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Koehler K905 Series Operation And Instruction Manual

Koehler K905 Series Operation And Instruction Manual

Automatic potentiometic titrator

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K905XX
Automatic Potentiometic Titrator
Operation and Instruction Manual
Koehler Instrument Company, Inc.
1595 Sycamore Avenue • Bohemia, New York 11716-1796 • USA
Toll Free: 1-800-878-9070 (US only) • Tel: +1 631 589 3800 • Fax: +1 631 589 3815
http://www.koehlerinstrument.com • e-mail: info@koehlerinstrument.com
Petroleum Testing & Analysis Instrumentation • Custom Design & Manufacturing

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Summary of Contents for Koehler K905 Series

  • Page 1 K905XX Automatic Potentiometic Titrator Operation and Instruction Manual Koehler Instrument Company, Inc. 1595 Sycamore Avenue • Bohemia, New York 11716-1796 • USA Toll Free: 1-800-878-9070 (US only) • Tel: +1 631 589 3800 • Fax: +1 631 589 3815 http://www.koehlerinstrument.com • e-mail: info@koehlerinstrument.com...
  • Page 3 ASTM D4739 This unit is tested before it leaves the factory, to ensure total functionality and compliance to the above specifications and ASTM standards. Test and inspection records are on file for verification. Jesse Kelly Application Engineer Koehler Instrument Company...
  • Page 5 C O N T E N T S SECTION 1 Introduction Specifications Features SECTION 2 Familiarization with instrument Front Panel – Keyboard Layout and Functions SECTION 3 Instrument Operation - Switching ‘ON’ the instrument 1) Develop Method  Generating the Quick Method ...
  • Page 6 5) Display  Display Result  Display Statistics  Display Calibration Data 6) Reprocess 7) Run  Run Last Method  Run New Method  Run Last Quick Method SECTION 4 Result Calculation Entering Blank Volume/Primary Dose Entering Constant related to Sample Automatic determining and storing of molarity Maintenance and cleaning of burette Maintenance and cleaning of electrode...
  • Page 7 SECTION 1 • Introduction • Specifications • Features Pg. No. 3 of...
  • Page 8 K905XX- AUTOMATIC POTENTIOMETRIC TITRATOR INTRODUCTION An Automatic Titrator is a combination of electrochemical potential measurement through electrode with microprocessor driven burette, thus increasing the accuracy of measurement. The instrument is capable of performing almost all basic titrametric functions and cater to all types such as 1) Aqueous 2) Non-aqueous 3) Redox 4) Precipitation / Argentometric 5) Complexometric / EDTA 6) Voltametric 7) Back titration with simplicity.
  • Page 9 Environmental Operating Conditions : Operation : Indoor. Temperature : Ambient to 45 °C Operating Temperature and humidity : +5 to 45°C Max, 5 to 90% non condensing. Storage Temperature and humidity : +5 to 45°C Max, 5 to 90% non condensing. e) Altitude in meters : up to 2000m Power : 110V/220V AC ±10%, 60/50Hz.
  • Page 10 FEATURES: contd… • Result calculation facility to obtain printout in different units such as molarity, factor, % assay (wt), % volume (ml), ppm, mg/l, mg/g, ml/g, g/l, mEq/l, mol/kg, TAN & TBN. • Reprocessing of threshold and recalculation of EP without performing the new run. •...
  • Page 11 SECTION 2 • Familiarization with Instrument • Front Panel – Keyboard Layout and Functions Pg. No. 7 of...
  • Page 12 K905XX - Automatic Potentiometric Titrator Familiarization with the Instrument : - 1) Titration Controller : System Control unit for controlling the Titration Unit. 2) Titration Unit : Consists of Burette Assembly having Gas tight syringe with teflon tipped plunger with luer fitting. The miniature 3-way valve is used to control the titrant flow.
  • Page 13 FRONT PANEL KEYBOARD LAYOUT : Key functions: L.H.S. Keys: Alphanumeric Dual Function (A~Z, 1~9), Zero (0) with Dash (-), Dot (.), Slash (/), Decimal point ( . ) and Clear Entry( CE ) Key. R.H.S. Keys: Functional Keys and RESET key. Description of Functional Keys: : To reset the instrument or re-initialize before RUN.
