Metrohm 799 GPT Titrino User Manual

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799 GPT Titrino, Short instructions for use

CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com

799 GPT Titrino

Short Instructions for Use

8.799.1023 04.2002 / pkl

Page 2

799 GPT Titrino, Short instructions for Use

Table of contents

1. Getting started .........................................................................1

1.1 Principle of data input ...........................................................2

1.2 Development of a method.....................................................3

1.3 Storing methods....................................................................7

1.4 Working with several dosing units ...................................... 10

2. Titration, dosing and measuring modes...............................12

2.1 Survey of the titration modes .............................................. 12

2.2 Mode DET and MET, parameters .......................................14

2.3 Mode SET, parameters .......................................................15

2.4 Mode KFT, parameters........................................................ 16

2.5 Mode STAT, parameters .....................................................17

2.6 Mode DOS, parameters ......................................................19

2.7 Mode DOC, parameters ......................................................20

2.8 Mode MEAS and CAL, parameters ..................................... 21

2.9 Mode TIP, parameters.........................................................22

2.10 Calculations ....................................................................... 23

3. Other functions ......................................................................25

3.1 Method memory ..................................................................25

3.2 User name, key <user> ..................................................... 27

3.3 Sample data, keys <smpl data> and <silo>.................... 27

3.4 Configuration, key <configuration>................................... 28

Index...........................................................................................30

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1.1 Principle of data input

799 GPT Titrino: Getting started

Summary of the most important signs

Signs in the Titrino dialog:

> Title of inquiry groups. Press <ENTER> to go to

the inquiries.

: Values can be chosen with keys <←> or <→>.

Signs that are used in the instructions for use <> sign for "key", e.g. <ENTER> or <←>.

Page 4

1.1 Principle of data input

799 GPT Titrino: Getting started

1 Getting started

This is a step by step introduction into the operation of the Titrino. You learn how to go round with the Titrino and you get an idea of the possibilities that the Titrino offers you.

1.1 Principle of data input

<↓>

<ENTER>

<←> or <→>

<ENTER>

2 x <QUIT>

Press <STOP> if the Titrino is busy. It is now in the inactive standby state. Then press the <CONFIG> key.

The first line indicates the "path", which means the place where you are right now: You pressed the <CONFIG> key and are now in the "configuration" inquiries. In the next lines you find a list of the inquiry groups of key <CONFIG>. They are all marked with ">". This sign means that you get to the inquiries with <ENTER>. The inquiry group ">monitoring" is inverted, which means that the cursor is placed on this line. You can move the cursor up and down with the <↑> and <↓> keys.

Set the cursor to ">auxiliaries" and open this inquiry group with <ENTER>.

The arrow in the lower right corner means that there are more inquiries. They appear if you move the cursor below.

Set the cursor to the inquiry "dialog:". You may select a different dialog language with the keys <←> or <→> (Key <→> "turns" forward, <←> backward).

Select any language and press <ENTER>.

Note the sign ":" in the text "dialog:". If you see this sign in the dialog text you can always use the <←> or <→> keys to select a value.

Readjust the language to "english" again.

Quit the inquiries in the <CONFIG> key pressing <QUIT> twice.

configuration >auxiliaries dialog: english date 2002-04-08 time 15:23 run number 0 auto start OFF start delay 0 s ↓

configuration >monitoring >peripheral units >auxiliaries >RS232 settings COM1 >RS232 settings COM2 >common variables >prep.dosing elements

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1.2 Development of a method

799 GPT Titrino: Getting started

1.2 Development of a method

You learn how to elaborate a method . First you select a titration mode. A general survey of the different titration modes is given on page 12.

Selecting the mode

<MODE>

<←> or <→>

<ENTER>

<START>

<STOP>

Press the <MODE> key. Select the mode DET with <←> or <→> keys, press <ENTER>, select the measured quantity "pH" and press <ENTER> again. DET stands for Dynamic Equivalence point Titration. In this titration, the size of the volume increments vary as a function of the slope of the titration curve. After each increment, a preset measured value drift (or time) is awaited until the next increment is added (so called "equilibrium titration"). After the titration, the equivalence points are evaluated automatically.

