operating instructions titration unit titroline alpha index..... 204 chapter 1 technical description...

Version 990818 E

105C O N T E N T S

Operating Instructions Titration UnitTitroLine alpha

C O N T E N T S PAGE

1 Technical description of the Titration Unit TitroLine alpha ............................ 107

1.1 Summary ............................................................................................................................. 107Declaration of Conformity .................................................................................................... 108

1.2 Warnings and safety information ......................................................................................... 111

2 Setup and first operation .................................................................................... 112

2.1 Unwrapping and setup of the Titration Unit TitroLine alpha ............................................... 1122.1.1 Installing the „Memory card“ ................................................................................................ 1122.1.2 Removing the „Memory card“ .............................................................................................. 1132.1.3 Installation of the stand bar ................................................................................................. 1132.2 Replacing the entire dosing unit .......................................................................................... 1142.3 Replacing the dosing unit .................................................................................................... 1172.4 Combining the Titration Unit TitroLine alpha with other devices ......................................... 119

3 Structure of the Titration Unit TitroLine alpha ................................................ 121

4 The connections of the Titration Unit TitroLine alpha .................................... 122

4.1 Measuring amplifier input / electrode signal ........................................................................ 122

5 Working with the Titration Unit TitroLine alpha .............................................. 123

5.1 Multifunction display ............................................................................................................ 1235.1.1 Contrast adjustment ............................................................................................................ 1235.2 Parameterization of the Titration Unit TitroLine alpha using a keyboard ............................ 1235.3 The menu system ................................................................................................................ 1265.4 „MODE“ ............................................................................................................................... 1285.4.1 <<MTH>> ............................................................................................................................ 1285.4.2 <<CALC>> ........................................................................................................................... 1455.4.3 <<DOC>> ............................................................................................................................ 1525.4.4 <<STD>> ............................................................................................................................. 1545.4.5 <<LIST>> ............................................................................................................................. 1555.4.6 <<PRN>> ............................................................................................................................. 1565.4.7 <<MEAS>> .......................................................................................................................... 1575.5 Menu „INIT“ ......................................................................................................................... 1575.5.1 <<TIME>> ............................................................................................................................ 1575.5.2 <<COPY>> .......................................................................................................................... 1575.5.3 <<CAL>> ............................................................................................................................. 1585.5.4 <<RS>> ............................................................................................................................... 1605.5.5 <<PASSW>> ....................................................................................................................... 1615.5.6 <<SYS>> ............................................................................................................................. 1625.5.7 <<CNTRY>> ........................................................................................................................ 1655.6 Menu „CAL“ ......................................................................................................................... 1665.7 Edit balance data ................................................................................................................. 1675.7.1 Use ...................................................................................................................................... 1675.7.2 Edit function (AD) ................................................................................................................ 1675.7.3 Edit function (ID) .................................................................................................................. 1685.7.4 Edit function (OW) ............................................................................................................... 1685.7.5 Edit function (DL) ................................................................................................................. 1685.8 Error messages ................................................................................................................... 1695.8.1 Titration error messages ..................................................................................................... 1695.8.2 Calibration error messages ................................................................................................. 169

Version 990818 E

106 C O N T E N T S (continuation)

PAGE

6 Method creation using the TitroLine alpha ...................................................... 170

6.1 Titration of sulphuric acid ..................................................................................................... 1706.2 Titration of an unknown acid ................................................................................................ 1786.3 Chloride in potable water ..................................................................................................... 1866.4 Water determination according to Karl-Fischer ................................................................... 1896.5 pHstat in soil samples .......................................................................................................... 194

7 Inputs/Outputs for data communication ........................................................... 198

7.1 Keyboard connection ........................................................................................................... 1997.2 Power connection ................................................................................................................ 1997.3 RS-232-C interfaces ............................................................................................................ 1997.4 Centronics interface ............................................................................................................. 2007.5 Controlling the Titration Unit TitroLine alpha via the RS-232-C interface ........................... 201

8 Maintenance and care of the Titration Unit TitroLine alpha ........................... 202

8.1 Maintenance and care of the titration unit ........................................................................... 2028.2 Maintenance and care of the burette unit ............................................................................ 202

9 Storage and transport ......................................................................................... 203

10 Index ..................................................................................................................... 204

107Chapter 1 Technical description

1 Technical description of the Titration UnitTitroLine alpha

1.1 SummaryThe Titration Unit TitroLine alpha is a self-contained titration computer enablingversatile titrations in laboratories owing to its processor and hardware.

Connections can be made with e.g.− Measuring sensors for pH-, mV-, °C measurements and Karl-Fischer titrations− Printer with a serial (RS-232-C) or parallel (Centronics) interface

- EPSON compatible -− Stirrer TM 125 (additional TZ 1848 power pack required)− Mini keyboard TZ 2825,

PC keyboard (multifunction PC keyboard or XT keyboard)− Personal computer for downloading results− Balance

It is possible to carry out pH, redox, Karl-Fischer, and pH-stat titrations with up to8 memorizable methods.

Examples of possible applications of the Titration Unit TitroLine alpha:− Acid/base determination in aqueous solutions, p and m value− Acid/base determination in non-aqueous solutions, e.g. TAN, TBN, and acid

number in polymers− Redox titrations such as iodometry, manganometry, chromatometry, and CSB

determination− Other mV titrations, e.g. chloride in water, halogenides side by side− Titrations using ion-sensitive electrodes, e.g. calcium, fluoride, copper,

sulphide− Water determinations according to Karl-Fischer− pH stat titrations e. g. in biochemistry and in soil samples− Indices such as OH number, iodine number or saponification number

These methods are mere examples; further applications can be found in foodtechnology, pharmaceuticals, biochemistry, photofinishing, environment, qualitycontrol, and process monitoring.

Owing to its connections the Titration Unit TitroLine alpha is very versatilein combination with other devices.

− One of the two RS-232-C interfaces is used for extensive data communicationwith a computer - personal computer - or to log data using a printer with anRS-232-C interface.

− The second RS-232-C interface enables the connection of a balance.− The Centronics is used to document data using a printer with a parallel inter-

face.− The standardized socket for a standard PC keyboard enables simple param-

eterization for many functions.− A 2-pole jack bush can be used to operate a TM 125 Magnetic Stirrer or a

TZ 1845 Stirrer.− The stirring speed is set on the stirrer.− lluminated multifunction LCD display with its corresponding dialogue menus

and a calibration system for pH electrodes enable safe operation with theTitration Unit TitroLine alpha.

Connections

Possible use

SCHOTT-GERÄTE GmbHIm Langgewann 5

D-65719 Hofheim am TaunusDeutschland, Germany, Allemagne

15. Oktober, October 15th, 15 Octobre 1996AGQSF 0000-A033-04/990303

KONFORMITÄTSERKLÄRUNGDECLARATION OF CONFORMITYDÉCLARATION DE CONFORMITÉ

Wir erklären in alleiniger Ver-antwortung, daß das Produkt

Titrator

TitroLine alpha

auf das sich diese Erklä-rung bezieht, übereinstimmt

mit den Normen

und mit dem normativenDokument

We declare under oursole responsibility that

the product

Titration Unit

TitroLine alpha

to which this declarationrelates is in conformity

with the standards

DIN 12 650, Teil 5,

ISO DIS 8655

and the normative document

Nous déclarons sous notre seuleresponsabilité que le produit

Titrateur

TitroLine alpha

auquel se réfère cette déclara-tion est conforme aux normes

et au document normatif

Technische Daten

Titrator TitroLine alpha

15. Oktober 1996

Translation of the legally binding German version




Technical data of the Titration Unit TitroLine alpha State October 15th, 1996

Conformity: DIN 12 650, Part 5, Conformity mark CE mark: Electromagnetic compatibility according to the Council Directive 89/336/EMC;

Generic emission according to standard EN 50 081, Part 1Generic immunity according to standard EN 50 082, Part 2Low-voltage directive according to the Council Directive 73/23/EWG,last modified by the Council Directive 93/68/EWGTesting basis EN 60 010, Part 1

Country of origin: Made in Germany

Burette portion: Technical data of the Interchangeable Units:Cylinder size: Volume size, selection via menu inputValve: Volume-neutral plug valve made of fluorocarbon polymersCylinder: 10 ml, 20 ml or 50 ml DURAN® borosilicate glass cylinderUV protection: Protective enclosure, brown, standardHoses: PTFE with brown UV protection

The following solutions may be used:− All common titration solutions, with the solutions referred to in the “Küster-Thiel” computing tables (Walter

de Gruyter Publishers) serving as guidelines.− Water and all non-aggressive inorganic solutions can be used as solutions. When working with inflamma-

ble substances the explosion-protection regulations of the employers' liability insurance association of thechemical industry have to be observed.

− With liquids with a higher viscosity (≥ 5 mm²/s), a low boiling point or a tendency to exhalation the fillingspeed can be adapted.

− Liquids with a viscosity above 20 mm2/s can not be dosed.

Interchangeabledosing unit

type no.

Volume[ml]

Int. ∅ tolerancesof the glass cylinders

[mm]

Accuracy*[%]

Smalleststep size

[ml]TZ 2051 10.0 0.004 0.15 0.002TZ 2052 20.0 0.005 0.15 0.004TZ 2055 50.0 0.008 0.15 0.01

*Accuracy: indicated in terms of measuring incertainty with a confidence level of 95%.

Measuring inputs: The built-in measuring inputs enable the following sensors to be connected:one pH/mV electrode,one temperature sensor (Pt 1000 Resistance Thermometer) andone double platinum electrode for Karl Fischer titration.

Measuring input: pH/mV input with 16-bit transducer for high-precision measurementresolution during titration and 4 smoothing stages of the measurement signalConnection: electrode socket according to DIN 19 262 or BNC socket and

reference electrode 1 x 4 mm socket

Measuringrange

Displayresolution

Accuracy*without sensor

Input resistance[Ω]

pH 0 ... 14 0,001 0.02 ± 1 digit > 1 • 1013U [mV] - 1900 ... 1900 0.1 1.0 ± 1 digit > 1 • 1013

® registered trademark for SCHOTT GLAS, Mainz

Translation of the legally binding German version




Measuring input: Measuring sensor port for Pt 1000 Resistance Thermometer,Connection: 2 x 4 mm sockets and 1 x 2 mm socket.

Measuringrange

Display resolution Accuracy*without sensor

T [°C] - 75 ... 175 0.1 0.2 K ± 1 digit

Measuring input: Karl-Fischer- (Dead-Stop) connector for double platinum electrodeoutput voltage: 100 mV, internally adjustable (60 ... 220 mV)connection: 2 x 4 mm sockets.

Measuringrange

Display resolution Accuracy*without sensor

I [µA] 0 ... 100 0.1 0.2 ± 1 digit

Display: LCD multifunction display with background lighting: approx. 65 x 110 mm,measuring value display 4½ digits with floating decimal point and unit, 18 mm high,4 alphanumeric lines each 8 mm high, additional control display, contrast adjustment

Calibration: automatically with 2 buffer solutions out of 8, sequence during calibration optional,3 freely definable buffers can be input. Default buffer solution according to DIN 19 266 and NBS or with integral pH values pH = 2.00; 4.00; 4.01; 6.87; 7.00; 9.08; 10.0; 12.45

Connections: DIN socket according to DIN 19 262 for pH/mV electrode orBNC and reference electrode 1 x 4 mm socket,2 x 4 mm and 1 x 2 mm sockets for Pt 1000 Temperature Sensor,2 x 4 mm sockets for double platinum electrode (KF titrations)

RS-232-C interfaces: ”Balance” for connecting an analytical weighing-balanceor Sample Changer TW alpha

”Computer” for connection of a PC for data memorization or of a printerwith a serial RS-232-C interface for documentation

Configuration of the RS-232-C interfaces: 1200, 2400, 4800, 9600 baud; word length 7 or 8 bits;stop bits: 1 or 2; parity: even or no (preset in 4 combinations)

Printer port: ”Printer” Centronics interface for connection of a printer with parallel interfaceKeyboard connection: ”Keyboard” TZ 2825 mini-PC-keyboard from SCHOTT-GERÄTE or

MF2 in XT modeStirrer connection: ”Stirrer” TM 125 Magnetic Stirrer, additional TZ 1848 voltage supply required and

TZ 1845 Stirrer with TZ 1583 connection cableMains connection: ”Power” 100 ... 240 V∼ (47 ... 63 Hz); 35 VA; via external TZ 1849 power packCasing material: Steel/polypropylene with glass ball reinforcement,

with interior metallization for shielding purposesFront-panel foil: PolyesterCasing dimensions: 148 x 310 x 210 mm (l x h x d) incl. cylinderWeight: 3.5 kgClimate: Environmental temperature: + 10 ... + 40 °C for operation and storage

Humidity according to EN 61 010, Part 1:80 % for temperatures up to 31 °C,linear decrease down to 50 % relative humidity at a temperature of 40 °C

*Accuracy: indicated in terms of measuring incertainty with a confidence level of 95 %.In addition the measuring incertainty of the sensor has to be taken into account as well.For instance, it is ∆ pH = 0.012 ... 0.03 according to DIN 19 266, item 3.

111Chapter 1 Technical description

1.2 Warnings and safety informationFor safety and functional reasons, the Titration Unit TitroLine alpha as well as theincluded power pack must basically be opened by authorized persons only; e. g.work at the electric appliance must only be carried out by trained specialists. Withunauthorized operation of the Titration Unit TitroLine alpha as well as careless ordeliberate damaging, the warrenty is no longer valid.

The Titration Unit TitroLine alpha corresponds to protection class III. It has beenbuilt and tested according to protective arrangements for electronic measuringinstruments EN 61 010 - 1:1993, part 1, and has left our plant in perfect conditionconcerning safety regulations. To maintain this condition and to guarantee safeoperation the user has to observe the instructions and warning marks which areincluded in these operating instructions. The power pack is manufactured andtested

according to EN 60 950 and corresponds to protection class I.

Before switching on, it has to be guaranteed that the adjusted operating voltageand supply voltage correspond. Operating voltage is indicated on the type platepower pack. The mains plug must only be inserted in a socket outlet with earthingcontact. The protective effect must not be invalidated by an extension line withoutearthed lead. Any interruption of the earthed lead inside or outside the

power pack or detaching the earthed lead connection could make the TitrationUnit TitroLine alpha dangerous. Deliberate interruption is not permissible. A powerpack other than the included power pack no. TZ 1849 must not be used.

It has to be guaranteed that fuses and rated current strength indicated are usedas substitute.

The Titration Unit TitroLine alpha must not be stored or operated in damp condi-tions.

If there is reason to believe that non-dangerous operation is not possible, theTitration Unit TitroLine alpha should be stopped and secured against unintentionaloperation.

Please note the corresponding operating instructions of other devices to be con-nected e.g. balance, printer, keyboard, PC.

For safety reasons the Titration Unit TitroLine alpha may only be used for the pur-poses described in the present operating instructions.

The Titration Unit TitroLine alpha is equipped with integrated circuits (EPROMs).These circuits (ICs) can be erased by X-rays or radioactive beams and UVbeams. While UV radiation is fully shielded by the device casing, X-rays or otherhigh-energy radiation may penetrate through the device casing the program to beerased.

When working with liquids other than common titration agents particular attentionshould be paid to the chemical resistance of the materials used for the TitrationUnit TitroLine alpha (ref. to chapter 1.2).

When working with liquids with a high vapour pressure and/or mixed substanceswhich are not referenced as suitable in chapter 1.2, the user is responsible for thesafe and proper operation of the Titration Unit TitroLine alpha.

During the upward movement of the cylinder a microfilm of the dosing liquid will inany case remain on the inner surface of the cylinder which is of no importancewith regard to the dosing accuracy. However, this negligent remainder of liquidmay evaporate, thus penetrate into the zone below the piston and corrode andeven dissolve the materials used there (ref. to chapter 8 „Maintenance and care ofthe Titration Unit TitroLine alpha").

Liquid on theinner surface

112 Chapter 2 Set up and first operation

2 Set up and first operation2.1 Unwrapping and set up of the Titration Unit

TitroLine alphaFunctions and dimensional accuracy of the Titration Unit TitroLine alpha as well asall peripherals are thoroughly checked in the factory.Please pay attention not to leave any of the small accessories in the package.

Packing list: 1 Titration Unit TitroLine alpha1 TZ 1583 low voltage cable for the connection of the TM 125

Magnetic Stirrer resp. TZ 1845 Stirrer1 mains cable1 TitroLine alpha dosing unit (10, 20 or 50 ml)1 TZ 1849 power pack1 „Memory card“ including device software1 Mini keyboard TZ 28251 stand rod support TZ 15161 stand rod TZ 15101 electrode double clamp Z 321

The Titration Unit TitroLine alpha may be placed on any flat surface. Plug themains cable into the cold-device plug on the power pack, then connect the 6-poleDIN plug to the Titration Unit TitroLine alpha. The screw connected has to betightened firmly. Only then should the power pack be connected to the mains!Prior to switching the Titration Unit TitroLine alpha on it has to be ensured that op-erating voltage and mains voltage are identical. The operating voltage is indicatedon the nameplate (see back panel of the Titration Unit TitroLine alpha).

If it is intended to work with a method which is already stored in the Titration UnitTitroLine alpha you may immediately proceed to chapter 5.4.4 <<STD>>.

2.1.1 Installing the „Memory card“The „Memory card" included with the Titration Unit TitroLine alpha has to beinstalled prior to the first operation of the Titration Unit TitroLine alpha. This isdone as follows:

− Separate the Titration Unit TitroLine alpha from the power pack and put it on itsleft side as seen from the front.

− Use a screw driver or a coin to open the two screws of the cover on the bottomof the Titration Unit TitroLine alpha.

− Remove the „Memory card" from its wrapping, and carefully insert it withoutapplying force with the back side (the side bearing the version number) up intothe guide bars.

− WARNING! It is possible to insert the card far enough only in one direction.− After installation attach the cover again with the two screws in order to prevent

the card from falling off.

If no „Memory card" is installed, the Titration Unit TitroLine alpha cannot beswitched on, the display remains dark.

After changing the method card, a RAM test (memory test) is performed after ini-tialization. This may lead to the disclosure of defective Ram modules. In case ofsuch a defect the Titration Unit TitroLine alpha will beep.

Packing listTitroLine alpha

Connection power pack

Important note

Installing the„Memory card“

113Chapter 2 Set up and first operation

2.1.2 Removing the „Memory card“If the Titration Unit TitroLine alpha is to be equipped with a new software version,the old software - contained on the „Memory card" - has to be removed first:− Separate the Titration Unit TitroLine alpha from the power pack and put it on its

left side as seen from the front.− Use a screw driver or a coin to open the two screws of the cover on the bottom

of the Titration Unit TitroLine alpha.− Press the eject key in the smaller opening and seize and remove the card

through the larger opening.The installation of the new card is described in chapter 2.1.1.Wrap up the old „Memory card" and send it to the following address:

SCHOTT-GERÄTE GmbHPostfach 1130D-65701 Hofheim

Password: Titration units

2.1.3 Installation of the stand bar

− The type no. TZ 1516 stand bar support is attached to the bottom plate of theTitration Unit TitroLine alpha using the screw.

− To do so, place the Titration Unit TitroLine alpha on its left side and attach thestand bar support to the bottom. Then screw in the stand bar.

