manual de titulador

Gebrauchsanleitung Titrator TitroLine alpha plus

Operating Instructions Titration Unit TitroLine alpha plus

Mode d'emploi Titrateur TitroLine alpha plus

Manual de instrucciones Titulador TitroLine alpha plus

Gebrauchsanleitung ........................................................................................................... Seite 1 ....... 82 Wichtige Hinweise: Die Gebrauchsanleitung vor der ersten Inbetriebnahme des Titra-tors TitroLine alpha plus bitte sorgfltig lesen und beachten. Aus Sicherheitsgrnden darf der Titra-tor TitroLine alpha plus ausschlielich nur fr die in dieser Gebrauchsanleitung beschriebenen Zwecke eingesetzt werden.

Bitte beachten Sie auch die Gebrauchsanleitungen fr die anzuschlieenden Gerte.

Alle in dieser Gebrauchsanleitung enthaltenen Angaben sind zum Zeitpunkt der Drucklegung gltige Da-ten. Es knnen jedoch von SCHOTT sowohl aus technischen und kaufmnnischen Grnden, als auch aus der Notwendigkeit heraus, gesetzliche Bestimmungen der verschiedenen Lnder zu bercksichtigen, Ergnzungen am Titrator TitroLine alpha plus vorgenommen werden, ohne dass die beschriebenen Ei-genschaften beeinflut werden.

Operating Instructions .................................................................................................... Page 83 .... 164 Important notes: Before initial operation of the Titration Unit TitroLine alpha plus please read and observe carefully the operating instructions. For safety reasons the Titration Unit TitroLine alpha plus may only be used for the purposes described in these present operating instructions.

Please also observe the operating instructions for the units to be connected.

All specifications in this instruction manual are guidance values which are valid at the time of printing. However, for technical or commercial reasons or in the necessity to comply with the statuary stipulations of various countries, SCHOTT may perform additions to the Titration Unit TitroLine alpha plus without changing the described properties.

Mode demploi ................................................................................................................ Page 165 .... 246 Instructions importantes: Prire de lire et dobserver attentivement le mode d'emploi avant la premire mise en marche du Titrateur TitroLine alpha plus. Pour des raisons de scurit, le Titrateur TitroLine alpha plus pourra tre utilis exclusivement pour les usages dcrits dans ce prsent mode d'emploi.

Nous vous prions de respecter galement les modes d'emploi pour les appareils connecter.

Toutes les indications comprises dans ce mode demploi sont donnes titre indicatif au moment de l'impression. Pour des raisons techniques et/ou commerciales ainsi qu'en raison des dispositions lgales existantes dans les diffrents pays, SCHOTT se rserve le droit d'effectuer des supplments concernant le Titrateur TitroLine alpha plus pour sries de dilution qui ninfluencent pas les caractristiques dcrits.

Manual de instrucciones ............................................................................................ Pgina 247.. 325 Instrucciones importantes: Primeramente, lean y observen atentamente el manual de instrucciones an-tes de la primera puesta en marcha del Titulador TitroLine alpha plus. Por razones de seguridad, el Titu-lador TitroLine alpha plus slo debe ser empleado para los objetivos descritos en este manual de instrucciones.

Por favor, respeten las indicaciones descritas en los manuales de instrucciones de los equipos antes de conectarlos.

Todos los datos contenidos en este manual de instrucciones son datos orientativos que estn en vigor en el momento de la impresin. Por motivos tcnicos y/o comerciales, as como por la necesidad de respetar normas legales existentes en los diferentes pases, SCHOTT puede efectuar modificaciones concernien-tes al Titulador TitroLine alpha plus sin cambiar las caractersticas descritas.

83 TABLE OF CONTENTS

TABLE OF CONTENTS PAGE

1..Technical properties of the TitroLine alpha plus Titration Unit ..........................85 1.1 Summary......................................................................................................................................85 1.2 Warning and safety information ...................................................................................................91

2..Set-up and first operation ......................................................................................92 2.1 Unwrapping and set-up of the TitroLine alpha plus Titration Unit...............................................92 2.1.1 Installation of the stand rod ......................................................................................................92 2.1.2 Connection of the optional TM 135 titration rig. .......................................................................92 2.1.3 Installation of the titration clip ...................................................................................................92 2.2 Installation of the TM KF Titration Stand and of the titration vessel ...........................................93 2.3 TA plus Interchangeable Unit:......................................................................................................96 2.4 Fitting and replacing an interchangeable unit ..............................................................................97 2.5 Replacing the glass cylinder ........................................................................................................98 2.6 Initial filling and rinsing of the complete interchangeable unit .....................................................99 2.7 Combining the TitroLine alpha plus Titration Unit with other devices........................................100

For a functional description, please refer to chapter 5, Working with the TitroLine alpha plus Titration Unit. In addition, please note the information provided with the devices being connected to the TitroLine alpha plus Titration Unit. ....................................................................................................100

3..Construction of the TitroLine alpha plus Titration Unit.....................................101

4..The connections of the TitroLine alpha plus Titration Unit ..............................102 4.1 Measurement-amplifier, A input channel , electrode signal.......................................................102 4.2 Measurement-amplifier, B input channel , electrode signal.......................................................102

5..Working with the titration unit .............................................................................103 5.1 Functioning of the keyboard.......................................................................................................103 Multifunctional graphics display: ...........................................................................................................103 Contrast setting: ....................................................................................................................................103 5.2 The start menu ...........................................................................................................................105 5.3 The mode menu .........................................................................................................................105 5.3.1 Changing a method..........................................................................................................106 5.3.2 Calculation menu item............................................................................................................127 5.3.3 TL alpha plus formulae editor.................................................................................................132 5.3.4 Documentation menu item .....................................................................................................138 5.3.5 Method management..............................................................................................................139 5.3.6 Create new method ................................................................................................................140 5.3.7 System settings ......................................................................................................................141 5.3.8 Measurement..........................................................................................................................150 5.3.9 Output .....................................................................................................................................151 5.4 The Cal menu.............................................................................................................................152

6..Method creation ....................................................................................................154 6.1 154

7.. In/Output for data communication ......................................................................155 7.1 Keyboard port.............................................................................................................................156 7.2 Power connector ........................................................................................................................156 7.3 Centronics-Interface...................................................................................................................156 7.4 RS-232-C-Interfaces ..................................................................................................................157 7.5 Loading the operating-system software via the RS-232-C interface .........................................157 7.6 Controlling the TitroLine alpha plus Titration Unit via the RS-232-C interface .........................158

8..Maintenance and care of the TitroLine alpha plus Titration Unit .............................159 8.1 Maintenance and care of the titrator section..............................................................................159

84 TABLE OF CONTENTS

8.2 Maintenance and care of the burette section.............................................................................159

9..Storage and transportation..................................................................................160

10Recycling and disposal ........................................................................................160

11Reference list ........................................................................................................161 Vers: 040714-E

Fig. 1

85

85Chapter 1 Technical properties

1 Technical properties of the TitroLine alpha plus Titration Unit 1.1 Summary The design of the TitroLine alpha plus Titration Unit is compact and very solid, and the device is highly versatile and variable to use. Its potential stretches from simple end-point titrations (EP) such as the de-termination of the total acid in wine, up to highly complex and difficult, non-aqueous titrations such as the determination of the total acid and base number in oils (TAN/TBN). As a matter of course, the automatic TitroLine alpha plus Titration Unit is also the ideal tool for pH-stat applications such as the determination of the enzyme activity, or for dead-stop titrations, such as the water determination according to Karl Fischer (KF).

The possibilities include pH, A, Karl Fischer, and pH-stat titrations with up to 50 methods which can be stored in memory. Examples of the possible applications of the TitroLine alpha plus Titration Unit include: 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 determinations Other mV titrations, e.g. chloride, halogenides next to each other Titrations using ion-sensitive electrodes, e.g. calcium, fluoride, copper, lead ions Water determinations according to Karl Fischer, bromine number in oils pH-stat titrations, e.g. for use in biochemistry or on soil samples indices such as OH number, iodine number, or saponification numbers. These methods are just examples; a lot of further applications can be found in food technology, pharma-ceutics, biochemistry, fotofinishing, environment, quality control, and process monitoring. Owing to its connections the TitroLine alpha plus Titration Unit is very versatile to use.