You are now ready to titrate. You titrate with the internal dosing unit D0, i.e. the Exchange Unit on the Titrino.

Mount an Exchange Unit with NaOH, c=0.1 mol/L on the Titrino. Plug a combined pH glass electrode into measuring input ("Ind I"). Pipette 2 mL HCI, c =0.1 mol/L into the titration vessel, dilute it with ca. 20 mL. dist. water, adjust the stirrer and press <START>.

During the titration the titration curve is displayed. To the left of the curve, the current measured values (pH and volume) are displayed. As soon as the Titrino has found an equivalence point, it will also be shown the left.

Let the titration continue for a short while, e.g. until ca. pH=11.50. Now stop it with <STOP>.

The equivalence point is displayed.

DET pH D0a ********

mode mode: DET measured quantity: pH

DET pH D0a ******** EP1 2.083 ml pH 7.64

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1.2 Development of a method

799 GPT Titrino: Getting started

Calculation of the result, entry of a formula

<DEF>

<ENTER>

<1>

<ENTER>

2 x <QUIT>

You may calculate results with the equivalence point. Press <DEF>.

Press <ENTER> to move on to the formula entry. The display now shows "RS? ". Press "1", i.e. the first formula.

You can now enter a formula. Note here the inscriptions in the right corner of the keys and the numbers. You can use mathematical operations, parentheses as well as the following symbols: EP# EP’s with 1-digit number, e.g. EP1. RS# Previously calculated results, e.g. RS1 in the sec-

ond formula.

C## Calculation values, e.g. C01. C00 is reserved for

the sample size. The meaning of the different cal-

culation values is given on page 24. Calculate the content of your hydrochloric acid in g/L: RS1=EP1*C01*C02/C00 EP*conc(titrant)*molar mass/sample size If you made a typing mistake, you can delete the symbols one by one with <CLEAR>. Confirm the formula with <ENTER>.

You may enter a text for the result output, see page 7. Enter the desired number of decimal places for the result. Select the unit g/I with <←> or <→> or enter a text as unit.

Quit the formula entry by pressing <QUIT> twice.

Instead of the equivalence point, the calculates result will be displayed. It is 0 because the calculation values C01 and C02 are still zero.

Entry of the calculation constants

<C-FMLA>

Press <C-FMLA>, to enter the calculation values. The constants which have been used in the formula are requested: C01: Concentration of your titrant = 0.1 mol/L C02: Molar mass of HCI = 36.47 g/mol

The result is recalculated.

def >formula RS1=EP1*C01*C02/C00

RS1 text RS1 RS1 decimal places 2 RS1 unit: g/l RS1 limit control: OFF

def >formula RS1=EP1*C01*C02/C00

def >formula >silo calculations >common variables >report >mean >temporary variables

C-fmla C01 0.0 C02 0.0

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1.2 Development of a method

799 GPT Titrino: Getting started

Entry of the sample size

You also need the sample size for the calculation of your

result. Enter it with the <SMPL DATA> key:

Place the cursor to "smpl size" and enter 2.

Select the unit "ml" for the sample size using the <←>

or <→> keys and confirm with <ENTER>.

The result is recalculated.

Viewing the titration curve

<←> or <→>

You can view the titration curve after the titration using

the <←> or <→> keys.

With the <↑> and <↓> you can trace the curve. To the

left the measured values of the current point are dis-

played. On the first line you will find the index of the

point.

At the equivalence point, you find its ERC (see Instruc-

tions for Use page 21, 22) and its volume.

Quit the curve display with <←> or <→> key.

Selection of the automatic report output

<DEF>

<↓>

<ENTER>

<←> or <→>

<ENTER>

2 x <QUIT>

If you have a printer connected, you can select the re-

port blocks to be printed out automatically at the end of

the titration.

Press <DEF> and place the cursor to ">report".

Press <ENTER> to define the report output.

(If you have your printer connected to COM2 press

<ENTER> once again.)

Select the individual report blocks with the <←> or

<→> keys. Use a ";" as delimiter between the report

blocks. If you wish to print out a curve and a full result

report, set "curve;full".

