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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: [email protected]

Petroleum Testing & Analysis Instrumentation • Custom Design & Manufacturing

K905XX

Automatic Potentiometic Titrator

Содержание K905 Series

Страница 1: ...ue 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 In...

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Страница 3: ...ce with the applicable standards set forth in this certification Specifications ASTM D664 ASTM D2896 ASTM D3227 ASTM D4739 This unit is tested before it leaves the factory to ensure total functionalit...

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Страница 5: ...ing Full Method 41 2 Function Standardization Calibration 45 mV indicator Priming 47 Priming 47 Burette Replacement 48 Manual Titration 49 3 Configuration Setting RTC Clocl 50 Balance Connectivity 50...

Страница 6: ...ance and cleaning of burette 68 Maintenance and cleaning of electrode 69 Appendix A Alphanumeric entry 70 Appendix B Error Codes 71 Appendix C Printer DIP switch setting 73 Appendix D Parameter select...

Страница 7: ...Pg No 3 of 89 SECTION 1 Introduction Specifications Features...

Страница 8: ...ults Molarity Assay wt volume ml ppm mg l mg g g l meq l mol kg TAN and TBN for oil samples Sensors 1 Electrodes for Potentiometric titration pH Ion Redox Precipitation a Any combination electrode wit...

Страница 9: ...OPY and for Calibration Three modes of titration incremental equilibrium and cut off by pH mode to perform almost all types of titration By selecting titration method instrument prints the type of app...

Страница 10: ...N having only titration parameter Error indication on Display helps user to trace the problem Titration run can be started with last run parameters Display of last run or default parameters while ente...

Страница 11: ...Pg No 7 of 89 SECTION 2 Familiarization with Instrument Front Panel Keyboard Layout and Functions...

Страница 12: ...tubing is for dispensing the titrant in reaction vessel 3 Stirrer Assembly Consists of Vortex stirrer with glass propeller with digital controller for variable speed regulation 4 Printer Output 25 Pin...

Страница 13: ...t or re initialize before RUN 2 To go back to previous entry 3 To Return to Main menu from any operation and to abort the titration during run 4 a To acknowledge functions b To enter titration paramet...

Страница 14: ...Pg No 10 of 89 SECTION 3 Instrument Operation Titration Method Development Function Methods...

Страница 15: ...with Display Display Display MAIN MENU 1 Develop Method To generate add Edit View Titration Method parameter Delete Copy Method Refer pages 13 2 Function To perform pH Calibration mV scan Burette Prim...

Страница 16: ...hod 2 Function 3 Config 7 4 Print 5 Display 6 Reprocess 7 Run 1 Quick method 2 Full method 1 Last Method 2 Edit Method 1 3 Copy Method Titration Type 1 Aq 2 Non Aq 3 Redox 4 Pr 5 EDTA 6 Back 7 Photo 8...

Страница 17: ...BC 5 MNO 0 0 0 0 0 Initial Dose 5 2000 l 100 Volume Limit Max 99999 l 10000 ENTER Interval 1 999 sec 5 5 MNO ENTER ENTER Titration End Criteria 1 EndPoint EP 2 VolumeLimit VL 1 Number of EP 1 9 1 ABC...

Страница 18: ...th 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 o...

Страница 19: ...onst 1 0 0001 999999 99 Conc 0 00001 99 9999 Derivative Threshold 1 32000 6 PQR 0 2 DEF 3 GHI 1 ABC 0 0 0 0 0 Conc 0 00001 99 9999 0 100 Conc 0 00001 99 9999 0 100 ENTER ENTER 1 BlankVolume 2 PrimaryD...

Страница 20: ...de Incremental Initial Dose l 100 Interval sec 3 Measurement Type Potentiometric Predispense Volume l 100 Predispense Dose l 50 Predispense Interval sec 0 Stir Time sec 0 VolLimit l 10000 Titr End Cri...

Страница 21: ...5 seconds 1 Run 2 View 1 Quick method 2 Full method 1 Last Method 2 Edit Method 1 3 Copy Method Method No 1 40 1 Last Method 2 Edit Method 1 3 Copy Method ENTER ENTER 1 ABC 3 GHI 1 ABC No of EP 1 Cal...

Страница 22: ...CONSTANT 1 PRINT REPORT None Enter ADMIN or USER Password ref Page 51 If method is already present Display reads Enter Sample and Titrant Name refer Appendix A for alphanumeric entries 1 Develop Meth...