One of the two RS-232-C interfaces (Computer) is used for extensive data communication with a com-puter (Personal Computer) The second RS-232-C interface enables up to 16 SCHOTT-Instruments devices to be operated within one daisy chain: TITRONIC universal, TITRONIC T110 plus, TITRONIC 110/T 200 and TW al-pha/TW alpha plus sample changer. It may also be used for connecting an analytical weighing-balance. The Centronics interface is used for the documentation of results, data, and curve printouts using a printer with a parallel interface. The standardized socket for a standard PC keyboard (German keyboard layout) enables simple parameterisation for many functions. One of the two 2-channel jack sockets can be used to operate a TM 125 magnetic stirrer or a TM 128 stirrer plus the TM KF titration rig. The other 2-channel jack socket can be used to connect a TM 125 magnetic stirrer and to control the TM KF titration rig (on/off). The stirring speed can be set on the stirrer/titration rig assembly. The illuminated graphics LCD display with its corresponding dialogue menus and status displays en-able safe operation of the TitroLine alpha plus Titration Unit.

SCHOTT Instruments GmbH Hattenbergstrae 10

55122 Mainz Deutschland, Germany, Allemagne

05. August, August 5st, 5 Aot 2002 AGQSF 0000-A070-00/020805

KONFORMITTSERKLRUNG DECLARATION OF CONFORMITY DCLARATION DE CONFORMIT

Wir erklren in alleiniger Verantwortung, dass das Produkt

Titrator

TitroLine alpha plus

auf das sich diese Erklrung be-zieht, bereinstimmt mit den Nor-

men

und mit dem normativen Dokument

We declare under our sole responsibility that the product

Titration Unit


to which this declaration relates is in conformity with the standards

DIN EN ISO 8655, Teil 3

and the normative document

Nous dclarons sous notre seule responsabilit que le produit

Titrateur


auquel se rfre cette dclaration est conforme aux normes

et au document normatif

Technische Daten

17.12.2003




Translation of the legally binding german version Technical data of the TitroLine alpha plus Titration Unit Release 17.12.2003

Conformity: DIN EN ISO 8655, Teil 3 Konformittszeichen

CE-Sign: EMC - Compatibility according to the directive 89/336/EEC of the Council;

Interference emission according to the EN 61 326 standard, Part 1 Jamming resistance according to the EN 61 326 standard, Part 2 Low-voltage directive according to the Directive 73/23/EEC pf the Council, as amended by the Directive 93/68/EEC of the Council

Testing basis: EN 61 010, Part 1 Country of origin: Made in Germany

The following solvents / titration reagents may be used: All common titration solutions Water and all non-aggressive inorganic and organic liquids can be used as solvents. When working with in-

flammable substances, the explosion-protection regulations of the employers' liability insurance association of the chemical industry have to be observed.

With liquids with a higher viscosity ( 5 mm/s), a low boiling point or a tendency to exhalation the filling and dosing speed may be adapted.

Liquids with a viscosity above 20 mm/s cannot be dosed.

Measuring input: A and B channel, pH/mV input with 16-bit transducer for high-precision readings resolution, galvanic insulation of the B channel from the A channel. 4 smoothening levels of the measurement signal are possible in the A channel. Termination: Electrode socket according to DIN 19 262; with the BNC version, a socket in-sert (Z 860) may be used. Reference electrode 1 x 4 mm socket

A channel Measurement range Over-range Display reso-lution

Measurement accuracy* without

sensor probe

Input resis-tance

[] pH A PH 0,0 ... 14,00 - 1, 0 ... 14,00 0,001 0,02 1 Digit > 1 1013 mV A U [mV] - 2000 ... 2000 - 2020 ... 1920 0,1 1,0 1 Digit > 1 1013

B channel Measurement range Over-range Display reso-

lution Measurement

accuracy* without sensor probe

Input resis-tance

[] pH B PH 0,0 ... 14,00 - 1, 0 ... 14,00 0,001 0,02 1 Digit > 1 1013 mV B U [mV] - 1800 ... 1800 - 1820 ... 1820 0,1 1,0 1 Digit > 1 1013

To ensure maximum accuracy of the readings we recommend to allow some reasonable time for the TitroLine alpha plus Titrator to warm up. Please note with regard to the B measurement channel: To maintain the galvanic insulation from the A channel, the connector of the temperature sensor probe must NOT be connected to the common earth in the case of single-rod electrodes with an integrated temperature probe. In this case a separate PT 1000 tempera-ture probe has to be used for temperature measurement or temperature compensation.




Translation of the legally binding german version Release 17.12.2003

Measurement input: Temperature probe - connector for a Pt 1000 resistance thermometer Connection: 2 x 4 mm - sockets and 1 x 2 mm socket.

Measurement range

Display resolution Measurement ac-curacy* without sensor probe

T [C] - 75 ... 175 0,1 0,2 K 1 Digit

Measurement input: Karl-Fischer (Dead-stop) connector for double platinum electrode Polarisation voltage variably adjustable from 10 200 mV.

Connector: 2 x 4 mm - sockets.

Measurement range

Display resolution Measurement ac-curacy* without sensor probe

I [A] 0 ... 100 0,1 0,2 1 Digit

* The measurement incertainty of the sensor probe has to be taken into account as well. Display: LCD graphic display with background illumination, approx. 69 x 69 mm, 128 x 128 pixels. Readings display: 4 digit display with floating point and unit, 14 mm high, 9 alphanumeric lines each

6 mm high, 4 softkeys for speedy operation of the titration unit during parameterisation and titra-tion. Additional control displays, contrast setting.

Calibration: Automatically with 2 buffer solution out of 8, sequence during calibration optional, 3 freely defin-

able buffers can be input. Default buffer solutions according to DIN 19 266 and NBS, or with integer pH values:

pH = 1,00; pH=4,00; ph=4,01; pH=6,87; pH= 7,00;

pH= 9,18; PH=10,00; Connections: A Measurement input: pH/mV input with electrode socket according to DIN 18 262 / or BNC

B Measurement input: pH/mV input with electrode socket according to DIN 18 262 / or BNC KF/A measurement input: Karl-Fischer (Dead-stop) connector for double platinum electrode (Connection sockets: 2 x 4 mm) Pt 1000 measurement input: Temperature sensor probe for P 1000 resistance thermometer (Connection sockets: 2 x 4 mm, 1 x 2 mm)





Power supply: Switch-over at the bottom panel of the device - 115 Volt, 50/60 Hz, fuse: 0.5 AT. - 230 Volt, 50/60 Hz, fuse: 0.25 AT. Power consumption 42 VA

RS-232-C-Interface: - RS-232-C interface with galvanic insulation via opto-coupler - Daisy-chaining is possible

Data bits: Adjustable, 7 or 8 bits (default value 7 bits) Stop bits: Adjustable, 1 or 2 bits (default value 2 bits) Start bit: Fixed 1 bit Parity: adjustable, even / odd / none Baud rate: adjustable: 1200, 2400, 4800, 9600, 19200 (default 4800 baud)

The baud rate can be changed via the software address (0 to 15), per software download and upload protocol: for operating-system software and methods pa-rameters - Protocol for operating-system upload. - Connections: RS-232-1 computer, daisy-chain input RS-232-2 TitroLine alpha plus Titration Unit, - TW alpha plus + TW alpha sample changers - TITRONIC T 110 plus piston burette, - TITRONIC T 110, T 200, T universal piston burette - Weighing-scales of the Mettler, Sartorius, Kern, Ohaus types; additional types upon request

Stirrer control: Stirrer off: Voltage smaller than 1.3 Volt Stirrer on: Voltage 3.3 Volt Printer connection: Printer Centronics interface (25-channel D-SUB socket) for connecting an Epson, HP-compatible printer with a centronics interface (parallel interface). Keyboard connection: Keyboard PS2 socket for connecting a TZ 2835 keyboard from

SCHOTT Instruments, or a German PC keyboard. StirrerConnection: Stirrer Start/stop signal for TM 135 and TM KF stirrers (TZ 1581)

12V DC out Power supply for a TM 135, TM 128 and TM KF stirrer (with cable TZ 1581)

Casing material: Stainless steel/polypropylene; with interior metallization for shielding Front membrane: Polyester Casing dimensions: 145 x 360 x 295 mm (W x H x D), height including dosing unit Weight: Approx. 4.1 kg for basic device

