Sie sind auf Seite 1von 84

Gebrauchsanleitung Operating Instructions Mode d'emploi Manual de instrucciones

Titrator TitroLine alpha plus Titration Unit TitroLine alpha plus Titrateur TitroLine alpha plus Titulador TitroLine alpha plus

Gebrauchsanleitung ........................................................................................................... Seite 1 ....... 82


Wichtige Hinweise: Die Gebrauchsanleitung vor der ersten Inbetriebnahme des Titrators TitroLine alpha plus bitte sorgfltig lesen und beachten. Aus Sicherheitsgrnden darf der Titrator 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 Daten. 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 Eigenschaften 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 antes de la primera puesta en marcha del Titulador TitroLine alpha plus. Por razones de seguridad, el Titulador 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 concernientes 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 1.2 Summary ......................................................................................................................................85 Warning and safety information ...................................................................................................91

2.. Set-up and first operation ......................................................................................92


2.1 2.1.1 2.1.2 2.1.3 2.2 2.3 2.4 2.5 2.6 2.7 Unwrapping and set-up of the TitroLine alpha plus Titration Unit...............................................92 Installation of the stand rod ......................................................................................................92 Connection of the optional TM 135 titration rig. .......................................................................92 Installation of the titration clip ...................................................................................................92 Installation of the TM KF Titration Stand and of the titration vessel ...........................................93 TA plus Interchangeable Unit:......................................................................................................96 Fitting and replacing an interchangeable unit ..............................................................................97 Replacing the glass cylinder ........................................................................................................98 Initial filling and rinsing of the complete interchangeable unit .....................................................99 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 4.2 Measurement-amplifier, A input channel , electrode signal.......................................................102 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 7.2 7.3 7.4 7.5 7.6 Keyboard port.............................................................................................................................156 Power connector ........................................................................................................................156 Centronics-Interface...................................................................................................................156 RS-232-C-Interfaces ..................................................................................................................157 Loading the operating-system software via the RS-232-C interface .........................................157 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
8.2

TABLE OF CONTENTS 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

Chapter 1 Technical properties

85

1
1.1

Technical properties of the TitroLine alpha plus Titration Unit


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 determination 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, pharmaceutics, 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 computer (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 alpha/TW alpha plus sample changer. It may also be used for connecting an analytical weighingbalance. 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 enable safe operation of the TitroLine alpha plus Titration Unit.

KONFORMITTSERKLRUNG DECLARATION OF CONFORMITY DCLARATION DE CONFORMIT


Wir erklren in alleiniger Verantwortung, dass das Produkt We declare under our sole responsibility that the product Nous dclarons sous notre seule responsabilit que le produit

Titrator

Titration Unit

Titrateur

TitroLine alpha plus


auf das sich diese Erklrung bezieht, bereinstimmt mit den Normen

TitroLine alpha plus


to which this declaration relates is in conformity with the standards

TitroLine alpha plus


auquel se rfre cette dclaration est conforme aux normes

DIN EN ISO 8655, Teil 3


und mit dem normativen Dokument and the normative document et au document normatif

Technische Daten 17.12.2003

SCHOTT Instruments GmbH


Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne
05. August, August 5 , 5 Aot 2002 AGQSF 0000-A070-00/020805
st

Translation of the legally binding german version Technical data of the TitroLine alpha plus Titration Unit
Conformity: CE-Sign: Release 17.12.2003

DIN EN ISO 8655, Teil 3 Konformittszeichen 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 inflammable 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 insert (Z 860) may be used. Reference electrode 1 x 4 mm socket Measurement range Over-range Display reso- Measurement Input resisA channel lution accuracy* without tance sensor probe [] pH A PH 0,0 ... 14,00 - 1, 0 ... 14,00 0,001 0,02 1 Digit > 1 1013 mV A - 2000 ... 2000 - 2020 ... 1920 0,1 U [mV] 1,0 1 Digit > 1 1013 B channel pH B mV B PH U [mV] Measurement range 0,0 ... 14,00 - 1800 ... 1800 Over-range - 1, 0 ... 14,00 - 1820 ... 1820 Display reso- Measurement Input resislution accuracy* without tance sensor probe [] 0,001 0,02 1 Digit > 1 1013 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 temperature probe has to be used for temperature measurement or temperature compensation.

SCHOTT Instruments GmbH


Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne
05. August, August 5 , 5 Aot 2002 AGQSF 0000-A070-00/020805
st

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 T [C] - 75 ... 175 Display resolution 0,1 Measurement accuracy* without sensor probe 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 I [A] 0 ... 100 Display resolution 0,1 Measurement accuracy* without sensor probe 0,2 1 Digit

Display: Readings display:

* The measurement incertainty of the sensor probe has to be taken into account as well. LCD graphic display with background illumination, approx. 69 x 69 mm, 128 x 128 pixels. 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 titration. Additional control displays, contrast setting. Automatically with 2 buffer solution out of 8, sequence during calibration optional, 3 freely definable 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;

Calibration:

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)

SCHOTT Instruments GmbH


Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne
05. August, August 5 , 5 Aot 2002 AGQSF 0000-A070-00/020805
st

Translation of the legally binding german version


Release 17.12.2003 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 with galvanic insulation via opto-coupler - Daisy-chaining is possible Adjustable, 7 or 8 bits (default value 7 bits) Adjustable, 1 or 2 bits (default value 2 bits) Fixed 1 bit adjustable, even / odd / none 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 parameters - 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 off: Voltage smaller than 1.3 Volt Stirrer on: Voltage 3.3 Volt Centronics interface (25-channel D-SUB socket) for connecting an Epson, HP-compatible printer with a centronics interface (parallel interface). Keyboard PS2 socket for connecting a TZ 2835 keyboard from SCHOTT Instruments, or a German PC keyboard. 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) Stainless steel/polypropylene; with interior metallization for shielding Polyester 145 x 360 x 295 mm (W x H x D), height including dosing unit Approx. 4.1 kg for basic device Approx. 4.9 for complete device including interchangeable unit (including empty reagents bottle) 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 Printer

RS-232-C-Interface: Data bits: Stop bits: Start bit: Parity: Baud rate:

Stirrer control: Printer connection: Keyboard connection: StirrerConnection: Casing material: Front membrane: Casing dimensions: Weight: Environment:

SCHOTT Instruments GmbH


Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne
05. August, August 5 , 5 Aot 2002 AGQSF 0000-A070-00/020805
st

Translation of the legally binding german version


Release 17.12.2003 Interchangeable units Compatibility: Coding of the cylinder size: Valve: Cylinder: Hoses: Bracket for storage bottle: Fastening for interchangeable unit: Materials: Dimensions: Weight: Dosing accuracy: Correctness: Precision: The units are compatible with those of the T 100, T 110/200 and T 100 plus piston burettes Automatic, mounting for the glass cylinder bears unmistakable code Volume-independent cone valve made of fluorcarbon polymers made of DURAN FEP hose set with UV-protection To fit glass bottle to DIN 12 036 and DIN 12 039 or rectangular glass or plastic bottle With automatic checking feature Borosilicate glass, fluorocarbon polymers, PPS, high-grade steel, polypropylene, acrylic glass, 145 x 260 x 270 mm (W x H x D) without reagents bottle Approx. 0.80 kg for TA 20 interchangeable unit (without reagents bottle) According to DIN EN ISO 8655, Part 3 0,1 0,3 % 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 interchangeable units: Interchangeable unit type no. TA 01 TA 05 plus TA 10 plus TA 20 plus TA 50 plus Volume [ml] 1,00 5,00 10,00 20,00 50,00 Tolerances of the i of the glass cylinders [mm] 0,003 0,003 0,003 0,003 0,003 Dosing mistakes* referred to 100 % volume [%] 0,3 0,15 0,1 0,1 0,1 Reproducibility [%] 0,10 0,07 0,05 0,05 0,05

SCHOTT Instruments GmbH


Hattenbergstrae 10 55122 Mainz Deutschland, Germany, Allemagne
05. August, August 5 , 5 Aot 2002 AGQSF 0000-A070-00/020805
st

91 1.2

Chapter 1 Warning and safety information

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 maliciously 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 observe 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 operating 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 materials 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, however, 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
2.1

Set-up and first operation


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

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 bottom panel. To complete, screw in the stand rod. Working with the TM 135 titration rig: please refer to chapter 2.1.2.