  • Page 14 SECTION 3 • Instrument Operation • Titration Method Development • Function • Methods Pg. No. 10 of...
  • Page 15 OPERATION : • Switching ‘ON’ the instrument and connecting the accessories: a) Connect interface cable between Controller Unit & Titration Unit. b) Connect the DC Adapter power cord to 230V AC/50 Hz, 5A socket of stabilized power supply with proper earth connection & insert the DC jack in the Controller Unit socket. c) Connect pH Electrode on the back side of the instrument.
  • Page 16 1. Titration Method Development • Developing the Quick Method : Follow the below mentioned instructions MEAS. TYPE Potentiometric TITR. TYPE Acid-Base Aqueous 0 µl TITR. MODE Incremental P.D.VOLUME 100 µl STIR TIME 5 sec INITIAL DOSE 10000 µl INTERVAL 5 sec VOLUME LIMIT TITR.
  • Page 17 µ Initial Dose (5-2000 l) : 100 ENTER Interval (1-999 sec) : 5 ENTER µ Volume Limit (Max. : 99999 l) : - . / - . / µ Volume Limit (Max. : 99999 l) : 10000 ENTER - . / - .
  • Page 18 • Viewing & Running the Last Quick Method : Follow the below mentioned steps . Details of last quick method to be viewed & run : MEAS. TYPE : Potentiometric TYPE : Acid-Base Aqueous : 0 µl MODE : Incremental PREDISPENSE VOLUME PREDISPENSE DOSE : 1000 PREDISPENSE INTERVAL : 0...
  • Page 19 Conc. (0.00001-99.9999) : 0.100 ENTER - . / - . / 1)BlankVolume 2)PrimaryDose 3)None : ENTER Constant Code (1-8) : ENTER Const 1 (0.0001-999999.99) : Const 1 (0.0001-999999.99) : 63 ENTER Sample Vol. (0.0001 – 999.99999 ml): 1.0000 Vol. Reqd : 0.9425 ml R : 0.1924 MOLARITY(S) 1)Repeat Run 2)Reprocess 3)Print : a) To repeat the same quick method with same parameters, select ‘1’...
  • Page 20 Constant Code (1- 8) : ENTER Const 1 (0.00001-999999.99) : Const 1 (0.00001-999999.99) : 63 ENTER Sample Vol. (0.0001 – 999.99999 ml) : 1.0000 Vol. Reqd : 0.9425 ml R : 0.1924 MOLARITY(S) 1)Repeat Run 2)Reprocess 3)Print : • Viewing Last Quick Method : 1)Quick method 2)Full method : 1)Last Method 2)Edit Method : 1 3)Copy Method...
  • Page 21 ENTER No. of EP Cal. By : 1st Deriv. Threshold : 15 ENTER 1)Run 2)View : • Copying Last Quick Method : Follow the below mentioned instructions 1)Quick method 2)Full method : 1)Last Method 2)Edit Method : 1 ENTER 3)Copy Method Method No.
  • Page 22 • Developing the Full Method : Follow the below mentioned steps Examples: TITRATION BY INCREMENTAL METHOD METHOD NO. SAMPLE NAME TITRANT NAME : NAOH MEAS. TYPE Potentiometric TITR. TYPE : Acid-Base Aqueous TITR. MODE Incremental P.D.CRITERIA : 0 mV 500 µl : 100 µl P.D.VOLUME P.D.DOSE...
  • Page 23 < Predispense Criteria (0-1000 mV) : 0 ENTER - . / µ Predispense Volume (0-95000 l) : 0 - . / - . / µ Predispense Volume (0-95000 l) : 500 ENTER Predispense Dose (5-1000) : - . / - . / Predispense Dose (5-1000) : 100 ENTER Predispense Interval (0-999 sec) : 0...
  • Page 24 Conc. (0.00001-99.99999 M1) : - . / Conc. (0.00001-99.99999) : 0.100 ENTER - . / - . / 1)BlankVolume 2)PrimaryDose 3)None : ENTER Constant Code (1-20) : ENTER Const 1 (0.00001-999999.9) : Const 1 (0.00001-999999.9) : 1 ENTER Print Report 1)Full 2)Select 3)Condensed ENTER 4)None : 4 Method No.
