Koehler K905 Series Guide

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: [phone] • Fax: [phone]
http://www.koehlerinstrument.com • e-mail: [e-mail]
Petroleum Testing & Analysis Instrumentation • Custom Design & Manufacturing
K905XX
Automatic Potentiometic Titrator

CERTIFICATE OF CONFORMANCE
Automatic Potentiometric Titrator
K905XX
This certificate verifies that part number K905XX, Automatic Potentiometric
Titrator, was manufactured in conformance 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 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

Pg. No. 1of 89
C O N T E N T S
SECTION 1
Introduction
5
Specifications
5
Features
6
SECTION 2
Familiarization with instrument
9
Front Panel – Keyboard Layout and Functions
10
SECTION 3
Instrument Operation - Switching ‘ON’ the instrument
12
1) Develop Method

Generating the Quick Method
13

Viewing & Running & Copying the Last Quick Method
15
Generating the Full Method
19

Viewing, Copying, Skipping & Running 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

Temperature Compensation
50

Printer Selection
51
Password Entry
51
Data Transfer
52

Resolution Selection
53

Titrant Temp Factor
53
4) Print

Printing Last Titration Result
54

Printing Data Table
55

Printing The Titration Analysis
Condensed Report
55

Printing the Titration Statistics Report
55
Printing pH Calibration Report
55
Printing Method Parameters
56

Printing mV v/s
µ
l Grapha Report
56

Pg. No. 2of 89
5) Display

Display Result
57
Display Statistics
57
Display Calibration Data
57
6) Reprocess
58
7) Run
Run Last Method
59

Run New Method
60

Run Last Quick Method
61
SECTION 4
Result Calculation
64
Entering Blank Volume/Primary Dose
65
Entering Constant related to Sample
66
Automatic determining and storing of molarity
68
Maintenance 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 selection table
74
Appendix E : Titration Type
76
Appendix F : Titration Modes
77
Appendix G : Method Parameters
78
Appendix H : Sample Analysis Parameters
79
Appendix I : Calculation Parameters
81
Appendix J : Standard Methods (41-50)
82
Appendix K : PC Setup instruction for Data Downloading
87
THE CONTENTS OF THIS MANUAL ARE SUBJECT TO CHANGE WITHOUT NOTICE.

Pg. No. 3of 89
SECTION 1
•Introduction
•Specifications
•Features

Pg. No. 4of 89
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. User can define
particular method for a specific titration.
SPECIFICATIONS :
Control : Micro-controller based.
Burette : 1ml, 5 ml or 10 ml capacity, interchangeable. 25 ml Optional.
Burette resolution : 1/10000 for 10 ml , 1/5000 for 5 ml and 1/1000 for 1 ml.
Filling time : < 20 seconds.
Principle : Volume determination by equivalence point, end point or pH STAT.
Modes of operation : a)Incremental b)Equilibrium c)Cut-off by pH d)pH STAT titration.
Methods : a)Acid-base b)Non-aqueous c)Redox d)Precipitation
e)Complexometric f)Back g)Photometric h) Thermometric.
mV range : ±3200 mV
Accuracy : ±0.1 mV (±0.0016 pH).
Amplifier Input Impedance : > 10 12 ohms.
End Point detection : a)Potentiometric b)Voltametric c)Thermometric and d)Photometric.
Cut-off criteria : a) Volume b)End point c)mV/pH.
Results : 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 with BNC connector,
b)Differential System comprising Sensing (Indicator) with BNC and
Reference (4mm banana connector). 2) Electrodes for
KF/Voltametric titration with TNC connector. 3) Temperature
(PRT/PT100) for ATC with 5-pin shell connector
Calibration : 3-point Calibration with user entered buffer values and
standardization (7pH)
Titration Head : Manual stand with swiveling arm for electrode, dispensing tip &
stirrer is provided as standards
Stirring System : Micro-controller based variable speed, high torque stirrer with
indication.
Data Storage : Non-volatile memory.
Method Storage : 50 methods with parameters.
Titrant Molarity storage : within Method data.
Input/Output Peripheral Interface : a) Parallel Port : 1 No. for printer.
b) Serial Port : 2 Nos. for Balance & PC.
Report Format : Selection of various formats -a) Method parameters b) Titration
analysis report c) Titration analysis condensed report d) Titration
data table e) Titration graphic report - 1) µl v/s mV 2) µl v/s First
derivative 3) µl v/s Second derivative 4) µl v/s time. f) Statistics
report g) Calibration report.
Keyboard : Alphanumeric splash water proof polyester soft keys.
Display : 40 x 2 line back lighted LCD display.
Convertibility : Can be used KF titrator for Moisture estimation with KF burette
system (Optional)