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 connection 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 cable. 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.

93 2.2

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

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 desiccation 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 manually. 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

Chapter 2 Set-up and first operation of the TitroLine alpha plus Titration unit Fig. 3 Hose connections (seen from behind)

1 2

PTFE filling hose: Storage bottle titration vessel PVC hose for overpressure in the storage bottle: Storage bottle receiver drier PVC hose for overpressure in the storage bottle: Receiver drier titration vessel Stand rod PTFE suction hose: Titration stand waste bottle PVC hose for vacuum in the waste bottle: Titration stand waste bottle GL 45 screwed connections with adapter for hose connections and screw connections Storage bottle 1 l, brown Receiver drier 100 ml *) see previos page Olives for connection of the PVC hoses Mains-unit connector U = 12 VWaste bottle 1 l, bright

4 5 6

8 9 10 11 12

95

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

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 continue 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 seconds 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

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

TA plus Interchangeable Unit:

11 1

2 12

10 9 3

7 6 5 4

Fig. 3

1 2 3 4 5 6 7 8 9 10 11 12

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

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

97 2.4

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

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 installation 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 adjusted. 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 interchangeable 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 interchangeable unit is presently in place. After inserting a different (or the same) interchangeable unit the burette 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. Caution: After each replacement, an automatic filling plus a float balancing will take place. For this reason, please DO NOT remove the interchangeable unit immediately, but only as soon as the device 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 interchangeable units contain a coding which communicates the size of the installed cylinder to the bottom section of the burette. This ensures accuracy of the dosed volume at any time.

Fig. 4

98 2.5

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

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 analysis accuracy, it is always recommended to replace the PTFE piston at the same time when a defect glass cylinder 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 observed. Fig. 5 Installation of the glass cylinder

99 2.6

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

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 <R/D> menu item. After the start of the rinsing routine, and depending on the setting, the appropriate 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 <<Status: Rinsing>>, 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 <<0.000 ml>> will appear in the case of interchangeable units from 1 to 10 ml, or <<0.00 ml>> with interchangeable units of 20 and 50 ml, respectively, and the display will show <<Status: Ready>> Please note: The initial filling / rinsing program is not suitable for changing titration media, solutions, and liquids 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 disassembly 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

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

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:

KF Pt

Electrode A

Electrode

1 RS-232-C

Printer Ref Centronics

Ref 230V:0.25 115V 0 5


I O

2
KeyStirrer 12V out

Fig. 6

Keyboard

Stirrer Printer Cable TZ 3088 TZ 3089 TZ 3084 TZ 3086 TZ 3087 TZ 3082 TZ 3083 TZ 3081 CentronicsCable TZ 2835 TZ 1581 TZ 1581

What is to be connected? RS 1 PC with cable, length 5 m or with cable, length 10 m Daisy-Chain, please refer to RS 2 RS 2 TitroLine alpha plus, T 110 plus TW alpha plus T 110, T 200, TW alpha T universal Sartorius weighing-balance Mettler AT weighing-balance Mettler AB-G, PG weighing-balance etc. Centronics Printer e.g. Epson Stylus Color 880/980, HP-Deskjet 920 / 970 etc. Keyboard keyboard Stirrer TM 135, TM 128 TM KF

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 Titration Unit.

101

Chapter 3 Construction of the TitroLine alpha plus Titration unit

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
4.1

The connections of the TitroLine alpha plus Titration Unit


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.
Smoothing stage 0 1 2 3 Input delay none weak medium strong Setting time 0s approx. 0,5 s approx. 2,5 s approx. 5 s Suitable for titrating media aqueous, polar aqueous, alcoholic solvent with non-polar portion non-aqueous, non-polar Examples Acid-base titration in water Acid-base titration in alcohol and weak acids or bases in water Titrations in alcohol/water mixtures TAN, TBN, acid-base titrations in halogenised solvents or aromatics

The selectable input delay (setting time) causes a smoothing of the measurement signal. The respective setting 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 measurement 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
5.1

Working with the titration unit


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 <MODE> overview menu to parameterise a method. Jump to the system parameters menu item Display of the <Calibration> menu for calibrating the A and B measurement channels Change of sign Takes you to the Dosing menu

<F1> <F2> <F3> <F4> <F5> <F6> <F7> <F8> <F9> <F10> Num Lock Prt Sc Sys Rq Scroll Lock <ESC> < > < > Cursor key 0...9 decimal point <ENTER> or <> <DEL> or < Backspace > Letters, ASCII characters All other keys

<START> <STOP> <EDIT PARAM.> <FILL> <STORE PARAM.> <MODE> <INIT> <CAL> +/DOS

<ESC> returns you to the previous menu level. Scrolling within the overview menu to select specific menus Within the specific menu items: Move the cursor to select parameters Input of method numbers, sample numbers, and parameters. Confirmation of the input parameters. Within the present operating instructions, both keys are referred to as <ENTER>. Deletion of the input digit/character above the cursor. 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. 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 deactivated 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 <III> 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:

Chapter 5 Working with the TitroLine alpha plus

Head line Line 1 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

01

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.

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.

105 5.2

Chapter 5 Working with the TitroLine alpha plus

The start menu


In principle, it is always possible to adapt the TitroLine alpha plus Titration Unit to your specific requirements. Yet, you also have the possibility of accessing the database containing approx. 100 default standard 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.

Titroline ready no. 1

01

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 corresponding 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 <Start/Stop> key. The rinsing and dosing parameters and the rinsing and dosing functions can be set after pressing the <R/D> key. Pressing the <C> key will initiate the calibration of the

5.3

The mode menu


<MODE> / <F6> is used to select the mode menu. This level can only be accessed using a connected keyboard. 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 change 1 method method management create method system settings measuring output new calculation

01

change method: This item can be used to change an existing method. 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 results of the last titration, as well as printout and display of the CAL data. New calculation: A re-calculation will be performed, if necessary with a modified formula. The specified documentation will be prepared once again

003

106
5.3.1

Chapter 5 Working with the TitroLine alpha plus

Changing a method
01
To activate the password feature, please use the Password item of the system menu (please refer to chapter 5.3.5, Hardware settings)

method creating Passwort Passwort eingeben

048

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

01

At this point a 18-digit alphanumeric method name can be input. 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 <Enter> or < > key will take you to the following menu item.

049

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

01

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 parameters: 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 several methods at this point.

032

107

Chapter 5 Working with the TitroLine alpha plus Overview of all elements of a method 032* 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.

sampler none 12 samples 16 samples 24 samples 24 samples COD

01

If no sample changer is selected, the system will take you directly to the menus used for the input of the sample description 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 programmed to the selected plate size. If COD titration is to be performed, please select the <<24 samples COD>> position.

050

108

Chapter 5 Working with the TitroLine alpha plus

Parameterisation of the sample ID

titration parameter sample ID manual automatic no

01

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 entering a sample ID

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

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

01

Sample weight manual: The weighing-in data which are inquired at the start of the method have to be input manually each time. Sample weight auto: Upon the start of the method, the balance 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 calculation. The calculation will take into account the sample quantity 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

179

Parameterisation of the sample quantity (sample weight)

titration parameter weight fix weight in g: 1.00000g

01

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 sample weight for all subsequent titrations of this method.

203

109

Chapter 5 Working with the TitroLine alpha plus

Parameterisation of the sample quantity (sample volume)

titration parameter volume fix volume in ml: 1.000 ml

01

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.

204 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:

titration parameter number titrations multi determinat. 1

01

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 determinations to be made. The results obtained are used to perform a statistical calculation 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!

208 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:

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

01

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 minimum 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 optimum minimum stirring time should be determined in experiments. 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.

104

110

Chapter 5 Working with the TitroLine alpha plus

Parameterisation of the rinsing function If the rinsing function is selected, the required parameters for controlling the various rinsing operations are inquired one after another.

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

01

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 sensors 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.

051 Once the rinsing type or number of desired rinsing positions selected, you set the rinsing duration (max. 99 s).

sampler rinsing time rinsing time in s : 5s

01

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.