− The magnetic stirrer attaches to the stand bar. The design of the attachment ofthe stirrer is pivoted. Please make sure after installation the fastening screwbetween stirrer support and stand bar points towards the piston burette so thatthis pivoting feature can be fully used.

Removing the„Memory card“

Fig. 1Installation ofthe stand bar


2.2 Replacing the entire dosing unit− Prior to replacing the dosing unit the piston has to be taken to its lowest posi-

tion. To do so, trigger the filling command by pressing the <FILL> key. As soonas the filling command has been executed the piston is in its downmost posi-tion.

− Rotate the retention ring (Figure 2) in such a way that the opening pointstowards the front.

− Now the dosing unit can be easily removed from its guide towards the frontside.

Fig. 2


Slide it to the valve support.

− Another dosing unit can now be installed.

Figure 3


− Subsequently remove the valve support by pulling it upwards. In this way theentire dosing unit, consisting of the top unit, the valve unit, the burette tip andthe reservoir can be replaced without dismantling any tube connection.

Installation− Insert the valve including its support into the valve housing. When inserting the

valve unit make sure that the interlock catch on the valve's axis points towardsthe front.

− Slide on the dosing unit, and close retention ring.− If required, start the rinsing cycle (ref. to chapter 5.5.6).

Fig. 4

Installation ofthe dosing unit


− If a different cylinder size was installed, the unit size has to be entered again(ref. to chapter 5.5.6).

2.3 Replacing the dosing unit− Prior to replacing the dosing unit the piston has to be taken to its lowest posi-

tion. To do so, trigger the filling command by pressing the <FILL> key. As soonas the filling command has been executed the piston is in its downmost posi-tion.

− Subsequently, dismantle the tube connection between the valve and the dosingunit at the valve, then rotate the retention ring so that the opening pointstowards the front side. Now the dosing unit can be easily removed from itsguide towards the front side.

Assembling the dosing unit is done in reverse order:

− A locking protection prevents the unit from being inserted in the wrong direc-tion. Please do not use any force when installing the unit. To adjust it, use thepiston extractor to pull out the piston almost to the lower edge.

− After pressing the dosing unit on a flat surface the piston is set to its properheight, and the dosing unit can be reinstalled easily.

− If required, start the rinsing cycle (ref. to chapter 5.5.6.3). If a different cylindersize was installed, the unit size has to be entered again (ref. to chapter5.5.6.2).

Replacement of a glass cylinder

− First of all the dosing unit has to be removed from the Titration Unit TitroLinealpha as is described in chapter 2.3.

− Then it is possible to loosen and remove the threaded cover cap (refer toFigure 5).

− The cylinder including the piston and the tube can now be removed from theprotective cage.

− Now it is also easy to dismantle the tube, the piston and the UV shield for thepurpose of cleaning or installing spare parts.

Replacingthe dosing unit

Assemblingthe dosing unit

Replacement ofa glass cylinder


1. Threaded cover cap2. Duran burette cylinder

10 ml type no. TZ 128120 ml type no. TZ 128250 ml type no. TZ 1285

3. PTFE piston with piston rod10 ml type no. TZ 127120 ml type no. TZ 127250 ml type no. TZ 1275

4. Centering ring5. UV shield type no.TZ 14306. Protective cage7. Combination of 2 and 3

10 ml type no. TZ 126110 ml type no. TZ 126210 ml type no. TZ 1265

Assembling of the dosing unit is done in reverse order:

− Carefully insert the piston into the glass cylinder from below.− Insert the UV shield into the protective cage. The protective cage will only fit in

one direction into the lower opening, if required it has to be rotated.− Place the cylinder with the protective cage downwards into the protective cage.− Screw on the cover, tighten it by hand.− Adjust the piston height by pressing it on a flat surface.− Push on dosing unit, lock retention ring.− Connect the tube between the valve and the Titration Unit TitroLine alpha.− Start rinsing cycle (ref. to chapter 5.5.6.3).− If a different cylinder size was installed, enter unit size again (ref. to chapter

5.5.6.2).

Caution:As a rule, the tubes and the cylinder will contain chemicals which will drain and/orbe splattered during disassembly. The relevant safety precautions applicable tothe handling of chemicals have to be observed.

Fig. 5Dissambleddosing unit

Assembly ofthe dosing unit


2.4 Combining the Titration Unit TitroLine alpha with otherdevices

The Titration Unit TitroLine alpha can be combined with the following devices:

− printer with RS-232-C interface (serial)− printer with Centronics interface (parallel)− personal computer with RS-232-C interface− TZ 2825 mini PC keyboard, or MF 2 Multifunction keyboard in XT mode− connected balance− Stirrer TM 125 with the enclosed TZ 1583 cable

4

When using the Titration Sample Changer TW alpha, the balance should beconnected at the RS 232 Port no. 2 of the sample changer.

Please notify: If a keyboard, a printer or a balance has been connected withthe TitroLine alpha, the titrator must be switched off and on againto start an initialization of the system.

Functioning is described in chapter 5 „Working with the Titration Unit TitroLinealpha". Please also observe the operating instructions of the devices connected tothe Titration Unit TitroLine alpha.

Device connections

Necessary cables for theconnection of peripheralunits please see fromdrawing below:


During the connection of a peripheral device which itself is supplied withvoltage, both devices must be switched off!

Connecteddevice

Connection onthe Titration UnitTitroLine alpha(Fig. 9)

Used cabletype no.

E x p l a n a t i o n s

Computer, PC RS-232-CComputer

TZ 1599 (2 m)TZ 1589 (10 m)

Data transfer using a suitable terminalprogram. When selecting the cableplease observe length (in brackets).

Printer, serial RS-232-CComputer

TZ 1591 Possibility of connecting printers withRS-232-C interface, note configurationoptions of the printer.

Printer, parallel CentronicsPrinter

TZ 2890Centronics cable

Connection of printers withCentronics interface-EPSON compatible-

TZ 2825 keyboard Keyboard Firmly installedcable

Required for parameterization.

TM 125 orTZ 1845 Stirrer

Stirrer TZ 1583 The stirrer is started at thebeginning of the titration.

Balance RS-232-CBalance

Balancespecification

Check back with SCHOTT-GERÄTEor consult the list in the annex.

Table 1Device connections

121Chapter 3 Structure of the Titration Unit TitroLine alpha

3 Structure of the Titration Unit TitroLine alpha

Fig. 7Complete set up

122 Chapter 4 The connections of the Titration Unit TitroLine alpha

4 The connections of the Titration UnitTitroLine alpha

4.1 Measuring amplifier input / electrode signal

The measuring amplifier input allows to connect one pH/mV electrode to theTitration Unit TitroLine alpha. A maximum of 500 measurement values can berecorded.The measuring input pH/mV can be used to adapt the smoothing of the meas-urement signal in four stages to the requirements of the titration. This is performedusing software commands of the Titration Unit TitroLine alpha.

pH/mV input with 16-bit measurement transducer for highly accurate measure-ment value resolution during tiration and with 4 smoothing stages of the mea-surement signal, electrode socket according to DIN 19 262.

Smoothingstage

Input delay Suitable fortitrationspeeds

Suitable fortitration media

Examples

0 none very fast aqueous, polar acid/base titration in water1 weak fast aqueous, alcoholic acid/base titration in alcohol and weak

acids or bases in water2 medium medium solvents with an

non-polar portiontitrations with ion-sensitive electrodes

3 strong slow non-aqueous,non-polar

TAN, TBN, acid/base titration inhalogenated solvents or aromatics

Input resistance Ri: 1 • 1013 ΩMeasuring range pH: 0.000 ...14.000Excess range pH: - 3.000 ...17.000Measuring range U: - 1900 mV ... 1900 mVThe selectable input delay (set time) causes the measuring signal to besmoothed. For measuring accuracy of 1% the respective set times of the4 smoothing stages are as follows:

0: 0 s1: approx. 0.5 s2: approx. 2.5 s3: approx. 5 s

This means that the input delay causes a delayed reaction time of the input ampli-fier. So it is, for instance, that with smoothing stage 3 (5 s) 99% of the measuringsignal will be received only after 5 seconds. In the case of very intense fluctuationof the measuring values, e.g. at the beginning of a titration, one has to select cor-respondingly long wait time in order to ensure the minimum set time. This meansthat one has to work with a fixed drift control, with the delay time being at least aslong as the respective set time resulting from the selected input delay.Karl-Fischer (dead stop) connector for double platinum electrodes;Output voltage U: 100 mV, internally variable (60...220 mV)Connection: 2 x 4 mm sockets.

Output voltage U: 100 mV (ex-factory set)internally adjustable from: 60 ... 220 mV (adjustable)

Current I: 0.0 ... 100.0 µA

Measuring input temperature-sensor port for Pt 1000 Resistance ThermometerConnection: 2 x 4 mm sockets resp. for N2042 2 mm socketTemperature T: - 75 °C ... + 175 °C

Electr. measuring input

Table 2Input delayMeasuring input pH/mV

KF Measuring input

Pt 1000Measuring input

123Chapter 5 Working with the Titration Unit TitroLine alpha

5 Working with the Titration Unit TitroLine alpha5.1 Multifunction display

HOLD RUN CAL 12

3

4

5

1. Status indicator

2. Display of measured value

3. Dimension/unit display

4. Dialog display

5. Control display

5.1.1 Contrast adjustment

Contrast adjustment to the text display. By pressing of the <ROLL DOWN> or the<ROLL UP> key in the „INIT“ menu, the contrast can be adjusted to the desiredviewing angle.

5.2 Parameterization of the Titration Unit TitroLine alphausing a keyboard

The Titration Unit TitroLine alpha can be parameterized flexibly for various tasks.This requires a mini PC keyboard TZ 2825 or a multifunction keyboard in XTmode.

Usually, there is an „AT/XT" (or PC) change-over switch at the bottom panel of anMF-keyboard. This switch has to be set to the „XT" (or PC) position. In the case ofkeyboards which detect the modus automatically, no setting is required. It is alsopossible to use an other mini PC keyboard as keyboard. In case of doubt the sup-plier will provide information as to whether a particular keyboard meets thisrequirement.

Fig. 8Multifunction display

Contrast adjustmentusing the keyboard

Keyboard MF

124 Chapter 5 Working with the Titration Unit TitroLine alpha

A keyboard which fill fit in every case is the TZ 2825 mini PC keyboard fromSCHOTT-GERÄTE. This keyboard is in membrane design, i.d. splashproof cover.

Fig. 9Keyboard mini PCType TZ 2825


Functions of the keyboardsIn combination with the Titration Unit TitroLine alpha, the keys of the keyboardperform predefined functions, listed on the following table (Figures 2 and 3).

Standard MF2 keyboardorstandard mini keyboard

Mini PC keyboardtype no. TZ 2825from SCHOTT

O p e r a t i o nwith the Titration Unit TitroLine alpha

<F1> <START> *) Start of the displayed method.

<F2> <STOP> *) Cancellation of the method. Cancellation of calibration anddisplay of the calibration values.

<F3> <EDIT PARAM.> Balance data editing.

<F4> <FILL> With <<CALC>> activation and deactivation of transfer parameters.Burette rinsing upon switching on, otherwise filling of the burette.

<F5> <STOREPARAM.>

After pressing this key the final position of the parameterization isreached and the following display appears <<check/store>>.This menu item than can be used to decide whether to store or not.

<F6> <MODE> *) Display of the „MODE“ survey menu to parameterize a method.

<F7> <INIT> *) Display of the „INIT“ survey menu for intitial parameterizationof the Titration Unit TiroLine alpha.

<F8> <CAL> *) Display of the „CAL“ menu for the calibration of the measurementchannels.

<F9> + / - Change in sign at <<titration end>> mV and input, factors,blank value in the <<CALC>> menu.

<ESC> <ESC> *) <ESC> returns you to the previous level.

ROLL DOWN ROLL DOWN *) Within a particular menu, the parameters are scrolled throughbackwards (scroll forward: <ENTER>). Within the menu items:scrooling through the parameters. Selection of the standardmethods on the <<STD>> menu.

ROLL UP ROLL UP *) Within the menu items: scrolling through the parameters.

< → > ← >

Cursor

< → > ← > *)

Cursor

Scrolling within the survey menu to select menu items.Within the menu items: Moving the cursor to select the parameters.Selection of the substances on the <<STD>> menu.

0...9,Decimal point

0...9,Decimal point

Input of method numbers, sample numbers and parameters.

ENTER> or< ↵ >

<ENTER> *) Confirmation of the input parameters. In the present operatinginstructions, both keys are referred to <ENTER>.

<DEL> <DEL> Deletion of an input digit/character under which the cursor ispositioned.

Letters,ASCII characters

Letters,ASCII characters

Alphanumeric input is possible. With a TZ 2825 upper case only.In combination with the MF keyboard upper and lower case.

All other keys No function.

Table 3Keyboard functions


5.3 The menu systemAfter switching on, the system fills and the following display appears:

50.0 ml

size ok? <ENTER>10 20 50 <up/down>

The size of the currently used interchangeable unit has to be confirmed using the<ENTER> key or selected using the <ROLL UP> or <ROLL DOWN> keys,respectively.

You can make a rinsing of the unit by pressing the <FILL> key. The number ofrinsing cycles can be set under the <INIT> item in the „Sys“ menu. To cancelrinsing, press <STOP>.

The highest menu level is the execution level of a method.

Here it is possible to start a titration using the <START> key. The <ROLL UP> keyand the <ROLL DOWN> key can be used to select the next method. Onlyactivated methods can be started or displayed.A method is activated by storing it on the „MODE“ menu.The bottom line shows the name of the method (if such a name exists).

<START>/<up/dwn>

1Mth

This menu set up is particularly user-friendly, since after switching on the methodlast used prior to switching off is always immediately available.

On the execution level any number can be entered. Only numbers between01 and 08 are permitted.

However, only „memorized" methods can be started, otherwise the following dis-play will appear for 3 seconds:

Mth1

<START>/<up/dwn>Mth. not pres.

After this error message, method no. 1 is displayed.

With the <↑↑↑↑> and <↓↓↓↓> keys you can move the head of a connected samplechanger up- or downwards. This may make sense, for instance, after cancelling amethod, prior to starting a new titration.

Fig. 10Execution level

Method number input


<START>/<up/dwn>

PASSW SYS CNTRYTIME COPY CAL RS

LIST PRN MEASMTH CALC DOC STD P1: 7.00 <START>

P2: 4.00

MODE INIT CAL

ESC ESC ESC

7.00 pH

CAL

1Mth

Mth1

Menu „MODE“ Menu „INIT“ Menu „CAL“

Possible input for the Titration Unit TitroLine alpha

The multifunction display of the Titration Unit TitroLine alpha requests the input ofmissing data and parameters via the front panel keyboard or a connected XT orMF keyboard. The system can be parameterized by simply selecting parametersfrom displayed menu lines, and this parameterization is even easier by selectingfrom approx. 100 standard parameters which are preset for various titrations.

All dialogue parameterization steps are included in the inquiry loop. The parame-ters are inquired and input by way of a dialog. Owing to the fact that the dialogueis arranged as an inquiry loop, one always returns to the starting point, i.e. „losingone's way" is excluded.

Scrolling forwards is done by pressing the <ENTER> key, scrolling backwardsrequires the <ROLL DOWN> key to be pressed. Modified data are taken over bypressing the <ENTER> key; if input data are not to be taken over, they can bedeleted by pressing the <ROLL DOWN> key.

Fig. 11Switching over

the menu levels

Possible input

<ENTER><ROLL DOWN>


5.4 „MODE“ menu

After pressing the <MODE> key, the following input menu will be displayed:

Mth CALC DOC STDLIST PRN MEAS

1Mth

Using these menu items it is possible to select methods from the existing pa-rameter sets and to adapt them to the desired requirements, to edit existing meth-ods and to create own ones, to enter calculation parameters, to select documen-tation parameters, and to output method listings, results, and data. The desiredmenu item is selected with the < ←←←← >, < →→→→ > cursor keys. The selected menu itemis confirmed by pressing the <ENTER> key.

5.4.1 <<Mth>> menuThis menu item can be used to edit the current method.

− Inquiry of the standard presettings which are valid for all types of titration(5.4.1.1)

− Selection of the titration types (5.4.1.2)

5.4.1.1 Standard parameters

After pressing the <ENTER> key the following image will appear on the display.The number of the selected method will appear in the unit display of the measurement-value display (Mth and number 1 to 8).

Mth1

change method yes no

If the selected method is to be modified, use the < ←←←← >, < →→→→ > cursor keys to setthe cursor under <<yes>>, and confirm with <ENTER>. Now it is possible tocheck and, if required, modify the method parameters. If all parameters are ed-ited,

Mth1

methodtest / store

will be displayed.

Important note If it is intended to work with a method which is already stored in the Titration UnitTitroLine alpha you may immediately proceed to chapter 5.4.4 <<STD>>.

Fig. 12„MODE“ menu

<<MTH>> menu

Change methods


If the modifications are to be taken over, the cursor must be positioned under<<store>>, followed by a confirmation using the <ENTER> key. If the parametersare to be checked again, leave the cursor under <<test>> and press the<ENTER> key.

As an alternative to repeatedly pressing the <ENTER> key the end position of theparameterization can also be reached by pressing the <F5> or<STORE PARAMETER> key, respectively. To store the data, the <<store>>menu item has to be selected and confirmed with <ENTER>.

Important note: If, when on the „INIT“ <<SYS>> menu (chapter 5.5.6.8):

SYSINI

Edit STD method on off

the selection is <<off>>, it is actually not possible to modify the titration parame-ters as such. In this case only the method name, the weighed-in quantity, or thesample volume menu items. Afterwards the system automatically proceeds to themethod <<test/store>> (see above).

Mth1

method name __

Here it is possible to enter a 16-digit alphanumeric method name.

Mth1

select weightwght. vol. none

Do you wish a weighed-in quantity or a volume within the method?

<<wght>> = weighted-in quantity

Mth1

weight auto man fix

If <<auto>> is selected, the transferred balance data of a connected balance willbe inquired automatically upon the start of the method (see chapter 5.7 „Edit ba-lance data“).

With <<man>> the display of the Titration Unit TitroLine alpha will ask for thebalance data upon the start of the method. The balance data have to be enteredmanually.

In the case of <<fix>> the display will appear:

Mth1

mth. wght. [g] 0.00000 <ENTER>

The input mass will be used for every titration within the method.If selected, a value has to be entered here. If no value is entered, 1.0 will besubstituted in order to avoid a division by zero in the calculation.

Storing methods

<STORE PARAMETER>

EDIT STD method

Enter method name

Weight/volume

Manual weighing-in

Fixed weighing-in


<<vol.>> = volume:

Mth1

volume man fix

After starting the method, if <<man>> is selected, the operator is asked for thesample volume on the display of the Titration Unit TitroLine alpha. The samplevolume has to be entered manually.

If <<fix>> is selected, the display appears:

Mth1

mth. vol. [ml] 0.0000 <ENTER>

The input sample volume will be used for every titration within the method. If se-lected, a value has to be entered here. If no value is input, 1.0 will be substitutedin order to avoid a division by zero in the calculation.

The originally weighted-in quantity or the volume will be taken into account in thecalculation if the formula contains a „Q". The originally weighted-in quantity or thevolume, respectively, will then be multiplied by the factor „Q" (see chapter 5.4.2„<<CALC>> menu“.

