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KARL FISCHER TITRATION

A method for determining the water content of samples.  A polarising current is applied to a pair of platinum
electrodes immersed in a solution containing iodine, pyridine, methanol and sulphur dioxide.  A polarising
current, typically 10 microamps, is applied to the electrodes and the resulting potential is monitored.

LIQUID JUNCTION

The point of contact between the sample and the reference electrode filling solution.

LEAK RATE

The reference electrode fill solution will inevitably leak into the sample solution.  An irregular leak rate may
cause the liquid junction potential to vary causing unstable or drifting readings.  Samples of small volume that
need to be retained can also suffer an unacceptable level of contamination.

MEMBRANE

In a pH electrode the membrane is a thin pH sensitive glass.  A potential difference is developed across the
membrane due to the formation of double layers with ion-exchange properties.

MILLIVOLT

Based on the SI unit of potential difference, electrical potential or e.m.f. such that the potential difference
across a conductor is 1 millivolt when a current of 1 milliamp flows through a resistance of 1 ohm.

MOLALITY

The concentration of a solution expressed as a number of moles of dissolved substance per kilogram of
solvent.

MOLARITY

The concentration of a solution expressed as the number of moles of dissolved substance per dm

3  

of solution.

MONOVALENT ION

An ion with a single positive or negative charge (Na+, H+, Cl-, etc).

NERNST EQUATION

A mathematical relationship which describes the theoretical behaviour of pH electrodes

E = Ex + 2.3 RT logai
                  nF

E is the potential, in millivolts, developed between the sensing and reference electrodes.
Ex varies with the choice of reference electrodes and is a constant.
2.3 RT

is the Nernst Factor. R is the gas constant, i.e. 8.31441J.K-1 mol-1.

   nF

T is the thermodynamic temperature (in K)
n is an integer with sign and magnitude corresponding to the charge on the ion.
F is the Faraday Constant and is equal to 9.648456 x 104 C.mol-1.
Ai is the activity of the ion to which the electrode is responding.
At T=25°C, E is equal to 59.16mV when n=1.

NOISE

Random and rapid changes in displayed electrode potential.  This is often due to the pick-up of strong static
charges or electromagnetic interference from adjacent equipment.

3345/REV A/08-99

46

Содержание 3345

Страница 1: ...MODEL 3345 ION METER OPERATING MANUAL 547 009 REV A 08 99...

Страница 2: ...Setting up parameters 3 6 Entering pH Buffer Values 3 7 pH Calibration Automatic 3 8 pH Calibration Manual 3 9 Error Codes 3 10 Good Practice Guidelines 3 11 mV MODE Setting up parameters 3 12 Tempera...

Страница 3: ...SECTION 4 MAINTENANCE General 4 1 Cleaning Re conditioning of Glass Electrodes 4 2 Ion Selective Electrodes 4 3 SECTION 5 OPTIONAL ACCESSORIES SECTION 6 INTERFACING GLOSSARY OF TERMS 3345 REV A 08 99...

Страница 4: ...ines are date and time stamped thus satisfying the requirements of Good Laboratory Practice GLP quality assurance protocols The units will store up to 100 readings which can subsequently be recalled o...

Страница 5: ...Recognition 2 4 7 9 and 10pH buffers with manual override facility Pre Programmed Ion NO3 ION ION2 ION ION2 H SCN Cu2 S2 CN I Br Characteristics Cl Hg 2 Cd2 Pb2 F Ag CO3 Ba2 NO2 ClO4 NH4 Ca2 K Calibr...

Страница 6: ...l adjacent to the power socket This adjustment should only need to be made on receipt of the instrument After initial adjustment the instrument will automatically adjust the contrast depending on the...

Страница 7: ...MENT SETUP mode using the arrow key and press the key Move the cursor to the LANGUAGE menu and select the appropriate language by using the arrow keys Once selected move to the EXIT option and press t...

Страница 8: ...for selection of modes of operation The selected mode is reverse highlighted 6 ICONS used in pH and Ion modes to prompt steps of calibration and sample measurement 7 ERROR MESSAGES displays error mes...

Страница 9: ...l functions Display select key Used to toggle between primary and secondary displays Used to enter the exponential part of a value e g to enter 1 3 x 10 3 the key sequence is 1 3 EXP 3 Help key Provid...