Approx. 4.9 for complete device including interchangeable unit (including empty re-agents bottle)

Environment: Ambient temperature: +10 ... +40 C for operation and storage Air 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





Interchangeable units Compatibility: The units are compatible with those of the T 100, T 110/200 and T 100 plus

piston burettes

Coding of the cylinder size: Automatic, mounting for the glass cylinder bears unmistakable code

Valve: Volume-independent cone valve made of fluorcarbon polymers

Cylinder: made of DURAN

Hoses: FEP hose set with UV-protection

Bracket for storage bottle: To fit glass bottle to DIN 12 036 and DIN 12 039 or rectangular glass or plastic bottle

Fastening for interchangeable unit: With automatic checking feature Materials: Borosilicate glass, fluorocarbon polymers, PPS, high-grade steel, polypropylene, acrylic glass, Dimensions: 145 x 260 x 270 mm (W x H x D) without reagents bottle Weight: Approx. 0.80 kg for TA 20 interchangeable unit (without reagents bottle) Dosing accuracy: According to DIN EN ISO 8655, Part 3 Correctness: 0,1 0,3 % Precision: 0,05 - 0,1 % (depending on the interchangeable unit being used)

Dosing accuracy of the TitroLine alpha plus Titration Unit when used with TA and TA plus inter-changeable units:

Inter-changeable unit

type no.

Volume

[ml]

Tolerances of the i of the glass cylinders

[mm]

Dosing mistakes* referred to 100 %

volume [%]

Reproducibility

[%]

TA 01 1,00 0,003 0,3 0,10

TA 05 plus 5,00 0,003 0,15 0,07

TA 10 plus 10,00 0,003 0,1 0,05

TA 20 plus 20,00 0,003 0,1 0,05

TA 50 plus 50,00 0,003 0,1 0,05

91

Chapter 1 Warning and safety information

1.2 Warning and safety information For safety reasons the TITRONIC T 110 Piston Burette may only be opened by authorised persons who are in charge of the observance of the relevant safety conditions. For example, work on the electrical equipment may only be performed by trained specialists. If the unit is opened without authorisation, or if it is damaged mali-ciously or through negligence the guarantee is void. The TitroLine alpha plus Titration Unit conforms to protection class I. It has been built and tested in accordance with EN 61 010 - 1:1993, Part 1, Protection Measures for Electronic Measuring Instruments and left the factory in perfect technical condition. In order to maintain this condition and ensure safe operation, the user must ob-serve all the instructions and warnings contained in these operating instructions. Before switching on it is to be ensured that the operating voltage matches that of the mains voltage. The oper-ating voltage is specified on the type plate at the bottom panel of the titration unit. The setting can be seen from voltage selector at the bottom panel of the titration unit. The mains plug may only be inserted into a socket with an earthed contact. The earth must not be eliminated by using an extension cable without an earthed wire. Any discontinuity in the earth wire inside or outside the device or the release of the earth wire connection may lead to the TitroLine alpha plus Titration Unit becoming hazardous. The earth wire must not be broken intentionally. When changing the operating voltage, the fuses have to be replaced in accordance with the information on the rear panel. The unit must not be stored or operated in wet rooms. If it has to be assumed that it is not possible to operate the TitroLine alpha plus Titration Unit safely, it is to be taken out of operation and secured to prevent its being put back into operation unintentionally. Please observe the corresponding operating instructions of the devices to be connected, i.e. weighing-scales, printer, keyboard, computer, electrodes. For safety reasons the TitroLine alpha plus Titration Unit is only to be used for the purposes described in the present operating instructions. The TitroLine alpha plus Titration Unit is equipped with integrated circuits ( flash memory and EPROMs). These circuits (ICs) can be deleted by X-rays or radioactive rays. X-rays or other high-energy rays are fully retained by the casing. When working with fluids other than conventional titration media, especially the chemical resistance of the ma-terials of the TitroLine alpha plus Titration Unit must be taken into account (please refer to chapter 1.1) When using liquids with a high vapour pressure and/or matters or mixed matters not qualified for use under chapter 1.1, the user will be responsible for the safe and proper operation of the TitroLine alpha plus Titration Unit. Each time the piston rises inside the cylinder a microfilm of the dosed fluid will remain on the internal wall of the cylinder, but this has not influence on the dosage accuracy. The negligible residue of fluid may evaporate, how-ever, and thus penetrate into the zone beneath the piston and corrode or dissolve the materials used there (cp. chapter 8, "Maintenance and care of the TitroLine alpha plus Titration Unit").

92

Chapter 2 Set-up and first operation of the TitroLine alpha plus Titration unit

2 Set-up and first operation 2.1 Unwrapping and set-up of the TitroLine alpha plus

Titration Unit Functions and dimensional accuracy of the TitroLine alpha plus Titration Unit as well as that of all accessories and peripherals are thoroughly checked in the factory. Please pay attention not to leave any of the small accessories in the package. For the scope of delivery, please refer to the enclosed parts list. The TitroLine alpha plus Titration Unit may be placed on any flat surface. The mains supply cable plugs into the cold-device socket at the back panel of the device. Prior to switching the device on, it has to be ensured that the operating voltage of the device matches that of the mains voltage. The operating voltage is indicated on the type plate (ref. to bottom panel).

2.1.1 Installation of the stand rod

Fig. 2 2.1.2 Connection of the optional TM 135 titration rig. The TM 135 magnetic stirrer is attached to the bottom of the titration unit using the appropriate TZ 1560 con-nection sheet. To begin, fasten the connection sheet to the titration rig, then attach it to the bottom panel of the titration unit. Screw the stand rod into the TM 135 titration rig. Power is supplied by a TZ 1581 connection ca-ble. Subsequently, push the TZ 303 electrode holder onto the stand rod. To do so, press the grey key. Power is supplied by a TZ 1581 connection cable. If the stirrer is to be switched on/off from the titration unit, the second TZ 1581 connection cable is to be used. The stirring speed cannot be controlled. The desired stirring speed is set at the adjustment knob. 2.1.3 Installation of the titration clip Subsequently, push the TZ 303 electrode carrier onto the stand rod. To do so, please press the grey key. Slip the Z 303 titration clip onto the stand rod. After pressing the retention key, it can be moved easily.

Working without titration rig: The TZ 1516 type no. stand rod bracket is mounted to the bottom plate of the titration unit using the screw. To do so, lay the titration unit on its left side, then fasten the stand rod bracket to the bot-tom panel. To complete, screw in the stand rod.

Working with the TM 135 titration rig: please refer to chapter 2.1.2.

93


2.2 Installation of the TM KF Titration Stand and of the titration vessel As a rule, you will place the titration rig directly to the right of the TitroLine KF Titrator.

Seen from the front: Connect the right hose olive located at the back panel of the titration rig and the hose olive on the desicca-

tion bottle (figure 3, item 9) using one of the short PVC hoses (figure 3, item 10 and item 3). Connect the other hose olive of the desiccation bottle to the hose olive of one of the square bottles (solvent

bottle) using the other short PVC hose (refer to figure 3, item 2). Connect the left hose olive at the backside of the titration rig and the hose olive on the waste bottle using

the longer PVC hose (figure 3, item 10 and 6). Insert the stand rod (figure 3, item 4) into the corresponding holder on the titration rig, then tighten it manu-

ally.

Use the knurled screw to fasten the titration vessel to the stand rod in such a manner that the bottom of the titration vessel sits directly on the upper surface of the titration rig.

Adjust the dosing and waste hoses as is shown in figure 3. This applies to the titration vessel, the storage bottle, and the waste bottle. Subsequently, tighten the screwed connections with the hoses on the titration vessel and on the bottles.

*) Fill the desiccation bottle (figure 3, item 9) up to two thirds with the enclosed 0.3 nm molecular sieve. Also, fill some molecular sieve into the desiccation pipe for the titration vessels. First, you should put some

of the enclosed cotton into the desiccation pipe, so no molecular sieve will fall into the titration vessel.

Fill the solvent into the 1 l solvent bottle. Instead of the square laboratory bottles coming with the device, it is also possible to use other reagents bottles with a GL 45 or S 40 (TZ 1795 adapter) thread.