The next display will be:

Mth1

titration modepH mV pHstat KF

5.4.1.2 pH titration

<<pH>> will cause a pH titration. The following display appears:

Mth1

input delay no medium

If you move the cursor < ←←←← > the following screen will appear:

Mth1

input delay medium strong

This parameter is used to set the response time of the input amplifier. This optionis particularly useful in the case of titration of aqueous solutions with a high ohmresistance, e.g. titration in non-aqueous solutions.

The individual stages represent the following delays (for 99% signal modification):none: the signal will not be delayedweak: the signal will be delayed by approx. 0.5 smedium: the signal will be delayed by approx. 2.5 shigh: the signal will be delayed by approx. 5.0 s.See chapter 4.1 „Measuring-amp card/electrode input".

Volume

Volume entered manually

Volume fix

Titration mode

pH titration

Input delay


The next selection is to define an increasing or decreasing titration.

Mth1

direction tit.increase decrea.

Mth1

predosing? yes no

Mth1

predos.. bur. [Ad] 1 <ENTER>

Mth1

predos. vol. [ml]10.0000 <ENTER>

You can connect a burette (e.g. TITRONINC® 97) to the Titration UnitTitroLine alpha for predosing a certain volume. Reverse titration would be a typicalexample for this. First you select predosing. In the second step you enter the ad-dress of the predosing burette. The final step consists of the output of the pre-dosing volume. By cable TZ 3095 a Piston Burette TITRONIC® 97 can be con-nected to the interface „balance“ of the Titration Unit TitroLine alpha.

The following menu item is used to specify whether pretitrating is to be performed.

Mth1

pre titration ? yes no

If pretitration is intended, the system will ask for the volume to be pretitrated.Pretitration is intended to add a larger dosage volume at one time, and to acceler-ate or optimize titration. The added dosage volume will be taken into account inthe result of the titration volume.

Mth1

pre tit. vol. [ml] 0.0000 <ENTER>

The next menu item defines the criterion for the titration end:

Mth1

titration end ml EQ+pH EQ+ml

Direction titration

Predosing

Pretitration

Pretitration volume

Titration end, criteria


If you move the cursor < ←←←← > the following screen will appear:

Mth1

titration endEQ+ml pH+ml all

and this screen will appear:

Mth1

titration endpH EQ ml EQ+pH

<<pH>> titration endThis menu item is used in pH titration to select various end criteria as a function ofthe pH value.

Mth1

tit. end [pH]pH 1endpt 2endpt

If <<pH>> is selected, the titration will be performed until an input pH value isreached. This kind of titration is used, for instance, if the course of the titration isknown and overtitration is permitted. Likewise, a safety function can be included incombination with other end criteria.The desired pH value is input in the following menu item:

Mth1

tit. end [pH] 11.000 <ENTER>

If <<1endpt>> is selected, titration to one predefined end point will be performed,i.e. titration is completed as soon as the pH value entered as end point is reached.This kind of titration is subject to rigidly defined rules and can only be influencedexternally by the type of the anticipated titration jump.

The end points titration are as follows:

Mth1

tit. endpt. 1 [pH] 11.000 <ENTER>

In the case of <<2endpt>>, titration will be performed to two predefined endpoints. This should be used for instance for p + m titrations. Both these types areautomatically controlled by the intensity of the anticipated titration jump. In thiscontext a selection out of five jump magnitudes has to be made for EP1 and EP2,respectively:

Mth1

EP1 : jump1 2 3 4 5

<<pH>> titration end

Input pH value

End point titration1 end point

End point titration2 end points


The settings are appropriate for the following applications:

Jump typeselection

Curve type Example Risks in case ofincorrect curve selection

1 steep jump HCl to NaOH Overtitration with differentparameters

2 medium jump Ethanoic acidto NaOH

1: titration too slow≥ 3: overtitration

3 weak jump Ethanoic acidto NH4OH

titration too slow

4 strongly bufferedsystems

highly carbonate-containing waters

titration too slowtoo many measurement points

5 Special applications Switch off automatic mode and replace by linear titra-tion

End point titration is not only controlled in dependence of the slope of the curve,but also by the distance to the set end point (pH). The smaller the distance to theend point, the smaller the individual dosing steps.

The last parameter inquired in connection with EP titration will be a delay time.The respective input end point has to be exceeded or reached over this period oftime in order to end titration.

Mth1

Ep delay 0-99[s] 3 <ENTER>

If two end points are to be found, this wait time applies to both end points.

Titration end <<EQ>>

If <<EQ>> is selected, an „equivalence titration" will been performed. This titrationwill continue until a certain number of equivalence points has automatically beenfound. The number of equivalence points to be searched for prior to the cancella-tion of the titration can be selected in the following menu item:

Mth1

number EQ1 2 3 4 5

Up to five „equivalence points" can be determined. Titration is ended as soon asthe specified number of EQs has been found. It is recommended to combine thiscriterion with other cancellation criteria. The following applies as a principle: Theflatter the jumps are and the higher the number of equivalence points is, thegreater is the risk that minor disturbances in the titration curve will lead to the can-cellation of the titration.

The number of calculated equivalence points and the related formulae are definedin the „Calc“ menu item.

End point titrationdelay time

Titration endequivalence point

Numberequivalence point


The following menu item is used to specify the sensitivity for the search forequivalence points:

Mth1

EQ sensitivity 1 2 3 4 5

Step Curve shape Example

1 very weak jump acetic acid next to hydrochloric acid

2 weak jump chloride in trace range, Ca/Mg mit ISE

3 medium jump phosphoric acid, both jumps

4 normal intense jump HCI/NaOH

5 very intense jump Redox-titration with very intense jump -CSB-

When working with high equivalence-point sensitivity, the „noise" alone can causethe abortion in the case of unsteady titrations!

NOTE: It is in any case recommended to combine this kind of titration with asecond cancellation criterion (e.g. pH or ml). This avoids overtitration or spillingover of the titration container if the number of found equivalence points is lowerthan the number of set equivalence points.

Titration end <<ml>>

<<ml>> is selected if a specified volume is to be titrated. This end criterion ismainly used as a safety function, for instance to avoid spilling over of the titrationcontainer.

Mth1

tit. end [ml]50.0000 <ENTER>

End of titration <<EQ + pH>>End of titration <<EQ + ml>>End of titration <<pH + ml>>End of titration <<all>>If a combination of various end criteria is selected on the menu, the titration will becancelled as soon as one criterion is fulfilled.If <<all>> is selected, all end criteria for pH, EQ and ml will be inquired.

If the titration end was defined, the control of the titration and the speed will be pa-rameterized.

Mth1

drift control fixed fast

Equivalence pointsensibility

Table 5Sensibilty stepstitration EQ


Combination ofend criteria

Drift control


If you move the cursor to the right the two other drift parameters will be displayedas well:

Mth1

drift control medium exact

The drift control ensures the quality of the measurement values. Owing to therespective drift control, the selected parameters <<fast>>, <<medium>>, <<ac-curate>> influence the duration of the titration process, i.e. an „accurate" driftcontrol will produce a more stable measurement value and thus a higher measu-ring accuracy on the one side, but also a longer measurement duration on theother.

If <<fixed>> is selected, a wait time is preset manually. The wait time defines thebreak between the dosing steps.

The wait time is input on the next menu item:

Mth1

delay 0-99 [s] 1 <ENTER>

The kind of titration control, i.e. linear or dynamic, is selected on the next menuitem:

Mth1

tit. control lin. dyn.

<<lin>> will cause the titration to be carried out in constant dosing steps, irrespec-tive of the change of the measured signal. The added dosage volume will alwaysremain constant. The desired volume is input in the next menu item:

Mth1

linear [ml] 0.0100 <ENTER>

Chapter 6.2 contains a titration curve with linear titration control.

If <<dyn>> is selected, dynamic titration will be performed. In this case the dosedvolumes of the individual dosing steps differ. The step width depends on therespective measurement-signal change. As a result, for instance, a minor mea-surement value change will cause a greater dosing step. This means that thevolume to be dosed doubles with a stable measurement value, always up to themaximum volume (of 0.3 ml). If a major measurement value change occurs,dosing continues with the minimum volume (0.02 ml). This feature allows dynamictitration to be much faster than linear titration since the dosing volume is alwaysoptimally adapted to the curve gradient.

Chapter 6.2 contains a titration curve with linear titration control.

<<fast>><<medium>>

<<exact>>

<<fixed>>

Delay time input

Linear titration control

Dynamic titration control


In the case of dynamic titration, four dynamic stages can be selected. This is donein the menu item:

Mth1

dynamic step 1 2 3 4

In the stages <<1>>, <<2>>, <<3>> preset parameters are used which haveproved effective in practice and experience with the TPC 2000 and the Titration-Controller TC 1200 computer titration system.

Dynamic step Application Example

1 usual pH titrations withmedium and strong jumpsmany mV titrations

HCI with NaOH

chloride with AgNO32 titrations with medium

or several jumpsHCI + acetic acid with NaOHor chloride + bromide with AgNO3CI in small quantities, iodometric titration

3 flat jumps at pH titrations(at special applications)

4 explicit statement at someSGH applications

In stage <<4>> the user can define and optimize parameters. It is possible to inputparameters for the „slope character" and the „dosage emphasis":

Mth1

dynamic para.SAP 0.150 <ENTER>

This parameter is referred to as „slope character". 0.1500 is an example.

The second parameter which is decisive for dynamic control is referred to as„dosing emphasis". It is entered as follows:

Mth1

dynamic para. DBP 0.850 <ENTER>

This parameter completes the parameterization for pH titration.0.8500 is an example.These parameters may be indicated in exemplary applications.

Dynamic parameters: The abbreviations used areSAP for „slope character"DBP for „dosing emphasis".

5.4.1.3 mV titrationFor a mV titration in analogy to pH titration. Compared to pH titration there aredifferences with regard to the titration end:

No end-point titration is possible. Only one mV end value can be entered.

Dynamic steps

Table 6Dynamic steps

Slope characterSAP

Dosing emphasisDBP

Titration mode <<mV>>


5.4.1.4 Karl-Fischer titrations

If the <<KF>> type of titration is selected, a different parameterization is required.The desired type of conditioning is selected from the following menu:

Mth1

KF conditioningstby. y per.no

<<Stby.>> In the case of KF titration it is possible to perform a „standby“ condi-tioning. In this case conditioning will always be performed if the value falls short ofthe set value. A titration can only be started in the conditioned state. If the cursoris used to select <<stby>> and this selection is confirmed by pressing <ENTER>,the menu will show:

Mth1

KF stby. condit. single endless

If you select <<single>> on this menu, the Titration Unit TitroLine alpha will startconditioning following start-up.

Mth1

KF stby. condit. single endless

In this stage conditioning can be completely cancelled using the <ESC> key in the„endless“ mode. As long as the value is exceeded the following message will bedisplayed:

Mth1

KF stby. condit.finishing <STOP>

If <STOP> is pressed in this stage, conditioning will be finished:

Mth1

KF condit. rdycontinue <START>

At this point „standby“ conditioning can be completely finished by pressing the<STOP> key. If <<START>> is pressed after the addition of the sample, the titra-tion begins.

Note:After finishing „standby“ conditioning the cylinder will be filled first. Prior to starting,one should wait until this filling process is completed. Subsequently the titrationwill be peformed like a normal KF titration.

Caution:If <<endless>> has been selected, „standby“ conditioning will resume immediatelyafter the results have been printed. In this mode a printer must be connected,otherwise the titration results will be lost. Likewise, no checking up of the resultswill be possible if „statistics“ was selected.

Titration mode <<KF>>

Conditioning selection

„Standby“ conditioning

„Single“ conditioning


If <<yes>> is selected, the titration proceeds until the desired µA end value isreached, i.e. the cell is „dry".

Mth1

KF condi ready continue <START>

If <<no>> is selected, KF titration up to the selected end point will be performeddirectly, i.e. without previous conditioning.

In the case of a <<perman.>>ent conditioning, titration is continued until the de-sired end value is reached. This end value is maintained until the <STOP> key ispressed.

This end value is selected in the following menu item:

Mth1

KF value [µµµµA] 10 20 30

In order to define the cancellation criterion for ending the titration, the next menuitem is used to set the time over which the selected measuring value has to bereached or exceeded, respectively (99 s max.).

Mth1

KF delay [s] 10 <ENTER>

The control parameters of the automatic control are set:

Mth1

KF step control 1 2 3 4 5

In the case of Karl-Fischer titration both predosing as well as pretitration are pos-sible. No other control parameters require setting.

KF Regulationstep

Application

1 samples with normal water content; unitary system

2 samples with low water content: unitary system

3 sample with normal water content but increased water release;unitary system and two-component system

4 samples with normal water content; two-component system

5 samples with low water content; two component system

„yes“ conditioning

Permanent conditioning

KF end value µA

KF end point delay

Table 7KF control step


5.4.1.5 pH-stat titrationsIn the case of pH-stat titration, a pH value (set value) is kept stable.

The first part of parameterization is similar to parameterization for a pH or mVtitration. Subsequently, the value to be kept stable is inquired.

Mth1

pHstat value 7.000 <ENTER>

The next menu will ask for an <<addition>>. This means that titration will be inter-rupted after reaching the set value for the first time (exceeding for a time of 2 s(seconds) and that it then is possible to enter a manual addition.

Mth1

pHstat add. vol. no man

If <<none>> is selected, the value will be kept stable immediately upon reachingthe set value.

With <<man>>, titration will stop upon reaching the set value, and a manual addi-tion can be made. Titration continues by depressing the <START> key.

The time basis for the measurement interval time is inquired in the next menu:

Mth1

pHstat interval sec min h

The time has to be entered at this point (max. 9999).

Mth1

interval [sec] 5 <ENTER>

The measurement-interval time refers to the wait time to be observed betweentwo measurement-value recordings. Titration control and additional dosing are in-dependent from this time.

The time basis for the overall titration time is inquired in the following menu:

Mth 1

pHst total time sec min h

The time has to be entered at this point (max. 9999).

Mth1

time length [sec] 60 <ENTER>

When selecting and coordinating these times one has to take into account that amaximum of 500 measurement values can be stored. If this limit is exceeded,titration is aborted.

pH-stat titrations

pH-stat value

pH-stat addition volume

pH-stat measurementinterval

pH-stat total time

pH-stat end point titration


In order to avoid overtitration during initial titration up to the set value, initial titra-tion is controlled in analogy to end-point titration. The required selection is made inthe following menu:

Mth1

adjust pHst jumphigh med low

The parameters for the pH-stat addition control the quantity and speed of the ad-dition in dependency on the reaction speed, the quantity of the nascent protonsand the buffering characteristics of the systems.

Mth1

pHstat control 0 1 2 3 4 5

If the accuracy of pH constancy is to be superior to pH = 0.1 units, only half asmuch protons can be neutralized with a 0.1 mol/l NaOH than in the case of apH constancy < 0.2 pH. The following table shows the dependency on the controlstages.

pH Constancy pH Constancy

Control stage ∆ pH < 0.1 ∆ pH < 0.2

1 max. 0.05 mMol H+-ions/min max. 0.1 mMol H+-ions/min



4 max. 1 mMol H+-ions/min max. 2.5 mMol H+-ions/min


Stage 0 is used to define the smallest proton quantities in unbuffered systems. Inthe case of stage 0 a 100 ml dosing unit has to be used in order to be able to dosethe required volumes.

The next menu item is used to set in terms of seconds (max. 9999) the timespecified between the start of a method and the start of titration (stirring time 1).To ensure a good mixture of the titration solution, stirring starts as early as duringthis wait time.

Mth1

wait. time 1 [s] 10 <ENTER>

At the same time the piston burette will be filled. If the filling time is lower than thethe wait time 1, the remaining time will be shown on the display:

7.000 pHwait. time 1 25s please wait

The wait time 2 (max. 9999 s) starts running after a possible pretitration.

7.000 pHwait. time 2 25s] please wait

pH-stat end valueinitial titration

Table 8pH-stat control steps

Wait time 1

Wait time 2


In the case of pH and ml titration it is possible to record the measurement valueprior to the start of pretitrating; this means that after the lapse of wait time 1 thesystem will wait until the measurement value has stabilized. During this time thedisplay will look as follows:

7.000 pHmV. value drift please wait

This measurement value can also be output during documentation. In the case ofpH, with a connected Pt 1000 sensor, the start and end temperatures will also berecorded. This function can be switched on or off in the <<DOC>> menu item.

If only the measurement value of a sample is to be determined, i.e. without titra-tion, this is possible. To ensure that a stabilized measurement value is read in,<<yes>> has to remain selected in the DOCU on the „automatic start-valuerecording" menu item.

After starting titration the wait time 1 will elapse, subsequently the system will waituntil the pH value has stabilized. The respective measurement value is recorded.

By selecting wait time 1 it is possible to obtain a thorough mixing of the solutionprior to the start of the recording of the measurement value. Wait time 2 should beset to 0, since it starts after the measurement value has stabilized. Otherwise themeasuring time would be prolonged. It is not possible to pretitrate.

5.4.1.6 Sample changer applications:The use of a Sample Changer TW alpha is to be parameterized as follows:

sample changer?yes no

If <<yes>> is selected you are asked to enter the plate size:

TW table size12 16 20 24 30 a

When starting the method the Titration Unit TitroLine alpha is programmed for theselected plate size. If a CSB titration is to be performed, select <<a>>. If <<a>> isselected, the Titration Unit TitroLine alpha asks the sample changer for the usedplate size. To enable this inquiry the Sample Changer TW alpha must be set tothe plate size and plate type on the back panel, i.e. to "CSB". These parametersettings take the height difference between CSB containers and beaker glassesinto account.

pH and mVmeasurement value

Measurementwithout titration

Sample changerapplications


Subsequently, the starting position of the sample plate is set:

TW start pos.1 <ENTER>

If the number of samples to be processed is always the same, it can be prede-fined as <<firm>> within a method; if the occurrence of samples varies perma-nently, the number will be inquired as <<variable>> after each start of themethod.

TW no. samplesvariable fixed

If <<fixed>> is selected, the number of samples is inquired.

TW no. samples1 <ENTER>

The next menu item is used to inquire the number of desired rinsing positions.The last three plate positions can be selected as rinsing positions. If, for instance,2 rinsing positions are desired with a 16 sample plate, positions 15 and 16 arerinsing positions.

TW no. rins. pos.0 1 2 3

If rinsing positions are actually selected, the next menu item will ask for the rinsingtime which has to be entered in terms of seconds (max. 99 s).

TW rins. time [s]10 <ENTER>

When connecting a Rinsing Unit TP 18 to the Sample Changer TW alpha there is- in addition to the three rinsing positions described above - the possibility of rins-ing the measuring sensor and burette tips at the titration position.

TP rinsing unit?yes no

If rinsing is to take place at the current titration position - i.e. the sample on whichtitration is completed - select <<yes>>.

TP rins. time [s]1 <ENTER>

The next menu item is used to set the cleaning time in terms of seconds:(max. 99 s).

Caution: The rinsing liquid will spill over the titration containerif the rinsing time is too long!


Stirring speed

Note: Adequate mixing of the sample prior to the start of titration hasa direct influence on the titration result!