052 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.

sampler waiting position first position second position no wait position

01

In order to avoid that the electrode will dry out after titration with its head up, you can define a position in which the electrode 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.

055

111

Chapter 5 Working with the TitroLine alpha plus

sampling assign position start position 1

01

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

056

sampler number samples variable number samples

01

With the <<variable>> 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.

057 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 type of titration selection pH selection mV selection uA selection KF selection pH-Stat

01

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

065

112

Chapter 5 Working with the TitroLine alpha plus

Initial measurement value

titration parameter initial meas. value yes no

01

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 defaulted internally in the form of quite a number of experiencebased applications.

244

Selection of the measurement channel

titration parameter select channel measuring channel A measuring channel B

01

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.

246

Attenuation of the A measurement channel

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

01

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 instance with titrations in non-aqueous solutions. The individual stages corresponds to the following timely delay (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

248

113

Chapter 5 Working with the TitroLine alpha plus

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

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

01

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 predefined end points. This is required for special methods, such as can be found in paper industry. Linear: Titration is performed with constant dosing steps, irrespective of the change of the measurement signal. The disadvantage 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 respective 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 result, less measurement points will be recorded in the flat part, whereas more measurement points will be recorded in the steep part of the curve.

068/ 250

pH/mV end point titration

titration parameter control EP 1 strong medium weak buffered minimal consumption

01

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

252

114

Chapter 5 Working with the TitroLine alpha plus

Subsequently, you may select the various end criteria as a function of the pH/mV value. These menus are cycled through up to three times as a function of the desired number of end points. Cycling is done separately for each end point.

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

01

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 titration will be ended.

255 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 <<fast>>, <<medium>>, <<accurate>> 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 measurement value, but also a slower course of the titration. If <<value>> is selected, a measurement value drift per minute will be indicated.

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

01

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

265

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

01

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

209

115

Chapter 5 Working with the TitroLine alpha plus

Increasing/decreasing titration After the input of the titration parameters for end point titration, you specify the expected direction of the titration:

titration parameter titration direction increasing decreasing automatic

01

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 titration if the end point has already been exceeded.

071 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.

titration parameter linear steps step size in ml 0.00 ml

01

Enter the desired volume in ml. Titration will always be performed with identical steps, irrespective 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).

096 Combining multiple end criteria If you selected linear or dynamic titration, this menu item will give you the opportunity of selecting and combining multiple end criteria.

titration parameter end of titration mL EQ M Val M Val + mL M Val + EQ mL + EQ mL + M Val + EQ

01

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 measurement 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 criterion which is reached will end titration. An ml criterion, for instance, will ensure that the beaker glass will not spill over, and therefore it should always be input.

268

116
mL end criterion

Chapter 5 Working with the TitroLine alpha plus

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

01

Enter the desired value in ml

092 EQ end criterion

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

01

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

274

EQ end criterion, type of jump

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

01

Depending on the intensity of the jump, this is the point to select the sensitivity of the inflection point to be determined. Special titrations may require an adaptation of the cancellation 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

275

117

Chapter 5 Working with the TitroLine alpha plus

Measurement value (M Val) end criterion

titration parameter enter end M Val: enter parameters 0.00

01

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

271 mL + EQ end criterion

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

01

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.

269 Selecting drift control

titration parameter drift control fixed waiting time fast medium exact set

01

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 titrations 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.

097

118

Chapter 5 Working with the TitroLine alpha plus

Input, fixed waiting time of drift control

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

01

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

098 Input, value of drift control

titration parameter drift control set 100.00 [mV/min]

01

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

276 Dynamic pH/mV titration

titration parameter dynamic control steep jump medium jump flat jump Dyn_Parameter

01

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 chloride Dyn_Parameter: This is the point to make detailed, application-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 smallest step width is to be titrated. - the slope (please refer to the 1st derivative) where the largest step width is to be titrated.

099

119

Chapter 5 Working with the TitroLine alpha plus

Input of the start stirring time (waiting time 1)

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

01

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

074 External titration burette You have the possibility of titrating using an external burette. Using the "titration burette <yes>/<no> 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 impossible 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.

titration parameter titrat. burette ext adress burette: 00

01

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.

279 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 pretitration pretitration in ml: 0.00 ml

01

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.

280

120

Chapter 5 Working with the TitroLine alpha plus

Input of reaction time

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

01

Following pretitration, a waiting time will run to ensure complete reaction. The first waiting time will run after predosing. If no predosing or pretitrating is performed, both waiting times will be added up.

078 Predosing

titration parameter predosing no 1 burette 2 burettes 3 burettes

01

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.

072 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.

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

01

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

286 The predosing burettes which can be used include: Piston burettes of the TITRONIC universal, TITRONIC 110, TITRONIC 200, and TITRONIC 110 plus types

121

Chapter 5 Working with the TitroLine alpha plus

Automatic filling of the burette

titration parameter fill dosing unit fill do not fill

01

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 volumes 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.

105 A titration type

titration parameter uA titrations one end point linear (EQ)

01

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, irrespective of the change of the measurement signal.

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

01

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 solvent 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 duration. Go on with method: Exit the input menu. Proceed with methods parameterisation.

217

122

Chapter 5 Working with the TitroLine alpha plus

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

01

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 singlecomponent reagent will be too slow. For safety reasons, two-component control is the default standard control method.

218

titration parameter KF settings polarisation volt 100mV

01

Polarisation voltage refers to the voltage being applied between 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!

281

titration parameter KF settings extraction time 0s

01

Extraction time: After the sample has been added into the titration vessel, a certain period of time has to be waited before the titration unit will start with the addition of the KF reagent. 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.

282

123

Chapter 5 Working with the TitroLine alpha plus

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

01

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.

219

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

01

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 cancellation. [g/min] means a higher value. In this case the l value will be multiplied by the titer.

221

titration parameter KF settings min/max time min time max time

01

1s 999s

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 extracted more quickly out of the sample. The min. titration duration 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.

220

124

Chapter 5 Working with the TitroLine alpha plus

pH-stat titration type In the case of pH-stat titration, a pH-value (set value) will be kept stable

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

01

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

109

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 add reagent no automatic manual

01

None: No further substance is to be added. The process of value preservation will start immediately. Automatic: The corresponding volume of a reagent will be added by dosing after the set value has been reached, then titration continues automatically. If 'automatic' is selected, the volume to be added and the address of the addition burette have to be entered. Manual: As soon as the set value is reached, titration will be stopped, and a manual addition can be made.

112

titration parameter set pH pH= 7.00pH Max.: 100 ml/min

01

Input of a pH value which is to be preserved during titration. The max. dosing or titrating speed is: 100 ml/min with a 50 ml interchangeable unit. It would be 10 ml/min in the case of a 5 ml interchangeable unit. The addition will slow down automatically when the set value is being approached.

115

125

Chapter 5 Working with the TitroLine alpha plus

Selection of the titration direction

titration parameter titration direction increasing decreasing automatic

01

Increasing: To be set in the case of base (NaOH) addition. Decreasing: to be set in the case of acid addition (HCl). Automatic: The direction will be recognised automatically.

401 Subsequently, the basis of the measurement interval time is to be specified. The term of 'measurement interval time' refers to the waiting time between two measurement reading recordings. Titration control and dosing are not affected by this time.

titration parameter measuring interval second minute hour day

01

Considering that the number of measurement values without data reduction is limited, a sensible interval should be defined for the measurement-value "pairs" to be stored. If, for example, a specific pH value is to be kept constant for five hours, one minute might be a recommendable measurement interval. (The measurement value will also be kept constant within this interval.) The result will consist in 300 measurement value pairs including consumption, pH value, and indication of time.

116 The window for entering the value is not shown here. The next thing to be specified is the overall duration of titration.

titration parameter duration total time second minute hour day month manual cancellation

01

Specify the total duration of pH-stat titration. Attention should be paid to the number of measurement values and a sensible specification of the measurement interval. Manual cancellation is always appropriate if the consumption of pH-stat titration and the reaction time cannot be estimated.