If you wish to inject liquids through a septum, unscrew the large screwed connector, and then put one of the enclosed septums into the opening. You can remove the black O-ring before. Subsequently, tighten the screw connector manually.

Screw the titration hose onto the valve of the titrator. All the other hose connectors as well as the threaded connections of the TZ 1770 or TZ 1772 titration vessel are already pre-mounted.

94


Fig. 3 Hose connections (seen from behind) 1 PTFE filling hose: Storage bottle titration vessel 2 PVC hose for overpressure in the storage bottle: Storage bottle receiver drier 3 PVC hose for overpressure in the storage bottle: Receiver drier titration vessel 4 Stand rod 5 PTFE suction hose: Titration stand waste bottle 6 PVC hose for vacuum in the waste bottle: Titration stand waste bottle 7 GL 45 screwed connections with adapter for hose connections and screw connections 8 Storage bottle 1 l, brown 9 Receiver drier 100 ml *) see previos page 10 Olives for connection of the PVC hoses 11 Mains-unit connector U = 12 V- 12 Waste bottle 1 l, bright

95


Power supply of the TM KF Titration Stand The power supply to the titration stand comes from the titrator. Connect the titration stand to the titrator using the enclosed low-voltage cable (please refer to figure 2, item 11 and figure 4, 12 V DC). Working with the titration stand

Dosing: Press the front part of the key rocker to pump solvent into the titration vessel. Additive dosing will continue as long as you press the key.

suck off: Press the back part of the key rocker to suck off solvent into the waste bottle. sucking off will con-tinue as long as you press the key.

Note: Please observe the filling level of the waste bottle. Prior to extracting the finish-titrated solution, please ensure that the waste bottle can accommodate at least this quantity of solution.

The built-in magnetic stirrer (stirrer for magnetic stirrer rod) will stir the liquids in the titration vessel. Use theturning knob on the front panel of the titration stand to set the stirring speed (figure 4). Fig. 4

Dosing Extraction

Stirring speed

Malfunction Problems might occur if the hoses were connected improperly, or if the pressure or vacuum systems should contain a leaking screw connection. This will lead to a cessation of the solvent discharge after only a few sec-onds after the start of the pump. So when checking the hoses, please pay particular attention to the tightness between the flanged connections and their adapters. The same applies to the hose connections of the receiver drier or the interchangeable desiccating tube unit.

Note: Wrinkled hoses will cause dosing and extraction problems. The tightness of the hoses including their connections should be checked on a regular basis. Replace defective items if necessary.

If solvent should coast out of the storage bottle during additive dosing, please place the bottle on a level below that of the titration vessel. Likewise, if solvent should coast out of the storage bottle during the change from dosing to extraction, you should wait for a few seconds during the change.

96


2.3 TA plus Interchangeable Unit:

Fig. 3 Items 1, 2, 3, 10, 11, and 12 are only available within the whole set.

1 Built-in valve TZ 3000 with automatic control 2 Hose between valve an titration tip 3 Titration tip 4 Inscription field 5 Locking feature with lower burette section 6 Cylinder pressure screw 7 UV- protection 8 Receptacle for reagents bottle according to DIN 12 036 and DIN 12 039 or rectangular glass or plastic bottle 9 Adjustment of reagents bottle 10 Suction hose to valve 11 Clamped screwing connection 12 FEP hose for valve cylinder connection

1

2

3

45

6

7

8

9

10

12

11

97


2.4 Fitting and replacing an interchangeable unit An interchangeable unit is installed by simply slipping it on over the guide rail from front to back. The installa-tion is completed when you can clearly here the mechanical retention device snap in. If you have problems during installation, the position of the PTFE piston in the glass cylinder has to be ad-justed. To adjust the piston, it is to be drawn downwards using the piston drawer provided, until the top edge of the PTFE piston is approx. 8 mm below the upper edge of the black pressure screw. The actual adjustment is now made by simply pressing the interchangeable unit onto a flat surface, for example a table top. To replace an interchangeable unit, the piston in the cylinder has to be set to the lower starting position. To do so, one has to initiate the filling operation (also refer to chapter 2.4, "Initial filling and rinsing of the entire inter-changeable unit"). Subsequently, the interchangeable unit can be easily removed towards the front by pressing the retention key on the left side of the unit (Fig. 4).

After removing the interchangeable unit, the signal tone will sound, and the display indicates that no in-terchangeable unit is presently in place. After inserting a different (or the same) interchangeable unit the bu-rette size is automatically recognised and displayed. When working with a square glass bottle, please use the clamping ring provided to prevent the reagents bottle from falling out of the holder.

Fig. 4

Caution: After each replacement, an automatic filling plus a float balancing will take place. For this reason, please DO NOT remove the interchangeable unit immedi-ately, but only as soon as the de-vice is again ready for the start of a titration. If a new interchangeable unit is installed without reagent, you have to initiate an "Initial filling" or "Rinsing" of the Piston Burette (please refer to chapter 2.4). The front parts of the inter-changeable units contain a cod-ing which communicates the size of the installed cylinder to the bot-tom section of the burette. This ensures accuracy of the dosed volume at any time.

98


2.5 Replacing the glass cylinder The hose between the cylinder and the valve is to be unscrewed from the cylinder (see Fig. 3, item 12). The UV protection is to be pulled down, and the black press screw (cp. Fig. 3, item 6) for the glass cylinder is to be loosened by turning it anti-clockwise and pulling it downwards. The cylinder with the piston inside can now be removed. A new cylinder with a piston is to be fitted in reverse order and then adjusted as described under chapter 2.3 "Fitting and replacing an Interchangeable Unit". Basically, it is to be ensured that only the intended cylinder size is fitted within an interchangeable unit, since otherwise the code in the interchangeable unit will not conform with the cylinder size. The result would be an incorrect dosage. For reasons of dosage and analy-sis accuracy, it is always recommended to replace the PTFE piston at the same time when a defect glass cyl-inder is replaced. This applies in particular if the glass is broken, since the sealing rings of the PTFE piston may be damaged by splinters of glass. Please note: As a rule, the hoses and cylinder contain chemicals which may escape or be sprayed around when the unit is dismantled. The relevant safety precautions for dealing with these chemicals have to be ob-served.

Fig. 5 Installation of the glass cylinder

99


2.6 Initial filling and rinsing of the complete interchangeable unit Initial filling of the burette unit is carried out by a rinsing program. You initiate the rinsing program using the keyboard in the menu item. After the start of the rinsing routine, and depending on the setting, the ap-propriate number of upward and downward piston strokes will be carried out. During the execution of the first-fill or rinsing program you have to place a waste container under the titration tip. After the start of the rinsing program, the display will show , and the piston will move to its bottom position.

Subsequently, the contents of the cylinder (air or old reagent) will be ejected, with fresh reagent being taken in. As soon as the top piston position is reached, the filling procedure is started during which fresh reagent is drawn in. When the lower piston position is reached, the complete contents of the cylinder will be ejected once again. Another filling cycle will take place, and after float balancing the message will appear in the case of interchangeable units from 1 to 10 ml, or with interchangeable units of 20 and 50 ml, respectively, and the display will show

Please note: The initial filling / rinsing program is not suitable for changing titration media, solutions, and liq-uids which widely differ in composition and/or concentration. Such cases require a careful cleaning of the parts coming in contact with the titration agents, such as intake tube, valve, glass cylinder, and titration tip (for disas-sembly procedure, please refer to chapter 2.4, Replacing a glass cylinder). After the execution of the program, the TitroLine alpha plus Titration Unit is ready for the next titration or dosing processes.

100


2.7 Combining the TitroLine alpha plus Titration Unit with other devices The TitroLine alpha plus Titration Unit may be combined with numerous devices of the SCHOTT-Instruments programme, please refer to the table below: Fig. 6

What is to be connected? Cable

PC with cable, length 5 m TZ 3088 RS 1 or with cable, length 10 m TZ 3089

Daisy-Chain, please refer to RS 2

TitroLine alpha plus, T 110 plus TZ 3084 TW alpha plus T 110, T 200, TW alpha TZ 3086 T universal TZ 3087 Sartorius weighing-balance TZ 3082 Mettler AT weighing-balance TZ 3083 Mettler AB-G, PG weighing-balance etc. TZ 3081

RS 2

Centronics Printer

e.g. Epson Stylus Color 880/980, HP-Deskjet 920 / 970 etc.

