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18.  Appendices 

18.1  pH Electrode Fundamentals 

pH  electrodes  are  generally  combination  electrodes,  where  the  pH  sensing  membrane  and  the 
reference  system  are  contained  in  a  single  body.  The  sensing  membrane  is  the  round  or  spear 
shaped  bulb  at  the  tip  of  the  electrode.  This  produces  a  voltage  that  changes  with  the  pH  of  the 
solution.  This  voltage  is  measured  with  respect  to  the  reference  section.  The  reference  section 
makes  contact  with  the  sample  solution  using  a  salt  bridge,  which  is  referred  to  as  the  reference 
junction.  A  saturated  solution  of  KCl  is  used  to  make  contact  with  the  sample.  It  is  vital  that  the 
KCl solution has an adequate flow rate in order to obtain stable, accurate pH measurements. 

18.1.1  Asymmetry of a pH Electrode 

An  “ideal”  pH  electrode  produces  0  mV  output  at  7.00  pH.  In  practice,  pH  electrodes  generally 
produce 0 mV output at slightly above or below 7.00 pH. The amount of variance from 7.00 pH is 
called the asymmetry.  

Figure 18-1 illustrates how asymmetry is expressed for a pH electrode. 

 

Figure 18-1 

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-400

-200

0

200

400

600

0

7

14

m

V

+1.00 pH Asymmetry

0.00 pH Asymmetry

-1.00 pH Asymmetry

Response of pH Electrode, as a Function of Asymmetry

pH

Содержание smartCHEM-pH

Страница 1: ...ub sections have also been included to enable you to find the information you need at a glance 2 Introduction The introduction has a diagram and explanation of the display and controls of the smartCHE...

Страница 2: ...Ltd ABN 30 009 773 371 Unit 6 253 Leitchs Road Brendale QLD Australia 4500 Phone 07 3205 8027 International 61 7 3205 8027 Fax 07 3808 4871 International 61 7 3808 4871 Email tps tps com au Web www t...

Страница 3: ...essages 25 5 Absolute Millivolt Mode 27 5 1 Selecting Absolute Millivolt Mode 27 5 2 Absolute Millivolt Calibration 27 5 3 mV Calibration Notes 28 5 4 mV Calibration Messages 29 6 Relative Millivolt M...

Страница 4: ...e RS232 Port 48 13 RS232 Port 49 13 1 Setting the Baud Rate 49 13 2 Sending Readings to the RS232 Port 49 13 3 RS232 Configuration 49 13 4 Communication and Statistical Software 49 13 5 Commands 50 13...

Страница 5: ...s This is essential to produce a waterproof seal Always replace the waterproof cap when a connector is not in use to maintain waterproof integrity Function and Menu Keys One Touch and Enter Keys Numer...

Страница 6: ...nually record readings into the Logger See section 12 1 Press to transmit current reading plus date and time to the RS232 port See section 13 2 Press to start and stop Automatic Datalogging See sectio...

Страница 7: ...121306 6 pH4 00 Buffer 200mL 121381 7 Plug Pack Power Supply 130048 8 smartCHEM Titro Handbook 130050 Options that may have been ordered with your smartCHEM Titro 1 Schott Universal Digital Piston Bu...

Страница 8: ...ny other can be entered during calibration Sensor Asymmetry Range 1 00 to 1 00 pH Sensor Slope Range 85 0 to 105 0 1 9 2 Absolute and Relative mV Ranges Resolution Accuracy 0 to 400 0 mV 0 to 1500 mV...

Страница 9: ...te month year hours minutes seconds Good Laboratory Practices Date time and results of last calibration for all parameters are stored This information can be recalled or sent to the RS232 port at any...

Страница 10: ...F1 Recall F2 Erase F1 Erase All F2 Erase Last F3 Print F4 Program F1 Secs F2 Mins F3 Hours F3 Mode F1 0 01pH F2 0 001pH F3 mV F4 Rel mV F5 Titrator F1 Titrator ON F3 Titrator OFF F4 Setup F1 pH Buffer...

Страница 11: ...rn the Automatic Titrator function OFF Press to quit without changing the current selection 3 In normal display mode the smartCHEM Titro will now prompt you to press to start the Standard Titration Fo...

Страница 12: ...ace to fit the entire Titration apparatus 2 If computer interfacing is desired connect the Serial cable 130041 to the Power RS232 socket of the smartCHEM Titro 3 Connect the AC DC Adaptor 130048 to th...

Страница 13: ...or full details on setting up this device The default factory settings should not need to be changed for use with the TPS smartCHEM Titro 5 Connect the pH sensor to the pH mV Ion socket and the Temper...

Страница 14: ...l band is the number of pH units or the number of Millivolts away from the end point at which titrant addition is slowed down to avoid overshooting The addition rate is slowed down from the maximum do...

Страница 15: ...set the proportional band 1 Select the Titration menu F4 Setup F6 Titr 2 Select F2 Prop from the menu The following screen is now displayed Enter Proportional Band 1 00pH Enter the proportional band f...