Страница 23: ...2000 l 100 Volume Limit Max 99999 l 10000 Predispense Volume 0 95000 l 500 Predispense Dose 5 1000 100 ENTER ENTER ENTER Interval 1 999 sec 5 5 MNO ENTER Predispense Criteria 0 1000 mV 0 Predispense...

Страница 24: ...1 ABC 1 BlankVolume 2 PrimaryDose 3 None Print Report 1 Full 2 Select 3 Condensed 4 None 4 3 GHI 4 JKL ENTER ENTER Constant Code 1 20 Const 1 0 00001 999999 9 1 Method No 1 Stored 1 ABC ENTER ENTER C...

Страница 25: ...APH 2 No Time l GRAPH 2 No 2nd DERIV GRAPH 2 No Enter ADMIN or USER Password ref Page 51 Enter Sample and Titrant Name refer Appendix A for alphanumeric entries 1 Develop Method 2 Function 3 Config 4...

Страница 26: ...lume Limit Max 99999 l 10000 Predispense Volume 0 95000 l 500 Predispense Dose 5 1000 100 ENTER ENTER Interval 1 999 sec 1 Predispense Interval 0 999 sec 0 5 MNO ENTER ENTER Titration End Criteria 1 E...

Страница 27: ...ensed 4 None 4 Titration Report 1 Y 2 N 1 Titration Data Table 1 Y 2 N 2 Titration mV l Graph 1 Y 2 N 1 Titration Derivative Graph 1 Y 2 N 2 Titration Time l Graph 1 Y 2 N 2 Titration 2nd Deriv Graph...

Страница 28: ...DERIV GRAPH 2 No Time l GRAPH 2 No 2nd DERIV GRAPH 2 No Enter ADMIN or USER Password ref Page 51 Enter Sample and Titrant Name refer Appendix A for alphanumeric entries Method No 1 40 Measurement Typ...

Страница 29: ...0 0 0 0 0 0 0 0 Initial Dose 5 2000 l 100 Volume Limit Max 99999 l 10000 Control Limit 0 14 pH 4 00 End Limit 0 14 pH 9 00 Predispense Volume 0 95000 l 500 Predispense Dose 5 1000 100 ENTER ENTER ENT...

Страница 30: ...1 Full 2 Select 3 Condensed 4 None 4 Titration Report 1 Y 2 N 1 Titration Data Table 1 Y 2 N 2 Titration mV ul Graph 1 Y 2 N 1 Titration Derivative Graph 1 Y 2 N 2 Titration Time ul Graph 1 Y 2 N 2 Ti...

Страница 31: ...1 PRINT REPORT Full Note To understand the meaning of each parameter please refer Appendix F H Enter ADMIN or USER Password ref Page 51 Enter Sample and Titrant Name refer Appendix A for alphanumeric...

Страница 32: ...EF 0 0 0 Initial Dose 5 2000 l 100 Volume Limit Max 99999 l 10000 Control Limit 0 14 pH 8 00 End Limit 0 14 pH 8 02 Predispense Volume 0 95000 l 0 ENTER ENTER Stat Interval 1 99 sec 5 5 MNO ENTER ENTE...

Страница 33: ...tive Threshold 1 32000 0 1 ABC 0 0 0 Conc 0 00001 99 99999 0 100 ENTER 1 BlankVolume 2 PrimaryDose 3 None Print Report 1 Full 2 Select 3 Condensed 4 None 4 3 GHI 4 JKL ENTER ENTER Constant Code 1 20 M...

Страница 34: ...Enter ADMIN or USER Password ref Page 51 If method is already present Display reads Enter Sample and Titrant Name refer Appendix A for alphanumeric entries 1 Develop Method 2 Function 3 Config 4 Print...

Страница 35: ...al 1 999 sec 5 MNO ENTER Predispense Criteria 0 1000 mV 0 0 ENTER ENTER 1 BlankVolume 2 PrimaryDose 3 None Titration End Criteria 1 EndPoint EP 2 VolumeLimit VL 1 Number of EP 1 9 Stir Time 0 999 sec...

Страница 36: ...r 4 5 seconds 1 Run 2 View Const 1 0 0001 999999 9 Print Report 1 Full 2 Select 3 Condensed 4 None 4 4 JKL ENTER Constant Code 1 20 Const 1 0 0001 999999 9 16 9 Method No 5 Stored ENTER ENTER Const 2...