118

126
pH-Stat pretitration

Chapter 5 Working with the TitroLine alpha plus

titration parameter amount set phase add volume not used

01

Frequently, the pH value to be kept constant must first be set. This process is referred to as set phase. This volume can then be added to the titration volume. It may also be taken into account in the calculation of the slope and consumption.

120

titration parameter pHStat [ml/min] very low low medium high very high

01

pH-stat titration allows titration with a firmly set pH value over a fixed period of time. The titration parameters depend on the added reagent volume and the speed of this addition. Very low: Applications in the range of up to 0.5 ml Low: Applications up to approx. 2 ml. Medium: Applications up to approx. 5 ml. High: Applications up to approx. 20 ml. Very high: Particularly high consumption.

121

127
5.3.2

Chapter 5 Working with the TitroLine alpha plus Calculation menu item

At this point, you can perform calculations or edit the calculation parameters of the currently selected methods. In addition, this menu can be used to select, create, or modify formulae.

calculations

01

New calculation: The result will be calculated once again. Formula selection EQ: Used for the calculation of one of several turning points Formula selection EP: Used for the calculation of one or several end points (EP) Formula selection KF: Calculation of the result in the case of KF titrationFormula selection pHst. : Calculation of the result in the case of pH Stat titration

formula formula formula formula

select select select select

EQ EP KF pHst.

106 Formula selection, calculate number of EQs

calculation calculate EQ(s) enter no. of EQs 1

01

Here the numbers of inflection points are set.

442 Formula selection EQ/EP

calculation calculate EQ(s) EQ 1 EQ 2 EQ 3 EQ 4 EQ 5

01

At this point you can select the formulae for the calculation of the respective inflection point (EQ). There are 5 EQs and 3 EPs possible. The selection of the formulae for the end points is done analogously.

390

128

Chapter 5 Working with the TitroLine alpha plus

calculations formula selection mL*F1*F2/Q (mL-B)*F1*F2/Q (mL1-mL2)*F1*F2/Q (B-mL)*F1*F2/Q Q*F1/((mL-B)*F2 (B*F3-mL*F1)*F2/Q

01

At this point you can select the formulae for the calculation of the respective turning point (EQ) or end point (EP). You may select one out of the following formulae: mL*F1*F2/Q: Normal formula (mL-B)*F1*F2/Q: Normal formula with consideration of blank value (mL1-mL2)*F1*F2/Q: Difference between two EQs or EPs (B-mL)*F1*F2/Q: Reverse titration Q*F1/((mL-B)*F2: Titer determination (B*F3-mL*F1)*F2/Q: Reverse titration with additional calculation factors

141

PLEASE NOTE: The formula for the <(mL1-mL2)*F1F2/Q> difference formation must only be used from the use of a minimum of 2 EPs or EQs.

Formula selection KF

calculations formula select KF (ml-B)*Tit*F1*F2/EW EW*F1*F2/ml-B*F3 ml*F1*F2*F3

01

At this point you can select the formulae for the calculation of a KF titration. (ml-B)*Tit*F1*F2/EW: EW*F1*F2/ml-B*F3: ml*F1*F2*F3:

404 Formula selection pH-stat

calculations formula select pHSt mL*F1*F2/Q (mL-B)*F1*F2/Q (Stg*F1*F2)/Q

01

At this point you can select the formulae for the calculation of a pH-stat titration. mL*F1*F2/Q (mL-B)*F1*F2/Q (Stg*F1*F2)/Q

405

129

Chapter 5 Working with the TitroLine alpha plus

Legend of the abbreviations used in the formulae: = The calculation uses the ml values as determined, i.e. also ml 1, ml 2 etc. = Factor 1 (multiplicative) = Factor 2 (multiplicative) = Factor 3 (multiplicative) = Quotient; will be multiplied automatically with the respective sample weight or sample volume in the calculation Tit = Titer of the titration solution B = Blank value (additive) Stg = Slope in the case of pH stat The following menu items can be used to enter the desired values. ml F1 F2 F3 Q

calculations enter F1 enter value 1.00000 from global memory

01

The factor may be any numeric value, for instance the molecular weight or molarity of the titration solution. It may also be taken from a global memory. This makes sense, for instance, in the case of a titre determination with a separate method.

339

calculations enter Q enter value 1.0000 from global memory

01

Normally, the quotient is located under the fraction bar. It serves first of all as a multiplicative factor used in the conversion of the sample weight. The sample weight is made in [g], but the calculation frequently requires [mg]. In the case of titer determination, the quotient is above the fraction bar.

342

calculations enter B enter value 0.00 from global memory

01

This item can be used to enter a value for the blank value. As an alternative, the value may be taken from a global memory which was calculated or determined in a different place (a different method). The value is used in an additive form.

146

130

Chapter 5 Working with the TitroLine alpha plus

The result consists of an identifier, a calculated value, and a unit (for instance %).

calculations enter unit unit

01

At this point, the unit may be entered (max. 11 characters).

344

calculations enter identifier identifier

01

At this point, the identifier may be input, for instance chloride (max. 11 characters).

345 On this menu you can select whether the calculation of the titration is to be done with arithmetically smoothed or "raw data".

calculations smoothing no smoothing weak smoothing medium smoothing strong smoothing

01

No smoothing: Raw data will be used. Weak/medium/strong smoothing: The degree of smoothing is sets by an arithmetic algorithm in such a way that smoothing with different strengths will occur. In principle, only the raw data will be stored in the devices. Smoothing is done only in the calculation. The smaller the degree of smoothing, the more accurate will the results be.

149

131

Chapter 5 Working with the TitroLine alpha plus

calculations no. decimals no. decimals 1

01

This menu item is used to enter the number of decimal digits of the result or the results, respectively.

103

calculations result into memory not into memory into global memory with number 1

01

Here you can store the result of the calculation. This value can be used in a different formula, but also in a different method If more than 1 EQ or EP have been calculated, only the last calculated value will be stored.

150 IMPORTANT: To document the statistics, a printer or PC has to be connected. A subsequent documentation of the individual values is no longer possible. Delete statistics

calculations statistics delete manual delete automated

01

If the statistics feature was activated, the statistics memory may be deleted at this point. Manual deletion: The statistics memory will be deleted. Automatic deletion: When a multiple determination is started, the statistics memory will be deleted automatically.

284

132
calculations

Chapter 5 Working with the TitroLine alpha plus

01

Selection end: You leave the calculation menu and return to the method creation selection. IMPORTANT: Standard deviation has to be selected to activate full statistics processing.

selection end selection standard deviation

335

calculations go back formula formula formula formula proceed to select select select select EQ EP KF pHSt.

01

If more than one EQ was selected, this is the point to select formulae and enter factors for further EQs.

101

5.3.3

TL alpha plus formulae editor

You can use the formula editor to create formulae of your and integrate them into methods.

calculations formula selection own formula

01

Within a method either predefined formulas or own formulas can only be used. Since many formulas contain the same numerical values (for example chloride in cheese, water...), these formulas can be predefined. They are selected in the methods from a list

181

133
calculations

Chapter 5 Working with the TitroLine alpha plus

01

own formula list formula editor print list export list

In this example the formula in formula editor was already created for another method and has to be selected only from a list in this case.

153

calculations own formula no. of formulas 1 no. of EPs/EQs 1

01

The number of the formulas must be entered in this method and the number of the EQs or EPs used in these formulas.

152

calculations formula list result: not into memory into global memory with number 1

01

It is decided here whether a result is supposed to be set for other methods and formulas availably. The result can be stored in one of 50 Global variables

155

134

Chapter 5 Working with the TitroLine alpha plus

calculations enter unit unit

01

Here the unit can be entered (at the most 11 signs).

159

calculations enter identifier identifier

01

Here the result name can be entered, for example chloride (at the most 11 signs).

160

135

Chapter 5 Working with the TitroLine alpha plus

calculations no. decimals no. decimals 0

01

Here one gives the number of the decimal places of the result and/or the results.