Confirm the entry with <ENTER> and quit the inquiries

with <QUIT>

smpl data id#1 or C21 id#2 or C22 id#3 or C23 smpl size 1.0 g smpl unit: g

def >report report COM1:curve;full

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1.2 Development of a method

799 GPT Titrino: Getting started

Press <PRINT> <REPORTS> <ENTER> to print your reports. Your printout will look as follows:

Identification of report type (cu = curve)

Start volume and method identification Scaling of curve axis

Instrument type with identification and program version

Initial pH

Volume and pH value of EP1

Calculated result

Entry of a stop criterion

<PARAM>

<↓>

<ENTER>

Entries <ENTER>

2 x <QUIT>

You don't want to stop your titration manually each time. Let us enter an automatic stop criterion.

Press <PARAM> and place the cursor to ">stop conditions". Press <ENTER> to go to this inquiry group.

The absolute stop volume. It can be used as a safety volume to prevent overflow of the titration vessel. Enter a value for the stop volume that appears suitable for your titration vessel.

Set the pH value, e.g. 11.5 as stop criterion. If several stop criteria have been set, the one that is reached first, applies.

Confirm the input with <ENTER> and quit the inquiry with <QUIT>.

Try another titration with this method.

parameters >stop conditions stop V: abs. stop V 99.99 ml stop pH aus stop EP 9 filling rate max. ml/min

'cu 799 GPT Titrino 01102 799.0010 date 2002-04-08 time 09:07 1 Start V 0.000 ml DET pH ********

1.0 ml/div dpH=2.0/div

−−−−−−−−−−−−−−−−

'fr 799 GPT Titrino 01102 799.0010 date 2002-04-08 time 09:07 1 pH(init) 2.88 DET pH ******** smpl size 2 ml EP1 2.083 ml 7.64 RS1 3.80 g/l manual stop

−−−−−−−−−−−−−−−−

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1.3 Storing methods

799 GPT Titrino: Getting started

1.3 Storing methods

You learn how to operate the method memories. The Titrino offers 2 types of method memories:

• Internal method memory, key <USER METH>

• External method memory on the card, key <CARD>

Storing a method in the internal method memory

<↓>

<ENTER>

Entries <ENTER>

<QUIT>

<ENTER>

Press <USER METH>, place the cursor to ">store

method" and press <ENTER>.

Press <CLEAR> to delete the existing method name

(********).

Open text entry with key <ABC>.

A field with letters and symbols appears. You can select

a letter with the cursor keys and confirm this letter with

<ENTER>. The letter then appears in the input field of

the method name.

Enter an identification for your method, e.g. HCl:

If you made a typing error you can delete the characters

one by one with <CLEAR>.

Quit the text input with <QUIT> when you completed

your name.

Confirm the name with <ENTER>. The method will be

stored in the internal method memory.

The method runs now under the identifier "HCl".

A list of contents of the method memory can be printed

with the key sequence <PRINT><USER

METH><ENTER>.

'um 799 GPT Titrino 01102 799.0010 date 2002-04-08 time 07:49 user methods bytes DET pH Titer_pH D0 190 DET U Blank D0 178 DET U Chloride D0 234 MET U Diazo D0 208 MET Ipol Br-Index D0 226 DET U Perox.No D0 172 DET pH HCl D0 108 remaining bytes 98684

------------

mode and meas.quantity

method name

dosing unit, that is being used

user methods >store method method name:

ABCDEFGHIJKLMNOPQRSTUVWXYZ abcdefghijklmnopqrstuvwxyz µ°!"#$&'()*+,-./ 0123456789

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1.3 Storing methods

799 GPT Titrino: Getting started

Recall a method from the internal method memory

<ENTER>

<←> or <→>

<ENTER>

Stored methods can always be recalled into the working memory.

Press <USER METH> and <ENTER> to go to ">recall method".

You can select a method with <←> or <→> or enter its name directly.

Recall the method with <ENTER>.

The method is now ready to work.

Method memory on the card

The card offers additional memory space for methods. It may be used e.g.