Centronics-Cable

Keyboard keyboard TZ 2835

TM 135, TM 128 TZ 1581 Stirrer TM KF TZ 1581

Please note: If a keyboard, printer, or weighing-balance is connected to the TitroLine alpha plus Titration Unit, the titration unit has to be switched off and on again in order to star the initialisation of the system. For a functional description, please refer to chapter 5, Working with the TitroLine alpha plus Titration Unit. In addition, please note the information provided with the devices being connected to the TitroLine alpha plus Ti-tration Unit.

Keyboard Stirrer

CentronicsRef

Electrode A

Ref

Electrode

Pt

KF

Printer

Stirrer Key-

1

RS-232-C

2

12V out

230V:0.25 115V 0 5

OI

Printer

101

Chapter 3 Construction of the TitroLine alpha plus Titration unit

3 Construction of the TitroLine alpha plus Titration Unit

Fig.7 The illustration shows the TitroLine alpha plus Titration Unit with an interchangeable unit TA 20 plus, a TM 135 magnetic stirrer, the TZ 2835 keyboard, the TZ 303 electrode holder and one measurement electrode.

102

Chapter 4 The connections of the TitroLine alpha plus Titration unit

4 The connections of the TitroLine alpha plus Titration Unit 4.1 Measurement-amplifier, A input channel , electrode signal The A input channel of the measurement amplifier enables a pH/mV electrode to be connected to the TitroLine alpha plus Titration Unit . A maximum of 1,000 measurement values can be recorded during one titration. If more measurement values are present, they will be stored through an automatic data reduction.

In the case of the pH/mV A channel, the smoothing of the measurement signal can be adapted in four stages to the requirements of the titration. This is done through the user surface of the TitroLine alpha plus Titration Unit.

Smooth-ing stage

Input delay Setting time Suitable for titrat-ing media

Examples

0 none 0 s aqueous, polar Acid-base titration in water 1 weak approx. 0,5 s aqueous,

alcoholic Acid-base titration in alcohol and weak ac-ids or bases in water

2 medium approx. 2,5 s solvent with non-polar portion

Titrations in alcohol/water mixtures

3 strong approx. 5 s non-aqueous, non-polar

TAN, TBN, acid-base titrations in halogen-ised solvents or aromatics

The selectable input delay (setting time) causes a smoothing of the measurement signal. The respective set-ting times of the four smoothing stages are as follows:

This means that the input delay causes a delayed response time of the input amplifier. For instance, in the case of smoothing stage 3 (5 s), 99% of the measurement signal are obtained only after five seconds. In the case of a very high variation of the measurement values, e.g. at the start of the titration, the minimum setting time has to be ensured by suitably long waiting times. For this reason, one should work with a fixed drift control, with the delay time being been at least as long as the setting time resulting from the selected input delay.

4.2 Measurement-amplifier, B input channel , electrode signal The B input channel of the measurement amplifier enables another a pH/mV electrode to be connected to the TitroLine alpha plus Titration Unit . The B measurement input is galvanically insulated from the measurement channel A. This ensures that the two measurement signals will not affect each other. To maintain this galvanic insulation, the two measurement potentials must not be connected to each other. The smoothing of the measurement signal cannot be adapted any further in the case of the B pH/mV meas-urement input. If the measurement signal needs to be smoothened, the A measurement input has to be used.

.

103

Chapter 5 Working with the TitroLine alpha plus

5 Working with the titration unit 5.1 Functioning of the keyboard In combination with the TitroLine alpha plus Titration Unit, the keys of the keyboard supplied with the unit have the predefined functions as specified in the table below:

Start of the method being displayed Cancellation of the method

Cancellation of calibration Direct move to method creation Filling of the dosing unit The current titration parameters are stored,

and you return to Method creation. Display of the overview menu

to parameterise a method. Jump to the system parameters menu item Display of the menu for

calibrating the A and B measurement channels + / - Change of sign DOS Takes you to the Dosing menu Num Lock

Prt Sc Sys Rq

Scroll Lock

returns you to the previous menu level. < > < > Cursor key

Scrolling within the overview menu to select specific menus Within the specific menu items: Move the cursor to select parameters

0...9 decimal point

Input of method numbers, sample numbers, and parame-ters.

or < >

Confirmation of the input parameters. Within the present operating instructions, both keys are referred to as .

or < Backspace >

Deletion of the input digit/character above the cursor.

Letters, ASCII characters

Letters, ASCII characters

Alphanumeric input is possible. In the case of TZ 2825, upper case only. With the MF keyboard, both upper and lower case.

All other keys Without any function. Multifunctional graphics display: The display is a LCD graphics display with a resolution of 128 x 128 pixels. It can be used to display charts,

such as an on-line curve during titration. The scaling of this graph depends on the end value which was specified as an end criterion in the case of a

pH or mV titration. If the pH or mV end criterion is supposed not to appear within a method, it may be de-activated retrospectively. However, the previously specified pH or mV end value will remain stored within the respective method and use for all future scaling operations.

It is also possible to display the current measurement value and the consumption instead of the on-line curve. (The display can be switched over during titration using the key.)

Contrast setting: The contrast is set using the Page-up or Page-down key, respectively. If nothing visible is left on the display, please press these keys until something becomes visible.

104


The menu system:

On the right side you can see four softkeys which are assigned to the keys as a function of the menu level you are currently on; they are designed to facilitate the devices parameterisation during input. The parameters are inquired and input in a dialogue. This kind of inquiry is particularly user-friendly, since after you will always be returned to the starting point each pass; in this way it is impossible to get lost.

One step backwards at input, or jump back to the preceding selection menu

Upward selection

Downward selection

Take over value (ENTER)

Start calibration

Parameterise, rinse, dose

START/STOP: Start of titration

Using STOP, you can stop running titration, dosing, and rinsing processes.

Head line Line 1 01 Headline Line 2 Input Line 1 Input Line 2 Input Line 3 Input Line 4 Input Line 5 Input Line 6 Input Line 7 Status Information

003

The display is divided up into 9 lines, with the two upper heading lines containing information about the currently active user-menu level. The lowest line shows status informations.

105


5.2 The start menu In principle, it is always possible to adapt the TitroLine alpha plus Titration Unit to your specific require-

ments. Yet, you also have the possibility of accessing the database containing approx. 100 default stan-dard methods for various applications quickly and conveniently. In this context, you can modify each method in such a manner that it will fit to your very specific tasks.

5.3 The mode menu / is used to select the mode menu. This level can only be accessed using a connected key-

board. The mode menu can be used to input all settings required for parameterisation, or for a change or the administration of methods as well as for the input of calculation and documentation parameters.

This menu may also be used to access the system settings. Below you find an overview of the major menu items.

mode 01 change 1 method method management create method system settings measuring output new calculation

003

change method: This item can be used to change an existingmethod.

management: Selection of standard methods, print, delete,copy and export methods.

new: Creation of a new method: system settings: Used to select the system parameters of the

titrator measuring: Performance of measurements (pH, mV, etc.) output: Printout and export of the curve and the titration re-

sults of the last titration, as well as printout and display of theCAL data.

New calculation: A re-calculation will be performed, if neces-sary with a modified formula. The specified documentationwill be prepared once again

Titroline ready 01 no. 1 Method 1 dosing unit size 20 ml

001

Start menu: The method which is available is always the one which was being worked with before the device was switched off. The upper right corner shows the method which is presently active. After entering the desired method number, the correspond-ing method name will be displayed. The desired method is selected by pressing the / keys. From the level of the Start menu, titration is started by pressing the key. The rinsing and dosing parameters and the rinsing and dos-ing functions can be set after pressing the key. Pressing the key will initiate the calibration of the

106


new method 01 method number 1 enter method name Methode -----1

049

At this point a 18-digit alphanumeric method name can be in-put.

You may enter a different method number. The arrow keys will take you to the next menu line.

If the selected method is to be changed, pressing the or < > key will take you to the following menu item.

5.3.1 Changing a method

method creating 01 selection sample handling/TW titration parameter calculations documentation reset statistics? method link

032

Sample handling/PW: This item is used to enter the sample ID, the type of the sample quantity, and the kind of sample changer.