Pg. No. 5of 89
Environmental Operating Conditions :
a) Operation : Indoor.
b) Temperature : Ambient to 45 °C
c) Operating Temperature and humidity : +5 to 45°C Max, 5 to 90%
non condensing.
d) 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. 40W.
Weight and dimensions :
Control Unit : 12 inch x 12 inch x 6 inch (W X D X H)
Titration unit : 12 x 16 x 16 (W X D X H)
with Vortex Stirrer
Magnetic Stirrer : 6 x 10 x 10 (W X D X H)
(For KF Titration - Optional)
System Weight : 9 Kg.
FEATURES:
•Advanced Micro-controller based user-friendly state-of-the-art product design with
alphanumeric splash waterproof polyester soft keys for keyboard and User interactive
software in dialogue mode for ease of operation.
•Quick interchangeable burette assemblies with intelligent recognition for its volume size.
Burette factor for dispensing correction is available for true end point volume.
•Alphanumeric entry of Sample Name, Titrant Name, Identification Number, Date & Time
with type of electrode used for authentication. Daily Auto Incremented Run number and
Factory entered CUSTOMER NAME & Instrument Sr.No. on report printouts make the
system foolproof and GLP compliant.
•Protection against invalid parameter entries during method generation.
•Storage of 40 User methods with parameters. (Plus10 not editable – Default methods)
•Two Tier - ADMIN & USER Password Protection for Method data during ADD/EDIT,
DELETE, COPY, 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
appropriate electrode.
•Automatic selection of Sensor Input as per titration method selected.
•During titration, the measured variable i.e. electrode potential (mV) or pH value is shown
on display together with dispensed volume and number of End Point (EP) detected.
•User selectable End Point (EP) evaluation up to 9 EP during the run, and calculation by
first, last, largest, all or selected EP with display of results and printout.
•Composite Differential Electrode Amplifier unit for potentiometric and voltametric / KF
titration, having BNC connectivity to various electrodes and temperature sensor for
indication.
•Capability to use as simple pH meter with display of pH, mV values & Temperature display.
•Facility to use as a dispenser for fixed volume dosing or dilution allows to perform manual
titration with user defined dose and mV indication.
•User Programmable selectivity for report format, complying with GLP requirements: a)
Report giving titration parameter and result. b) Data table giving mV, pH, δmV, mV/ml, 2nd
Deriv. and volume. c) Graphics report giving mV v/s µl titration curve. d) Graphics report 1st
deriv. graph v/s µl titration curve e) Graphics report of 2nd deriv curve. f) Report of method
parameters for 50 methods. g) Condensed report of titration parameters and results. h)
Auto evaluation report for multi EP samples - EP1, EP2-EP1 & EP3-EP2 etc. available.
The reports can be obtained even after resetting/power off / power fail conditions or Run
Aborted.

Pg. No. 6of 89
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.
•Display and printout of daily Auto Incremented Run (AIR) number which makes system
foolproof and GLP compliant.
•Statistic function with run selectivity for finding Mean, SD, RSD & CV of last 10 repeat run
results could be viewed or printed.
•Real Time Clock (RTC) for time display and report printout with run time indication.
•Special Method Compliant to ASTM D664, D2896 & D4739 for TAN and TBN analysis for
oil samples.
•Automatic evaluation of molarity determination of titrant.
•Quick Method for Trial analysis RUN 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 entering or running method.
•Display of stir time after pre-dispensing (with selectable dose and time).
•Escape and Back keys for better user interaction.
•Vortex stirrer for homogeneous stirring with glass propeller (provides chemical inertness).
•Digital Speed control of vortex and magnetic stirrer with indication.
•Availability of optional in situ accessory for Titration Vessel heating to perform titration
from ambient+10°C to 80 °C. Cooling can be achieved with external chiller.
•PC Compatibility – RS232 interface for Data Downloading to Result Data Capturing
Software (Ethernet based) or Windows Hyper Terminal Software (Optional).
•Balance interface for automatic sample weight transfer.
•K905XX can be converted to perform Karl Fischer titration by just changing burette
assembly.