• as a backup-medium for the internal method memory

• as an extended method memory, where the methods

can be organized in various directories

• if every user wants to store his methods on his own card

• for exchanging methods between various laboratories, apparatus, and/or users

The card has a battery, which should be exchanged periodically, see page 91 of the Instructions for Use.

As an example, perform a backup from the internal method memory to the card. If the card is not formatted, see page 91 of the Instructions for Use.

<CARD>

<↓>

<ENTER>

<←> or <→>

<ENTER>

Press <CARD> and place the cursor to ">backup".

Confirm this function with the key <ENTER> and give a name for the backup directory. If you wish to overwrite an existing directory, choose a name with <←> or <→>. Then press <ENTER>

The backup will be effected.

user methods >recall method method name: ********

user meth. >backup dir.name: Backup

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1.3 Storing methods

799 GPT Titrino: Getting started

Printing a list of contents of the card

The following card reports can be printed:

'ad 799 GPT Titrino 01102 799.0010 date 2002-04-08 time 07:49 card label: Appl.799 dev.label: KF Titr. bytes KFT Ipol TarTiter D0 150 KFT Ipol H2OTiter D0 150 KFT Ipol Blank_KF D0 132 KFT Ipol KF-Blank D0 206 KFT Ipol KF D0 170 remaining bytes 121892

------------

Current directory

name of the current directory

remaining bytes on this card

'cd 799 GPT Titrino 01102 799.0010 date 2002-04-08 time 07:50 card label: Appl.799 dev.label:

directory: user meth. Acid Tit.NaOH Tit.HCl W-Liquor bytes: 620

directory: KF Titr. TarTiter H2OTiter Blank_KF KF-Blank KF bytes: 808 remaining bytes on card: 121892

------------

Contents of the whole card

Press <←> or <→> repeatedly until

"mem card" appears in the display.

bytes that are being used in the directory "user meth."

methods in this directory

the directory "KF Titr." contains 5 methods

Page 12

1.4 Working with several dosing units

799 GPT Titrino: Getting started

1.4 Working with several dosing units

Here you will learn how to work with several dosing units. Several dosing units can be used

• if a working station will be permanently installed for specific analysis, e.g. having a dosing unit specially prepared for Karl Fisher titrations

• if several titrations are being carried out in the same sample. The linking of various methods is possible with TIP (Titration Procedure), see page 85 of the In- structions for Use.

• for addition of auxiliary solutions

Selection of the dosing unit in the titration method

The dosing unit is selected in the method. The method runs always with the selected dosing unit. Connect the dosing unit D1 and arm it with an Exchange Unit (the Dosino with a Dosing Unit, resp.).

<PARAM>

<ENTER>

<↓>

<←> or <→>

<ENTER>

2 x <QUIT>

Recall the method "HCl" from the user memory: Press <USER METH>, then <ENTER>. Select the method name "HCl" with the keys <←> or <→> and recall the method with <ENTER>.

The dosing unit of this method is D0, i.e. the Titrino itself.

To change the dosing unit, press <PARAM>, then <ENTER>. You are now in the inquiry group ">titration parameters". Place the cursor on "dos.element:". Choose the dosing unit with keys <←> or <→>: internal D0: Dosing unit of the Titrino external D1: External dosing unit, connected to 1 or 2. Choose e.g. "external D1", confirm the input with <ENTER> and quit with the key <QUIT>.

The display shows now e.g. "DET pH D1 HCl". D1 means, that in this method the external dosing unit D1 is being used. Start the method. After the titration "D1a" appears in the display. "a" means "active", the dosing unit D1 is now active.

DET pH D1 HCl

parameters >titration parameters dos.rate. max. ml/min signal drift 50 mV/min equilibr.time 26 s start V: OFF pause 0 s dos.element: internal D0

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1.4 Working with several dosing units

799 GPT Titrino: Getting started

Manual dosing

• to prepare an Exchange Unit (or Dosing Unit, resp.)

• for quick dosing

If you press the key <DOS>, the dosing unit from the method is working. This dosing unit appears in the display. If you wish to dose with another dosing unit, use the key <PREP> to select the dosing unit and press <DOS> to dose.