Titration parameters: Selection of the titration type and the pa-rameters: selection of the titration type (pH, mV, A, Karl-Fischer or pH-Stat)

Calculation: This item is used to calculate the parameters of the selected method, or for the creation, inquiry, or administration of formulae

Documentation: Selection of the type of documentation reset statistics?: This item can be used to reset the statistics

memory of the current method. Method link: With more complex jobs, it is possible to link sev-

eral methods at this point.

method creating 01 Passwort Passwort eingeben

048

To activate the password feature, please use the Password item of the system menu (please refer to chapter 5.3.5, Hard-ware settings)

107


Overview of all elements of a method 50

Sample parameters/TW: General settings, sample ID, sample quantity, sample changer

65

Titration parameters: Control of the titration (type, speed) 106 Calculation: Calculation of the results 107

a. Documentation: Output of the titration including result

441

Statistics reset: Reset of the statistics memory of the current method.

108

Method interlinkage: Run next method automatically.

* The numbers are equivalent to the numbers of the menues displayed. A method is not completely defined and parameterised unless or until all the above settings have been made. Sample parameters/TW menu item At this point a decision is made as to the use of a sample changer and the processing of the sample. This is the only menu which can be used to influence the attribution of sample descriptions and the selection of a sample quantity or sample volume.

If no sample changer is selected, the system will take you di-rectly to the menus used for the input of the sample descrip-tion and the sample weight or volume, respectively.

If the use of the TW alpha sample changer is specified, the first thing to do is to select a plate size. At the time the method is started, the TL alpha sample changer will be pro-grammed to the selected plate size.

If COD titration is to be performed, please select the position.

sampler 01 none 12 samples 16 samples 24 samples 24 samples COD

050

032*

108


Parameterisation of the sample ID Parameterisation of the sample quantity (sample volume/sample weight) Parameterisation of the sample quantity (sample weight)

titration parameter 01 sample ID manual automatic no

079

Manual: A manual sample ID is prompted for input upon the start of a method and has to be entered using the external keyboard.

Automatic: Only active if a sample changer is being used. At the beginning, a master value is to be input which will then be counted upwards automatically.

None: Titration will start directly, without the possibility of en-tering a sample ID

titration parameter 01 sample amount weight manual weight automatic weight fix volume manual volume fix no

179

Sample weight manual: The weighing-in data which are in-quired at the start of the method have to be input manually each time.

Sample weight auto: Upon the start of the method, the bal-ance data transmitted from a connected balance will be taken over automatically.

Sample weight fixed: Within the method, the input mass is used for each titration. If selected, a value has to be input at this point. If no value is input, 1.0 will be substituted in order to avoid a division by 0 in the calculation.

Sample volume manual: The sample volume has to be input manually after the start.

Sample volume fixed: The sample volume entered here will be used for each titration within the method. If selected, a value has to be input at this point. If no value is input, 1.0 will be substituted in order to avoid a division by 0 in the calcula-tion. The calculation will take into account the sample quan-tity or volume if the formula contains a "Q". The quantity or volume, respectively, will be multiplied by the factor "Q".

None: No sample quantity or sample volume is desired

titration parameter 01 weight fix weight in g: 1.00000g

203

At this point, the value for the desired sample quantity is to be input. The sample weight entered here will be used as a fixed sam-ple weight for all subsequent titrations of this method.

109


Parameterisation of the sample quantity (sample volume) Input for multiple determination (statistics) As soon as you have made the desired settings for the balance data and the sample volume, you will be taken to the following menu item: Parameterisation of the sample changer If a sample changer is to be used, you will be taken to the input of the desired stirring speed after selecting the plate size to be used:

Please note: Proper mixing of samples prior to the start of the titration will have a direct influence on the titration result!

You can select one out of 10 possible stirring-speed stages. A value of 6, for instance, makes sense

Please note: When using a TW alpha sample changer with stirrer, a mini-mum stirring time of 15 seconds should be set from below, since this stirrer has a startup time of approx. 10 seconds. Likewise, when using high-walled COD containers, the opti-mum minimum stirring time should be determined in experi-ments.

The stirring speed refers only to the stirrer in the sample changer. The stirring speed on a connected TM 135 is to be set manually.

titration parameter 01 stirrer speed step 1-10 enter value : 7

104

titration parameter 01 number titrations multi determinat.

1

208

If more of than one determination is to be made on one and the same sample, this is the point to input the number of de-terminations to be made.

The results obtained are used to perform a statistical calcula-tion of the mean value and the standard deviation as soon as a value greater than 1 is entered.

The calculation, however, has to specify the formula to be used for the preparation of the statistics!

titration parameter 01 volume fix volume in ml: 1.000 ml

204

At this point, the value for the desired sample volume is to be input. The sample volume entered here will be used as a fixed sample volume for all subsequent titrations of this method.

110


Parameterisation of the rinsing function If the rinsing function is selected, the required parameters for controlling the various rinsing operations are in-quired one after another. Once the rinsing type or number of desired rinsing positions selected, you set the rinsing duration (max. 99 s). Warning: If the selected rinsing duration is too long, the rinsing liquid may spill over the titration vessel! If desired, you may subsequently determined the waiting position of the electrode.

Do not rinse: No rinsing will take place Rinse with TP: If you connect a rinsing device, for instance a

TP 20, you have the possibility of rinsing the measuring sen-sors and burette tips at the titration position. WARNING: Please note the capacity of the titration vessel!!

One position/two/three positions. At this point, the number of the desired rinsing positions is inquired. The possible rinsing positions always refer to the last three plate positions. If, for instance, in the case of a 16 sample plate, two rinsing positions are desired, the positions 15 and 16 are rinsing positions.

sampler 01 rinsing do not rinse rinse with TP one position two positions three positions

051

In order to avoid that the electrode will dry out after titration with its head up, you can define a position in which the elec-trode may remain, for instance over night. In practice, it makes sense after finishing titration on the first sample to replace the first sample by a KCl solution and to define the first position as "waiting position". After the titration of the last sample, the sample changer will move to the waiting position and immerse its head into the beaker glass.

sampler 01 waiting position first position second position no wait position

055

If a rinsing device is connected, the rinsing duration will determine the rinsing volume. Considering that in this case rinsing is done at the titration position into the sample on which titration was just finished, the max. capacity of the titration vessel should be observed. As a rule, 5 seconds should be sufficient. Using rinsing positions, the optimised rinsing time depends on the application.

sampler 01 rinsing time rinsing time in s : 5s

052

111


At this point, the parameterisation of the processes of the sample changer is completed, and you can proceed with the parameterisation of sample processing; please refer to "Sample description". Once sample processing has been parameterised, the parameterisation of the titration as such starts. 5.3.1.1 Titration parameters menu item pH/mV titration type The parameterisation of mV titration is done in analogy to pH titration

titration parameter 01 type of titration selection pH selection mV selection uA selection KF selection pH-Stat

065

- The present example illustrates the selection of pH or mV. - A titrations are performed using a double platinum elec-

trode and in the form of A deadstop titration (e.g. bromine index).

- KF titration is used for water determination with special

equipment. - pH Stat is a form of titration where a defined pH value is

kept constant over a specified period of time.

The starting position may be specified explicitly. In the case of method interlinkage it is possible to enter dif-ferent starting positions.

sampling 01 assign position start position 1

056

With the setting, the number can be re-defined for each titration process. The number will be inquired after each start of the method.

The number of the samples to be processed can be specified within the method.

sampler 01 number samples variable number samples 1

057

112


Initial measurement value Selection of the measurement channel Attenuation of the A measurement channel

titration parameter 01 initial meas. value yes no

244

At this point, you may select whether an initial measurement value is to be recorded prior to the start of titration.

An initial measurement value will be recorded "exactly" and also documented automatically. Before an initial value will be recorded, a specific drift value has to be fulfilled. The drift value is defined in terms of reading/time and is de-faulted internally in the form of quite a number of experience-based applications.

A measurement input: Channel for pH and mV titrations. B measurement input: Channel for pH and mV titrations.

The B measurement channel is galvanically separated from the A measurement channel.

titration parameter 01 select channel measuring channel A measuring channel B

246

titration parameter 01 input delay no / water weak / alcohol medium / organic strong / unpolar

248

These parameters are used to determine the response time of the input amplifier. This is particularly beneficial in the case of titrating solutions with a high Ohmic resistance, for in-stance with titrations in non-aqueous solutions.