  • Page 25 • TITRATION BY EQUILIBRIUM METHOD: METHOD NO. SAMPLE NAME TITRANT NAME : NAOH MEAS. TYPE Potentiometric TITR. TYPE : Acid-Base Aqueous TITR. MODE Equilibrium P.D.CRITERIA : 0 mV 500 µl : 100 µl P.D.VOLUME P.D.DOSE P.D.INTERVAL 5 sec STIR TIME : 5 sec 100 µl INITIAL DOSE...
  • Page 26 µ Predispense Volume (0-95000 l) : 0 - . / - . / µ Predispense Volume (0-95000 l) : 500 ENTER Predispense Dose (5-1000) : - . / - . / Predispense Dose (5-1000) : 100 ENTER Predispense Interval (0-999 sec) : 0 ENTER Stir Time (0-999 sec) : 5 ENTER...
  • Page 27 Conc. (0.00001-99.99999) : - . / Conc. (0.00001-99.99999) : 0.100 ENTER - . / - . / 1)BlankVolume 2)PrimaryDose 3)None : ENTER Constant Code (1-20) : ENTER Const 1 (0.0001-999999.99) : Constant (0.0001-999999.99) : 1 ENTER Print Report 1)Full 2)Select 3)Condensed ENTER 4)None : 4 Titration Report 1)Y 2)N : 1...
  • Page 28 • TITRATION BY pH CUTOFF ( END) VALUE.:- METHOD NO. SAMPLE NAME : HCl TITRANT NAME NAOH MEAS. TYPE : Potentiometric TITR. TYPE Acid-Base Aqueous TITR. MODE : Cutoff pH P.D.CRITERIA 0 mV : 500 µl 100 µl P.D.VOLUME P.D.DOSE P.D.INTERVAL : 5 sec STIR TIME...
  • Page 29 µ Predispense Volume (0-95000 l) : 0 - . / - . / µ Predispense Volume (0-95000 l) : 500 ENTER Predispense Dose (5-1000) : - . / - . / Predispense Dose (5-1000) : 100 ENTER Predispense Interval (0-999 sec) : 0 ENTER Stir Time (0-999 sec) : 5 ENTER...
  • Page 30 Derivative Threshold (1-32000) : - . / - . / Derivative Threshold (1-32000) : 500 ENTER Conc. (0.00001-99.99999) : - . / Conc. (0.00001-99.99999) : 0.100 ENTER - . / - . / 1)BlankVolume 2)PrimaryDose 3)None : ENTER Constant Code (1-20) : ENTER Const 1 (0.0001-999999.99) : Const 1 (0.0001-999999.99) : 1...
  • Page 31 • TITRATION BY PH STAT METHOD: FOR ENZYME KINETIC STUDY. e.g. say pH to be maintained is 8 pH.±0.02pH METHOD NO. SAMPLE NAME ENZYME TITRANT NAME NAOH MEAS. TYPE Potentiometric TITR. TYPE Acid-Base Aqueous TITR. MODE pH stat P.D.CRITERIA 0 mV 0 µl P.D.VOLUME STIR TIME...
  • Page 32 µ Predispense Volume (0-95000 l) : 0 ENTER Stir Time (0-999 sec) : 5 ENTER µ Initial Dose (5-2000 l) : 100 - . / - . / µ Initial Dose (5-2000 l) : 100 ENTER Stat Interval (1-99 sec) : 5 ENTER µ...
  • Page 33 µ Minimum Control Dose (5-500 l) : 10 ENTER Derivative Threshold (1-32000) : - . / - . / Derivative Threshold (1-32000) : 200 ENTER Conc. (0.00001-99.99999) : - . / Conc. (0.00001-99.99999) : 0.100 ENTER - . / - . / 1)BlankVolume 2)PrimaryDose 3)None : ENTER Constant Code (1-20) :...