Страница 16: ...ct a Negative or Positive value for the Endpoint 3 The direction of the titration process can now be selected For pH Titrations For mV and Relative mV Titrations STD Parameters Titration Direction F1...

Страница 17: ...lay is shown in normal display mode 4 00pH 25 0 oC 0 00mL 12 00 00 Press F6 to start STD Titration If the Automatic Datalogging function is programmed as per section 12 2 an additional prompt informs...

Страница 18: ...232 compatible printer Press to exit and return to the opening screen 3 5 12V DC Switched Output Optional When the smartCHEM Titro is in Standard Titrator mode the 12V DC output can be activated manua...

Страница 19: ...e 1 Select the Mode menu F3 Mode Mode F1 0 01pH F2 0 001pH F3 mV F4 Rel mV F5 Titrator The arrow indicates the current selection Press to select pH mode with 0 01 pH resolution Press to select pH mode...

Страница 20: ...menu is now displayed Select Secondary Buffers F1 4 00 9 23pH F3 4 00 10 06pH The arrow indicates the current selection Press to select pH4 00 and pH9 23 as the Secondary Buffers Press to select pH4 0...

Страница 21: ...21 5 If you wish to use a pH buffer other than one of those listed above its value can be keyed in during calibration Make sure that pH versus Temperature data for the buffer is known...

Страница 22: ...orrect order For the pre programmed buffers see section 4 2 this order can be any one of the following First Point Second Point Third Point pH6 88 or pH7 00 pH4 00 pH9 23 or pH10 06 pH4 00 pH6 88 or p...

Страница 23: ...ually set see sections 7 1 and 7 4 NOTE For real temperature readings the decimal point is shown by a when the temperature readout is not calibrated 4 Remove the wetting cap from the pH sensor Rinse t...

Страница 24: ...bility press to disable the Automatic Stability Function 9 The meter is now 1 point calibrated Note that a will not be removed until a 2 point calibration has been performed Rinse the pH and Temperatu...

Страница 25: ...point calibration should be performed at least monthly Of course more frequent calibration will result in greater confidence in results 5 All calibration information is retained in memory when the sma...

Страница 26: ...mmetry 3 If a 2 point calibration has been successfully performed the smartCHEM Titro will display the following message and the asymmetry and slope of the electrode Slope Asymmetry Calibration OK 0 1...

Страница 27: ...Cal Change to 2 point F1 Yes F2 No Press to proceed with a 2 point calibration The second slope currently in memory from the previous 3 point calibration will be deleted Press to cancel without re ca...

Страница 28: ...s eg ISE s and solutions please substitute them when carrying out this procedure 1 Plug the Redox sensor into the pH mV Ion BNC socket Temperature compensation is not applicable for Millivolt mode so...

Страница 29: ...sable the Automatic Stability Function 7 The smartCHEM Titro is now calibrated for mV and is ready for use in this mode Discard the used samples of standard Rinse the Redox sensor in distilled water a...

Страница 30: ...et 10 0mV 2 If a mV calibration has failed the smartCHEM Titro will display the following message and the failed offset value of the sensor Calibration Failed Offset 100 0mV 3 The smartCHEM Titro has...

Страница 31: ...nown standard Relative mV cannot be Zeroed when the smartCHEM Titro is in Automatic Titration mode as the is used to start the titration process 1 Plug the Redox sensor into the pH mV Ion BNC socket T...

Страница 32: ...mediately without waiting for complete stability press to disable the Automatic Stability Function 8 The smartCHEM Titro Relative mV mode is now zeroed and is ready for use The readout can be re zeroe...

Страница 33: ...rature throughout the beaker 4 Select Temperature Calibration F1 Calibrate F3 Temperature The Temperature Calibration screen is now displayed for example Enter Actual Temperature _ 24 0 OC The current...

Страница 34: ...tion Messages 1 If a temperature calibration has been successfully performed the smartCHEM Titro will display the following message and the offset of the sensor Calibration OK Offset 0 1 OC 2 If a tem...

Страница 35: ...alibrate F3 Temp 4 The current temperature setting is now displayed For example Enter Manual Temperature 25 0 OC Menu Quits 5 Enter the temperature of the sample using the Numeric Keypad Press to save...

Страница 36: ...parameters have not stabilised in case user intervention is required 2 When ALL parameters have stabilised all highlighting will be removed and the will change to a All readings are now frozen For exa...

Страница 37: ...is applied again The highlighting is provided to give the operator a visual indication of exactly which parameters have not stabilised in case user intervention is required 2 When ALL parameters have...

Страница 38: ...As each parameter becomes stable the highlighting is removed If any parameter subsequently becomes unstable the highlighting is applied again The highlighting is provided to give the operator a visua...

Страница 39: ...ht menu F4 Setup F3 Backlight 3 The Backlight menu is now displayed BACKLIGHT F1 On F2 Off F3 Energy Saver The arrow indicates the current selection Press to set the Backlight to be on continuously Pr...