Pg. No. 7of 89
SECTION 2
•Familiarization with Instrument
•Front Panel – Keyboard Layout and
Functions

Pg. No. 8of 89
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. Two Teflon tubings are
fitted with finger tight fittings. The left side tubing is for titrant
aspiration and the right side 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 D type connector – Centronic Parallel port interface
5) Display : 40 X 2, Back lighted, LCD display.
6) Key Board : Multi-function tactile keyboard as shown below.
7) Electrode Connection: Differential input with BNC and 4mm Banana Connector.
8) Temperature sensor : 5 pin Shell connector
9) Balance connectivity : RS232C – DB9.
10) PC Connectivity : RS232C – DB9 for data downloading to Result Data
Capturing Software (Ethernet based) (Optional) or
Windows HyperTerminal or any other terminal software.

Pg. No. 9of 89
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:
1] : To reset the instrument 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 parameters.
c) To stop continuous monitoring of mV read by electrode in Scan mode.
5] : To cancel the wrong entries.
6] : To enter decimal point during numeric entries. To Add / Remove the Beep
during run.
7] : To Start / Stop Stirrer Manually.
RESET
ESC
ENTER
CE
BACK
•
BEEP
STIRRER
ON/OFF

Pg. No. 10 of 89
SECTION 3
•Instrument Operation
•Titration Method Development
•Function
•Methods

Pg. No. 11 of 89
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.
d) Connect printer through appropriate cable to the backside of the instrument.
e) Connect the Vortex stirrer to the backside of Stirrer control unit.
f) Turn the power switch ‘ON’, with beep sound the LCD display shows the Model & the
firmware version 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 Priming, Burette
change or Manual titration. (Refer pages 45)
3) Config :- System Settings – Clock/date, Balance, Temperature
compensation, Printer, Password setting, Titrant temperature
factor., Data Transfer, Resolution (Refer pages 50)
4) Print :- Titration report, Statistics, Method parameter, pH Calibration
report. (Refer pages 54)
5) Display :- Titration result, Statistics, pH Calibration data. (Refer pages 57)
6) Reprocess :- Data Reprocessing (Refer pages 58)
7) Run :- To Perform titration with desired method (Refer pages 59).
AUTO TITRATOR Vx.x
AT 10 ml Burette Assembly detected
1)Develop Method 2) Function 3)Config.
4)Print 5) Display 6) Reprocess 7)Run
Wait…
A

Pg. No. 12 of 89
1. Titration Method Development
•Developing the Quick Method : Follow the below mentioned instructions
MEAS. TYPE : Potentiometric TITR. TYPE : Acid-Base Aqueous
TITR. MODE : Incremental P.D.VOLUME : 0 µl
STIR TIME : 5 sec INITIAL DOSE : 100 µl
INTERVAL : 5 sec VOLUME LIMIT : 10000 µl
TITR. END CRIT. : End Point NO. OF EP : 1
CAL. BY : 1 st EP DERIV.THRESH.: 50
1)Develop Method 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)Thermo : 1
1
ABC
1
ABC
2
DEF
1
ABC
Select titration mode
1)Incr. 2)Equil. 3)Cutoff(pH) 4)pHstat: 1
1
ABC
Initial Dose (5-2000 µl) : 50
1
ABC
0
- . /
0
- . /
Predispense Volume (0-95000
µ
l) : 0
ENTER
Stir Time (0-999 sec) : 5
5
MNO
ENTER
Measurement Type
1)Potentiometric 2)Voltametric :
1
ABC
ENTER
ENTER
ENTER
Predispense Dose (5-10000
µ
l) : 1000
ENTER
Predispense Interval (0-999 sec) : 0
ENTER