  • Page 34 • TITRATION BY MULTIPLE END POINT METHOD: METHOD NO. SAMPLE NAME : HALIDES TITRANT NAME AgNO MEAS. TYPE : Potentiometric TITR. TYPE Precipitation TITR. MODE : Incrimental P.D.CRITERIA 0 mV : 0 µl P.D.VOLUME STIR TIME 5 sec : 100 µl INITIAL DOSE INTERVAL 5 sec...
  • Page 35 Predispense Criteria (0-1000 mV) : 0 ENTER - . / µ Predispense Volume (0-95000 l) : 0 ENTER - . / Stir Time (0-999 sec) : ENTER µ Initial Dose (5-2000 l) : - . / - . / µ Initial Dose (5-2000 l) : 100 ENTER...
  • Page 36 Constant Code (1-20) : ENTER Const 1 (0.0001-999999.9) : Say – 16.9, Press keys 1,6, dot & 9 Const 1 (0.0001-999999.9) : 16.9 ENTER Const 2 (0.0001-999999.9) : Say – 11.9, Press keys 1,1, dot & 9 Const 2 (0.0001-999999.9) : 11.9 ENTER Const 3 (0.0001-999999.9) : Say –...
  • Page 37 TITRATION METHOD FOR BLANK & BACK TITRATION:- Back-titrations may be used in volumetric analysis where direct titrations cannot be used for technical reasons such as Sample solubility, Trace of impurities, and slow reaction. For example, when a compound is not soluble in water, or where it contains impurities, which interfere with direct titration, an excess of the titrant may be added, and the excess then determined by titration (i.e.
  • Page 38 Select titration mode ENTER 1)Incr. 2)Equil. 3)Cutoff(pH) 4)pHstat: 2 Predispense Criteria (0-1000 mV) : 0 ENTER - . / µ Predispense Volume (0-95000 l) : 0 Enter 1,8,0,0,0 and ENTER µ Predispense Volume (0-95000 l) : 18000 ENTER Predispense Dose (5-1000) : - .
  • Page 39 Calculation by ENTER 2)Largest 3)Last 4)All 5)Select : 1 µ Minimum Control Dose (5-500 l) : - . / µ Minimum Control Dose (5-500 l) : 10 ENTER Derivative Threshold (1-32000) : - . / - . / Derivative Threshold (1-32000) : 300 ENTER Conc.
  • Page 40 • METHOD FOR BACK TITRATION:- METHOD NO. 7 (BACK Titration) SAMPLE NAME Sample + NaOH TITRANT NAME MEAS. TYPE Potentiometric TITR. TYPE Back TITR. MODE Equllibrium P.D.CRITERIA 0 mV 500 µl P.D.VOLUME 10000 P.D.DOSE P.D.INTERVAL 5 sec STIR TIME 30 sec 200 µl INITIAL DOSE EQ.
  • Page 41 µ Predispense Volume (0-95000 l) : 0 Enter 10000 and ENTER µ Predispense Volume (0-95000 l) : 10000 ENTER Predispense Dose (5-1000) : - . / - . / Predispense Dose (5-1000) : 500 ENTER Predispense Interval (0-999 sec) : 0 ENTER Stir Time (0-999 sec) : - .
  • Page 42 µ Minimum Control Dose (5-500 l) : 10 ENTER Derivative Threshold (1-32000) : - . / - . / Derivative Threshold (1-32000) : 300 ENTER Conc. (0.00001-99.99999) : - . / Conc. (0.0001-99.99999) : 0.100 ENTER - . / - . / 1)BlankVolume 2)PrimaryDose 3)None : ENTER Blank Volume (0.0001-99.9999ml) :...
  • Page 43 Entering Method for TAN & TBN ( ASTM D664, ASTM D2896 & ASTM D4739) Note : Select following Titration methods numbers for TAN & TBN • Method No. 39 for ASTM D2896, which is indicated on printout. • Method No. 38 & 40 are respectively for ASTM D664 and D4739 for which buffer values should be entered as following, the same is indicated on printout.
  • Page 44 • Viewing the Titration Methods : All the 50 methods can be scanned for checking or modifying the parameters individually. Say Method No.1 has to be viewed before performing analysis. 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)Quick method 2)Full method : 1)Add/Edit method 2) Copy method ENTER...