Страница 40: ...ul calibration as shown in the following example where the last pH calibration has failed smartCHEM T V1 0 T1234 31 12 04 13 00 mV Offset 10mV 31 12 04 12 00 pH Asymmetry 0 10pH 00 00 00 00 00 pH Slop...

Страница 41: ...to be reminded that calibration is due every week Press to be reminded that calibration is due every 2 weeks Press to be reminded that calibration is due every 4 weeks Press to switch the GLP Calibrat...

Страница 42: ...ed on the same day of the week as when the function was first activated even if the unit is not calibrated on that day For example if the GLP Calibration Alarm is triggered weekly on a Monday and the...

Страница 43: ...erification New Access code _ Re Enter to Verify Re enter the access code as per the previous step Press to quit without enabling the Access Code system 5 The smartCHEM Titro now confirms that the Acc...

Страница 44: ...nging the Access Code 4 The smartCHEM Titro now prompts you to re enter the access code for verification New Access code _ Re Enter to Verify Re enter the access code as per the previous step Press to...

Страница 45: ...pped as required When any period greater than Zero is programmed Datalogging starts and stops automatically during a titration procedure 1 Select the Logger menu F2 Logger 2 Select F4 Program from the...

Страница 46: ...ts and stops automatically during a titration procedure When the smartCHEM Titro is logging into its own memory the display will look like this 7 00pH 25 0OC 31 12 04 Log 1 12 00 00 The log number wil...

Страница 47: ...Press and to move forwards and backwards through the records Press and hold or to scroll continuously through the readings The rate is slow enough to allow the operator to see trends in the data as it...

Страница 48: ...t of a PC 3 Ensure that the baud rate for the printer or PC and the smartCHEM Titro are the same If necessary alter the baud rate of the smartCHEM Titro see section 13 1 The smartCHEM Titro uses XON X...

Страница 49: ...alogging See section 12 2 for details Press while recalling data on the display see section 12 3 to send that record to the RS232 port 13 3 RS232 Configuration The smartCHEM Titro RS232 configuration...

Страница 50: ...trument serial number and number of logged readings in memory for example smartCHEM T V1 0 T1234 2340 cr where are spaces Note that the number of logged readings is right justified The is used interna...

Страница 51: ...following pH for pH readout mV for Absolute Millivolts readout mVR for Relative Millivolts readout TTTTT is Temperature data 5 characters right justified uuu is the Temperature unit description which...

Страница 52: ...mmand section 13 5 the computer must respond with a character after receiving each line For example smartCHEM T V1 0 T1234 31 12 2004 13 00 mV Offset 10 0mV 01 04 2004 12 00 pH Asy 0 10pH 01 04 2004 1...

Страница 53: ...ext Files prn txt csv 3 Navigate to the folder where your data file is stored and double click it to start the Text Import Wizard Note The default data folder for the WinTPS software is C My Documents...

Страница 54: ...ed into a single column to ensure that the X axis is correctly formatted if the data is to be charted later Press Next after all the column breaks have been inserted 6 Simply press Finish at step 3 of...

Страница 55: ...show the current date for example Date is now 31 12 04 Enter Date 31 31 04 dd mm yy 5 Use the Numeric Keypad to enter the current date then press Alternatively press menu to quit and retain the curren...

Страница 56: ...are sure that you wish to initialise ALL parameters or just the Slope B from a 3 point pH calibration The latter is only offered when a 3 point pH calibration has actually been performed Initialise F...

Страница 57: ...ry has been lost or corrupted Switch the meter OFF for 5 seconds and switch back ON If the problem persists return the unit to TPS for service Waiting for Burette Press Menu to exit The smartCHEM Titr...

Страница 58: ...rm place Replace standards or buffers Unstable readings 1 Reference Electrolyte chamber needs to be refilled 2 Reference junction blocked 3 pH glass bulb not clean 4 Bubble in pH glass bulb 5 Faulty c...

Страница 59: ...ensor for repair or replace sensor Displays flashing M when Temperature sensor plugged in 1 Faulty instrument socket 2 Faulty Temperature sensor Return the instrument to the TPS factory for service Re...

Страница 60: ...referred to as the reference junction A saturated solution of KCl is used to make contact with the sample It is vital that the KCl solution has an adequate flow rate in order to obtain stable accurat...

Страница 61: ...lly produce slightly less than this The output of a pH electrode is expressed as a percentage of an ideal electrode For example an ideal electrode that produces 59 16mV pH unit has 100 Slope An electr...

Страница 62: ...arisation output for Karl Fischer titrations This titration is a method for determining minute quantities of water in non aqueous liquids The TPS Double Platinum electrode part no 122237 has two conne...

Страница 63: ...ulty The following test can be performed to help determine if the smartCHEM Titro or the pH or Redox electrode is faulty 1 Initialise the smartCHEM Titro see section 15 2 Disconnect the pH or Redox el...

Страница 64: ...at this equipment is in need of repair please re read the manual Sometimes instruments are received for repair in perfect working order This can occur where batteries simply require replacement or re...

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