Страница 37: ...stimate Blank Volume SAMPLE NAME NaOH TITRANT NAME HCl MEAS TYPE Potentiometric TITR TYPE Acid Base Aqueous TITR MODE Equllibrium P D CRITERIA 0 mV P D VOLUME 18000 l P D DOSE 500 l P D INTERVAL 5 sec...

Страница 38: ...0 0 2 DEF 0 0 Initial Dose 5 2000 l 200 Volume Limit Max 99999 l 22000 Predispense Volume 0 95000 l 18000 Predispense Dose 5 1000 500 ENTER ENTER ENTER Predispense Criteria 0 1000 mV 0 Predispense In...

Страница 39: ...erivative Threshold 1 32000 3 GHI 0 1 BlankVolume 2 PrimaryDose 3 None Print Report 1 Full 2 Select 3 Condensed 4 None 4 3 GHI 4 JKL ENTER ENTER Constant Code 1 20 Method No 6 Stored 8 VWX ENTER ENTER...

Страница 40: ...R Password ref Page 51 If method is already present Display reads Enter Sample and Titrant Name refer Appendix A for alphanumeric entries 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6 Repro...

Страница 41: ...Max 99999 l 22000 Predispense Volume 0 95000 l 10000 Predispense Dose 5 1000 500 ENTER ENTER ENTER Predispense Interval 0 999 sec 0 5 MNO ENTER ENTER Titration End Criteria 1 EndPoint EP 2 VolumeLimi...

Страница 42: ...1 Run 2 View Derivative Threshold 1 32000 300 Derivative Threshold 1 32000 3 GHI 0 1 BlankVolume 2 PrimaryDose 3 None Print Report 1 Full 2 Select 3 Condensed 4 None 4 1 ABC 4 JKL ENTER ENTER Constant...

Страница 43: ...N 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 pr...

Страница 44: ...ial Dose l 100 Concentration 0 10000 Measurement Type Potentiometric Predispense Criteria mV 0 Predispense Volume l 500 Interval sec 5 VolLimit l 10000 Titr End Crit EndPoint No of EP 1 Cal By 1st Der...

Страница 45: ...50 titration methods can be scanned independently If the method scanned is not present or earlier entered display shows Print Report None ENTER Method does not exist 1 Add Edit method 2 Copy method 3...

Страница 46: ...5 seconds 1 Quick method 2 Full method Copy to Method No Copy from Method No Method No 1 copied from Method No 41 ENTER ENTER 1 ABC 2 DEF 2 DEF 1 ABC 4 JKL 1 ABC 1 Develop Method 2 Function 3 Config...

Страница 47: ...1 50 Method No 1 Skipped 1 Quick method 2 Full method 1 Individual 2 All Method No 1 40 Skipped ENTER ENTER ENTER ENTER ENTER 1 ABC 2 DEF 3 GHI 1 ABC 1 ABC 1 ABC 2 DEF 3 GHI 2 DEF 1 Add Edit method 2...

Страница 48: ...splay reads After 4 5 seconds Note 1 The offset shown here is now memorized for future measurements analysis 2 If the offset is out of the range more than 30 mV the display shows Check the buffer or c...

Страница 49: ...limit provided in the instrument is 80 to 120 c Resetting the Calibration data to Default Values If instrument calibration done by buffers is not required and needs to be resetted press 2 the system...

Страница 50: ...ctors Initially PRIME function can be repeated 2 to 3 times to clean system The PRIME is also used for adding fixed volume as per program parameter Primary Dose P Dose is added After 4 5 seconds Primi...

Страница 51: ...etection and returns to Main Menu 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...

Страница 52: ...the ENTER key After ESC key is pressed system initializes and data table report from main menu can be printed 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6 Reprocess 7 Run 1 pH Calibration...

Страница 53: ...the titration Run Display 3 Temperature Compensation 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 Tem...

Страница 54: ...NTER 1 ABC Temp compensation 1 Manual 2 Auto Temperature 20 120 25 ENTER 2 DEF 5 MNO Temp Compensation 1 Manual 2 Auto ENTER 2 DEF 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6 Reprocess 7...

Страница 55: ...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 3 GHI 5 MNO 1 Admin P W 2 User P W 2 DEF Enter Admin Pas...