103

calculations smoothing no smoothing weak smoothing medium smoothing strong smoothing

01

Do not smooth: Is worked with raw data. Weak Smoothing / Average-Strong Smoothing / Strong Smoothing: The degree of smoothness is set by a mathematical algorithm so that a smoothing is received in different strengths. Only the raw data are stored fundamentally in the device. The smoothing occurs only during the calculation. The smaller the degree of smoothness is, the more precise the results are. Normally a smoothing is not necessary. It can improve, however, the result safety very restless titration curves. By means of the first derivation of the titration graphics a judgement is slightly possible.

149

calculations selection end selection standard deviation

01

End selection: The calculation menu is left and goes back to the selection method creation. CAUTION: In the case of standard deviation selection the statistic is activated.

335

136

Chapter 5 Working with the TitroLine alpha plus

Create an formula with the editor:

calculations own formula formula list formula editor print list export list

01

The Formula editor selection will take you to the menu for creating own formulae.

153

calculations formula editor no. 1 formula name Fo-----------1 overwrite

01

170

calculations enter formula EQ1 * 35.45 * 0.1 * 100 / (1000 * W)

01

The formula is input like normal text using the keyboard. A formula used to calculate chloride in terms of % would then look as follows: EQ1 * 35.45 * 0.1 *100 / (1000 * W) The equivalence point is a variable and referred to as EQ1. Five EQs from 1 to 5 are possible. The molecular weight 35.45 is input in the form of a number incl. a decimal point. The operators include the asterisk (*) for multiplication and the slash (/) for division. The other arithmetic factors (e.g. 0.1 for the molarity and 100 for the conversion to % and 1000 for the conversion of G to mg) are to be typed, accompanied by a blank.

161

137
calculations

Chapter 5 Working with the TitroLine alpha plus

01

formula editor formula selection new formula print formula formula exporting

The formula which was just created may be printed or output via the RS interface. At this point it is also possible to select the formula right away to integrate it into the method.

169181

calculations own formula no. of formulas 1 no. of EPs/EQs 1

01

The input to be made here includes the number of formulae included in this method and the number of EPs or EQs to be used within these formulae.

152181

Functions +, -, *, / (), (-1) Arithmetic operators EQ1 .. EQ5 Equivalence points EP1 .. EP3 End points EV End volume, consumption at the end of titration W Weighed-in quantity V Volume pattern M1 .. M50 Global memories (ln Zahl) Natural logarithm to the base of e (lg Zahl) Logarithm to the base of 10 (ex Zahl) Exponent to the base of e (sq Zahl) Square root 123.456 Numeric value Editing: Negative values to be entered between brackets Del key: The character at the cursor position will be deleted Backspace: The character to the left will be deleted Arrow keys: Direct cursor movement to desired position Number of characters: 140 characters on 8 lines

138

Chapter 5 Working with the TitroLine alpha plus

Input: Directly at cursor position Examples:: Citric acid mg/litre EP1 * 64.04 * 0.1 * 1000 / V EP1 End point 64.04 equivalent weight of citric acid 0.1 NaOH mol/l concentration 1000 Conversion ml to litres V Pattern in ml (sample quantity) Chloride % EQ1 * 35.45 * 0.1 * 100 / ( 1000 * W) EQ1 Equivalence point 35.45 Mol weight of chloride 0.1 AgNO3 concentration 100 Conversion to % 1000 Conversion g to mg W Weighed-in quantity in g

5.3.4

Documentation menu item

titration parameter documentation no documentation short documentation std documentation detail documentat. GLP documentation shortlist

01

No documentation: The results will not be output on the printer. In this way, for instance, the device can be used for measuring, dosing, and setting of the pH value without wasting paper. Short documentation: Output of the method name, date, time, and result. Standard documentation: In addition to the short documentation, the titration chart will be printed. detail documetation: Besides to the standard documentation the formula with all values is printed GLP documentation: All attitudes are printed, including the method parameter. shortlist

107

139
5.3.5

Chapter 5 Working with the TitroLine alpha plus Method management

This menu item can be used to administer, edit, print, etc. existing methods.

method management meth. 1 delete meth. 1 print meth. 1 copy meth. 1 export standard methods print list export list

01

Delete method 1: Firstly, the current method number is displayed as the one to be deleted. However, it can be overwritten by the desired number. When confirming the selection with <enter> or < >, the selected method will be deleted without security prompt. Print method 1: All parameters of the selected method will be printed on the connected printer. The current method can be stored under a new number. Subsequently, this new method can be modified in a time-saving manner. Export method: The term of export refers to its output via the RS interface 1 in the form of a text file. Standard methods: At this point, a method can be selected or edited from a selection of standard methods. print list: A list containing names and numbers of the working methods. export list: During export, this list will be output in ASCII via the RS-1 interface

004

Standard methods

atandard methods selection print list export list

01

Selection: This item is used to select the standard methods of the respective titration modes. Print list: A lists containing the numbers and names of the working methods will be printed.* export list: If exported, this list will be output through the RS 1 interface in ASCII form.* *Not in version 1.0

036

standard methods selection std.meth. pH titrations mV titrations uA titrations KF titrations pH-Stat

01

This item is used to preselect the titration type of the standard method.

037

140

Chapter 5 Working with the TitroLine alpha plus

Example: pH titration type

standard methods selection pH end point acids EQ acids org Solv acids end point bases EQ bases org Solv bases

01

At this point, you may select the type of pH titration, for instance end point acids.

038

standard methods method Citric acid store as number of method 1

01

The selected standard method will appear under 'method'. Using the and keys, you may select a different standard method. Below, please enter the desired method number under which the standard method is to be stored.

045 5.3.6 Create new method

With this menu item you can create a completely new method according to specific requirements. If password protection is active you will first be prompted to enter the password. If the password protection is off, pressing <ENTER> or < >will take you to the following menu item:

new method method number 1 enter method name. Methode 1

01

Here you may entered the number and the name of the new method to be created. To correct erroneous input, press the < Backspace> key. If you press the <ENTER> or < > key, you will be taken to the selection (032) dialogue window. This window can be used to program all desired parameters for the new method. (please refer to chapter 5.3.1, page 21).

243

141
5.3.7

Chapter 5 Working with the TitroLine alpha plus System settings

At this point, the general device-specific settings for the TitroLine alpha plus Titration Unit are made, such as language, password protection, etc.

system settings system settings language calibration setting dos speed/filltime delete all methods user hardware

01

Language: You may select between German, English, French, and Spanish. Calibration setting: This item is used to define which buffers are to be used for calibration. Dosing speed/filling time: Setting of the dosing speed and filling time. Delete all methods: All user methods will be deleted. Hardware: Settings required for RS parameters, date and time, printer selection etc.

007

Calibration setting

system settings

01

calibration setting buffer selection temperature: 25.00 C new buffer sensor management

Buffer selection: At this point, you may select up to two buffers out of a set of standard buffers and freely definable buffers to be used for pH calibration. Presently not yet active! Temperature: The temperature for calibration is to be set manually here, if no Pt 1000 is connected. A Pt 1000 will be recognised automatically, and in this case its temperature reading will be used. New buffer: To be used for the definition of own buffers. The march of temperature of the buffer may be input from 10C to 40C in steps of 5C.! Sensor management: This item is to be used to attribute names to sensors (electrodes). They are provided with calibration data which can then be documented together with the name of the sensor in a form which is suitable for FDA/GLP. Presently not yet active! Validation: If validation is active, a pH end point titration is only possible with a valid and correct calibration. Presently not yet active!

017

Buffer selection

calibration setting buffer selection calibration 2 point selection buffer 1 selection buffer 2 selection buffer 3 end selection

01

This item is used to define the buffers for calibration. We recommend calibration using two buffers, as a rule 4.00 and 7.00. Calibration can be carried out with 1 to 3 buffers. The buffers are selected in a row (please refer to fig. 094). All buffers once selected, the setting of the calibration data is completed by End of selection.

018

142

Chapter 5 Working with the TitroLine alpha plus

calibration setting selection buffer 1 standard buffer own buffer

01

Standard buffer: Ex-works predefined buffer. Each buffer can be selected from a list (buffer pH 1,0 - 4,0 4,01 - 6,87 - 7,0 - 9,18 - 10,0) which is provided either by SCHOTT Instruments, or by the device manufacturer for the specific application case. Own buffer: At this point you can select buffers which were previously self-defined by the user inclusive of their temperature march.