  • Page 45 Print Report : None ENTER 1)Add/Edit method 2) Copy method 3) Skip method 4) View : NOTE : 50 titration methods can be scanned independently. If the method scanned is not present or earlier entered, display shows : Method does not exist !! Pg.
  • Page 46 • Copying the Titration Method : Say Method No.1 has to be copied from Method No. 41. Follow the below mentioned instructions 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)Quick method 2)Full method : 1)Add/Edit method 2) Copy method 3) Skip method 4) View : Copy to Method No.
  • Page 47 • Skipping the Titration Method : Say Method No.1 has to be skipped so memory can be made free to add new method. a) To skip individual method : 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)Quick method 2)Full method : 1)Add/Edit method 2) Copy method 3) Skip method 4) View :...
  • Page 48 FUNCTION PARAMETERS 1) pH Calibration :- for pH measurement or pH titrations. Standardization is done at 7 pH and Calibration can be done for acid and base buffer. Calibration can be performed for 3 point with 2 buffer (one on acidic side and other on basic side).
  • Page 49 Enter if stable mV (std) ENTER mV = +177.0 T : 25.0° Remove the pH electrode from 4 pH buffer and rinse it thoroughly with distilled water. Sock dry the electrode with tissue paper to remove the excess DI water and put the electrode in Base buffer (say 9 pH).
  • Page 50 2) Using instrument as pH / mV indicator ( mV scan ) For pH measurement ensure that the instrument is properly calibrated before measurement. Place the beaker containing sample whose pH is to be measured. Insert the clean and dried electrode such that it gets immersed in the sample. Now start the stirrer and proceed as following 1)Develop Method 2) Function 3)Config.
  • Page 51 4) Replacing the burette assembly 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)pH Calibration 2)mV scan 3)Prime 4)Burette Change 5)Manual Titra : Do you wish to change the ENTER Burette Assembly 1)Y 2)N Wait … To remove the Burette Assembly After removing the Screw Now remove the screw Screw has been removed...
  • Page 52 5) Performing Manual Titration 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)pH Calibration 2)mV scan 3)Prime 4)Burette Change 5)Manual Titra: Titration Dose (5-10000 ul) : - . / - . / Titration Dose (5-10000 ul) : 100 ENTER After refilling burette Wait ..
  • Page 53 CONFIG PARAMETERS 1) Setting RTC (Clock) 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)Clock/Date 2)Balance 3)Temp. 4)Printer 5)PW 6)Data Xfer 7) Resol. 8) Tit. Temp. Fct. Set Clock and Date 1)Y 2)N : Min : Hour : Day : Month : Year ENTER : 17 : 12...
  • Page 54 a) For Manual Temperature compensation Temp. Compensation 1)Manual 2)Auto : ENTER Enter the sample temperature after measuring it with external thermometer (25) Temp.compensation 1)Manual 2)Auto ENTER Temperature (20-120) : 25 Screen returns to main menu. b) For Automatic Temperature compensation Temp.
  • Page 55 Admin Password saved To enter User Password 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)Clock/Date 2)Balance 3)Temp. 4)Printer 5)PW 6)Data Xfer 7) Resol. 8) Tit. Temp. Fct. 1)Admin P/W 2)User P/W : To change User P/W Enter Admin Password : After entering Admin Password Set User Password :...
  • Page 56 7) Resolution selection 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1)Clock/Date 2)Balance 3)Temp. 4)Printer 5)PW 6)Data Xfer 7) Resol. 8) Tit. Temp. Fct. Result Resolution : 1)1 2)2 3)3 4)4 Enter the required result resolution, Say 4 1)Develop Method 2) Function 3)Config.
  • Page 57 PRINT 1) Printing Report After the titration is over, the result is stored in non-volatile memory, which can be printed for report generation. The Hardcopy of titration can be taken for : i) Result ii) Data iii) Graph (mV v/s µl or 1st derivative of mV v/s µl ) iv) Condensed Report Care has been taken for printing in DRAFT mode.
  • Page 58 • Printing Data Table 1)Develop Method 2) Function 3)Config. ENTER 4)Print 5) Display 6) Reprocess 7)Run 1)Result 2)Data 3)Condensed 4) Statistics 5) Cal. Repo 6) Method 7) Graph Titration Data Table is printed and screen returns to main menu. • Printing the Titration Analysis Condensed Report Follow the below mentioned instructions :...