When using a Sample Changer TW alpha the stirring speed is set as follows:

stirring speed0 1 2 3 4 5 6 7 8 9 10

Ten stirring speed options are available.

The next menu item is used to set in terms of seconds (max. 9999) the timespecified between the start of a method and the start of titration (stirring time 1).To ensure a good mixture of the titration solution, stirring starts as early as duringthis waiting time.

wait. time 1 [s]10 <ENTER>

At the same time the piston burette will be filled. If the filling time is lower than thewait time 1, the remaining time will be shown on the display:

wait. time 25splease wait

The subsequent stirring time 2 (max. 9999 s) starts running after a possible pre-dosage or titration. It is used to ensure an adequate mixture of the added solu-tions.

wait. time 2 [s]10 <ENTER>

Caution: With a Sample Changer TW alpha with a stirrer, a minimum stirringtime of 15 seconds should be set from below, since this stirrer has a"start-up time" of approx. 10 s. Likewise, when using high CSB con-tainers, the minimum stirring time should be determined by way ofexperiment.

In the case of pH and ml titration it is possible to record the measurement valueprior to the start of pretitrating; this means that after the lapse of stirring time 1 thesystem will wait until the measurement value has stabilized. During this time thedisplay will look as follows:

m. value driftplease wait

This measurement value can also be output during documentation. In the case ofpH, with a connected Pt 1000 sensor, the start and end temperatures will also berecorded. This function can be switched on or off in the <<DOC>> menu item.

Stirring speed

Minimum stirring time


5.4.1.7 Automatic invocation of a methodThe following menu can be used to enter the number of the method to be startedautomatically upon termination:

next method no. xx <ENTER>

If 0 is entered, no subsequent method will be started.

If the input is a number from 1 to 08, the respective method will be invoked upontermination of the current method. In combination with the transfer memories, thismakes it possible to perform complex courses of methods.

Example: Titer determination and subsequent measurements with the SampleChanger TW alpha, taking into account the previously determined titer, multipledeterminations including their statistical evaluation.

Caution: It has to be ensured that the method invoked has been "activated" orcreated by way of storing. Otherwise unforeseen performances mayoccur, for instance going back to the first method. When working withthe sample changer the automatic work with further samples thereforeis not secured.

5.4.1.8 Recording of measurement values without titrationIf the measurement value of a sample is to be determined without titration, thiscan be done by selecting titration end <<ml>> in the creation of the method. Thetitration will be finished immediately without addition of a solution. The use of aSample Changer TW alpha is possible.

In order to make sure that a stabilized measurement value is read in, <<ja>> (yes)must remain selected in the DOKU at the "wait start value".

After the start of the titration the stirring time 1 will elapse. Upon the lapse of thistime the system will wait until for example the pH value has stabilized. Subse-quently, the respective measurement value will be stored. In this way, and in com-bination with a TZ 280 Sample Changer, it is possible to to determine the pH ormV value and the temperature for entire measurement series.

Selecting the stirring time 1 will cause the solution to be well stirred prior to thestart of the take-up of the measurement value. Stirring time 2 should be set to 0,since it will run off only after the stabilization of the measurement value and wouldotherwise only prolongate the measuring time.

Automatic invocationof a method

Recording ofmeasurement valueswithout titration


5.4.2 <<CALC>>

5.4.2.1 Calculation of resultsThis menu item can be used to edit the processing parameters for the currentlyselected method. The cursor is placed under <<CALC>>. After pressing the<ENTER> key the following display will appear:

Cal1

change calculat. yes no

If a calculation is to be performed or if the calculation parameters of the selectedmethod are to be edited, place the cursor under <<yes>> and press <ENTER>.The following display will appear:

Cal1

calculation <ESC> edit RUN

<<Edit>> is selected.

If a calculation is to be performed using measurement data which were alreadyrecorded, place the cursor under <<RUN>> and confirm this selection with the<ENTER> key. If the calculation formulae are to be edited, place the cursor under<<EDIT>> and confirm with <ENTER>. If neither editing nor calculating is to beperformed, leave the menu by pressing the <<ESC>> key.

Now it is possible to check and, if required, modify the calculation parameters.Scrolling forward can be done using the <ROLL DOWN> key. Modified data willbe taken over by pressing the <ENTER> key, <ROLL DOWN> can be used forscrolling backwards; if the entered data are not to be taken over, they can bedeleted by pressing the <ROLL DOWN> key.

The following parameters are available for calculating the results:

Note: Depending on the method created<<EP>> will appear in the case of end-point titrations<<EQ>> will appear in the case of equivalence-point titrations<<ml>> will appear in the corresponding formula in the case of all other

titrations

1. Number of equivalence points. Use the < ←←←← > , < →→→→ > cursor keys to select thenumber from the following options:

Cal1

Number of EQ0 1 2 3 4 5

2. On the following menu one of the permanently preset calculation formulae canbe selected using the <ROLL UP> or <ROLL DOWN> key:

Cal1

select <up/dwn>* (EQ1*F*F2)/Q

<<CALC>> menu

Calculation of results

Change calculation

Calculation <<Edit>>

Number ofequivalence points

Choice ofcalculation formulae


For orientation purposes, the first calculation formula is marked with a * on the leftmargin.

3. The abbreviations used in the formulae have the following meaning:

ml = ml; here, calculation is continued with the determined ml valuesEPn = EP1 to EP2; the respectively found end point in terms of mlEQn = EQ1 to EQ2; the respectively calculated equivalence point in

terms of mlF = Factor 1 (multiplicative)F2 = Factor 2 (multiplicative)C = Factor 3 (multiplicative)Q = Quotient; is automatically multiplied by the respective weighed-

in quantity or preset weight in the calculationB = Blank value (additive)

The formulae are: (example for an endpoint titration):

Formula 1: (EQ1 • F • F2) / QFormula 2: (EQ1–B) • F • F2 / QFormula 3: (EQ[n] – EQ [n-1]) • F • F2 / QFormula 4: (B – EQ1) • F • F2 / QFormula 5: Q • F /((EQ1–B) • F2)Formula 6: (F • F2) / EQ1Formula 7: (B • C – EQ1 • F ) • F2 / QFormula 8: (Stg • F • F2) / QFormula 9: C • EQ1 – F • EQ2 • F2 / QFormula 10: C • EQ2 – F • EQ1 • F2 / Q • (EQ1 • F • F2) / QWith two end points for EP2, the following formula can be used for the limereserve:Formula 11: (((EP2 – EP1) • F) – B) • F2 / Q

Note:Formula 3 can only be selected if the number of EP/EQs is greater than 1.

Formula 5 can only be selected if EQ = 0.

Formula 8 applies to pH-stat titrations only.

In the case of pH-stat titrations one may choose only between formula 1

and formula 8.

In the case of formula 1 Epn will be substituted by ml.

EQ is replaced by EP in the case of endpoint titration.

Meaning of theabbreviations used inthe calculation formulae

Content of thecalculation formulae


Example no. 1:EQ1 = 4.376 mlWeighted-in qty. = noneF = 0.25F2 = 1Q = 0.1Selected formula = formula no. 1: EQ • F • F2 / Q

4.376 • 0.25 • 1= _____________ = 10.94

0.1Example no. 2:EP1 = 11.245 mlWeighted-in qty. = 2.3478 gF = 0.1F2 = 1.002Q = 0.8B = 24.98 mlSelected formula = formula no. 4: (B - EP1) • F • F2 / Q

(24.98 - 11.245) • 0.1 • 1.002= _______________________ = 0.733

0.8 • 2.3478

Cal1

input unit: <ENTER>

4. A 6-digit unit can be entered in alphanumeric form and in capital and small let-ters.

Cal1

input name: <ENTER>

5. An 8-digit name can be entered in alphanumeric form and in capital and smallletters.

Calculation examples

Input unit

Input name


Depending on the number of selected equivalence points, the result formulae,formulae parameter, unit, and name can be inquired up to two times.

In the case of a pH-stat titration, an inquiry will be made at this point to knowwhether a measurement-value optimization is to be performed prior to the calcula-tion of the result.

Cal1

pHst. calc. optim. yes no

If <<yes>> is selected, the measurement values will be subjected to an arithmeticoptimization. Depending on the number of measurement values involved, therequired calculation time may be up to several minutes.

The following parameters will be output as result of the pH-stat titration:

Slope [ml/s] corresponds to the speed of proton formation(= reaction speed)

Ordinate section [ml] corresponds to the consumption of base required toneutralize the free acid of the sample

Correlation coefficient shows whether the data form a straight line. A valuebetween 0.95 and 1.00 is usually a reliable indication ofa straight line.

Initial RMS-value shows the degree of smoothness of the compensationstraight line. A small RMS value means a smoothcurve. The initial RMS corresponds to the value whenall measurement points are considered.

Number of points used shows the number of the measurement points used forcalculation. In the case of an optimization, the numberof the measurement values considered may be smallerthan the number of the available measurement values,since measurement „freak values" are omitted.

Optimized RMS value shows the value after the omission of the measure-ment „freak values".

Subsequently, it has to be specified whether the calculation of the titration resultsis to be made using the smoothed or the „raw" data.

Cal1

smoothing? yes no

The raw data are not lost here.

The number of digits following the decimal point can be selected using the nextmenu.

Cal1

decimal places1 2 3 4 5 6 7 8

Three decimal places are preset; it is, however, possible to specify up to 8 decimalplaces for special applications.

In the documentation the factors are always shown with 6 digits, weighted-inquantity and pattern with 5 digits each.

pH-stat optimization

pH-stat titrationresult parameters

Smoothed data

Digits


5.4.2.2 Statistic functionIf a measurement series is to be evaluated statistically, this is specified in the fol-lowing menu:

Cal1

statistics yes no

If <<yes>> is selected, the kind of statistical processing can be specified in thefollowing menu item.

Cal1

choice of stat.avg. std. vari

<<avg:>> Averaging is performed.

<<std:>> An average will be calculated, and the standard deviation isdetermined in addition.

<<var:>> This option performs a calculation of average value, standarddeviation and, in addition, of the variation coefficient (in termsof % VC).

The number of values to be statistically evaluated can be specified in the followingmenu item:

Cal1

statistic nos. 2 <ENTER>

Here the minimal number for the average value is 2, and at least 3 values have tobe specified for the standard deviation.

In the case of individual measurements, each started by pressing <START>, thecorresponding calculation will be performed upon reaching the <<statistic num-ber>>.

IMPORTANT! To document the statistical evaluations, a printer or PC must beconnected. A subsequent documentation of the individual values is no longer pos-sible.

The Titration Unit TitroLine alpha is equipped with a memory for up to 30 sampleresults. This memory can be deleted using the following menu. This is necessaryat the beginning of a measurement series.

Cal1

statistic new yes no

If <<yes>> is selected, the memory will be deleted.

Statistics

Averagestandard deviation

variation coefficient

Statistic number

Statistic new


5.4.2.3 Storing transfer parametersThe Titration Unit TitroLine alpha offers the possibility of working with up to5 transfer memories. These transfer memories can be accessed from anymethod. This means, they are not specific to a certain method. Invoking thetransfer memories is done in the <<CALC>> menu in the following menu item:

Cal1

result - > memoryno 1 2 3 4 5

If <<no>> is selected, no transfer memory is defined. If the cursor keys are usedto select one of the <<M1 M2 M3 M4 M5>> memories, the calculated result willbe copied into the selected transfer memory at the end of a titration. If the statis-tics function has been activated, it is always the respectively new calculated aver-age value which will be copied into the selected transfer memory.

An assignment of a result or average value, respectively, will be marked by thefollowing symbol during the printout of the results “ > „.

When calculating several EPs or EQs, the result of the EP or EQ last calculatedwill be assigned to the selected memory.

5.4.2.4 Assigning transfer parametersThe transfer memories can be assigned to the factors, quotients, and blankvalues. To do so, the <Fill> key (TZ 2825 mini-keyboard) has to be pressed in thecorresponding menu item. With a MF keyboard this is done by pressing the <F4>key. The following menu will appear:

Cal1

Factor: F =M1 M2 M3 M4 M5

The desired transfer memory is selected using the < →→→→ > or < ←←←← > cursor keys.

If a memory assignment is to be deleted, this is done by pressing the <Fill> key inthe case of the TZ 2825 mini-keyboard or the <F4> in the case of a MF keyboard,respectively.

The assignment of a transfer memory to a factor, quotient, or blank value will bemarked by „Mx" in the documentation.

If more than one EQ or EP is selected, the assignment of a transfer memory in thecalculation formula is possible to the last EQ or EP only.

After all parameters have been entered, the following display appears:

Cal1

calculationtest / store

Transfer memories

Global memories

Assigning transferparameters

Deleting thememory assignment

Calculationtest/store


5.4.2.5 Checking up

<<test>> has been selected. If the modifications are to be taken over, the cursorhas to be positioned under <<store>>, followed by a confirmation with the<ENTER> key. If the parameters are to be checked again, leave the cursor under<<test>> and press the <ENTER> key. All menu items can be checked again. If<<store>> was selected, the display will appear again:

Cal1

calculation <ESC> edit RUN

and the calculation can be started by pressing <<RUN>>. During the calculationthe following display is shown:

Cal1

calculation RUN please wait

If the desired number of EPs was calculated, the display

Cal1

calculation OKresult end rep.

will appear. Using the < ←←←← > and < →→→→ > cursor keys, one of the menu items canbe selected. The selected menu item is activated by pressing the <ENTER> key.Returning to the „MODE“ menu can be done by pressing the <ESC> key.

Cal1

calculation OKresult <up/dwn>

<<Result>> = the calculated results can be displayed by pressing<ROLL UP> or <ROLL DOWN>.

<<End>> = the calculation mode is exited, the „MODE“ menu will be dis-played.

<<rep.>> = the <<Edit RUN>> display is shown again. The calculationparameters can be modified again, or the calculation canbe restarted.

If the calculation of the desired number of equivalent points was impossible, thefollowing message will be displayed:

Cal1

calc. ERROR <ESC>no. calc. EQ <EQ>

Checking-up in<<CALC>>

<<RUN>>

Display results

Calculation errors


If the following message appears in the course of a pH-stat titration, the number ofmeasurement values was to small.

Cal1

calc. ERROR <ESC>not enough pts.

After confirmation with the <ESC> key the following display is shown again:

Cal1

calculation OKresult end rep.

5.4.3 <<DOC>>This menu item is used to select the parameters to be printed in a protocol. Withthe basic setting all parameters are set to output. The menu item is selected usingthe < ←←←← >, < →→→→ > cursor keys. After pressing the <ENTER> key the followingquestion appears:

Doc1

change document. yes no

If the documentation parameters of the selected method are to be edited, use the< ←←←← >, < →→→→ > cursor keys to place the cursor under <<yes>>, followed by pres-sing the <ENTER> key. You will be asked:

Doc1

sample ident. yes no

This point is used to define whether a sample designation (sample identification)is to be assigned. If this is the case, the cursor has to be positioned under<<yes>>, followed by pressing the <ENTER> key.

After entering the sample designation the documentation items are completed.The printout of the protocol will contain all items marked with <<yes>>, as far asthese items were considered within the method.

Doc1

method number:output: Y N

The cursor is positioned under <<Y>> (yes) or <<N>> (no), depending on whetherthe parameter is to be output or not.<<Y>> = output, <<N>> = no output.

Error message:not enough pointspH-stat

Documentation<<DOC>>

Change documentation

Documentationsample designation

Documentationmethod number


A selection can be made from the following parameters:method number: number of the methodmethod name: name of the methodsample ident.: sample designationdate/time: date and timeweight: sample weight [g]volume: sample volume [ml]pre-tit. vol.: volume which was pretitratedtitration vol.: volume which was titratedcalibration dates: electrode parameters and date of the last calibrationcal user name: name of the person performing the last calibrationelectrode ID: electrode identification descriptionresults: printout of the fully calculated resultsCALC parameters: calculation parameters of the selected

calculation formulastart value: this item is used to specify whether a starting

measurement value is to be recorded in the case ofa pH or mV titration

data/graphics: output of the titration data or of a graphic chartmethod head: output of one out of 5 freely selectable method heads

The menu item

Doc1

data / graphicsoutput: Y N

is used to select the output of either data or a graphic chart.If <<yes>> is selected here, the following display will appear:

Doc1

choice output data graphic

If <<graphic>> is selected, the next menu item will ask for the type of graphicchart:

Doc1

choice outputml 1st deriv. t

<<ml>> will cause the output of a graphic chart showing the ml on the X axis andthe respective measurement value on the Y axis.

If <<1st deriv.>> is selected in the case of an EQ titration, the output will show theml on the X axis and the first derivation on the Y axis.

The <<t>> option shows the time on the X axis and the measurement values onthe Y axis.

<<Data>> requires no further parameterization.

Documentation,content, choice

Documentationdata/graphics

Documentationchoice data/graphic

Documentationgraphic

Output of the graphic


Except for the selection of the method head, all settings are made using the cur-sor only. The following menu item can be used to select and enter one out of5 freely selectable method heads of 5 lines each (each line 16 characters long).From each method, the respectively set method head will be accessed, e.g. 5-linemethod head no. 2.

ATTENTION! The heads are not specific for certain methods, but generally valid.

Doc1

method head no 1 2 3 4 5

If <<no>> is selected, no method head will be output.

If one of the 5 method heads is selected, the following prompts will appear:

Doc1

head no.: 1r:1 __

This item can only be used to describe the respective head (X) and its correspon-ding line (x). All 5 lines have to be acknowledged by pressing <ENTER>.

The standard setting of all documentation parameters is „YES", with the exceptionof „data/graphic chart". Since a data/graphic chart output can involve long print-outs, this output has to be specifically set to „YES" in order to reduce paper con-sumption and to save time during protocol preparation.

After all parameters are entered the display

Doc1

documentationtest /store

is shown. <<test>> is selected. If the modifications are to be taken over, the cur-sor has to be positioned under <<store>>, followed by a confirmation with the<ENTER> key. If the parameters are to be checked again, leave the cursor under<<test>> and press the <ENTER> key. All menu items can be checked again. If<<store>> was selected, the „MODE“ menu will be displayed after saving.

5.4.4 <<STD>>

This menu item can be used to select a parameter set from a number of standardparameter sets. Upon pressing the <ENTER> key the unit display will show<<STD>> together with the number of the selected standard parameter set. Thedialogue display will ask you with the following screen to select a group:

STD10

acid base mVpHstat KF ?

This screen is used to select the respective titration group. If you have decided ona certain group, confirm your decision with the <ENTER> key.

Documentationmethod head

Store documentation

Standard parameter sets<<STD>>

Group selection


Group definition:

<<acid>> An acid is to be titrated.<<base>> An alcaline solution is to be titrated.<<mV>> A mV titration is to be performed.<<KF>> A Karl-Fischer titration is to be performed.<<?>> You can scroll through all groups.

At this point it is also possible to directly select a standard parameter set via thekeyboard. To do so, enter the corresponding number, followed by a confirmationwith the <ENTER> key. The first example name of this titration will then be shownon the following menu screen:

STD10

next meth. (<-/->)hydrochlor. acid

Here you can use the < ←←←← > < →→→→ > cursor keys to scroll through the entire group.The unit display will show the standard parameter number corresponding to thename.If one is at the end of a group the following message will appear for about2 seconds:

STD10

next meth. <-/->)! end of list

Here it is also possible to select a parameter set by entering the number directly.Confirm with <ENTER> after having selected a parameter set. The following menuwill appear:

STD10

->work. method no. _store <ENTER>

This menu is used to enter the method number of the desired working method un-der which the standard method is to be stored and possibly further edited.8 working methods are available. If a specific working method is already occupied,this will be indicated by an acoustic signal and the number you input will bedeleted. You have to enter a different number. If no free working method is avail-able you have to delete one (ref. to chapter 5.5.2.2 „Deleting a method" and tochapter 6.2 „Titration of an unknown acid“).