Страница 56: ...s 7 Run 1 Clock Date 2 Balance 3 Temp 4 Printer 5 PW 6 Data Xfer 7 Resol 8 Tit Temp Fct 3 GHI 6 PQR Titrant Temp Factor 0 900 1 100 1 ABC ENTER 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6...

Страница 57: ...ayed If number of doses exceeds 199 during any titration run graph cannot be printed error message is displayed If first derivative value is out of range 32000 to 32000 during any titration run graph...

Страница 58: ...libration Report with Buffer values and Slope is printed along with the last calibration date is printed and screen returns to main menu 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6 Reproc...

Страница 59: ...can be print Note Printouts of Graphs are not available if Data Transfer mode selected to PC 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6 Reprocess 7 Run 1 Result 2 Data 3 Condensed 4 Stat...

Страница 60: ...evelop Method 2 Function 3 Config 4 Print 5 Display 6 Reprocess 7 Run 1 Result 2 Statistics 3 Cal Data 5 MNO 1 ABC Vol Reqd 0 9425 ml Result 0 1924 Molarity T Readings 2 10 Skip Reading 0 10 ENTER ENT...

Страница 61: ...0 00001 99 99999 Derivative Threshold 1 32000 6 PQR 0 2 DEF 3 GHI 1 ABC 0 0 0 Conc 0 00001 99 99999 0 100 ENTER 1 BlankVolume 2 PrimaryDose 3 None 3 GHI ENTER Constant Code 1 8 Constant 0 0001 999999...

Страница 62: ...ated to weight and balance mode is AUTO screen shows After pressing Print key of balance screen changes to After pressing ENTER key to acknowledge on instrument screen changes to 1 Develop Method 2 Fu...

Страница 63: ...he screen changes to b Run new method Press ENTER to acknowledge and contine the run or ESC to exit to main menu Enter Identification No refer Appendix A for alphanumeric entries 1 Develop Method 2 Fu...

Страница 64: ...od If last method is quick method Press ENTER to acknowledge ESC to exit Quick Method starts with the mentioned para 1 Develop Method 2 Function 3 Config 4 Print 5 Display 6 Reprocess 7 Run 1 Last Met...

Страница 65: ...ml or after 2 doses Ctrl Lt for pH titration exceeds sample pH error message is displayed the titration run is aborted and suitably printed Constant 0 0001 999999 99 1 Conc 0 00001 99 99999 1 ABC 0 1...

Страница 66: ...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...

Страница 67: ...Refer Pg No 70 S1 Weight or Volume of the sample in ml gm b Direct Titration with Blank or Primary dose The result is calculated according to the following formula Result M1 EP1 E0 C1 S1 where EP1 Tit...

Страница 68: ...which will require end point volume more than the burette volume and ii to reduce the titration time e g if the titrant volume required for neutralization is about 7 ml and the installed burette asse...

Страница 69: ...is to be determined for liquid solid samples respectively Code no 12 19 are reserved and used for solid samples Sample is taken by weight gm e g Entering Constant value 1 in Code no 1 for Sample Volu...

Страница 70: ...AN 56 1 19 TBN 56 1 20 1 Z1 Valency of the titrant Mol wt Eq Wt Z2 Valency of the sample Eq Wt depends upon the nature of titration reaction M Molar Mass gms C Concentration of sample mol L TAN Millig...

Страница 71: ...tubing with suitable solvent is recommended Do not dry the Non glass parts in oven Never place O rings or rubber washers in organic solvents like chloroform carbon tetra chloride 1 Select the Burette...

Страница 72: ...electrode is extremely dirty clean it with 0 1 N hydrochloric acid soapsuds or detergent as necessary for a short time and clean it thoroughly with pure water 3 The electrode which has been left dry...

Страница 73: ...numeric characters can be entered for any alphanumeric entry e g To enter Sample Name say 2 HEXANE Please follow sequence of operations NOTE Press 2 means press the button twice Press 4 Press 3 Press...

Страница 74: ...n exceeds sample pH error message is displayed and the titration run is aborted and Run aborted is printed on report If the second element is 0 i e this condition occurs only after resetting the syste...

Страница 75: ...values are not within specified range error message is displayed If the method parameters are not suitable for running the method by changing burette error message is displayed If the entered paramet...