The individual stages corresponds to the following timely de-lay (for a signal change of 99%): None: The signal will not be delayed Weak: The signal will be delayed by approx. 0.5 s Medium: The signal will be delayed by approx. 2.5 s Strong: The signal will be delayed by approx. 5.0 s

113


Subsequently, you select the way in which the titration is to be performed: Selection of titration type (pH/mV) pH/mV end point titration

titration parameter 01 control EP 1 strong medium weak buffered minimal consumption

252

The parameters for end point titration depend on the type of the curve: Strong: Strong jump with a steep rise Medium: Medium jump with less steep rise, for instance, with

acetic acid Weak: Flat jump without significant rise Buffered: A flat curve portion ahead of the end point as is the

case, for instance, with tartaric acid Minimum consumption: E.g. for the titration of blank values

titration parameter 01 pH titrations one end point two end points three end points linear (EQ) dynamic (EQ)

068/ 250

One end point: Titration will be carried out to ONE predefined end point, which means titration will be finished as soon as the measurement value which was input as end point will be reached. This kind of titration is subject to a given regulation which will be influenced by the curve to be expected, and by the drift.

Two end points: In this case, titration is performed to TWO pre-defined end points. This kind of titration may be used, for instance, for p + m valued titrations.

Three end points: Titration is performed to THREE pre-defined end points. This is required for special methods, such as can be found in paper industry.

Linear: Titration is performed with constant dosing steps, ir-respective of the change of the measurement signal. The dis-advantage of linear titration control is found in the range of the equivalence point, since, as a rule, only very few date points are found there

Dynamic: Dynamic titration will be performed. In this case the dosed volumes of the individual dosing steps are different in their magnitude. The step distance depends on the respec-tive rise of the titration curve. As a result hereof, for instance, larger dosing steps may be performed in a more flat curve portion. This means that the volume to be dosed will double up to the maximum volume. If the titration curve becomes steep, dosing will continue at minimum volume until the set value is reached. This feature means that a dynamic titration will be performed considerably faster than a linear one, since the dosing volume is optimally adapted to the curve. As a re-sult, less measurement points will be recorded in the flat part, whereas more measurement points will be recorded in the steep part of the curve.

114


Subsequently, you may select the various end criteria as a function of the pH/mV value. These menus are cy-cled through up to three times as a function of the desired number of end points. Cycling is done separately for each end point. After the definition of the titration end, the control and the speed of titration are to be parameterised. The drift control feature ensures the quality of the measurement values. It defines the time when a measurement value will be taken over after the addition of the titration agent. The selected , , parameters have an influence on the titration duration owing to the drift control, which means that an "accurate" drift control will cause a stable measurement value and thus an enhanced certainty of the meas-urement value, but also a slower course of the titration. If is selected, a measurement value drift per minute will be indicated.

titration parameter 01 enter value EP 1 end[pH]: 7.00 steps[ml] 0.00 ml delay[ s]: 10 s

255

End [pH]/[mV]: Titration is performed up to an input pH/mV value.

Step [ml]: At the end of titration, after the end point was reached for the first time.

Delay [s]: Delay time upon the lapse of which the input end point has to be exceeded or reached, respectively, so that ti-tration will be ended.

titration parameter 01 EP speed fast medium exact value: 100 ml/min

265

Fast / medium / exact: These criteria influence the duration of titration. End point titration will be performed at various speeds: Fast titration will be finished within less than one minute, accurate titration will take longer (approx. 4 to 5 min-utes)

Under the 'value' item you can enter a drift which has to be fallen short of in order to end to titration

titration parameter 01 total consump.titr. final consumpt.ml 50.00 ml

209

The ml end criterion will define the cancellation criterion for ti-tration. As a rule, it will be used as a safety criterion to pre-vent the titration vessel from spilling over.

115


Increasing/decreasing titration After the input of the titration parameters for end point titration, you specify the expected direction of the titra-tion: Parameterisation of linear titration: In the case of linear titrations, titration is done in constant dosing steps and irrespective of the change of the measurement value. The volume being dosed remains the same all the time. Combining multiple end criteria If you selected linear or dynamic titration, this menu item will give you the opportunity of selecting and combin-ing multiple end criteria.

titration parameter 01 titration direction increasing decreasing automatic

071

Increasing: The initial measurement value is below the end point.

Decreasing: The initial measurement value is above the end point.

Automatic: Titration starts without any verification of the initial measurement value. The above criteria are intended to prevent an end point titra-tion if the end point has already been exceeded.

titration parameter 01 linear steps step size in ml 0.00 ml

096

Enter the desired volume in ml. Titration will always be performed with identical steps, irre-spective of the course of the curve. A great many titrations in organic media are performed in this way (mostly in combination with fixed waiting times).

titration parameter 01 end of titration

mL EQ M Val M Val + mL M Val + EQ mL + EQ mL + M Val + EQ

268

mL: Titration will be ended as soon as the input ml value has been reached.

EQ: Titration will end as soon as the specified number of EQs has been reached (inflection point of the titration curve).

M Val: Titration will be ended as soon as the specified meas-urement value has been reached. The measurement value depends on the specified titration type (pH or mV).

M Val + mL / M Val + EQ / mL + EQ / mL + M Val + EQ: In practice, a combination of criteria is used. The first criterionwhich is reached will end titration. An ml criterion, for in-stance, will ensure that the beaker glass will not spill over, and therefore it should always be input.

116


mL end criterion EQ end criterion EQ end criterion, type of jump

titration parameter 01 total consump. titr. final consumpt.ml 50.00 ml

092

Enter the desired value in ml

titration parameter 01 number end points EQ 1 EQ 2 EQ 3 EQ 4 EQ 5

274

This item is used to specify the desired equivalence points at which titration will be cancelled.

titration parameter 01 end of titration steep jump medium jump flat jump value dev. 8.00

275

Depending on the intensity of the jump, this is the point to se-lect the sensitivity of the inflection point to be determined.

Special titrations may require an adaptation of the cancella-tion criteria in the form of an input of a numerical value for the derivative. The values vary from 1 (weak jump) to 1000 (strong jump). As a hint strong jump: > 300 medium jump: > 10 weak jump: < 5

117


Measurement value (M Val) end criterion mL + EQ end criterion Selecting drift control

titration parameter 01 enter end M Val: enter parameters 0.00

271

The measurement value to be input here depends on the specific titration type: pH, mV, A.

titration parameter 01 total consump. titr. final consumpt. ml 50.00ml

269

At this point you should enter the maximum volume upon reaching of which a titration is to be cancelled. This criterion is used to prevent excessive titration, i.e. that the titration vessels volume will not suffice.

titration parameter 01 drift control fixed waiting time fast medium exact set

097

Drift control decides when a measurement value is taken over after the addition of the titration reagent.

Fixed waiting time: The waiting time following the addition of the titration agent is always constant. PLEASE NOTE: In the case of difficult, non-aqueous titra-tions such as TAN/TBN, or inhibited chemical reactions such as the determination of aromatic amines through diazotising it is necessary to set a constant waiting time. This bears the disadvantage that the duration of titration is frequently longer than with the other drift criteria.

Fast/medium/exact: The measurement value resulting from an addition of titration agent will always be taken over as soon as it has stabilized over a certain period of time. In the case of acid/base titration in aqueous media, the selection of fast or medium as a criterion is recommended.

Set: The value of the drift may be set at this point in terms of mV/min.

118


Input, fixed waiting time of drift control Input, value of drift control Dynamic pH/mV titration

titration parameter 01 drift control set 100.00 [mV/min]

276

Special requirements of the application may make it neces-sary to enter a value here in terms of mV/min.

titration parameter 01 fixed waiting time waiting time in s: 0.00s

098

Waiting time between two titration steps in seconds Can be set in steps of 1 second up to 999 s.

titration parameter 01 dynamic control steep jump medium jump flat jump Dyn_Parameter

099

The selection of the type of jump has an influence on titration control and will improve the result of titration. Steep leap, such as in the case of hydrochloric acid with

NaOH Medium jup, such as in the case of chloride with silver nitrate. Flat jump, such as in the case of trace determination of chlo-

ride Dyn_Parameter: This is the point to make detailed, ap-plication-specific settings

- the smallest step width for the steep jump range - the largest step width for the flat portion of the titration curve- the slope (please refer to the 1st derivative) where the small-est step width is to be titrated. - the slope (please refer to the 1st derivative) where the larg-est step width is to be titrated.