5.4.5 <<LIST>>This menu item allows to print out different information of the methods:

<<list>> Output of a list of the stored methods<<content>> Output of the selected (actual) methods<<STD>> Output of the methods stored under <<STD>>

Mth1

output methodlist content STD

The <<RS>> or <<Centronics>> output destination is specified in the <<PRN>>menu item.

Standard parameter setsdirect selection

Standard parameter setselection with cursor

Standard parameter setsstored in methods

Output under <<List>>


5.4.6 <<PRN>>This menu item can be used to output various method parameters. After selectingthis menu item and pressing the <ENTER> key, the following display will appear:

Mth1

output viaRS centronics

This item is used to specify the output destination. Output can be done via thebuilt-in Centronics or RS-232-(Computer) interface. After selecting the output in-terface, the following display will appear:

Mth1

choice sourceres. gra. docu. TW

This menu item is used to select the data to be output. The following data can beoutput:

<<Res.>> Results including designations and units.

<<Dat.>> The list of the measurement points of the titration curve if <<DOC>><<Dat.>> has been selected.

<<Doc.>> The documentation list selected under <<DOC>>.

<<MR.>> Output of all results of a method at statistic.

ATTENTION! Does not apply to statistical processing! The statisticaldata will be lost here. If a statistical evaluation is to be performed, aprinter or PC has to be connected and documentation has to be doneusing <<results>> or <<Doc>>.

<<Gra.>> Output of a graphic if <<DOC>> <<Graphic>> has been selected.

Mth1

Auswahl Graphik ml 1st Abtlg. t>

At this point the desired graphic presentation can be selected irrespective of thesetting in the <<DOC>> menu. This selection does not influence the graphics set-ting selected in <<DOC>>.

After selecting the output-data source and pressing the <ENTER> key, the datawill be transmitted. Upon completion of the transmission, the following display ap-pears:

Mth1

transfer finished <ESC>

After pressing the <ESC> key, the menu „MODE“ appears again.

Print

Output via <<PRN>>

Output data

<<Res.>>

<<Dat.>>

<<Doc.>>

<<MR.>>

<<Gra.>>

Transfer finished


5.4.7 <<MEAS>>This menu can be used for „on-line" measurements. The menu items

select modepH mV µµµµA temp

will be shown. The desired measurement range (measuring channel: pH, mV, mAand temperature) is selected using the < ←←←← >, < →→→→ > cursor keys and confirmingwith the <ENTER> key. The <<take measurement>> function is left by pressingthe <ESC> key.

5.5 „INIT“ menuAfter pressing the <INIT> key on the execution level, the input menu is displayed:

PASSW SYS CNTRYTIME COPY CAL RS

In this „Init“ menu you can rinse the interchangeable unit of the Titration UnitTitroLine alpha by pressing the <FILL> key. The number of rinsing cycles can beset in the „Sys“ menu. To cancel rinsing, press <STOP>.

5.5.1 <<TIME>>This menu item is used to set the internal clock. The hour is inquired first. It canbe entered via the keyboard. A space or full stop must be included between theindividual input items. If nothing is to be changed, the <ENTER> key will take youstep by step down to the basic menu. Only valid input will be taken over; in case oferroneous input the initial value will appear. The input mode can be left by press-ing the <ESC> key.

5.5.2 <<COPY>>This menu item is used to copy or delete methods. The desired function has to beselected from the menu.

The selection menu provides the following commands:

5.5.2.1 Copy methodThe * on the left margin marks the following function:

function<up/dwn>*COPY No. -> No.

In the function <<COPY No.> No.>> the following menu is shown:

COPY No. X toNo. __ <ENTER>

Instead of __, the method number into which the method X is to be copied has tobe entered. X is always the current method. Copying can only be performed to un-occupied methods.

„On-line“ measurements

Fig. 13„INIT“ menu

Time setting with<<TIME>>

<<COPY>> menu

<<COPY>> menuselection

Copy method


The following display appears during copying:

COPY active

5.5.2.2 Delete method

If the <<delete no.>> function is selected, the following menu will appear afterdepressing the <ENTER> key:

DELETENo. _ <ENTER>

The first method number shown is the current one. However, this method can beoverwritten by the method number 1 to 8 to be deleted. After acknowledgement ofthe number with the <ENTER> key the following menu item appears:

delete No. XAre you sure?

If you are certain to delete number X, acknowledge it with <ENTER>; if not, leavethe menu using the <ESC> key. The following display appears during deletion:

delete active

5.5.3 „CAL“ menuThis item can be used to define the validation parameters for electrode calibration.After pressing the <ENTER> key, the following display will appear:

CALINI

change CAL/VAL yes no

If the curser is placed under <<yes>> and <ENTER> is pressed, the buffer valueswill be inquired:

CALINI

buffer1 <up/dwn>pH= 7.00 <ENTER>

This item can be used to select the desired buffer out of 8 options using the<ROLL UP>, <ROLL DOWN> keys. 8 buffers are firmly predefined. 3 additionalbuffers can be freely defined as described in paragraph „input of freely definablebuffer values“. After acknowledging the selected buffer with <ENTER>, the sec-ond buffer can be selected.

CALINI

buffer2 <up/dwn>pH= 4.00 <ENTER>

Delete method

„CAL“ menu

Selection of buffer values


The temperature courses of the buffers are memorized in the Titration UnitTitroLine alpha.

pH = 2.99 4.01 7.00 10.004.00 6.87 9.18 12.45

Please note that the selected buffers must have a minimum distance of 1.5 pHand that one and the same buffer is not selected twice. The order defined herehas to be observed in a subsequent calibration. Next, the temperature compensa-tion will be inquired:

CALINI

temp. comp. auto man

<<man>> can be used to set the temperature at which the titrator will perform apH measurement without temperature sensor. 25 °C are preset. When using aTemperature Sensor (e.g. Pt 1000) a temperature compensation will be per-formed automatically.

CALINI

man temp. [°C] 25.00 <ENTER>

The next item is intended to define important data for validation:

CalINI

CAL validationY 2Pt N Res

<<Y:>> With this option a pH method can only be started after a valid calibra-tion has been performed. Single-point calibration is not possible.

<<2-Pt:>> Only a 2-point calibration will be allowed, however, the start of amethod is always possible.

<<no:>> No validation and no other restrictions.<<Res:>> The calibration data are set to the ex-works settings.

Zero point: pH = 7.00Slope: 98%Buffer1: pH = 7.00Buffer2: pH = 4.00

The following menu item can be used to enter the name of the person(16 characters) calibrating the Titration Unit TitroLine alpha.

CALINI

CAL User Name __

For the next question you can type in an alphanumeric identification of the elec-trode with 16 characters.

CalINI

electrode ID __

The next menu item can be used to enter up to three freely definable buffers. Thebuffers entered will later on appear in addition to the firmly programmed buffers.

Temperaturecompensation

Automatic temperaturecompensaton

Validation of thecalibration

Identificationof the electrode

Input of three freedefinable buffers


CALINI

Input bufferno No1 No2 No3

If <<1>>, <<2>> or <<3>> is selected, the buffer values for the buffer temperaturetable will be inquired.

CALINI

bu.No.X inp. 0 °CpH = 0.00 <ENTER>

Subsequently, the pH value of the buffer will be inquired starting with 0 °C. Thebuffer pH values are inquired in increments of 5 °C (0 °C to 95 °C).

Although it is not necessary to enter the entirety of the pH values of the buffer, thefollowing points should be observed:

− In order to enable the Titration Unit TiroLine alpha to recognize that a newbuffer is to be added, the 25 °C value of the buffer has to be entered.

− In addition, the pH values above and below the future measurement tempera-ture, at which calibration is to be performed, have to be entered. Example:Calibration temperature is 15 °C. The values to be entered now are the 10 °C,15 °C and 20 °C as well as the 25 °C pH values of the buffer.

− All prompts have to be acknowledged by pressing <ENTER> (even if nopH values are entered), until the menu item <<buffer input>> appears again.In order to continue with the „CAL“ menu, use the cursor to collect <<no>> onthe <<buffer input>> picture after the input is completed and the temperaturecourse is memorized.

CALINI

CAL validation test finishing

This item can be used to decide whether the input is to be tested again, orwhether the input is completed.

5.5.4 <<RS>>This menu item is used to parameterize the RS-232-C interfaces. Both interfacesRS-232-(balance) and RS-232-(computer) can only be parameterized with identi-cal parameters.

The first option is to select the baud rate. The selection is made using the < ← >,<→→→→> cursor keys.

RSIni

RS baud rate 1200 2400 4800

Buffer temperature table

Store Cal validation

Parameterization of theRS-232-C interfaces

<<RS>>baud rate


Afterwards the remaining parameters can be selected from four predefined sets.

RSIni

WortStopPARI<up> 7 2 No

Word = data bit; Stop = Stop bit; Pari = parity

Set 1: <<7 2 No>>Set 2: <<8 2 No>>Set 3: <<7 1 Even>>Set 4: <<8 1 Even>>

In the following menu the address is used to set the device’s address.

RSIni

RS address xx <ENTER>

This address will be leading when the RS-232 interface is used for printing.This completes the configuration of the two RS interfaces.

5.5.5 <<PASSW>>

If desired, this menu item can be used to protect the 3 main menus, i.e. „MODE“,„INIT“, and „CAL“ by a password in such a manner that these menus can only becalled up if the user knows the respective password. If the current passwordshould be „lost", there is a „Master" password which can be used to restore theforgotten password. If necessary, the „Master" password can be obtained fromSCHOTT-GERÄTE.

The following prompt asks whether a password should be activated:

active password: yes no

If <<yes>> is selected and confirmed by pressing the <ENTER> key, the desiredpassword can be entered. The input menu can be left using the <ESC> key. If apassword is entered here, a maximum of 8 alphanumeric characters are available.From this time on, the menus can not be reached without password. If <ENTER>is pressed, the Titration Unit TitroLine alpha reports <<active password>> andreturn to the „INIT“ menu. And if the „INIT“ menu is left again, the password hasto be entered in order to return into the menu.

To delete the password, press the <INIT> key.

input password---------- <ENTER>

Enter the password and confirm with <ENTER>. If an incorrect password is en-tered, <<wrong password>> will be displayed. Afterwards, the Titration UnitTitroLine alpha returns to the basic menu. By pressing the <INIT> key, a new at-tempt has to be made. If the correct password has been entered, the „INIT“ menuwill be displayed. Again, the cursor has to be used to select <<PASSW>>, fol-lowed by a confirmation with the <ENTER> key.

The input request is displayed again and the current password has to be enteredagain.

<<RS>>data bit; stop bit; parity

<<RS>> address

<<PASSW>> menu

Active password

Password input


passwordchange delete

If <<change>> is selected here, this item will request to check the old passwordor to enter a new one.

change password________ <ENTER>

If <<delete>> is selected, you will be asked:

delete password yes no

In case of <<no>> the system returns to the „INIT“ menu.

If <<yes>> is selected, the following display appears:

password deleted

All menus can now be accessed without restrictions.

5.5.6 <<SYS>>Some specific device parameters are adjustable under this menu point.

5.5.6.1 <<BEEPER>>This menu item is used to switch the acoustic signal on and off. You are asked:

SYSIni

Beeper on off

If <<on>> is selected, an acoustic signal will sound with each key stroke.If <<off>> is selected, the acoustic signal will only sound in the case of erroneousoperation and input. This warning signal can not be switched off.

5.5.6.2 Select interchangeable unit sizeThis menu item can be used to select the size of the interchangeable unit if thecheck unit function was disabled. Since the Titration Unit TitroLine alpha is notequipped with an automatic unit-size detection, the current size has to be set aftera change of the unit.

SYSIni

dosing unit vol. 10 20 50

The selection is made using the < ←←←← > and < →→→→ > keys and confirmed with the<ENTER> key.

5.5.6.3 Number of rinsing cycles

Deleting the password

<<SYS>> menu

<<Beeper>

Select interchangeableunit size


This menu item is used to select the number of rinsing cycles or to start rinsing,respectively.After a change of the interchangeable unit, or for the purpose of filling a cylinder,the piston has to draw in the liquid first, so a „rinsing" routine is required.

− The piston will first move upwards; at this time the valve will be in the „dosingposition“. Subsequently, the contents of the cylinder (air or old reactant) will beejected.

− After arriving at the top position the valve will be switched over to the „filling"position. This is when the filling process begins, with new reactant being drawnin.

− To ensure that the hoses are free of air, rinsing should be performed twice. Aslong as the rinsing routine is running a waste-liquid container has to be placedunder the titration tip.

− This process will be repeated in accordance with the input number.

SYSIni

repeat rinsing 1 <FILL/ENTER>

Input number of rinsing cycles, maximum 9. After pressing the <FILL> or, in thecase of a MF keyboard, the <F4> key the Titration Unit TitroLine alpha will start toprocess the preselected number of rinsing cycles. The <ENTER> key will take youto the next menu.

Please note: The first-fill or filling program is not suitable for changing titrationagents, reactants, or liquids which are considerably different with regard to theircomposition and/or concentration. Such cases require thorough cleaning.

5.5.6.4 Select main display

This menu item is used to select the contents of the large measurement valuedisplay (main display) during titration.

SYSIni

main displayvolume meas.val

If you select <volume> here, the measurement value display will show the dosedvolume, while the dialogue display will show the measurement value. If you select<meas. value>, the measurement value display will show the measurementvalue, while the dialogue display will show the volume.This selection does not affect the display of the results after the completion of a ti-tration process.

5.5.6.5 Select unit check function

This menu item is used to specify whether the interchangeable unit has to be con-firmed after each power-up. If a Titration Unit TitroLine alpha is frequently usedwith different interchangeable units, the unit check function should be kept active.If always the same interchangeable unit is used, the unit check may be deacti-vated.

SYSIni

dos. unit check on off

<<Number ofrinsing cycles>>

Rinsing routine

Select main display

Unit check function


With <<on>> the following menu will be displayed after each start-up:

ml50.0

size OK? <ENTER>10 20 50 <up/dwn>

If the volume displayed corresponds to the volume of the interchangeable unit,use the <ENTER> key to get to the execution level. If the volume has to bealtered, this can be done using the <ROLL UP> or <ROLL DOWN> keys, respec-tively.

If you press the <FILL> key while on this menu, the Titration Unit TitroLine alphawill initiate the rinsing process (ref. to chapter 5.5.6.3).

5.5.6.6 Automatic filling

This menu item is used to specify whether the burette is supposed to fill automati-cally after the completion of a titration.

SYSIni

fill at tit. end on off

If you select <<on>> here, an automatic filling process will occur at the end of atitration (time benefit).

In the case of sample-change methods, too, filling of the burette is performed atthe end of the titration.

If you select <<off>>, the piston will stop in any position, and filling will only occurafter the start of the next titration.

5.5.6.7 Editing <<STD>> methods

In the case of a method selected from the <<STD>> standard methods menu thebasic parameterization can only be changed with regard to the method name anda weighed-in quantity or a sample volume. All the remaining parameters areblocked in order to prevent inadvertent changes in the method parameters. Ifsome of these parameters are actually to be changed, this block can be lifted upon the following menu item by selecting <<on>>.

SYSIni

Edit STD method on off

From that point on all the parameters of the method can be freely edited. How-ever, if you should make a mistake or an unintentional change, you can still returnto the standard method. The standard method always remains unchanged. Youcan make the required changes in one of the 8 standard methods.

If <<off>> is selected, only the name, the weighed-in quantity or sample volumecan be edited.The <CALC> or <DOC> parameters can be changed at any time.

This point was the last one of the <<SYS>> menu. Press the <ENTER> key to getback to the „INIT“ menu.

Unit check on

Automatic filling

Editing<<STD>> methods


5.5.6.8 Setting the filling timeIf the viscosity or the vapour pressure of the liquid to be dosed is too high, thefilling time has to be adjusted appropriately. Filling times between 30 s / 100%filling volume and 999 s / 100% filling volume are possible. As a rule a filling speedreduction to 30 s / 100% filling volume will suffice.

SYSINI

filltime s30.00 <ENTER>

Warning! The set filling time depends on the selected method. This is valid for allmethods.

5.5.6.9 Setting the dosing speedThe maximum adjustable dosing speed per minute corresponds to twice thedosing volume of the dosing unit used, e.g. 100 ml / min in the case of a 50 mldosing unit. Depending on the dosing unit used dosing speeds from 0.01 ml / minto 100 ml / min can be input.

SYSINI

dosspeed ml/min100.00 <ENTER>

Warning! Setting the dosing speed is independent of the selected method. Thisis valid for all methods.

5.5.7 <<CNTRY>>

The <<CNTRY>> item is used to select the devices „language“. Several lan-guages are available, among others: German, English and French. The desiredlanguage is selected using the <ROLL UP> or <ROLL DOWN> key and con-firmed with the <ENTER> key.

language <up/dwn>english <ENTER>

If a new language is selected here, it will take about 3 seconds until the TitrationUnit TitroLine alpha starts working again. The display shows:

language Init please wait

Subsequently the display text and the documentation will be in the selected lan-guage.

CAUTION: If the Titration Unit TitroLine alpha is switched off during language ini-tialization, it may happen that two languages are active in later use. If this is thecase, a new language has to be selected again, in order to subsequently activaterespectively initialize the initially desired language.

<<CNTRY>> menu

Language selection


5.6 „CAL“ menu

Pressing the <CAL> key takes the Titration Unit TitroLine alpha to the calibrationmode.

The measurement value display will show the current buffer, and the text displaycontains the following message:

P1: 7.00 <START>P2: 4.00

7.00 pHCAL

The electrode has now to be immersed into buffer 1, followed by pressing the<START> key. The following message will appear:

CAL 7.00 pHcalibration P1 please wait

If the pH value was identified for buffer 1, but the value is not yet stable, the follo-wing message will be displayed:

CAL 7.00 pHbuffer 1 stable please wait

After the first buffer is accepted, you are requested:

CAL 4.00 pHrinse electrode + in P2<START>

If a single-point calibration is desired, the <Stop> key has to be pressed here. Inthis case the next two menu points are omitted. In the case of a single-point cali-bration only the zero point will be corrected, the slope will remain as it is.

If a 2-point calibration is to be performed, the electrode has to be rinsed and sub-sequently be immersed in buffer 2. After pressing the <START> key the followingmessage will appear:

CAL 4.00 pHcalibration P2 please wait

If the pH value was identified for buffer 2, but the value is not yet stable, the follo-wing message will be displayed:

CAL 4.00 pHbuffer 2 stable please wait

<CAL> calibration mode

Figure 14Calibration mode

Start calibration

Single-point calibration

2-point calibration


If the determined calibration data are o.k., the display will show:

calibration o.k.

Subsequently, zero point, slope, and, again, the basic menu will be displayed.

Warning! The chosen buffer selection can be modified on the „INIT“ menu.