  • Page 59 • Printing Method Parameters Follow below mentioned instructions 1)Develop Method 2) Function 3)Config. ENTER 4)Print 5) Display 6) Reprocess 7)Run 1)Result 2)Data 3)Condensed 4) Statistics ENTER 5) Cal. Repo 6) Method 7) Graph Parameter Report is printed along with empty methods & screen returns to main menu. 1)Individual 2)All To print single Prog.
  • Page 60 DISPLAY 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run 1) Displaying Titration Result Follow below mentioned instructions 1) Result 2) Statistics 3) Cal. Data Vol. Reqd : 0.9425 ml After 4-5 sec screen Result : 0.1924 Molarity (T) Result - 1)Print 2)Reprocess 3)Display 4)Display Stat.
  • Page 61 REPROCESSING THE RESULT FOR DIFFERENT RESULT UNITS : Derivative Threshold (1-32000) : - . / Derivative Threshold (1-32000) : 20 ENTER Calculation by ENTER 2)Largest 3)Last 4)All 5)Select : 1 Conc. (0.00001-99.99999) : - . / Conc. (0.00001-99.99999) : 0.100 ENTER - .
  • Page 62 RUNNING METHOD : Follow below mentioned instructions : 1)Develop Method 2) Function 3)Config. 4)Print 5) Display 6) Reprocess 7)Run a) Run last method 1)Last Method 2)New Method : If last method is quick method, Press ENTER to acknowledge : Run Quick Method ENTER If last method is full method, Press ENTER to acknowledge : Run Method 1...
  • Page 63 Method No. 1 Wait ..starts with the 00 : 00 : 18 mentioned para. Disp.Vol. : XXX ul # RN BV 10 TITRA 25.0° mV : 00 : 00 : The instrument displays volume and corresponding mV after every dosing. After detecting the Titration end criteria, the exact volume required for endpoint and result is displayed : Wait ..
  • Page 64 Method No. 2 Wait ..00 : 00 : 24 starts with the mentioned para. Disp.Vol. : XXX ul # RN BV 10 TITRA 25.0° mV : 00 : 00 : 38 The instrument displays volume and corresponding mV after every dosing. After detecting the Titration end criteria, the exact volume required for endpoint and result is displayed : Vol.
  • Page 65 Vol. Reqd : 0.9425 ml 1)Repeat Run 2)Result 3)Print : a) To repeat the same quick method with same parameters, select ‘1’ option. b) To print the data table report for quick method, select ‘3’ option. c) To get result for the quick method enter sample analysis parameters as following by selecting ‘2’...
  • Page 66 SECTION 4 • Result Calculation • Entering Blank Volume / Primary Dose • Entering Constant Related to Sample • Automatic Determining and Storing of Molarity • Maintenance and Cleaning of Burette • Maintenance and Cleaning of Electrode • Appendix A — K Pg.
  • Page 67 • Result Calculation a) Direct Titration :- The result is calculated according to the following formula : Result = M1 * EP1 * C1 / S1 where, = Titrant consumption up to the equivalence point in ml. = Concentration of titrant in mol./lit . = Calculation constant to convert the raw result into the desired unit.
  • Page 68 • Entering Blank Volume / Primary Dose a) Blank Volume : Blank Volume is the titrant volume required for neutralizing the known amount of solvent/distilled water taken for dissolving the sample. In certain titrations a small part of titrant is consumed by the solvent before actual sample endpoint is obtained.
  • Page 69 • Entering CONSTANT related to Sample Enter Constant value by selecting appropriate code no [refer Appendix-B(Pg.75), J(Pg.86)] for automatic calculation of results in units (%, factor, molarity, ppm etc). Code no 1 - 7 : are reserved and used for Liquid samples. Sample taken by volume (ml).
  • Page 70 CONSTANT CODES Suitable selection of constant code no. allows printout of the associated unit with result. 1) Constants (1-8) for sample taken by Volume (ml.) CODE NO. UNITS FORMULA MOLARITY(S) Z1 / Z2 % VOL. (M*Z1) / ( Z2*10 *δ ) MG / L ( M*1000 *Z1) / Z2 ( M*1000 *Z1) / ( Z2*δ...