119


Input of the start stirring time (waiting time 1) External titration burette You have the possibility of titrating using an external burette. Using the "titration burette / menu item you can select whether you wish to work with an external titration burette. The illustration below shows the inquiry of the address for the desired external titration burette. Please note: In the case of pH Stat and Karl Fischer titrations the use of an external titration burette is impos-sible for system reasons. In the case of EP titrations the titration speed has to be set to less than 4 ml/min (20 ml interchangeable unit) or to accurate. The external burettes which may be used include, for instance, piston burettes of the TITRONIC universal, TITRONIC 110, TITRONIC 200, and TITRONIC 110 plus types. Pretitrating

titration parameter 01 start mix time [s] enter value : 1 s

074

Prior to commencing titration, it is possible to run a stirring time. This stirring time can be used for mixing a sample prop-erly. The starting stirring time (0-999) proceeds prior to the initial measurement value and pretitration. durchmischen.

titration parameter 01 titrat. burette ext adress burette: 00

279

This item is used to input the address which is set as address on the desired external burette.

The address of the external burette is set either using the software, or by means of the rotary switch at the back panel of the device, depending on the type of the burette.

titration parameter 01 pretitration pretitration in ml: 0.00 ml

280

Pretitration is intended to add a larger dosage volume (0.01 - 100 ml) at one time, and to accelerate or optimise titration. The added dosage volume will be taken into account in the result of the titration volume.

120


Input of reaction time Predosing If predosing is to be done using one or more burettes, the address of the burette(s) and the desired predosing volume have to be specified here. The predosing burettes which can be used include: Piston burettes of the TITRONIC universal, TITRONIC 110, TITRONIC 200, and TITRONIC 110 plus types

titration parameter 01 reaction time [s] waitung time in s: 0s

078

Following pretitration, a waiting time will run to ensure com-plete reaction.

The first waiting time will run after predosing. If no predosing or pretitrating is performed, both waiting times will be added up.

titration parameter 01 predosing no

1 burette 2 burettes 3 burettes

072

At this point you specify whether predosing is to be done at all, and if yes, how many burettes are to be used. Up to three different predosing burettes can be used in one method. The typical applications include, for instance, reverse titration with thiosulfate in iodometry, or sample preparation with pH value setting using buffers.

titration parameter 01 pretitration 1 adress burette: 00 predosing in ml: 0.01ml

286

If predosing is to be done (0.01 - 100 ml), this is performed using an external burette. At this point, the address of the bu-rette and the predosing volume are to be entered.

121


Automatic filling of the burette A titration type The input of the parameters for a A titration is done in analogy with the parameterisation of a pH/mV titration. However, only titration to one end point is possible. Karl Fischer titration type

titration parameter 01 fill dosing unit fill do not fill

105

Filling: An automatic filling process takes place at the end of a titration

Do not fill: No filling is performed, neither at the beginning, nor at the end of titration. In the case of small titration vol-umes and automation using the sample changer, this can save time! PLEASE NOTE: The burette can be filled at any time by pressing the unlatch button or the F4/FILL key.gefllt werden.

titration parameter 01 KF settings type of reagent polarisation volt extraction time end criteria drift stop min/max time go on with method

217

Reagent type: In the case of KF titration, a distinction is made between a single-and a two-component reagent. In the case of single-component reagents, all the reagent components required for titration are contained in the titration agent. This means that reaction speed is somewhat slower than in the case of a two-component reagent. In the latter case the sol-vent components contain a serial of constituents.

Polarisation voltage: Setting of the voltage between the two pins of the double platinum electrode.

Extraction time: Setting of the waiting time which is required to either dissolve the sample or to extract the water from an insoluble sample.

End criteria: The end criteria consist of a current value in terms of A with a specified cut-off time and/or a drift value in ml/min.

Drift stop: Setting of a drift stop, should this be desired. The value can be input in terms of l/min.

Min./max. time: Depending on the sample to be analysed, this is the item to enter the minimum or maximum titration du-ration.

Go on with method: Exit the input menu. Proceed with meth-ods parameterisation.

titration parameter 01 uA titrations one end point linear (EQ)

251

One end point: Titration will be carried out to ONE predefined end point, which means titration will be finished as soon as the A value which was input as end point will be reached. This kind of titration is subject to a given regulation which will be influenced by the titration leap to be expected and by the drift.

Linear: Titration is performed at constant dosing steps, irre-spective of the change of the measurement signal.

122


titration parameter 01 KF settings one comp. reagent. two comp. reagent

218

The control of a single-component reagent is based on the assumption of a slower reaction time.

If a two-component reagent is being used, the selection of single-component control will lead to clear over-titration. The selection of two-component control when using a single-component reagent will be too slow. For safety reasons, two-component control is the default standard control method.

titration parameter 01 KF settings polarisation volt 100mV

281

Polarisation voltage refers to the voltage being applied be-tween the two platinum pins of the double platinum electrode. The current strength readings change as a function of the voltage being applied. The standard set value is 100 mV. This value, however, may be modified according to specific requirements; 10-200 mV may be set. If other solvents are being used, the titrations may be optimised by modifying the polarisation voltage. This value, in combination with the A criterion, may also be used for adapting to different solvents. In principle, the following is true: Higher voltage = Slower titration!

titration parameter 01 KF settings extraction time 0s

282

Extraction time: After the sample has been added into the ti-tration vessel, a certain period of time has to be waited be-fore the titration unit will start with the addition of the KF re-agent. This waiting time is necessary, either to dissolve the sample or to extract the water from an insoluble sample (therefore the description "extraction time".) The extraction time can be set in a range from 0 to 9999 s.

123


titration parameter 01 KF settings end criteria cutoff curren 20 uA cutoff time 10 s

219

End criteria: The end criteria decide when titration will stop. Cut-off current: The cut-off current, in terms of A, can be

set variably between 1 and 100 A. Its standard setting for all methods is 20 A, and as a rule this value does not require any change.

Cut-off time: As soon as the set cut-off current has been reached, the cut-off time starts to run. If the value drops back below the set value again, the cut-off time resumes at 0. If the set cut-off current is exceeded for a period exceeding the cut-off time, titration will stop. The standard set value is 10 seconds.

titration parameter 01 KF settings min/max time min time 1s max time 999s

220

Min. time: Min. titration duration is a very suitable parameter for samples out of which the water is extracted only very slowly. In the case of such samples it makes sense to have the water reacted away by the addition of KF reagent as early as during extraction. This means that the water will be ex-tracted more quickly out of the sample. The min. titration du-ration can be set from 0 to 9999 s. The standard value for all samples is set to 1 s.

Max. time: The max. titration duration is used on samples which create an increased drift towards the end, and where no stable end points will occur, for instance, caused by a slow extraction of water. The max. titration duration can be set from 0 to 9999 s. The standard value for all samples is set to 9999 s.

titration parameter 01 KF driftstop no [l/min] [ug/min]

221

Drift stop: Some humidity will penetrate from the environment into each titration vessel, even if it seems to be very closely sealed. This humidity will consume KF reagent. The term of 'drift' refers to the reagent consumption over time. The drift will be displayed automatically during conditioning and in the course of titration. It is indicated in terms of l/min. The drift can be used very beneficially as a criterion for can-cellation. [g/min] means a higher value. In this case the l value will be multiplied by the titer.

124


pH-stat titration type In the case of pH-stat titration, a pH-value (set value) will be kept stable pH-stat unbuffered After selecting the titration parameters for pH-stat titration, the following screen will be displayed and ask for an addition. This means that after the first reaching of the set value (exceeding 2 s), titration will be interrupted, and a manual addition can be made.

titration parameter 01 pHStat set phase unbuffered strong buffered flat jump medium jump steep jump

109

The set phase of titration corresponds to an end point titration. The titration parameters are set analogously. Unbuffered: There is a strong rise, for instance with hydro-

chloric acid Strong buffered: The titration curve contains a flat section, for

instance in the case of citric acid. Flat jump: Example acetic acid with NH4OH (ammonium hy-

droxide) Medium jump: Phosphate, first jump Steep jump: Strong acid with strong base

titration parameter 01 set pH

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