5.7 Edit balance data5.7.1 UseIt is possible to use the keyboard to view and edit balance data on the display.This function is only active if the initially weighed-in quantity was set to <<auto>>(= automatic) in the <<MTH>> method:

Mth1

weight auto man fix

The function „EDIT PARAMETER“ is selected by pressing the key on the menustart <EDIT PARAMETER>:

Bal edt

Balan(AD): 1 of 12weig. = g

The bracketed abbreviation following <<balance>> indicates the selected editingmode. If <<1 of 12>> is displayed, this indicates which memory position wasselected and how many memory positions are occupied.Example: <<3 of 8>>, <<wght. = 1.02103 g>> means that 1.02103 g were input inthe third memory position and that a total of 8 positions are being occupied.

If no balance data are present the following display will appear:

Baledt

Balan(AD): 0 of 0weig. = 0.00000 g

At this point it is possible to use the keyboard to input balance data, or havebalance data taken over via the RS interface if a balance is directly connected.This means that the Titration Unit TitroLine alpha can be used for titration withoutthe necessity of entering balance data when working off methods.

5.7.2 Edit function <<(AD)>>

The individual functions are selected using the <ROLL UP> or <ROLL DOWN>key. You can use the <<(AD)>> (= adding) function to enter balance data one byone in the data memory of the Titration Unit TitroLine alpha. Each input value willautomatically be attached to the existing list. While entering a value, the followingdisplay will appear:

Baledt

Balan(AD): new 1weig. = 1.21 g

Confirm the value with the <ENTER> key.

Edit balance data

<EDIT PARAMETER>

Balance data adding<<(AD)>> Edit function


Baledt

Balan(AD) : 1of 1weig. = 1.21345 g

You may enter further balance data. The other three edit functions require at leastone balance datum.

5.7.3 Edit function <<(IN)>>

The <<(IN)>> (= insert) function allows you to insert data in any position in anexisting list of balance data. Use the cursor key to move to the position where youwish to insert a new balance datum.

Example: You wish to insert another value in a list of 5 balance data between the3rd and the 4th value. Press the cursor <↑> or <↓> key until the display shows3 of 5. You select the <<(IN)>> function using the <ROLL UP> or<ROLL DOWN> key.

Baledt

Balan(IN): 3of 5weig. = 1.23456 g

Now you enter a value (e.g. 2.5678). which has to be confirmed with <ENTER>key. All the following balance data will be moved to the positions 5 and 6. The fol-lowing screen will be displayed:

Baledt

Balan(IN): 3of 6weig. = 2.56780 g

The list is now made up of 6 values.

5.7.4 Edit function <<(OW)>>

Using the <<(OW)>> (= overwrite) function it is simply possible to overwrite thebalance values without changing the order of the values. By pressing the cursorkey <↑↑↑↑>, <↓↓↓↓> the corresponding balance date can be selected.The <<(OW)>> function is selected with the <ROLL UP> and <ROLL DOWN>keys. The following screen will be displayed:

Baledt

Balan(OW): 3of 6weig. = 2.56780 g

This value can be overwritten. Confirm your input with the <ENTER> key.

5.7.5 Edit function

The <<(DL)>> (= delete) edit function can be used to remove existing values froma list of balance data. By pressing the cursor key <↑↑↑↑>, <↓↓↓↓> the correspondingbalance date can be selected. The <<(DL)>> function is selected with the<ROLL DOWN> or <ROLL UP> keys:

Baledt

Balan(DL): 3of 6weig. = 2.56780 g

Pressing the <ENTER> key will delete the value displayed. All other values abovethe deleted value in the list move will one position downwards. After deletion, the

Balance data inserting<<(IN)>> Edit function

Balance data overwriting<<(OW)>> Edit function

Balance data deleting<<(DL)>> Edit function


system will automatically change to the <<(AD)>> mode in order to avoid inad-vertent deletion of further values:

Baledt

Balan(AD): 3of 5weig. = 1.23456 g

In our example only 5 values are left in the list.

5.8 Error messages5.8.1 Titration error messages

balance interface balance data ?

Possible error causes should be checked in the following order:

− Are balance data saved in the Titration Unit TitroLine alpha?− Are RS-232-C transfer parameters of the balance correct?− Is a balance connected to the Titration Unit TitroLine alpha?

If these possible error causes can be excluded, the defective Titration UnitTitroLine alpha should be returned to the Application Laboratory of SCHOTT-GERÄTE GmbH.

5.8.2 Calibration error messages

ERRORwrong buffer

This occurs if the selected buffer does not correspond to the buffer solution usedduring calibration.

ERROR adjustment time

The electrode's set time is too long (> 1 min.) In such a case the electrode has notbeen soaked in water or is too old.

ERROR temp. drift

Temperature was not yet stable during calibration. Observe the tempering time ofthe measurement sensor! If necessary, use a temperature measurement sensorwith a shorter setting time or adapt the temperature difference respectively.

Error messages:balance data

Calibration:error message

wrong buffer


adjustment time


temperature drift

170 Chapter 6 Method creation

6 Method creation using the Titration UnitTitroLine alpha

The present chapter describes the method creation in practice. Based on selectedapplication examples you will find a description of how to proceed in the creationof method with regard to the individual steps of titration parameter, calculationformula and documentation.

6.1Titration of a strong acid (sulphuric acid)6.2Titration of an unknown acid6.3Chloride determination in potable water6.4Water determination according to Karl-Fischer in a solvent extract6.5pH-stat titration in soil samples

Every application example contains a detailed description of the individual menuitems of the TitroLine alpha. Please read the other examples as well, even if youare only interested in example 6.1.

Attention: A graphic printer has to be connected with the Titration UnitTitroLine alpha.

6.1 Titration of sulphuric acidTitration of sulphuric acid with caustic soda will serve as an application example. Itwill be shown how you can very easily create a method using the preset standardtitration parameters without having any previous experience in this sector.

After switching the TitroLine alpha on you are on the start menu or on the execu-tion level of a method, respectively. Pressing the <MODE> key will lead you to the„MODE“ menu:

Mth1

MTH CALC DOC STDLIST PRN MEAS

On this menu you use the cursor to select the <<STD>> menu and press the<ENTER> key to get to the next level:

STD10


You wish to titrate an acid? You select the <<acid>> menu:

STD10

next meth. <-/->)hydrochlor. acid

The first item appearing on the screen will be <<hydrochloric acid>>. Press thecursor until <<sulphuric acid>> appears.

STD10

next meth. (<-/->)sulphuric acid

Titration of a strong acid

„MODE“ menu

<STD> menu

Sulphuric acid

171Chapter 6 Method creation

Confirm your selection with the <ENTER> key. You now will be prompted underwhich working methods the parameter for sulphuric acid are to be stored:

STD10

->work.method no. _ store ENTER>

Enter 1 and confirm with <ENTER>. The parameters will now be stored in theworking method 1. Subsequently you will be back on the „MODE“ menu:

Mth1


The titration parameters are preset. In theory you would now be able to start titra-ting. However, it is both sensible and necessary to create a calculation formulaspecific to sulphuric acid. Use the cursor to select the <<CALC>> menu, confirmyour selection with the <ENTER> key.When you are asked:

Cal1


you use the cursor key to select <<yes>>.You will be asked whether a new calculation is to be performed:

Cal1

calculation (ESC). edit RUN

Confirm <<Edit>> with the <ENTER> key. You will be prompted for the number ofequivalence points (EQs) to be calculated. Since only one equivalence point is an-ticipated in the case of sulphuric acid, use the cursor key to select <<1>>:

Cal1

Number of EQ 0 1 2

The next thing to be selected is the calculation formulae:

Cal1

select. (up/dwn)* EQ1*F*F2/Q

You confirm this formula with the <ENTER> key. This formula can also be used totake into account sample volumes or the weighed-in quantity. You can now enterthe factors to be used for the calculation of the sulphuric acid one after another. Inthis example the calculation of the concentration is to be performed in terms ofmg/l.Conc. NaOH: 0.1 mol/lNormality NaOH: 0.995Factor H2SO4: 4.9 mgConversion factor to 1 liter: 1000

Working method

Input ofcalculation formulae

Number ofequivalence points

Selection of thecalculation formula


You then proceed to the following combination:

1 ml NaOH 0.1 mol/l correspond to 4.9 H2SO4.The conversion factor 1000 and the factor for the H2SO4 are combined to thefactor 4900.

Now you enter the numeric values one after another:

Cal1

Factor: F =4900 <Enter>

Cal1

Factor: F2=0.995 <Enter>

Cal1

quotient: Q=1.0000 <Enter>

Cal1

input unit:mg/l <Enter>

Cal1

input name:H2SO4 <Enter>

Cal1

smoothing? yes no

Cal1

decimal places1 2 3 4 5 6 7 8

Cal1

statistics yes no

Cal1

result -> memoryno 1 2 3 4 5

Factors inputCalculation H2SO4

Input unit

Input name


Cal1

calculationtest / store

After selecting <<store>> and confirming with the <ENTER> key you can leavethe calculation menu by pressing <ESC>. Press <ESC> again and you are backon the start menu of the Titration Unit TitroLine alpha.

− Connect the pH electrode− Fill the dosing unit with NaOH− Pattern the sample, and dilute it with distilled water− Start titration by pressing the <START> key:

Mth1

<START> / (up/dwn)sulphuric acid

So what is happening now? Titration will continue until the equivalence point hasbeen found. The result is calculated and printed on the connected printer. You willobtain a rather extensive printout which is preset in the <<DOC>> output. Theprintout will look as follows:

Start methodsulphuric acid

.....method number 1 method: sulphuric acid

titration start: 14:42:36 12.08.94 titration end: 14:44:19 12.08.94

titration volume: = 5.0600 ml

calibration data time/date: 20:20:20 20.20.20 slope: 98.0 % zero point: pH = 7.00 name: electrode ID:

start value pH =2.189 start temperature =25.0 °C end temperature =25.0 °C

titration results

EQ 1: 6.744 pH 4.9956 ml CALCULATION parameter smoothing: no factor =4900.000000 factor 2 =0.995000 quotient =1.000000 according formula 1: EQ1*F*F2/Q > H2SO4 = 24356.0 MG/L

Figure 15Standard printout

documentation


The documentation contains, among other things, for instance the date, the cali-bration data of the electrode, the method number. One the one hand it mightprobably not suit your ideas about how the result should be documented, on theother hand neither the sample volume nor the weighed-in quantity were taken intoaccount. To correct this you press the <MODE> key to return to the „MODE“menu:

Mth1


Use the cursor to select the <<MTH>> menu item, confirm your selection with the<ENTER> key. You are now prompted to know whether you would like to modifythe method.

Mth1


Place the cursor on <<yes>>, confirm your selection with the <ENTER> key.

Mth1

method name:sulphuric acid _

The name is preoccupied by sulphuric acid. You can take the name over or simplyoverwrite it. You continue with the <ENTER> key. The standard setting of theweighed-in quantity is <<none>>.

Mth1


This means that the calculation was performed with the preset value of 1. Youwould like to pipette the sample. Therefore you use the cursor to select <<vol.>>and confirm your selection with the <ENTER> key. The next prompt asks youwhether the sample volume should be input manually or as a fixed value:

Mth1

volume man fix

Please select <<man>>. This means that you will be prompted for the samplevolume at each start. This is the only item which has to be changed in the methodat this point. Please press the <ENTER> button. You will be taken to the menuitem where the method can be stored.

Mth1

methodtest / store

You select <<store>> and confirm your selection with the <ENTER> key. You arenow back on the „MODE“ menu:

Mth1


Modification of thesulphuric acid method

Method name

Select weighed-inquantity

Manual sample volume

Store method


You might now like to adapt the documentation to your requirements. Thereforeyou select the <<DOC>> menu item and confirm your selection with the <ENTER>key. You will first be prompted to know whether the documentation is to be modi-fied:

Doc1

change document. yes no

Please select <<yes>>, and confirm your selection with the <ENTER> key. Youwill be asked whether a sample identification is to be performed:

Doc1


The following displays will ask you a series of questions to know whether you wishany further documentation. If you wish the corresponding printout, make yourselection using the <<y>> or <<n>> and confirm them with the <ENTER> key.

Doc1

method number:output: Y N

Doc1

method name:output: Y N

Doc1

date / time:output: Y N

Doc1

weight:output: Y N

Please confirm <<yes>> with <ENTER>. Even if you selected the output of theweighed-in quantity in the documentation, no weighed-in quantity will be printed,since no weighed-in quantity was selected in the titration method. This applies toother items in the documentation as well.(Please refer to the documentation printout in Figure 15).

Doc1

volume:output: Y N

Doc1

pre-titr. vol.:output: Y N

Modification of thedocumentation for

sulphuric acid

Documentationsample identification

Documentationmethod number

Documentationmethod name

Documentationdate and time

Documentationweighed-in quantity

Documentationsample volume

Documentationpretitration volume


Doc1

titration vol.:output: Y N

On the next three menu items you use the cursor to select <<N>> and confirmyour selection with the <ENTER> key:

Doc1

calibr. dates:output: Y N

Doc1

cal. - user - name:output.: Y N

Doc1

electrode - ID:output.: Y N

Doc1

results:output.: Y N

Please confirm with <ENTER>.

Please select within the next two menus.

Doc1

CALC - parametersoutput.: Y N

Doc1

wait start valueoutput.: Y N

Doc1

data / graphics:output.: Y N

Please use the cursor to select <<Y>> and confirm with it.

Documentationtitration volume

Documentationcalibration data

Documentationuser name

Documentationelectrode ID

Documentationresults

Documentationcalculation parameters


Please confirm within the next four menus with <ENTER>.

Doc1

choice output data graphics

Doc1

choice outputml 1st deriv. t

Selection x axe y axe<<ml>> ml meas. valuewith EQ: <<1st>> deriv. ml 1st deriv.<<ml/t>> time ml<<t>> time meas. value

Doc1

method head: no 1 2 3 4 5

Doc1

documentation:test / store

Please use the cursor to select <<store>>, and confirm your selection with the<ENTER> key. You are now back on the „MODE“ menu. <ESC> will return you tothe start menu or the execution level, respectively.

You should best pattern a sample with a defined sulphuric acid volume and startthe modified sulphuric acid method by pressing the <START> key. You will beprompted for the sample identification

Pos1

sampl 1 ident: __

and the sample volume:

Pos1

sampl 1 volume: 1.0000 <ENTER>

Please enter the sample identification and the sample volume on the keyboardand and confirm your selection with the <ENTER> key. The TitroLine alpha willtitrate again until it finds the equivalence point.

Printout of themeasurement curve

Store documentation

Start of the modifiedsulphuric acid method

Sample ident input

Sample volume


The result will be calculated, and the documentation will be output on the printer:

In addition to the standard printout (exhibit 15) the titration curve including the cal-culated result will be output. For routine application we recommend for reasons oftime to fashion the documentation as short as possible (please refer to the expla-nation contained above in this same chapter 6.1).

6.2 Titration of an unknown acidAnother titration example is intended to exercise the use of the actual titrationparameters. In the first example the standard parameters for sulphuric acid wereselected, and the method was modified in the documentation and calculation only.In order to make further changes you must first remove the safety lock for pa-rameter modification in the „INIT“ menu, <<SYS>> (also cp. chapter 5.5.6.7).This safety lock prevents inadvertent changes of the suggested standard pa-rameters.

The next example is intended to create a method for an acid which is not con-tained in the parameter selection of the Titration Unit TitroLine alpha. You onlyknow that it is an organic acid which is well soluble in water. But you do not knowwhether it is a strong or very weak acid.On the start menu you select <MODE>, <<STD>> and <<acid>> to get to theselection of standard parameters for acid titration.

Figure 16Printout of the modifiedsulphuric acid method

Titration of anunknown acid


Mth1


STD10


STD15

next meth. (<-/->)testtitr. acid

Please press the cursor until <<testtitr. acid>> appears on the screen, and con-firm your selection with the <ENTER> key. Store the parameters under workingmethod 2:

STD15

->work. method no. _ store <ENTER>

To obtain a curve printout you have to select the „graphics“ option in the „docu-mentation“ section. To do so, you go to the <<DOC>> menu where you, as in theprevious example, either press the <ENTER> key to get in the Data/Graphicsselection menu or, as in the present example, press the <ROLL DOWN> keythree times.

Mth2


Doc2

change document yes no

Doc2


At this point you have to press the <ROLL DOWN> key three times:

Doc2

documentation:test / store

Doc2

mthod head: no 1 2 3 4 5


Doc2


Please select <<Y>> and confirm your selection with the <ENTER> key. Subse-quently you simply press the <STORE PARAM.> key to store the documentation.If desired, the titration curve will be printed. If the signification of the coordinates isnot changed, the printout will occur in the usual form: y axis = pH and x axis = ml.If you wish you can, as in the example above, modify the calculation and themethod at this point. Subsequently, you weigh-in or pipette your sample and diluteit with water. The <ESC> key will take you to the <<START>> menu.

Mth2

<START>/ (up/dwn)testtitr. acid

You start the titration with the <START> key.

The documentation printout could, for instance, look like this:

Start acid test titration

Figure 17Documentationacid test titration


As you can see, the measurement curve was further included as in the sulphuricacid method. Since the titration was designed as a test method, it will takesomewhat longer then the sulphuric acid method. This is due to several reasonswhich have to be explained in context with the titration parameters.

But in order to be now able to change the actual titration parameters you must firstchange the option on the „INIT“ <<SYS>> menu.

From the start menu the <INIT> key will take you to the „INIT“ menu:

TIME COPY CAL RSPASSW SYS CNTRY

Use the cursor to select <<SYS>> and press the <ENTER> key until the followingmenu item appears:

SYSIni

edit STD method on off

Use the cursor to select <<on>>, and confirm your selection with the <ENTER>key. Then press <ESC> one time. You will be back on the start menu. The<MODE> and <ENTER> key will take you to the <<MTH>> menu:

Mth2


Use the curser to change to <<yes>> and confirm your selection with the<ENTER> key. The next two steps, i.e. method name and weighed-in quantity,are described (see at the beginning of chapter 6.1). Please compare the descrip-tions. After confirming the sample volume or weighed-in quantity menu itemwith the <ENTER> key you will see the screen:

Mth2


Since you wish to titrate an acid and are working in the acqueous medium, yousimply confirm the selection <<pH>> with <ENTER>.

Mth2

input delayno short

The input delay can be switched off of the case of titration in water or polar sol-vents (see chapter 4.1). Confirm the selection <<no>> with <ENTER>.

Mth2


„INIT“ menu

<<SYS>> menu

Titration type <<pH>>

Input delay

Titration direction


When titrating an acid with a caustic solution the titration direction will run from alow pH value to a higher pH value, i.e. in an increasing manner. So you confirmthe <<increase>> selection with the <ENTER> key.

Mth2

pre titration? yes no

Since you do not yet know the minimum consumption, it would not make sense toadd a larger titration solution volume an the start of the titration. Therefore youconfirm this <<no>> selection with the <ENTER> key, too.This is where to input the end criteria for a titration.