Страница 10: ...rm connections 5 KARL FISCHER 2 x 4mm sockets Polarised output Karl Fischer titrations are enabled by the provision of a 10 A polarising current output 6 ANALOG OUT 2 x 4mm sockets Analog output propo...

Страница 11: ...o last calibration details RECALL recall mode for stored readings SETUP used to set up mode specific parameters instrument and clock set up parameters pH CONC STORE ABS RECALL SETUP pH pH mode CONC co...

Страница 12: ...be s are connected ENDPOINT SUPPRESS allows specific endpoint time to be entered for sample under test If the sample is known to have a slow stabilisation point then the endpoint can be suppressed to...

Страница 13: ...box appears To default to the original value press the key again ENDPOINT SUPPRESS Select the ENDPOINT SUPPRESS menu using the key and use or key to highlight options The value may be adjusted by sel...

Страница 14: ...on to prompt CAL REMINDER Select CAL REMINDER menu using the key and use arrow key or press to highlight options Select ON or OFF option as required and press to confirm INTERVAL HH Select the INTERVA...

Страница 15: ...tout will be initiated at that interval START start time set STOP stop time set AUTO CAL PRINT Select AUTO CAL PRINT menu using the key and use arrow key or press to highlight options Select ON or OFF...

Страница 16: ...me in units of hours minutes seconds using the numeric keys and then press to confirm ALARM POINTS SUB MENU EXIT menu escape key XX HIGH ALARM if the reading exceeds this value an alarm warning will a...

Страница 17: ...me in units of hours minutes seconds using the numeric keys and then press to confirm DATE Select the DATE menu using the key and use or key to highlight options The value may be adjusted by selecting...

Страница 18: ...he instrument has the facility to disable the secondary display allowing the the use of 1 sensor only This can be achieved by entering the INSTRUMENT SET UP and setting the SECONDARY CHANNEL option to...

Страница 19: ...and sensor input to be viewed and changed ALARM POINTS used to view and change alarm points for the selected mode and channel INSTRUMENT SETUP used to select the next set up menu for instrument param...

Страница 20: ...essing the key again will default to the original value Once the correct value is entered pressing the key will update the display to the new value corrected to 3 decimal places If you wish to abort p...

Страница 21: ...o calibrate the instrument select the CALIBRATE menu option using the arrow keys The electrode s should be placed into the first buffer solution and the reading allowed to stabilise the endpoint symbo...

Страница 22: ...the CAL 2 buffer value If a one point calibration only is required select the EXIT option using the arrow keys and pressing The instrument will return to the pH mode The icon will then change to show...

Страница 23: ...ature actual temperature will be displayed The instrument will then return to the main pH display Once calibration is completed the instrument is now ready to perform sample measurement Rinse electrod...

Страница 24: ...etting cap with pH4 buffer Reference pH 2 Electrodes should be stored a away from direct sunlight b in a vertical position c within their specified temperature range 3 Always ensure the electrode is u...

Страница 25: ...e specific test being carried out pH Redox and Ion Selective electrodes can all be used in this mode Most of these determinations will require the preparation of calibration curves or other analytical...

Страница 26: ...ng the numeric keypad and pressing This mode is suitable for determinations using Redox and Ion Selective Electrodes and has the additional benefit of being able to zero any offset voltage developed b...

Страница 27: ...erence electrodes are the calomel mercurous sulphate and double junction The calomel is the most widely used of the three and contains a saturated potassium chloride filling solution Potassium chlorid...

Страница 28: ...ard and test solutions to eliminate effects of differences in activity The temperature must be kept constant between samples and standard Within the linear range of the electrode two standards are suf...

Страница 29: ...ty to be entered The value entered will give a 1mV change in recorder output ION allows the ion selective electrode being used or channel using the arrow keys This allows the instrument to check the s...

Страница 30: ...eys and press REC O P 1mV Enter SETUP menu and select REC O P 1mV Adjust the reading as required using the numeric keys and press ION Enter SETUP menu and select ION Select the required ion selective...

Страница 31: ...ERS menu option using the arrow keys and pressing Selecting this menu allows access to five settings Values can be entered in any order and do not need to be incremental or decramental Adjustments can...

Страница 32: ...for temperature actual temperature will be displayed The icon will then change to show the CAL 2 buffer value If a one point calibration only is required select the EXI T option using the arrow keys...