  • Page 71 • Determination of Molarity: Standardizing 0.1 M Sodium Hydroxide (NaOH) by Potassium Hydrogen Pthalate (KHP). Enter Constant related to Standard taken volumetrically in Code 7 or enter in Code 12 if Standard is taken by weight (Refer Page 71) Constant Value = (M • Z1 ) / (1000 • Z2 ) = (204.22 • 1)/(1000• 1) = 0.2042 in Code 12.
  • Page 72 MAINTENANCE AND CLEANING OF ELECTRODES The glass electrode should be cleaned occasionally in moderately concentrated acid and kept in suitable buffer when not in use. See also the maintenance instructions packed with the electrode as set forth by the makers. The following procedure should be adopted for cleaning the glass electrode: 1) Rinse the electrode in pure water by changing water for more than 3-4 times, and wipe off water with clear filter paper or absorbent cotton.
  • Page 73 APPENDIX A ALPHANUMERIC ENTRY Alphanumeric entries are done to enter a Sample name, Titrant name (ENTER key) and Identification no. (RUN mode). Maximum 20 alphanumeric characters can be entered for any alphanumeric entry. e.g. To enter Sample Name : say 2 HEXANE. Please follow sequence of operations SAMPLE NAME : NOTE: Press(2) means press the button twice.
  • Page 74 APPENDIX B ERROR CODES # If the number of doses exceeds 200, ERROR 1 during any titration run, titration run is aborted, error message is displayed and ‘Run aborted’ is printed on report. # If the titration run volume exceeds 99.99 ERROR 1 ml, during any titration run,...
  • Page 75 APPENDIX B ERROR CODES (Contd.) # If the electrode’s offset or buffer values Incorrect Buffer or Faulty Electrode are not within specified range, error message is displayed. # If the method parameters are not suitable Check Method Parameter for running the method by changing burette, error message is displayed.
  • Page 76 APPENDIX C PRINTER DIP SWITCH SETTINGS The printer has twelve DIP switches grouped in two groups, mounted on the back panel. DIP switch 1-1 is the switch at the far left side, and the one at the far right is DIP switch 2-4. The following table summarizes the settings of switches for WIPRO LX - 800 printer.
  • Page 77 APPENDIX D PARAMETER SELECTION TABLE PARAMETER DESCRIPTION DEFAULT LIMITS Incremental Mode PREDISPENSE Maximum 95000 µl. Initial Predispense Volume VOLUME PREDISPENSE Dosing size after each pre- Factor of PDV & In steps of DOSE dispense interval 1/1000th of burette. PREDISPENSE Time between two doses 0 to 999 sec in step of 1 sec INTERVAL during predispense...
  • Page 78 APPENDIX D PARAMETER SELECTION TABLE (Contd..) PARAMETER DESCRIPTION DEFAULT LIMITS Cutoff pH Mode PREDISPENSE Maximum 95000 µl. Initial Predispense Volume VOLUME PREDISPENSE Dosing size after each pre- Factor of PDV & In steps of DOSE dispense interval 1/1000th of burette. PREDISPENSEI Time between two doses 0 to 999 sec in step of 1 sec...
  • Page 79 APPENDIX E TITRATION TYPE TYPE 1 : ACID-BASE In acid-base titration, an acid is determined by titration with a base, or − vice-versa. The essential reaction is between H and OH , giving water. The pH at the end-point depends on the dissociation constants of the reactants and products. It includes strong acid - strong base (e.g.
  • Page 80 APPENDIX F TITRATION MODES MODE 1 : INCREMENTAL In this mode of titration fixed dose can be given at fixed interval of time up to the number of selected end point. This is used for determining sequential endpoints in multi-component sample. The titration is performable up to maximum 9 endpoints evaluation.
  • Page 81 APPENDIX G METHOD PARAMETERS a) INITIAL DOSE (µL) : This is dispense volume of titrant in µl. This volume gets added periodically during sample run. Dose selection should be such that significant change of mV value occurs after addition of every dose. Minimum dose that can be set is 5 µl. 1/5th of the burette volume is the maximum dose that can be entered in all modes of titration.