Mth2


Use the cursor until the following display appears:

Mth2


Confirm the selection titration end <<all>> with the <ENTER> key. This meansnow that all the three possible end criteria are combined with each other and couldlead to a cancellation of the titration: One pH value, one consumption in terms ofml and one or two detected equivalence points (turning points). In the <<acid testtitration>> method only two criteria were combined, namely <<pH>> and<<ml>>. The end criterion for pH was automatically set to 12 in the<<acid test titration>> method, the end criterion for ml was set to 50. Thismeans that titration will only stop after a pH value of 12 or a consumption of 50 mlhas been reached.

Please look carefully at the curve in Figure 17 and consider whether youshould change the end criteria for <<pH>> and <<ml>>.The third end criterion you enter is the number of the equivalence points causing acancellation. The curve of the acid indicates only one turning point (ref. toFigure 17). For this reason you select the number 1 when you are asked for theEQ number.

If now an equivalence point is found in the course of the titration, titration will stopdespite the fact that the pH value and m value end criteria have not yet beenreached. Since the differences between the turning points may be considerable, asensitivity for finding the equivalence points has to be entered. The sensitivityscale extends from <<1>> to <<5>>. A sensitivity level of <<1>> means very highsensitivity, so that even very weak turning points will be detected during titration. Asensitivity level of <<5>> means a very low sensitivity in finding equivalencepoints.

The first prompt will ask for the pH value:

Mth2

tit. end [pH] 12.000 <ENTER>

Please input the value <<11.0>> and confirm with the <ENTER> key.

Pretitration

Selection titration end

<<all>><<pH>><<ml>><<EQ>>

<<pH>> titration end


Mth2

number EQ 1 2

Please confirm the selection <<1>> with the <ENTER> key.

Mth2

EQ sensibility 1 2 3 4 5

Move the cursor to the sensitivity level <<3>>. Sensitivity level <<4>> is preset andapplies to strong acids such as hydrochloric acid and sulphuric acid. However,from the course of the curve one can see that the acid under concern is a weakone. Please confirm with the <ENTER> key.

Mth2

tit. end [ml]50.0000 <ENTER>

The ml value here is just a mere safety criterion. Confirm the value <<50.00000>>with the <ENTER> key.

The following three menu items are related to the speed of measuring, thatmeasns drift control and titration control. The next prompt will appear:

Mth2

drift control middle exact

The drift control decides when a measurement value is to be taken over after thetitration addition. If you are on this menu item and use the cursor to move to theleft you will see the following screen:

Mth2

drift control fixed fast

So you can chose from four different drift criteria. The <<fixed>> drift controlalways causes a constant wait time after the titration addition. In the case of diffi-cult titrations in non-acqueous media such as TAN/TBN, or with inhibited chemicalreactions such as the determination of aromatic amines by way of diazotation, aconstant wait time has to be set. A disadvantage of this setting consists in that thetitration duration will often be longer than with the three other drift criteria.

The <<fast>>, <<middle>>, and <<exact>> will not wait over a fixed period oftime, but take over the measurement value after the TitroLine alpha every time themeasurement value has reached a certain stability over a certain time. In the caseof acid/alcaline titration in acqueous medium one would as a rule select the 'fast'or 'middle' drift criterion.

Use the cursor to move back to <<middle>> and confirm your selection with the<ENTER> key.

Number equivalencepoints

Equivalencepoint sensitivity


Drift control

<<fixed>> drift control

<middle>> drift control


Mth2

tit. control lin. dyn.

This screen allows you to decide whether titration control is dynamic or linear.

Linear titration control means that the entire titration will be performed with a con-stant step width. Figure 18 shows a titration curve recorded with a step width of0.2 ml. The disadvantage of linear titration control becomes only obvious in therange of the equivalence point, since as a rule there are only very few measure-ment points. This renders the calculation of the equivalence point more difficult,and the results may be inaccurate.

Titration control

Linear titration control


In contrast, dynamic titration control will cause a titration with different step widths.In the flat section of a titration curve titration will proceed with large step widths,while titration in the steep section will be performed with small steps (refer toFigure 19). This means that as a rule dynamic titration will be performed fasterthan linear titrations, and more measurement points will be found in the range ofthe turning point. Evaluation becomes more certain and exact.

The acid test titration was performed with a linear step width of 0.05 ml. However,the measurement curve of the unknown acid shows a marked turning point. It istherefore advisable in order to save time and to take up more measurement pointsin the equivalence-point range to perform the next titration using a dynamic

Figure 18Linear titration

Dynamic titration control

Figure 19Dynamic titration


titration setting. To switch over to dynamic titration control move the cursor to<<dyn>> and confirm your selection with the <ENTER> key.

Mth2

dynamic step 1 2 3 4

Here you can select from 3 fixed preset dynamic stages -1 to 3- and one freelyadjustable stage -4- (also refer to chapter 5.4.1.2).In simplified terms one can in principle say with regard to stages 1 to 3:stage 1 for intense and medium jumps, stage 3 for very weak jumps.Confirm selection 1 with the <ENTER> key.

Mth2

wait time 1[s] 10 <ENTER>

The waiting time 1 will run off as long as the dosing unit is being filled. It is pro-vided as a safety feature in order to ensure that the equilibria can establish prior topretitration and/or the taking up of the start pH value. Use the <ENTER> key toconfirm the waiting time of 10 s. For the same reason a second waiting time isrequired after pretitration and/or the taking up of the start pH value.

Mth2

wait time 2[s] 10 <ENTER>

If no pretitration or taking up of a start pH value was selected, change the waitingtime from 2 to 0 and confirm this setting with the <ENTER> key. This input savestime, and although a different input would be nothing else but a delay of the titra-tion, it is yet of no influence on the result. To conclude, memorize the method. Usethe <ESC> key to exit the „MODE“ menu.Prepare a new sample of the acid, and start the method with <START>. Pleasecompare the curve you will obtain this time with the first titration in the acid testtitration method. If you do not agree with the result you will have to change thecontrol parameters of the method and start another titration.

6.3 Chloride in potable waterThis example shows how to perform a titration using a ready-made applicationinstruction for the TitroLine alpha. It is intended to determine chloride in water(drinking water). We simply assume that no method was stored for this applicationunder <STD>, an assumption which is of course not true: it is stored as <STD>method no. 34.An application instruction does not only contain a complete description of thesample preparation, the appliances, electrodes and chemicals used, but also aprintout of the method and the calculation formula.

The annex contains an example of an application instruction.

Dynamic steps

Wait time 1

Wait time 2

Application instructionsfor the Titration UnitTitroLine alpha


Figure 20 shows a method printout of the chloride method. The printout in anapplication instruction is identical. You should now proceed step by step.

You are back on the start menu or execution level of a method:

Mth2

<START> / (up/dwn)testtitr. acid

Use the keyboard to enter number 3, i.e. as 03. Then use the <MODE> key to geton the „MODE“ menu, subsequently press <ENTER>.

Mth3


Move the cursor to <<yes>> and confirm your selection with the <ENTER> key:

Mth3

mthod name: _

Here you enter the name CL IN POT. W. (chloride in potable water). Please con-firm your selection with the <ENTER> key.

Mth3


Considering that we are dealing with a liquid sample and that the result is to becalculated in terms of ml, you select sample volume on this menu item. Pleaseanswer all the following menu items about the sample volume under <<MTH>>

Figure 20Method contents

chloride in potable water

************************ * method contents 3 * ************************ time: 13:53:51 date: 15.08.94 method:CHLORIDE IN D.W.

selected weight: volume = : man

titration mode: mV direction tit.: increase pretitration: no titration end: EQ+mV+ml number EQ = 01 EQ sensibility = 02 mV end =320.0 ml end =25.000 drift control: exact titration control: dynamic dynamic step: 01 stirr. time: 1 = 0015 s stirr. time: 2 = 0000 s

CALCULATION parameter smoothing: no factor =0.010000 factor 2 =35453.000000 quotient =1.000000 according formula 1: EQ1*F*F2/Q

Input method name

Select weighed-inquantity


according to the pattern of the method printout contained in Figure 20. Afterstoring the method you will be back on the „MODE“ menu. To enter the calcula-tion formula, move the cursor to <<CALC>> and press the <ENTER> key.

Cal3


Use the cursor to select <<yes>>. You will then be prompted whether the calcula-tion is to be edited:

Cal4

calculation (ESC) edit RUN

Confirm <<Edit>> with the <ENTER> key. For further details please refer to themethod printout. When you are asked for the decimal places, please enter 1. Thefollowing questions asking for the places, please enter 1. The following questionsasking for statistics and the result memory should be answered with <<no>>.Please store the calculation.

To compare the method created with with the pattern in Figure 20, simply print themethod. The printout is done on the <<LIST>> menu item in the „MODE“ menu.

Mth3


To do so, you go to the <<LIST>> menu item and press <ENTER> once. The fol-lowing screen will appear:

Mth3

output methodlist content STD

Move the cursor to <<content>> and press <ENTER>. The contents of themethod will now be printed. Please compare this printout thoroughly with the print-out in Figure 20. If the contents is totally identical, you should now modify only thedocumentation according to the description under the <<DOC>> menu item.

Practical way of proceeding:

− Connect an Ag 6280 to the pH/mV measurement input.− Pattern 100 ml of drinking water in al 150 ml beaker glass.− Acidify the solution slightly with 1 ml HNO3 (δ = 1.40 g/ml diluted 1/1).− Titrate with AgNO3 0.02 mol/l.

Editing <<CALC>>

<<LIST>>

Method printout


A printout of the documentation should roughly look like this one:

6.4 Water determination according to Karl-FischerWater determination according to Karl-Fischer is one of the most frequently usedtitration methods. For this titration process the Titration Unit TitroLine alpha fea-tures a special titration control which you will learn in this chapter.

As an example of a Karl-Fischer titration we take the determination of water inalcoholic plant extracts. Despite the fact that there are 3 standard methods for KFin the <<STD>> menu, we will create the method on the basis of an application in-struction.

Fig. 21Documentation printout

Chloride in potable water

Water determination inalcoholic plant extracts


Figure 22 shows a printout of this KF method:

You are back on the start menu or execution level of a method:

Mth3

<START> / (up/dwn)Cl, potable water

Use the keyboard to enter number <4>, i.e. as <04>. Then use the <MODE> keyto get on the „MODE“ menu, subsequently press <ENTER>. Again, you will beasked:

Mth4


Move the cursor to <<yes>> and confirm your selection with the <ENTER> key.

Mth4

method name: _

You enter for example the name KF EXTRACT. Confirm the name with the<ENTER> key.

Mth4

select weightwght. vol none

Since we are weighing in the sample and want the result to be calculated in termsof %, you move the cursor to <<wghd.>> and press the <ENTER> key.

Fig. 22KF EXTRACTmethod printout ************************

* method contents 4 * ************************ time: 14:06:46 date: 19.08.94 method: KF EXTRAKT

selected weight: weight : man

Titration mode: KF KF conditioning: yes KF value: 10.0 KF delay: 20 s KF step control: 01 pretitration: no

stirr. time: 1 = 0010 s stirr. time: 2 = 0020 s

CALCULATION parameter smoothing: no factor =5.000000 factor 2 =1.000000 quotient =10.000000 according formula 1: ml*F*F2/Q

Start menu

Edit method

Method name input

Selection ofweighed-in quantity


Mth4

weight auto man fix

We assume that in this example an analytical balance is connected to theTitroLine alpha. Therefore you select <<auto>> and confirm your selection withthe <ENTER> key. The next screen will show the selection of the titration type:

Mth4


Use the cursor to select <<KF>> and confirm your selection with the <ENTER>key.

Mth4

KF conditioning yes no perman.

Prior to the actual titration you would like to titrate the solvent in dry (condition).Therefore you use the cursor to select <<yes>> and confirm your selection withthe <ENTER> key.

Mth4

KF value [µA] 10 20 30

The KF end value is the value where titration is to end. The end value in terms of[µA] is preset to <<20>>. Use the cursor to select <<10>> and confirm your selec-tion with the <ENTER> key. The next item is the

Mth4

KF delay [s] 20 <ENTER>

KF duration in [s]. This is the period of time over which the end value has to re-main stable. Confirm the value of <<20>> with the <ENTER> key.

Mth4

KF step control 1 2 3 4 5

In this context please refer to the explanations in chapter 5.4.1.4. However, mostKF titrations can be performed with step 1. Confirm the selection step 1 with the<ENTER> key.

The following parameters should be entered according to the pattern (Figure 21)in the method.

Automatic weighing in

KF titration type

KF conditioning

KF end value

KF delay

KF control steps


After storing the method you are back on the „MODE“ menu. To enter the calcu-lation formula, move the cursor to <<CALC>>, then press the <ENTER> key.

Cal4


Use the cursor to select <<yes>>. You are know asked whether the calculation isto be edited:

Cal4

calculation ESC>. edit RUN

Confirm <<Edit>> with the <ENTER> key. For the remaining details please referto the method printout. When asked for the decimal places, please enter <2>. Thefollowing questions concerning statistics and result memory should be answeredwith <<no>>. Please store the calculation.

In order to compare the method created with the application pattern, print themethod. The detailed way of proceeding is described in chapter 8.3.

As a matter of course, you can perform a routine KF titration without a printout of ameasurement curve. However, for a better evaluation of a KF titration, you shouldadopt the following settings for the curve printout in the <<DOC>> menu:

Doc4


Please use the cursor to select <<yes>> and confirm your selection with the<ENTER> key.

Doc4

choice output: data graphics


Doc4

choice output::ml 1st deriv. t

The best way to evaluate a KF titration is an ml/time curve. With this curve onecan for instance see whether additional water occurs as a result of a side reactionand is erroneously recorded as well. Therefore you use the cursor to select <<t>>this time, and confirm your selection with the <ENTER> key.

Edit <<CALC>>

Measurementcurve printout

Type of curve printout

ml/time curve


− Connect a Pt 1400 electrode to the KF measurement input.− Pattern approx. 30 ml methanol in the titration reservoir.− First titrate the solvent in dry (conditioning).− Weigh in the sample in a disposable syringe placed on the analytical balance.− Inject the sample through the septum into the titration reservoir.− Then weigh the syringe again. The difference on the display is the actual

weighed-in quantity which is taken over into the TitroLine alpha by pressing thePrint key.

− Now the actual titration begins.

A printout of the documentation might look like this one:

Practical way ofproceeding

Figure 23Water determinationin alc. plant extracts


6.5 pH-stat in soil samplesThe last application example describes the creation of a method for a pH-stattitration. It is intended to set a soil sample to a very specific pH and keep in con-stant over a defined time.

You are back on the start menu or the execution level of a method:

Mth4

<START> / (up/dwn)KF EXTRAKT

Use the keyboard to enter number 5, i.e. as 05. Then use the <MODE> key to geton the „MODE“ menu, subsequently press <ENTER>. Again, you will be asked:

Mth5


Move the cursor to <<yes>> and confirm your selection with the <ENTER> key.

Mth5

method name: _

You enter for example the name PHST SOILSAMPL. Confirm the name with the<ENTER> key.

Mth5


The sample will be weighed in, but in this application the result always refers to aconstant weighed-in quantity of 10 g. here, you simply press the <ENTER> key.

Mth5


Then use the cursor to select <<pHstat>> and press <ENTER>.

Mth5

input delay none short

Since we are working in the acqueous medium, you confirm the selection<<none>> with <ENTER>.

Mth5


Since titration is performed with an acid in the present case, you use the cursor toselect <<descending>>.

Start menu

Edit method

Method name input

pH-stat type of titration

Input delay

Titration direction


Confirm your selection with the <ENTER> key. You will be asked:

Mth5

pre titration ? yes no

Also confirm this selection with the <ENTER> key.

Mth5

pHst value 7.000 <ENTER>

Enter the value 2.000. This means that the sample will first be set to a pH value of2.0. Confirm your selection with the <ENTER> key.

Mth5

pHst add. vol. none man

Since no substance is intended to be added after the pH setting, you confirm thepreset option with the <ENTER> key.

The next four questions refer to the measurement duration and intervals for takingover the measurement values.

Mth5

pHstat interval sec min h

The measurement values are to be recorded intervals of less than one minute.You therefore confirm the preset option <<sec>> with the <ENTER> key. Whenyou are prompted for the duration on the next menu item

Mth5

interval. [sec] 5 <ENTER>

you enter 30 sec. Confirm your selection with the <ENTER> key. The next promptwill be for the overall time.

Mth5

pHst total time sec min h

Titration is to be performed over 45 min. You therefore use the cursor to select the<<min>> unit and confirm your selection with the <ENTER> key. The next promptwill be for the duration:

Mth5

time length [min] 60 <ENTER>

Here you enter the number 45 and confirm your selection with the <ENTER> key.

Pretitration

pH-stat set value

pH-stat addition

pH-statmeasurement interval

unit selection

pH-statmeasurement interval

duration

pH-stat overall timeunit selection

pH-stat overall timeduration


The next prompt will be for the initial titration of the set value:

Mth5

pHst adjust. jumphigh met. low

This initial titration is equivalent to the end point titration control. Please refer tothe explanations in chapter 5.4.1.2. In the present case you select <<low>>, sinceno intense jump is to be anticipated with pH 2.0, and therefore overtitration is un-likely to occur.The next menu item is used to set the actual pH-stat control:

Mth5

pHstat control0 1 3 4 5

Please select the control stage 5. Stage 5 is particularly suitable for pH-stat in soilsamples, since a large quantity has to be added within a short time. Compared tothis, stage 0 is for suitable very low consumption only (only practical with a 10 mldosing unit)! Confirm this selection with the <ENTER> key. For the wait times 1and 2 you should enter the following values:

Wait time 1 = 3 sec. and wait time 2 = 0 sec. Please store the method.

Here again, the calculation formula for pH-stat titration is selected and modifiedunder the <<CALC>> menu item. With pH-stat titration you can select betweentwo different formulae. Use the <ROLL DOWN> or <ROLL UP> keys to select thefollowing formula:

Cal5

select . (up/dwn)* ml*F*F2/Q

Confirm your selection with the <ENTER> key. Enter the following values for thefactors, the unit, and the name:

Factor Factor 2 Quotient Unit Name1 1 1 ML CONS.

As soon as you have confirmed all entries with <ENTER>, the next prompt willappear:

Cal5

pHst. calc. optim. yes no

Confirm the selection with the <ENTER> key. After the titration you can use therecorded data for an optimization.

Confirm the following three questions by simply pressing <ENTER>. To finish, youstore the calculation. The <ESC> key will take you back to the „MODE“ menu.

Please set the graphics selection under the <<DOC>> menu item as follows:

Doc5

choice output data graphics


pH-stat initial titration

pH-stat additing control

Wait times

<<CALC>> calculationformulae pH-stat

Calculation formulafactors input

Optimize pH-statevaluation

store pH-stat evaluation

pH-stat graphic printout


Doc5

choice outputml meas.v/t ml/t

Please use the cursor to select <<ml/t>> and subsequently <<no>> in the methodhead. Please confirm your selection each time with <ENTER>.