094

Temperature compensation

calibration setting temperature compens manual automatic

01

Manual: Setting of the temperature at which the titration unit will work in the case of a pH measurement without temperature sensor. The default setting is 25C. Automatic: If a temperature sensor (Pt 1000) is used, temperature compensation will be performed automatically.

022 New buffer If the default standard buffers should not be sufficient, or if a special buffer is required, it may be defined at this point.

calibration setting new buffer new buffer 1 value 7.00pH

01

New buffer: Specification of the number. Value: Input of the value, for instance: 2.45.

024

143

Chapter 5 Working with the TitroLine alpha plus

calibration setting deviation/degree : 10 7,00pH 15 7,00pH 20 7,00pH 25 7,00pH

01

It is not necessary to enter all of the pH values of the buffers, but please note the following: To enable the TitroLine alpha plus Titration Unit to recognise that a new buffer is being recorded, the 25 C value of the buffer has to be entered. In addition, the pH values above and below the later measurement temperature at which calibration is to be performed have to be entered. Example: The calibration temperature is around 15C. This means that the 10C, 15C and 20C as well as the 25C pH value of the buffer have to be input. After pressing the <ENTER> key, you may input the next four values in the temperature range from 30 to 45 C.

025

Sensor management

calibrate init. sensor management yes no

01

Yes: At this point you may store the Information regarding the sensor be used. No: Proceed with the inquiry of validation information

126

calibrate init. sensor management new sensor delete sensor print list export list

01

new sensor: Used to activated a new sensor, for instance an N 62 glass electrode. delete sensor: Here you may select and delete a sensor. print list: Used to create a printout of the list of the currently defined sensors including the calibration data. export list: The exported list contains the same information as the printouts and will be output in the form of a text file via the RS 1 interface

129

144

Chapter 5 Working with the TitroLine alpha plus

sensor management new sensor sensor 1 sensor name Charge Nr.

01

At this point you can input a name for the sensor, e.g. N 62 no. 12345

130

sensor management Sensor pH mV uA C 1

01

This is the point where you specify the type of the sensor.

190 Dosing/Filling

dosing dosing speed. dosing speed max. filling time max. set filling time set dosing speed back 100.00ml/min 20 s

01

Dosing speed max.: The dosing speed is set to be max. possible value (100 ml/min) Filling time max.: The filling speed is set to the max. possible value. (20 s) Set filling time: For samples with a higher viscosity, for instance, the filling time can be extended between 20 s to 999 s. Set dosing speed: The dosing speed may be adapted to the application in a range between 0.01 ml/min to up 100 ml/min. Default setting: max. speed = 100 ml/min, shortest filling time = 20 s

013

145

Chapter 5 Working with the TitroLine alpha plus

The menu items below are used to specify the desired filling time.

filling time

01

input via keyboard 20s

If the liquid to be dosed has a too high viscosity or a too high vapour pressure, the filling time has to be adapted. The possible filling times stretch from 20 s / 100% filling volume and 999 s/100% filling volume. As a rule, a reduction of the filling speed to 20 s / 100% filling volume should be sufficient. Please note! The set filling time applies irrespectively of the selected method, i.e. it applies to all methods.

033

fill automated always after titration after dosing never

01

This menu is used to select whether and when the burette is to be filled after the end of a titration. Always: Automatic filling will take place at the end of each titration After titration: Only after a titration is filled automatically. After dosing: Only after dosing it is filled automatically. Never: Upon the end of titration, the piston remains in any position, and the burette will only be filled with the start of the next titration. The standard setting is always

035

dosing speed dosing speed ml/min 100.00ml/min

01

The max. adjustable dosing speed per minute corresponds to double the dosing volume of the dosing unit being used, for instance: 100 ml/min with a 50 ml dosing unit. Depending on the dosing unit, dosing speeds from 0.01 ml/min up to 100 ml/min may be input. Please note! The set dosing time applies irrespectively of the selected method, i.e. it applies to all methods. The max. speed is defaulted.

034

146

Chapter 5 Working with the TitroLine alpha plus

Dosing speed / Filling time: To get to the Rinsing/Dosing window, please press <ESC> on the main menu. You may also use the R/D key on the built-in keyboard.

rinsing/dosing rinsing dosing set rinsing set dosing

01

Rinsing: After pressing the ENTER key, the system will rinse. Dosing: After pressing the ENTER key, the system will dose. Set rinsing: specification of the number of rinsing cycles. Maximum 3 rinsing cycles. Set dosing: The volumes may be selected or preset. Please note: Some volumes are predefined for working without an external keyboard. The standard setting for dosing is 0.00 ml.

005

Set rinsing

set rinsing rinse once rinse two times rinse three times

01

Rinse once: One rinsing cycle will be carried out. Rinse two times: Two rinsing cycles will be carried out. Rinse three times: Three rinsing cycles will be carried out.

Normally, two rinsing cycles are performed in the course of initial filling. If the device contains one and the same reagents and is not used over a certain period of time, single rinsing may frequently be sufficient.

010

dosing set dosing input via keyboard 1 ml 2 ml 5 ml 10 ml 20 ml 50 ml

01

Input using the keyboard also enables the input of odd volumes, such as 1.234 ml. The default values are available for making a selection without using an external keyboard. Check, if defined volume can be dosed with the actual dosing unit in required accuracy. (please refer to Technical Data)

011

147
Hardware settings

Chapter 5 Working with the TitroLine alpha plus

system settings hardware RS parameter date/time beeper password printer sampler

01

RS parameters: Configuration of the RS interface Date/Time: Setting of date and time Beeper: On/off of the acoustic signal Password: Possibility of entering a password in order to protect the method parameters, the system settings, and the method management. Printer: Selection of the desired printer Sample changer: This menu is used for moving the sample changer manually.

178 RS-parameters

RS parameter RS adress 01

01

This item is used to select the RS interface. Two RS interfaces are available. Interface 1 is used for connecting a PC or a serial printer or for daisy-chain data transmission, interface 2 is used for a weighing balance or for daisy-chain data transmission. The term of daisy chain refers to a concept where the first device is connected through the first RS interface to the PC; subsequently, the second device is connected through its first RS interface to the second RS interface of the first device. Each device requires a different address (or number).

240

RS Com 1 word 7, 8, 7, 8, 7, 8, stop 1, 1, 1, 1, 1, 1, parity no no odd odd even even

01

Selection of the possible combinations for the settings required for RS interface 1. The default setting is 7, 1, no. PLEASE NOTE: The parameters have to match those of the connected device.

014

148

Chapter 5 Working with the TitroLine alpha plus

RS Com 1 baud rate 2400 baud 4800 baud 9600 baud 19200 baud

01

Selection of the data transmission rate of the RS interface. The default setting is 4800 baud. PLEASE NOTE: The parameters have to match those of the connected device..

238 Date / Time

date/time year 2000y

01

Year, month, day, hour, minute, second are inquired one after another. Each input has to be confirmed with <ENTER>. The units are not to be input, since they will be attached automatically.

026 Password If desired, a password may be entered here. Method creation, method management, and the system settings can only be called up if the user knows the suitable password. In case the current password should be lost, there is a "master password" which may be used to retrieve the lost one. If required, you may obtain this "master password" from SCHOTT GERTE.

system settings password activated yes no

01

Yes: A password consisting of min. 5 up to max. 11 alphanumeric characters can be input. Afterwards, the corresponding menu is can only be called up using the password. No: The corresponding menus will not be protected.

241

149

Chapter 5 Working with the TitroLine alpha plus

system settings password enter password repeat password

01

A password has to have a minimum length of 5 and a maximum length of 11 characters. The first input field was selected. Pressing the < > key will take you to the second input field. As soon as you press the < > and the ENTER key, the password will be stored.

Please note: If the two passwords do not match, the password protection is not in place, and the input has to be repeated.

125 Printer

system settings HP LowRes HP HiRes Epson LowRes Epson HiRes RS export

01

At this point, the appropriate printer may be selected. Examples: - Epson ESC/P2: Epson Stylus Color 880 - Epson ESC/Raster: Epson Stylus C 70 / C 80 - HP Deskjet: Almost all HP printers with PCL III The selected driver will be activated, if the < > and the ENTER key are pressed.For reasons of speed, we recommend the HP low resolution mode. RS export: If the RS export setting is set, the result will be output through the RS interface in the form of a text file.