Страница 33: ...s of the ion are unstable of unknown concentration or toxic This method is also used when the sample ion concentration is high and known addition procedures produce small changes in potential Alternat...

Страница 34: ...sed as a delete key starting from the lowest digit If you wish to alter the entered value keep pressing this key until a blank box appears Pressing the key again will default to the original value Onc...

Страница 35: ...splay will now give a reading and the second icon will flash to indicate that a measurement is in progress Pressing CONTINUE again and the key will cause the third icon to flash requesting that the kn...

Страница 36: ...ration is found using Where Cm Concentration of mixture Cs Concentration of standard Vs Volume of standard Cu Concentration of previous sample Vu Volume of previous sample To perform a measurement the...

Страница 37: ...essing the key will update the display to the new value Select STANDARD CONC using the arrow key Press Adjust the reading as required using the numeric keys If a mistake is made the key can be used as...

Страница 38: ...asurement sequence will commence as before Selecting STORE will allow the displayed reading to be stored On completion of measurements selecting EXIT and pressing will return the instrument to the CON...

Страница 39: ...without storing the reading To store a reading in a specific location use the arrow keys to select the required location and press If no other key is pressed within 5 seconds the reading will be auto...

Страница 40: ...elect the RECALL mode using the arrow keys and press Select RECORD by using the arrow keys and pressing ENT Select the specific location to be deleted by using the arrow keys Move to the DELETE menu o...

Страница 41: ...rameter proceeds by pressing The first part of the parameter is highlighted and can be adjusted to the required value using the arrow keys If further adjustment is required move the highlighted cursor...

Страница 42: ...OR CLEANING OF GLASS ELECTRODES NOTE Epoxy bodied electrodes should not be cleaned with aggressive solvents DEPOSIT CLEANING AGENT General deposits Mild detergent solution Inorganic coatings Commercia...

Страница 43: ...e 1 00E0 1E 3 1000mV Buffered Electrode Potential Analog Outputs Each sensor input has a buffered analog output which is available on the 25 way D socket 25 way D Socket pin 14 sensor 1 buffered outpu...

Страница 44: ...ng plus sample number Sending an ASCII C causes a printout of the last calibration parameters same as printout after performing a calibration Sending an ASCII P causes downloading of stored readings S...

Страница 45: ...ections are available on the 25 way D socket pin 12 sensor 1 open collector transistor low alarm output pin 13 sensor 1 open collector transistor high alarm output pin 10 sensor 2 open collectortransi...

Страница 46: ...ASYMMETRY POTENTIAL The potential developed across a glass pH membrane when both sides of the membrane are in contact with an identical solution This term is also used to define an electrode potential...

Страница 47: ...es has dissociated Expressed as K A B AB DIVALENT ION A doubly charged ion S is a divalent anion Ca Mg are divalent cations DOUBLE JUNCTION REFERENCE ELECTRODE Used in place of a single junction refer...

Страница 48: ...ired before an equal electrode response is seen INTERNAL REFERENCE ELEMENT A reference electrode situated within the glass pH sensing electrode IONIC STRENGTH I units mol m 3 mol g The total effect of...

Страница 49: ...cross a conductor is 1 millivolt when a current of 1 milliamp flows through a resistance of 1 ohm MOLALITY The concentration of a solution expressed as a number of moles of dissolved substance per kil...

Страница 50: ...t potential reference elec trode POTENTIOMETRY A method of directly measuring wither concentration or activity of a sample solution by comparison with results from two or more known standards The temp...

Страница 51: ...pH meters are equipped with a control to enable electrodes to be calibrated when developed potentials are non Nernstian This is often called the slope control SOLID STATE ION SELECTIVE ELECTRODE Membr...

Страница 52: ...on of Conformity JENWAY Model 3345 Ion Meter complies with the following European Standards EN 50081 1 1992 Electromagnetic compatibility Generic emission standard EN 50082 1 1992 Electromagnetic comp...

Страница 53: ...l 41 41 541 5877 Fax 41 41 541 5878 Email General Information Sales info kesn ch Accounts Department accounts kesn ch USA O ce 233 Rogue River Highway 425 Grants Pass Oregon 97527 5429 USA Tel 1 503 2...

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