Doc5

pHst. online DOCoutput.: Y N

Here you can output the measurement values during titration on a connectedprinter or PC. For this test please select the <<N>> (no) option and confirm withthe <ENTER> key. Please store at the end. <ESC> will take you back to the exe-cution level of the Titration Unit TitroLine alpha.Practical way of proceeding:− Connect for instance a pH 6280 to the pH/mV measurement input.− Weigh in 10 g of a soil sample in a beaker glass.− Dilute with distilled water to approx. 100 ml.− Titrate with HCl 1.0 mol/l.

pH-stat onlinedocumentation

Figure 24pH-stat in soil samples

198 Chapter 7 Inputs/Outputs for data communication

7 Inputs/Outputs for data communication

1 Electrode connection2 Reference electrode connection3 Power switch4 KF connection5 Temperature measurement connection6 Mains connection7 Printer connection (Centronics)8 Stirrer connection9 Balance connection (RS-232-C)

10 Keyboard connection11 Computer connection (RS-232-C)

Figure 23Rear view of theTitroLine alpha

199Chapter 7 Inputs/Outputs for data communication

Connection Electrode-Application Electrode Plug

on electrode Socket

on unitcable

pH titration, „hydrous so-lutions“

N 6280 A (DIN) „Electr.“ K1A

pH titration, „non hydroussolutions“

N 6480

Redox titration Pt 6280Chloride titration Ag 6280Karl-Fischer titration Pt 1400 NN

(4mm banana)„KF“ K1NN

Temperaturemeas./compensation

W 2130 NN(4mm banana)

„Pt 1000“ 9907/21

Titration withion sensitive electrodes

TZ 1101TZ1103TZ 1105

A (DIN) „Electr.“ K1A

Reference B 3520 N banana „Ref.“ B1A

7.1 Keyboard connectionThe keyboard port is used to connect the type no. TZ 2825 PC mini keyboard or aMF 2 multifunction keyboard for PCs. The port can handle PC and XT data for-mats. When using a different keyboard make sure that the keyboard is set to„XT mode".

7.2 Power connectionOnly the original power pack TZ 1849 suppliedby SCHOTT-GERÄTE may be connected.

7.3 RS-232-C interfacesThe Titration Unit TitroLine alpha is equipped with a Centronics interface (parallel).It is used to output result protocols, diagrams etc. via a printer with Centronicsinterface. The plug-in port for this interface is located on the rear panel (figure 6,item 7).

Pin configuration of the Centronics interface:

Pin no. Configuration Pin no. Configuration1 Strobe 14 NC2 - 9 Data 0 - Data 7 15 ERROR10 Acknlg 16 Init11 Busy 17 GND12 PE 18 - 25 GND13 SLCT

Electrode connection

Keyboard connection

Power pack TZ 1849

RS-232-C interfaces

RS-232-CPIN configuration

data transfer parameters

200 Chapter 7 Inputs/Outputs for data communication

7.4 Centronics interfaceThe Titration Unit TitroLine alpha is equipped with two serial interfaces(RS-23 2-C) for data communication with other devices. The plug-in ports of theseinterfaces are located on the back panel of the Titration Unit TitroLine alpha.Socket „1" is used to establish the connection with a computer or printer with a se-rial interface. The „balance“ socket can be used to connect a balance.

PIN configuration of the RS-232-C interfaces:

Pin no. Configuration Pin no. Configuration1 shielding, protective ground 2 T x D data output3 R x D data input 4 RTS5 CTS 7 digital ground

Please note:The data transfer parameters are set in the „INIT“ menu with the <<RS>> menuitem using software commands. All devices communicating among each othermust have the same transfer parameters.The transfer parameters are ex-factory set to 4800 baud, 7 bits, 2 stop bits, andNo Parity.

Possible parameters: Baud rate 1200, 2400, 4800, 9600The remaining parameters are: Data bits Stop Parity

7 2 no8 2 no7 1 even8 1 even

Centronics interface

PIN configuration of theRS-232-C interfaces

Setting the datatransfer parameters

201Chapter 7 Inputs/Outputs for data communication

7.5 Controlling the Titration Unit TitroLine alpha via theRS-232-C interface

The following commands can be used to control the Titration Unit TitroLine alphavia the RS-232-C (1) interface:

<aa> stands for the address of each unit (always two digits).The commands marked with a * can only be used in the executive level.

Command Answer: Action:*aaVE Version: 95/17 Output version number*aaRH Ident: TitroLine alpha Report Hardware aaRS Status: READY/MODE/INIT/CAL Report status (where am I?) aaRC aalast command Repeat last command aaRA aa unit 10 ml Ask for unit size aaSH aaY Titration stop*aaSM aaY Start of a method

(possible only in main menu)aaSP 7,50 OOY In the case of pH-stat titration,

the desired pH value can besent to the TL alpha priorto titration

*aaMC01...09 aaY Method change(possible only in main menu)

*aaFD aaY Measure dead stop function*aaFP aaY Measure pH function*aaFV aaY Measure mV function*aaFT aaY Measure temperature functionaaO OOM:1.912 pH „Online measurement“, an

0.080 ml online measurement value isoutput.

aaM Measurement value Measure within the setMeasuring range

*aaQE aaY Stirrer on*aaQA aaY Stirrer off*aaLL Output method list via RS computer*aaLI Output method contents via RS computer*aaLC Output calibration parameters via RS computer*aaLR Output result printout*aaLD Output data*aaLO Output documentation*aaLM Output measurement series*aaMM aaY Device in mode „MODE"*aaMI aaY Device in mode „INIT"*aaMK aaY Device in mode „CAL" aaSK aaY Start calibrationaaES aaY „ESC" one step backwardsaaEX aaY Function „Exit“ back to the execution level*aaBF aaY Burette is filling*aaBA1/2/5 aaY Set burette unit: 10 ml/20 ml/50 ml

Hint: Commands for small volumes can notbe performed, if the volume is too small to dose.

*aaDB01.12 aaY Burette is dosing volume without filling anddisplay is set to zero

*aaDA1.12AAY Burette is dosing volume without fillingwith addition

*aaGDM20.3 aay Dosing speed in ml/min

Every command must be typed separately and terminated with <CR> <LF>. Everyanswer will be sent back after being finished.

External controlling viathe RS-232-C interface

202 Chapter 8 Maintenance and care

8 Maintenance and care of the Titration UnitTitroLine alpha

8.1 Maintenance and care of the titration unitOperation has to be preserved by control and maintenance works. These mainte-nance or service works include:

− Visual control: Front-membrane display

− Measurement ranges: mV 3 values - nominal / actualpH 6 values - nominal / actual°C 3 values - nominal / actual

− Function: Karl-Fischer titration (dead-stop)

− Interface functions, measuring amplifier, control behaviour, dialogue system,keyboard function, stirrer connection, printer output.

− Once per quarter, the electrical contacts have to be checked, if the pistonburette is used in premises with an occasional occurence of corrosive mattersin their atmosphere.

8.2 Maintenance and care of the burette unitTo retain the function of the Titration Unit TitroLine alpha the following mainte-nance and inspection work is to be carried out.

Maintenance intervalsNormal operation:

− As a rule, all maintenance of the Titration Unit TitroLine alpha has to be per-formed at intervals of 6 months max.

Under particular stress

− Once per quarter, the glass cylinder has to be inspected visually in order tocheck for damages and in addition a test according to DIN 12 650, part 6, orISO DIS 8655, part 3, has to be carried out. These verifications are particularlynecessary if solutions have been used which are likely to attack glass, e.g.alkaline, fluoride or phosphatic solutions.

− If there is suspicion that a solution is attacking the glass excessively the main-tenance intervals are to be reduced accordingly.

In case of disturbances

− The work has to be carried out immediately if a disturbance, an error oranother defect becomes obvious.

Maintenance work to be carried out

− Check the piston and the cylinder for visible signs of mechanical damage, suchas cracks, fractures and damage of the surface.

− Check the piston rod for corrosion.− Check the hoses, screw unions and seals for signs of visible damage, con-

tamination and leaks.− Check the electrical plug contacts for corrosion and mechanical damage (on

Titration Unit TitroLine alpha and cables).− Defect parts must be repaired or replaced with new ones. Defect glass parts

must always be replaced.− After each maintenance operation, a test for metrological reliability according to

DIN 12 650, part 6, or ISO DIS 8655, part 3, has to be carried out.

Normal operation

Particular stress

In case of disturbances

203Chapter 9 Storage and transport

Periods without operation

− If the dosing units for the Titration Unit TiroLine alpha are not used over a longperiod of time, the liquids contained in the system, in particular aggressive so-lutions, have to be drained. If the liquid is left in the system, one has to reckonwith corrosion and a alteration of solutions used over the time. Since the stateof the art does not provide plastic hoses which are absolutely free of diffusionoccurences, this precaution measures apply in particular to the hose-line sec-tion.

Cleaning

− The dosing units can be cleaned using a piece of cloth soaked in normal wateror a household cleansing agent containing ethanol. In general, short-term im-mersion in, or rinsing with, water or ethanol is not harmful, but this methodshould only be applied in extreme cases.

− The casing of the lower section can also be cleaned using a piece of cloth anda household cleansing agent. The lower and rear side have to be cleaned dry.In no case must water penetrate into the interior of the lower section.

9 Storage and transportIf the Titration Unit TitroLine alpha has to be stored or transported, the originalpacking material will provide optimal protection of the Titration UnitTitroLine alpha. In many cases, however, the original packing material is no longeravailable, so that an equivalent packing material has to be used. Sealing the bot-tom part in a foil is advantageous.

The selected place of storage should be a room with temperatures between + 10and + 40 °C and a max. air humidity (rel.) of up to 70 %.

If dosing units are to be stored temporarily, or transported, all liquids contained inthe system, especially aggressive solutions, have to be drained. Please refer tochapter 8.2 „Maintenance and care of the burette unit".

Dosing units

Casing

Original packing material

Place of storagetemperatures

204 Chapter 10 Index

10 Index

Address...........................................................161Applications.....................................................107Application instructions ...................................186Automatic invocation of a method...................144Average

standard variation ........................................149variation coefficient......................................149

Bal...................................................................167Balance data

adding..........................................................167deleting ........................................................168edit ...............................................................167error messages ...........................................169inserting .......................................................168overwriting ...................................................168

Baud rate.........................................................160Beeper.............................................................162Buffer temperature table .................................160Buffer values selection ....................................158

Cal. user name................................................153CALC parameters ...........................................153Calculation

changing ......................................................145checking-up .................................................151choice of formulae .......................................145edit ...............................................................145errors ...........................................................151examples .....................................................147formula types ...............................................146formulae...............................................171, 196formulae abbreviations ................................146number of equivalence points......................145parameters ..................................................145RUN.............................................................151test/store......................................................151

Calibration2-point..........................................................166error message

adjustment time .......................................169temperature drift ......................................169wrong buffer .............................................169

single-point ..................................................166start..............................................................166

Calibration dates .............................................153Calibration mode .............................................166Care of the TitroLine alpha..............................202Casing .............................................................203Centronics interface ........................................200Chloride determination ....................................170Chloride in water .....................................187, 189Cleaning ..........................................................203Clock ...............................................................157Combining with other devices .........................119Commands TitroLine alpha.............................201Conditioning, permanent .................................138Connections ....................................................107Connections of devices ...................................120

Contrast adjustment display........................... 123Conversation fact ........................................... 153Cursor keys .................................................... 128Curve printout................................................. 192Cylinder .......................................................... 111

Data bit ........................................................... 161Data transfer parameters ............................... 200Data/graphics ................................................. 153Date/time ........................................................ 153Decimal places ............................................... 148Deleting the memory assignment................... 150Device connections ........................................ 119Digits .............................................................. 148

following the decimal point.......................... 148Display............................................................ 123Display results ................................................ 151Display, main selection................................... 163Disturbances .................................................. 202Documentation

acid test titration.......................................... 180calculation parameters................................ 176changing ..................................................... 152content, choice............................................ 153data/graphics .............................................. 153date and time .............................................. 175DOC............................................................ 152graphic, type ............................................... 153method head............................................... 154method name.............................................. 175method number .......................................... 152results ......................................................... 176sample designation..................................... 152sample identification ................................... 175sample volume............................................ 176storing ................................................. 154, 177titration volume ........................................... 176user name................................................... 176weighed-in quantity ..................................... 176

Documentation printout .................................. 189Dosing emphasis............................................ 136Dosing steps

constant ...................................................... 135individual ..................................................... 135

Dosing unitreplacing ..................................................... 114

Dosing units.................................................... 203Drift control ..................................................... 183

fixed ............................................................ 135Duration of the titration ................................... 135Dynamic steps........................................ 136, 186Dynamic titration............................................. 185Dynamic titration control................................. 185

Edit <<CALC>> .............................................. 192Edit method ............................................ 190, 194Edit parameter................................................ 167Edit STD method.................................... 129, 164

205Chapter 10 Index

Editing <<CALC>> ..........................................188Electrode calibration........................................158Electrode ID ....................................................153Electrode, identification ...................................159Electrode, connection......................................198End criteria, combination.................................134End point titration

1 end point...................................................1322 end points .................................................132delay time ....................................................133

End point titration formulae .............................146EPROM ...........................................................111Equivalence point

sensibility .....................................................134sensitivity .....................................................183

Equivalence points ..........................................171Error messages...............................................169Execution level ................................................126External controlling..........................................201

Factors input ...........................................172, 196Filling, automatic .............................................164First operation .................................................112

Glass cylinder..................................................117

Inputname....................................................147, 172unit .......................................................147, 172delay ....................................122, 130, 181, 194possibilities ..................................................127

Karl-Fischerconditioning .................................................191control parameters ......................................138control steps ................................................191delay ............................................................191end point delay ............................................138end value .............................................138, 191titration type .................................................191

KeyboardMF ...............................................................123mini PC ........................................................124

Keyboard connection.......................................199Keyboard functions .........................................125

Language selection.........................................165Linear titration .................................................185Linear titration control......................................184Liquid of the inner surface...............................111LIST.........................................................155, 188List of the stored methods...............................155

Mains connection ............................................198Maintenance of TitroLine alpha.......................202Measurement curve printout ...........................192Measurement value display ............................163Measurement values

maximum.....................................................122Measurement without titration .........................141Measuring amplifier.........................................122Measuring input

electrode ..................................................... 122Pt 1000 ....................................................... 122

Memory cardinstalling...................................................... 112removing ..................................................... 112

MenuCAL..................................................... 158, 166CALC .......................................................... 145CNTRY ....................................................... 165COPY.......................................................... 157INIT ............................................................. 157MODE ................................................. 128, 170MTH............................................................ 128PASSW....................................................... 161STD............................................................. 170SYS............................................................. 162

Menu levels .................................................... 127Method

creation ....................................................... 170head............................................................ 153name................... 129, 153, 174, 187, 190, 194number........................................................ 153number input............................................... 126printout........................................................ 188

Methodsactivated ..................................................... 126changing ..................................................... 128copy ............................................................ 157delete .......................................................... 157storing ......................................................... 129

Mini keyboard ................................................. 107ml/time curve.................................................. 192Modification

documentation ............................................ 175Modification of the method ............................. 174Multifunction display ....................................... 123

Normal operation............................................ 202

On-line measurements................................... 157Output data..................................................... 156Output under List............................................ 155Output via PNR .............................................. 156

Packing list ..................................................... 112Packing material............................................. 203Parameters, optimizing................................... 136Parity .............................................................. 161Particular stress.............................................. 202Password

active .......................................................... 161deleting ....................................................... 162input ............................................................ 161

Periods without operation............................... 203Peripheral device............................................ 120pH-stat

additing control ........................................... 196addition ....................................................... 195addition volume........................................... 139calculation formulae.................................... 196control ......................................................... 140duration....................................................... 195

206 Chapter 10 Index

end point titration .........................................139error message, not enough points...............152evaluation optimizing ...................................196evaluation, storing .......................................196graphic printout............................................196in soil samples .............................................194initial titration................................................195measurement interval..........................139, 195online documentation ..................................197quantity ........................................................140set value ......................................................195speed...........................................................140titrations .......................................................139total time ......................................................139type of titration .............................................194unit selection................................................195value ............................................................139wait time 1 ...................................................140wait time 2 ...................................................140

pH-stat optimization ........................................148pH-stat titration................................................170

result parameters ........................................148formula 8......................................................146

PIN configuration of RS-232-C interfaces.......200PNR, print........................................................156Power pack .............................................112, 199Power switch ...................................................198Pre-tit. volume.................................................153Pretitration.......................................131, 182, 195Pretitration volume ..........................................131Printer..............................................................107Printout of the curve ........................................177Printout of the sulphuric acid method..............178

Quality of measurement values.......................135Rear view TitroLine alpha ...............................198Recording of meas. values without titration ....144Results ............................................................153Results of calculation ......................................145Rinsing cycles .................................................163Rinsing routine ................................................163RS ...........................................................155, 160RS-232-C

interfaces .....................................................199parameterization..........................................160pin connection .............................................199

Safety information ...........................................111Sample changer applications ..........................141Sample ident. input .........................................177Sample identification. ......................................153Sample volume ...............................................177Sample volume, manual .................................174Scrolling ..........................................................127Select weight ...................................................174Selection

calculation formulae.............................145, 171Sensor.............................................................107Slope character ...............................................136Smoothed data................................................148Stand bar installation.......................................113Standard parameter

group selection ........................................... 154parameter setsdirect selection............................................ 155STD............................................................. 154stores in methods ....................................... 155printout, documentation .............................. 173

Start menu.............................................. 190, 194Start method................................................... 173Start of the sulphuric acid method.................. 177Start value ...................................................... 153Start value, automatic..................................... 141Statistic

minimal number of results .......................... 149new ............................................................. 149number........................................................ 149

Statistics ......................................................... 149Stirrer.............................................................. 107Stirring speed ................................................. 143Stop bit ........................................................... 161Storage temperatures..................................... 203Store method.................................................. 174STORE PARAM. ............................................ 180Store parameter ............................................. 129Sulphuric acid................................................. 173Switching on ................................................... 111

Temperature compensation ........................... 159automatic .................................................... 159

Temperature measurement connection ......... 198Test titration acid ............................................ 179Time setting.................................................... 157Titrating direction............................ 131, 181, 194Titration control............................................... 184

dynamic ...................................................... 135linear ........................................................... 135

Titration endall ................................................................ 182criteria ......................................................... 131EQ............................................................... 182ml ................................................ 134, 182, 183pH ....................................................... 132, 182selection...................................................... 182

Titration example............................................ 178Titration mode ................................................ 130

Karl-Fischer ................................................ 137mV .............................................................. 136

Titration of a strong acid................................. 170Titration of an unknown acid .................. 170, 178Titration of sulphuric acid ............................... 170

Titration parametersmodifying .................................................... 129

Titration speed................................................ 134Titration start .................................................. 126Titration type pH ............................................. 181Titration volume.............................................. 153Transfer of

global memories ......................................... 150memories.................................................... 150

Transfer finished ............................................ 156Transfer parameters

assigning..................................................... 150

207Chapter 10 Index

Unit check .......................................................163Unit check on ..................................................164Unit size...........................................................162

Validation of the calibration .............................159Validation parameters .....................................158Validation, store Cal ........................................160Valve support ..................................................116Volume............................................129, 130, 153

entered manually .........................................130fix .................................................................130

Wait time 1 ..................................................... 186Wait times ...................................................... 196Water determination....................................... 189

in alcoholic plant extracts............................ 189according to K.F.......................................... 170in alc. plant extracts .................................... 193

Weighed-in quantity................................ 187, 190Weighing-in

fixed ............................................................ 129manual ........................................................ 129

Weight .................................................... 129, 153Working method............................................. 171

operating instructions titration unit titroline alpha index..... 204 chapter 1 technical description...

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