...
  • Page 64 Single piece of the electrode main unit is not available for sale. When replacing the main unit of electrode, purchase the combination type fluoride ion selective electrode including Note Note the ion electrode tip (3200693774). Use this up before the expiration date displayed on the bottle.

  • Page 65: Troubleshooting

    roubleshooting This chapter describes the measures to take when accurate measurement is not possible. When accurate measurement is not possible........... 54...

  • Page 66: When Accurate Measurement Is Not Possible

    hen accurate measurement is not possible When accurate measurement is not possible, check the following. Table 2 Check list Check item Solution View in video Are the temperatures The standard solution in of the standard calibration and the sample solution and sample solution in measurement shall solution the same? have almost the same...
  • Page 67 Check item Solution View in video Is the temperature of A gradual rise in solution the solution being temperature due to the magnetic stirred rising? stirrer generating heat may cause an apparent potential drift. Reduce the influence of the temperature changes by covering ―...
  • Page 68 Check item Solution View in video Has the internal Replace the internal solution solution been before each measurement. replaced? If not, the internal solution concentration will change and it will cause measurement errors. “How to clean the electrode” (page 44)) Is there a sufficient Make sure that the surface of the amount of internal...
  • Page 69 Check item Solution View in video Has the composition If the standard solution has and concentration of expired, replace it with a new one. a standard solution Use up the standard solution changed? within approximately 3 months after opening the bottle. ―...

  • Page 71: Reference

    eference This chapter describes general matters regarding ion selective electrodes. Ion selective electrodes....60 Measurement principle of ion selective electrode ............62 About activity..............64 Characteristics of fluoride ion selective electrode ......66 Measurement range...........66 Impact of pH...............67 Impact of temperature ..........68 Impact of stirring............69 Impact of coexistent ions..........70 Response time ............71...

  • Page 72: Ion Selective Electrodes

    on selective electrodes The ion concentration is measured as the potential difference between an ion selective electrode and a reference electrode which are soaked into the sample solution and connected with an ion meter or a meter with an ion measurement function.

  • Page 73: Fig. 5 State Of Liquid Junction Of Reference Electrode

    Mechanism with which the reference electrode maintains a stable potential The reference electrode generates the potential that is used as the reference against the potential measured with the V ≈ 0 ion selective electrode. That potential needs to be stable with very little variation no matter what kind of sample Fig.

  • Page 74: Measurement Principle Of Ion Selective Electrode

    easurement principle of ion selective electrode If specific ions exist in the sample solution, the ion selective membrane of the ion selective electrode generates a potential that corresponds to the concentration of those ions. The generated potential is measured as the potential difference on the basis of the reference electrode using an ion meter or meter with an ion measurement function.

  • Page 75: Fig. 6 Relationship Between Monovalent Cation Concentration (Activity) And Electrode Potential

    If the ion concentration (activity) is set to the logarithmic axis, a linear relationship like in the graph below is created between the electrode potential measured with the ion selective electrode and the ion concentration (activity). ∆2.303 RT/nF Potential gradient 59.16 mV/decade (at 25ºC) Ion concentration (activity) Fig.

  • Page 76: Fig. 7 Difference In State Of Solution Depending On Ion

     About activity The ion concentration can be accurately measured by performing calibration and measurement using a TISAB. The following describes the relationship between the ion concentration and activity, and the reason for adding a TISAB. Distance Distance The concentration increases The number of solvent Solvent...

  • Page 77: Table 4 (Example) Activity Coefficient For Monovalent Ion

    The activity is a concentration of ions in the solution that is corrected using a coefficient called the activity coefficient, and the relationship between them can be expressed with the following relational expression. Activity (a) = Activity coefficient () · Ion concentration (C) Table 4 shows the relationship between the ion concentration and the activity coefficient.

  • Page 78: Characteristics Of Fluoride Ion Selective Electrode

    haracteristics of fluoride ion selective electrode  Measurement range The range where linearity is established between the logarithm of the ion concentration and the electromotive force is called the measurement range. In general, the range for measuring ion concentration using ion selective electrodes is a maximum of around 110 mol/L and a minimum of around 110...

  • Page 79: Fig. 9 Impact Of Ph On Fluoride Ion Selective Electrode

     Impact of pH The usable pH range is determined depending on the type and the structure of the ion selective electrode. In general, this range is smaller when the concentration of the ions to be measured is lower. Also, depending on the ion selective electrodes, the components of the ion selective membrane may be dissolved by the pH or the electrode potential may change due to the impact of the pH.

  • Page 80: Table 5 Relationship Between Temperature Of Ion Selective Electrode And Theoretical Slope

     How to prepare a sample solution Either use TISAB ( Page 21), or adjust the pH of the sample solution as described in the following procedure.  If the pH of the sample solution exceeds 8, adjust the pH in the range of 5 to 8 by adding hydrochloric acid.

  • Page 81: Table 6 Relationship Between Temperature Of Chloride Ion Selective Electrode

    Table 6 Relationship between temperature of chloride ion selective electrode and theoretical slope Temperature Theoretical slope of fluoride ion selective electrode [°C] [mV/decade] -54.20 -56.18 -58.16 -59.16 -60.15 -62.13 -64.11 If the temperature of the sample solution in measurement differs from the temperature of the standard solution in calibration, perform calibration again.

  • Page 82: Impact Of Coexistent Ions

     Impact of coexistent ions Although ion selective electrodes have good selectivity with respect to the ions to be measured, they may react to the other ions. The ions which interfere the measurement of the concentration of the ions to be measured are called “interfering ion”. Therefore, when using the ion electrode method, it is important to know the effects of coexistent ions and take measures to avoid them.

  • Page 83: Response Time

     Response time The response times of ion selective electrodes differ depending on factors such as the type and structure of the electrode, and type and concentration of ions. In general, the response time tends to be shorter when the ion concentration is high and longer when the ion concentration is low.

  • Page 84: Standard Solutions

     Standard solutions  Selecting standard solutions  Perform calibration using standard solutions of 100 mg/L and 1000 mg/L. Approximate concentrations can be measured.  For more accurate measurements, prepare standard solutions which have the following concentration relationship for calibration. Standard solution with low concentration <...

  • Page 85: Material

    aterial This chapter describes the specifications, external dimensions, and consumables of the product. Specifications......... 74 External dimensions ...... 75 Consumables........76...

  • Page 86: Specifications

    pecifications The following table shows the specifications of the product. Table 7 Specifications of combination type fluoride ion selective electrode Item Description Operating temperature range 0°C to 50°C Internal electrode Ag/AgCl (silver/silver chloride) electrode Internal solution 3.3 mol/L KCl Liquid junction Movable sleeve type Wetted part (part contacting , PSU...

  • Page 87: External Dimensions

    xternal dimensions 16.5 O.D. [Unit: mm]...

  • Page 88: Consumables

    onsumables Consumables can be purchased from your nearest local representative by notifying the product name and the part number. Table 8 Consumables Specifica- Product name Model Part number tions Fluoride ion selective 6561S- 3200693774 electrode Fluoride ion selective 7661S Electrode 3200693606 electrode tip 1000 mg/L fluoride ion...
  • Page 89 31, Miyanonishi-cho, Kisshoin Minami-ku, Kyoto 601-8306, Japan http://www.horiba-adt.jp For any questions regarding this product, please contact your local agency, or inquire from the following website. http://global.horiba.com/contact_e/index.htm...

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