Страница 76: ...izes the settings of switches for WIPRO LX 800 printer Switch Number Position SW 1 1 DOWN OFF SW 1 2 UP ON SW 1 3 UP ON SW 1 4 DOWN OFF SW 1 5 DOWN OFF SW 1 6 UP ON SW 1 7 UP ON SW 1 8 UP ON SW 2 1 UP...

Страница 77: ...E LIMIT Maximum volume of titration 10000 than initial dose and than predispense volume Maximum 99 999 ml END CRIT By VolLimit or EP EP 9 EP or VL max Equilibrium Mode PREDISPENSE VOLUME Initial Predi...

Страница 78: ...1 sec VOLUME LIMIT Maximum volume of titration 10000 than initial dose and than predispense volume Maximum 99 999 ml END CRIT By VolLimit or EP EP 9 EP or VL max CTRL LIMIT pH at which dose control st...

Страница 79: ...titrants are potassium permagnate KMnO4 potassium di chromate K2Cr207 iodine I2 potassium iodide KIO3 potassium bromate KBrO3 and sodium hypochlorite NaClO The most important reducing agents are ferro...

Страница 80: ...erred for higher reproducibility and accuracy This mode minimizes titration time while maintaining high precision The data of titration curve are checked for the presence of an equivalence point If an...

Страница 81: ...of reaction etc for Equilibrium and Cut off modes For slow weaker reactions increase the equilibrium factor value suitably c INTERVAL sec This is the delay time between dose for Incremental end point...

Страница 82: ...is the maximum predispense dose that can be entered d PREDISPENSE INTERVAL sec This is the delay time between predispense doses given in predispensing for all modes of titrations 0 999 sec e THRESHOL...

Страница 83: ...in the range 0 0001 to 10000 m BUFFER VALUE mV This is the buffer value entered for Method 38 and 40 i e for ASTM D664 D4739 respectively The endpoint can be calculated for the entered buffer value t...

Страница 84: ...lume required for titration This is determination of titrant consumed for neutralization by equivalent volume of solvent to be used along with the sample Blank volume ranges from 0 0001 99 9999 ml d C...

Страница 85: ...nt 1 THRESHOLD 300 MIN CONTROL DOSE 10 l MOLARITY mol lit 1 0000 BV PD NONE None CONSTANT 0 2042 CONSTANT CODE 12 REPORT None Method 42 Standardizing 0 1 M HCl against METHOD NO 42 TITRANT CONC 0 1 M...

Страница 86: ...dPoint 1 THRESHOLD 100 MIN CONTROL DOSE 10 l MOLARITY mol lit 1 0000 BV PD NONE None CONSTANT 0 2042 CONSTANT CODE 12 REPORT None Method 44 Standardizing 0 1 M HClO4 against KHP METHOD NO 44 TITRANT C...

Страница 87: ...EndPoint 1 THRESHOLD 300 MIN CONTROL DOSE 10 l MOLARITY mol lit 1 0000 BV PD NONE None CONSTANT 0 1732 CONSTANT CODE 12 REPORT None Method 46 Standardizing 0 02 M KMnO4 against Na Oxalate METHOD NO 4...

Страница 88: ...RITERIA EndPoint 1 THRESHOLD 300 MIN CONTROL DOSE 5 l MOLARITY mol lit 1 0000 BV PD NONE None CONSTANT 0 0356 CONSTANT CODE 12 REPORT None Method 48 Standardizing 0 02 M Hg NO3 2 against NaCl METHOD N...

Страница 89: ...EndPoint 1 THRESHOLD 100 MIN CONTROL DOSE 10 l MOLARITY mol lit 1 0000 BV PD NONE None CONSTANT 0 0584 CONSTANT CODE 12 REPORT None Method 50 Standardizing 0 1 M EDTA against ZnSO4 METHOD NO 50 TITRA...

Страница 90: ...lectivity in function menu Printer or Personal computer 2 All reports a Result Report b Data c Condensed Report d Statistical Data e Calibration Report of pH f Methods which are available for printing...

Страница 91: ...Open COM When a free Com port is selected The COM port Properties Pop up will be displayed on the screen Set the Comm Port Properties Baud 9600 Data bits 8 Parity none Stop bit 1 Flow Control None or...

Страница 92: ...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 Ctrl Key as Terminal key Backspac...

Страница 93: ...roperties window Click OK Icon on the Properties window to complete the settings Now once again Save the Session to store the settings To Generate the Icon for the TITRA connectivity with PC right cli...

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