Pg. No. 13 of 89
1)Run 2)View :
Derivative Threshold (1-32000) : 50
Volume Limit (Max. : 99999 µl) :
Derivative Threshold (1-32000) :
1
ABC
5
MNO
0
- . /
0
- . /
0
- . /
0
- . /
0
- . /
Initial Dose (5-2000
µ
l) : 100
Volume Limit (Max. : 99999 µl) : 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
1
ABC
ENTER
ENTER
Quick Method Stored
ENTER
ENTER
Calculation by
1)1st 2)Largest 3)Last 4)All 5)Select : 1
ENTER
1
ABC

Pg. No. 14 of 89
•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
MODE : Incremental PREDISPENSE VOLUME : 0 µl
PREDISPENSE DOSE : 1000 PREDISPENSE INTERVAL : 0
STIR TIME : 5 sec INITIAL DOSE : 100 µl
INTERVAL : 5 sec VOLUME LIMIT : 10000 µl
TITR. END CRIT. : End Point NO. OF EP. : 1
CAL. BY : 1 st EP DERIV.THRESH. : 50
Display Press
Quick Method RUN
starts with the
mentioned para.
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’ option.
1)Develop Method 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
1)Run 2)View :
Running Quick Method ...
ENTER
1
ABC
1
ABC
1
ABC
1
ABC
1)Sample Weight 2)Sample Volume :
2
DEF
Disp.Vol. : XXX
µ
l # RN BV 10 TITRA+
250° mV : 00 : 00 : 39
Conc. (0.0001-99.9999) :
0
- . /
1
ABC
.
Sample Volume (0.0001-999.99999 ml) :
Wait .....
00 : 00 : 24
ENTER
Vol. Reqd : 0.9425 ml
1)Repeat Run 2)Result 3)Print :
1
ABC
Calculation by
1)1
st
2)Largest 3)Last 4)All 5)Select : 1
ENTER

Pg. No. 15 of 89
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 reprocess/ recalculate result in different result unit or to evaluate endpoint by
changing the threshold , select ‘2’ option.
Derivative Threshold (1-32000) : 20
Const 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)PrimaryDose 3)None :
1)BlankVolume 2)PrimaryDose 3)None :
3
GHI
3
GHI
ENTER
ENTER
Constant Code (1-8) :
Const 1 (0.0001-999999.99) : 63
Vol. Reqd : 0.9425 ml R : 0.1924 MOLARITY(S)
1)Repeat Run 2)Reprocess 3)Print :
1
ABC
ENTER
ENTER
ENTER
Calculation by
1)1st 2)Largest 3)Last 4)All 5)Select : 1
ENTER
Sample Vol. (0.0001 – 999.99999 ml): 1.0000
.

Pg. No. 16 of 89
•Viewing Last Quick Method :
1)Quick method 2)Full method :
1)Last Method 2)Edit Method : 1
3)Copy Method
1)Run Method 2)View :
ENTER
1
ABC
1
ABC
2
DEF
Const 1 (0.00001-999999.99) :
6
PQR
3
GHI
Type : Acid-Base Aqueous
Mode : Incremental
Initial Dose (µl) : 100
Interval (sec) : 3
Measurement Type :
Potentiometric
Predispense Volume (
µ
l) : 100
Predispense Dose (µl) : 50
Predispense Interval (sec) : 0
Stir Time (sec) : 0
VolLimit (µl) : 10000
Titr. End Crit. : EndPoint
Constant Code (1- 8) :
Const 1 (0.00001-999999.99) : 63
Vol. Reqd : 0.9425 ml R : 0.1924 MOLARITY(S)
1)Repeat Run 2)Reprocess 3)Print :
1
ABC
ENTER
ENTER
ENTER
ENTER
ENTER
ENTER
ENTER
ENTER
Sample Vol. (0.0001 – 999.99999 ml) : 1.0000