  • Page 82 APPENDIX H SAMPLE ANALYSIS PARAMETERS a) PRE-DISPENSE CRITERION (mV) : This is the mV value difference after which predispense will automatically stop and programmed doses will be given (0-1000). The value ‘0’ allows the use of Pre dispense Volume function in which programmed doses are given at fixed minimum time of the system.
  • Page 83 APPENDIX H SAMPLE ANALYSIS PARAMETERS (contd.) i) STAT RUN TIME (sec) : This is the time for which pH-Stat titration should be continued after attaining set pH value. Run time can be entered for the range of 1-9999 sec. j) VTIME 1 (sec) : This is the time at which one wants to calculate the volume consumed during pH stat titrations.
  • Page 84 APPENDIX I CALCULATION PARAMETERS a) CONCENTRATION : This is the molarity of titrant to be considered for result calculation. For standardization of titrant, before run the value entered is 1 and then evaluated value gets transferred in respective code. Concentration value ranges from 0.0001-99.9999 mol/lit.
  • Page 85 APPENDIX J Standard Methods (41-50) : Method 41 : Standardizing 0.1 M NaOH against KHP METHOD NO : 41 TITRANT CONC : 0.1 M (appx.) SAMPLE NAME : KHP TITRANT NAME : NAOH MEASURE. TYPE : Potentiometric SAMPLE WEIGHT : 100 mg (apx) TITRATION TYPE : Acid-Base Aq.
  • Page 86 APPENDIX J Standard Methods (41-50) contd ... : Method 43 : Standardizing 0.1 M Alc. KOH against KHP METHOD NO : 43 TITRANT CONC : 0.1 M (appx.) SAMPLE NAME : KHP TITRANT NAME : Alc. KOH MEASURE. TYPE : Potentiometric SAMPLE WEIGHT : 100 mg (apx) TITRATION TYPE...
  • Page 87 APPENDIX J Standard Methods (41-50) contd ..: Method 45 : Standardizing 0.1 M NaNO2 against Sulphanilic Acid METHOD NO : 45 TITRANT CONC : 0.1 M (appx.) SAMPLE NAME : SULPHANILIC ACID TITRANT NAME : NANO2 MEASURE. TYPE : Potentiometric SAMPLE WEIGHT : 100 mg (apx) TITRATION TYPE...
  • Page 88 APPENDIX J Standard Methods (41-50) contd ... : Method 47 : Standardizing 0.1 M Na2S2O3 against KIO3 METHOD NO : 47 TITRANT CONC : 0.1 M (appx.) SAMPLE NAME : KIO3 TITRANT NAME : NA2S2O3 MEASURE. TYPE : Potentiometric SAMPLE WEIGHT : 25-30 mg (ap) TITRATION TYPE : Redox...
  • Page 89 APPENDIX J Standard Methods (41-50) contd ..: Method 49 : Standardizing 0.1 M AgNO3 against NaCl METHOD NO : 49 TITRANT CONC : 0.1 M (appx.) SAMPLE NAME : NACL TITRANT NAME : AGNO3 MEASURE. TYPE : Potentiometric SAMPLE WEIGHT : 40 mg (apx) TITRATION TYPE : Precipitation...
  • Page 90 APPENDIX K K905XX – Data Downloading Capability to Personal Computer Installation/setup Instructions: The instrument software has been incorporated with RS232C protocol interface for transferring the printable data to PC having standard data terminal software Windows - Hyper terminal. Features of PC data transfer, 1.
  • Page 91 If the COM port chosen is not free or being used by another application a pop up screen will be displayed with message “Unable to Open COM”. When a free Com port is selected The COM port Properties Pop up will be displayed on the screen.
  • Page 92 Now From the terminal window FILE menu select the Properties tool to set the Terminal Emulation mode and Data Line Once You click on the Properties menu - Properties window will appear. Select Settings option to set the Emulation mode and function setting. Function:- Arrow &...
  • Page 93 Click the ASCII setup icon to enter the setting window. Click the Boxes as shown in the graphics for  Line end with line feed,  Echo typed characters,  Append line feed to incoming line ends,  wrap lines that exceed terminal width, ...