315 Sample changer (TW)

sampler TW head up TW head down TW advance TW reverse stirrer off filling Bueretts

01

TW head up: The titration head moves up. TW head down: The titration head moves down. TW advance: The next sample will be approached. TW reverse : The preceding sample will be approached. stirrer off: filling bueretts: The burettes are filled.

395

150
5.3.8 Measurement

Chapter 5 Working with the TitroLine alpha plus

This item can be used to select the desired measurement range for the display of the desired measurement unit.

measure pH pH mV mV C uA A B A B

01

pH A: Display of the pH value of a pH electrode on the A measurement input. pH B: Display of the pH value of a pH electrode on the B measurement input. Both measurement inputs are potentialcontrolled, i.e. both electrodes may be of the single-rod type with built-in reference electrode. mV A: Display of the mV value of an electrode on the A measurement input. mV B: The mV value of the electrode on the B measurement input is shown in analogy to the pH value. C: Display of the temperature. A: display of the A value of a connected double platinum electrode.

008

Measurement pH A/B, example: B measurement channel

measure

01 B

Display of the A value of a pH electrode on B measurement input.

measuring channel

-0.000 pH
25.0 C

300

151
5.3.9 Output

Chapter 5 Working with the TitroLine alpha plus

This menu can be used to output various data - via the printer interface.

output print titration show titration print calibr. data show calibr. data print result list print meas. value

01

Print titration: The documentation of the last titration will be printed. The setting of the method will be used. Show titration: The titration result will be shown on the display. Print cal data: The currently valid calibration data will be output. Show cal data: The currently valid calibration data will be displayed. Print result list: The calculated results of the last 24 samples will be printed in the following order: Name of the sample, Method, Date/Time, Result, value, unit Print meas. value: TEXT???????

009

show calibr. data sensor 1 slope: -59.00 pH zero point: 7.00 pH proceed

01

Display of the slope % and the zero point of the electrode in term pH.

337

show calibr. data validated: temperature 25.00 C buffer 1 4.00 pH buffer 2 7.00 PH buffer 3

01

Display of the selected buffer and the manual temperature. Validation: Indication whether validation is active or not.

Validated: Currently without any meaning.

338

152 5.4

Chapter 5 Working with the TitroLine alpha plus

The Cal menu

Calibration is called by pressing the <F8> key or < >. Calibration is defaulted to an automatic 2-point calibration with the 4.00 and 7.00 DIN buffers. From System settings - Set calibration you may select two out of seven preset buffer solutions. The following DIN 9266 buffers and NBS buffers are available: 1,00; 4,00; 4,01; 6,87; 7,00; 9,18 und 10,00. It is also possible to define buffers of your own.

calibration sensor measuring channel measuring channel A B

01

Selection of the measurement channel to be calibrated. A distinction is made between channel A and B. To proceed, press <ENTER>

131

calibration buffer 1 rinse electrode dip into buf. Buffer 7.00pH

01

An acoustic signal will ask you to start calibration.. Immerse the rinsed electrode into the buffer solution, then start calibration with the <ENTER> key.

132

For the second buffer a new invitation in the form of an acoustic signal will be issued after calibration.

calibration buffer checking expected pH: 4.00 pH measvalue: -144.8 mV 25

01

The display will show the buffer value and the current mV value of the electrode. Considering that the theoretical mV value is pH 59.16, it is possible to give an estimation as to the correctness of the current values.

133

153

Chapter 5 Working with the TitroLine alpha plus

calibration buffer 2 rinse electrode dip into buf. Buffer 4.00pH

01

The way of proceeding is analogous for the second buffer. With <ENTER> you confirm that the electrode is immersed.

132 To leave the calibration mode, please press the <ENTER> key at this point.

The following error messages may appear:

calibration error slope slope is out of specification zero point: 7.00 pH slope: 108,2 %

01

If an incorrect steepness is detected in the course of calibration, this message will be output. Please check your buffer solutions first, then the electrode.

136

calibration error buffer buffer is wrong

01

The way of proceeding is analogous for the second buffer. With <ENTER> you confirm that the electrode is immersed.

137 Upon the successful calibration of the electrode, the zero point and the slope will be displayed. To leave the calibration mode, pressed the <ENTER> key.

154

Chapter 6 Method creation

6
6.1

Method creation

155

Chapter 7 In/Output for data communication

In/Output for data communication

KF Pt

Electrode A

Electrode B

1 RS-232-C 2 Keyboard

Printer Centro-

Ref

Ref
230V:0.25 AT

I 0

Stirrer

12V

out

1 2 3 4 5 6 7 8 9 10 11

Electrode connector pH A/mV A and pH B/mV B Connector for reference electrode channel A and B Mains switch KF connector Connector for temperature-measurement sensor Mains connector Printer connector (Centronics) Stirrer connector (Stirrer) Connector for weighing balance (RS-232-C) Keyboard connector Computer connector (RS-232-C)

156

Chapter 7 In/Output for data communication

Typical applications with available electrode and piston options Application PH titration, aqueous solutions PH titration, non-aqueous solutions Redox- titrations Chlorid- titrations Karl-Fischer- titrations Temperaturemeasurement/ compensation Titration with ion-sensitive electrodes Reference Electrode N 6280 Connection Stecker Buchse an Elektrode am Gert A (DIN)/BNC A or B Electrode cable K1A/ K1BNC

N 6480 LiCl/Eth. Pt 6280 AgCl 62P7 TZ 1106 NN (4mm banana type) W 2130 NN (4mm banana type) TZ 1101 A (DIN) TZ1103 TZ 1104 B 2920 N banana type

KF Pt 1000

K1NN 9907/21

A or B Ref.

K1A B1A

7.1

Keyboard port

The keyboard port is used to connect the TZ 2835 PC keyboard. The device cannot be parameterised without an external keyboard being connected.

7.2 7.3

Power connector Centronics-Interface

Please ensure that the mains voltages matches the voltage set at the bottom panel of the device.

The TitroLine alpha plus Titration Unit is equipped with a Centronics interface (parallel). It is used to output result protocols, charts etc. on a printer with the same interface. The plug-in port for this interface is located on the back panel (figure 6, item 7, Centronics / Printer)). Pin configuration of the Centronics interface: Pin no 1 29 10 11 12 13 Meaning Strobe Data 0 - Data 7 Acknlg Busy PE SLCT Pin no 14 15 16 17 18 - 25 Meaning NC ERROR Init GND GND

157 7.4

Chapter 7 In/Output for data communication

RS-232-C-Interfaces

The TitroLine alpha plus Titration Unit is equipped with two serial interfaces (RS-232-C) for data communication with other devices. The plug-in ports of these interfaces are located on the back panel of the device. The Computer socket is used to establish the connection with a computer or printer with a serial interface. The Balance socket can be used to connect a weighing-balance. Pin no 1 3 5 7 9 Meaning n. c. T x D data input Digital Mass n .c n .c Pin no 2 4 6 8 Meaning R x D data output n. c. n. c. CTS

Please note: The data-transmission parameters are to be set in the Systems settings and <<RS>> menu. The transfer parameters of all devices communicating with each other have to be the same. The ex-works settings of the transmission parameters are: 4800 baud, 7 bit, 2 stop bits, no parity. Optional parameters: Baudrate 1200, 2400, 4800, 9600, 19200 The remaining parameters are as follows: Data bits Stop Parity 7 1 no 8 1 no 7 1 odd 8 1 odd 7 1 even 8 1 even

7.5

Loading the operating-system software via the RS-232-C interface

The TitroLine alpha plus Titration Unit is equipped with a FLASH memory for storing the OS software. This FLASH memory enables new software versions to be loaded down via the RS 232 C interface from a PC onto the TitroLine alpha plus Titration Unit. This is a convenient feature if enhancements and improvements of the functions of the TitroLine alpha plus Titration Unit lead to the generation of a new software version. To use this feature, you need a PC with a free serial interface, the download software from SCHOTT, and a serial data cable of the TZ 1581 type. For the way of proceeding, please refer to the operating instructions of the download software. IMPORTANT NOTE: After the download of the software, the two middle keys of the TitroLine alpha plus Titration Unit have to be pressed simultaneously with the device being switched on. This will initiate an internal data reset which is indispensable in view of the devices proper functioning. It is also possible to update the standard methods using the RS interface. In this case, too, the required data are to be downloaded into the device through the RS interface.

158 7.6

Chapter 7 In/Output for data communication

Controlling the TitroLine alpha plus Titration Unit via the RS-232-C interface

The following commands can be used to control the TitroLine alpha plus Titration Unit via the RS-232-C / Computer interface: <aa> steht fr die Adresse des jeweiligen Gertes (immer zweistellig). Reply Action Version: 060602-01 Output of version number Ident: TL alpha plus Hardware report Status: READY/MODE/INIT/CAL Report status (where am I?) aaRC Last command Repeat last command aaRA aa UNIT: 10 ml Inquiry of unit size aaSM aaY Start of a method aaMC01..08 aaY Method change aaFD aaY Measure dead stop function aaFPA+B aaY Measure pH A + B function aaFVA+B aaY Measure mV A + B function aaFT aaY Measure temperature function aaM Measurement value Measure within the set measuring range aaO OOM:1.912 pH Online measurement, output of 0.080 ml an on-line measurement value aaQE aaY Stirrer on aaQA aaY Stirrer off aaLC Output of calibration values via RS computer aaLD Output of datav aaBF aaY Burette is filling aaDB01.12 aaY Burette is dosing volume without filling and zero-setting. Please note: Commands involving small volumes which cannot be dosed will not be executed. aaDA01.12 aaY Burette is dosing volume without filling, with volume addition aaGF30 aaY Filling time in seconds (30 s min.) aaGDH 11.3 aaY Dosing rate in ml/h aaGDM20.3 aaY Dosing rate in ml/min Each command must be entered separately and concluded with <CR> <LF>. All replies will be returned to the computer after each action has been completed. Command aaVE aaRH aaRS

159

Chapter 8 Maintenance and care of the TitroLine alpha plus Titration unit

8
8.1

Maintenance and care of the TitroLine alpha plus Titration Unit


Maintenance and care of the titrator section

Proper functioning of the device has to be maintained by check and maintenance work. This maintenance or service work include: Visual control: Measurement ranges mV: pH: C: Front-membrane display 3 values - nominal/actual 6 values - nominal/actual 3 values - nominal/actual

Function:

Karl Fischer titration (dead-stop)

Interface functions, measuring amplifier, control behaviour, dialog system, keyboard function, stirrer connection, printer output. Once per quarter, the electrical contacts have to be checked if the titration unit is used in premises with an occasional occurrence of corrosive matters in their atmosphere.

8.2

Maintenance and care of the burette section

Proper functioning of the TitroLine alpha plus Titration Unit has to be maintained by check and maintenance work. Maintenance intervals Normal operation: In a larger sense, the valve and the glass cylinder are parts which are subject to wear and tear; this means, that the glass surface may be damaged by the use of chemicals. This wear and tear may lead to inaccurately dosed volumes. For this reason, the dosing accuracy of the device is to be verified. As a rule, the max. intervals for carrying out all maintenance work is 6 months. Under particular stress:

Once per quarter, the glass cylinder has to be inspected visually in order to check for damages, and in addition a test according to DIN EN ISO 8655, Part 6, has to be carried out. These inspections are particularly necessary if solutions were used which are likely to attack glass, e. g. alkaline, fluoride, or phosphatic solutions. If there is any suspicion that a solution is attacking the glass excessively, the maintenance intervals are to be reduced accordingly.

In case of disturbances: The work has to be carried out immediately if a disturbance, an error, or another defect becomes obvious. Maintenance work to be carried out

Check the piston and the cylinder for visible signs of mechanical damage, such as 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, contamination, and leaks. Check the electrical plug contacts for corrosion and mechanical damage (on the titration unit and on the cables). Defective parts must be repaired or replaced by new ones. Defective glass parts must always be replaced. After each maintenance operation, a test for metrological reliability according to DIN EN ISO 8655, Part 6, has to be carried out.

160

Chapter 8 Maintenance and care of the TitroLine alpha plus Titration unit

Periods without operation

We If the dosing units for the TitroLine alpha plus Titration Unit are not used over a long period of time, the liquids contained in the system, in particular aggressive solutions, have to be drained. If the liquid is left in the system, one has to reckon with corrosion and an alteration of solutions used over the time. Since the state of the art does not provide plastic hoses which are absolutely free of diffusion occurrences, these precaution measures apply in particular to the hose-line section.

Cleaning

The dosing units can be cleaned using a piece of cloth soaked in normal water or a household cleansing agent containing ethanol. In general, short-term immersion in, or rinsing with, water or ethanol is not harmful, but this method should only be applied in extreme cases. The casing of the lower section may also be cleaned using a piece of cloth and a household cleansing agent. The bottom and rear side have to be cleaned dry. In no case must water penetrate into the interior of the lower section.

Reproducibility of results

The measurement results or analysis results depend on a variety of factors. Please check the plausibility of the measurement results or analysis results at regular intervals, and carry out the required reliability tests. In this regard, please adhere to the usual validation procedures.

Storage and transportation

If the TitroLine alpha plus Titration Unit has to be stored over some time, or to be dislocated, using the original packing will be the best protection of the device. However, in many cases this packing will not be available any more, so that one will have to compose an equivalent packaging system. Sealing the lower section in a foil is hereby recommended. The devices should be stored in a room with a temperature between +10 and +40C, and the (relative) humidity of the air should not exceed 70 %. If dosing units are to be stored over some time, or to be dislocated, the liquids contained within the system, in particular any aggressive solutions, have to be drained; also refer to chapter 8.2, Maintenance and care of the burette section.

10

Recycling and disposal

The present titration unit and its packing material were mainly made from materials which can be disposed of and recycled in an environmentally friendly manner. Please note: The main printed board contains 2 lithium batteries. Batteries should not be made part of the domestic waste. They will be taking back at no charge by the manufacturer and forwarded to proper reuse or disposal. Should you have any questions regarding disposal, please contact SCHOTT Instruments.

Reference List

161

11

Reference list

Care..23 Cleaning...24 Computer connector Connector for temperature sensor probe...18 Connector for weighing-balance..18 Control of the TitroLine alpha22 Cylinder..9 Electrode connector.. 18 EPROMs.9 First operation..10 Keyboard connector19 Mains connector Mains switch Mains voltage Maintenance.9 Measurement amplifier.17 Measurement sensor..3 Mini keyboard3 Operating voltage Periods without operation..24 Printer.3 Printer port18 Safety information..9 Set-up10 Stirrer..3 Stirrer connector..18 Storage..80 Warning information 9

162
Notes:

163
Notes:

Typ / Type / Type / Tipo:

TitroLine alpha plus

Bescheinigung des Herstellers


Wir besttigen, dass das oben genannte Gert gem DIN EN ISO 9001, Absatz 8.2.4 berwachung und Messung des Produkts geprft wurde und dass die festgelegten Qualittsanforderungen an das Produkt erfllt werden.

Suppliers Certificate
We certify that the equipment was verified according DIN EN ISO 9001, part 8.2.4 Monitoring and measurement of product and that the specified requirements for the product are met.

Certificat du fournisseur
Nous certifions que le produit a t vrifi selon DIN EN ISO 9001, partie 8.2.4 Surveillance et mesure du produit et que les exigences spcifies pour le produit sont respectes.

Certificado del fabricanteNosotros certificamos que el equipo est verificada conforme a DIN
EN ISO 9001, parte 8.2.4 Sequimento y medicin del producto y que las especificaciones requeridas para el equipo son respetadas y cumplidas.

Printed in Germany

SCHOTTInstruments GmbH Postfach 24 43 D-55014 Mainz Hattenbergstrae 10 D-55122 Mainz

Tel.: +49 (0)6131/66-5111 Fax: +49 (0)6131/66-5001 E-Mail: titration@schottinstruments.com www.schottinstruments.com

EDV 008 27 007 4

Version 040714 ME