<PREP>

<QUIT>

Press <PREP>. In the display appears "internal D0 prep", i.e. the dosing unit of the Titrino has been selected.

Press <PREP> again. In the display appears "external D1: prep".

Press the key <DOS> on the Titrino: The external dosing unit D1 doses. If you press the key <STOP/FILL> on the Titrino, it will fill again.

With <START>, the function "prep" is started. This prepares the dosing units. (The parameters for "prep" are under the key <CONFIG>, in the group ">prep.dosing elements"). Attention: With the function "prep", liquid will be expelled!

If the dosing unit D1 is a Dosino, you can empty the dosing unit completely (e.g. for cleaning). Choose the function "empty" with the key <←> or <→> and start with <START>. Attention: With the function "empty", liquid will be expelled!

Quit the selection of dosing units with <QUIT>.

internal D0 prep

Page 14

2.1 Survey of the titration modes

799 GPT Titrino: Titration, dosing and measuring modes

2 Titration, dosing and measuring modes

This chapter gives you a survey over the titration, dosing and measuring modes. You will find the parameters of all modes. The standard values are printed in bold face in the following tables.

2.1 Survey of the titration modes

DET

Dynamic Equivalence point Titra-

tion

MET

Monotonic Equivalence point Titra-

tion

Titration

Reagent feeding: Variable volume increments, depending on the slope of the curve.

Drift controlled ("equilibrium titration")

and/or

after a fixed equilibration time.

Reagent feeding: Constant volume increments, independent of the slope of the curve.

Drift controlled ("equilibrium titration")

and/or

after a fixed equilibration time.

Evaluation

The evaluation of EP' s is based on the zero crossing of the second derivative with a Metrohm correction for the distortion of the curve from superimposed jumps. Can be combined with selectable recognition criteria.

Recognition criteria: as for MET

The evaluation of EP's is based on the Fortuin interpolation.

Recognition criteria: all EP's only the last EP only the greatest EP EP windows

Applications

Suitable titration mode for most problems. Specially recommended if jumps lie very close together and for very flat jumps.

Note: The reagent feeding algorithm is based on measured data. The curve should therefore not deviate markedly from S-shape.

For

• slow titration reactions (diazotations, coupling reactions)

• sluggish electrode response.

V/mL

U/mV

V/mL

U/mV

Page 15

2.1 Survey of the titration modes

799 GPT Titrino: Titration, dosing and measuring modes

If you are looking for more information to the different quantities, you will find the display text as a keyword in the index of the Instructions for Use.

SET, KFT

Endpoint Titration

STAT

Holding a measured value

DOC

Controlled dosing

Titration to preset end-point.

The reagent addition is controlled such that a preset measured value is adhered to as accurately as possible.

The dosing function is controlled such that a nominal measured value is adhered to as accurately as possible. The nominal measured value follows a linear ramp.

Volume that has been dispensed up to the endpoint (EPX in mL).

Evaluation of

• rates dV/dt in the set time windows and the mean rate over the entire measuring point list.

• volumes associated with a preset time (fix V).

• times associated with a preset fraction of the total volume (fix time).

The total volume (C41) and the time needed for dosing (C42) can be used for calculation.

• For rapid, quantitative determinations in analytical chemistry. Requirement: EP of the titration reaction is known and does not change during a determination series.

• If an excess of titrant must be avoided.

• KFT: Determinations of water contents.

For

• the controlled dosing to a preset endpoint in the synthesis laboratory.

• activity determinations, e.g. of enzymes.

• kinetic investigations (first order kinetics).

Sweeping a measured value gradient for reaction formulations in the syntheses laboratory.

V/mL

U/mV

continuously

Control range

t/s

V/ml

rate

t/s

U/mV

V/ml

set

Page 16

2.2 Mode DET and MET, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.2 Mode DET and MET, parameters

Display Meaning Input range

>titration parameters meas.pt.density min.incr. [V step] dos.rate signal drift equilibr.time start V: start V factor

dos.rate pause dos.element: meas.input: temperature

Measuring point density. Minimum increment for DET. Volume increment for MET. Dosing rate for increments. Drift for measured value acquisition. Waiting time for value acquisition. Type of start volume: absolute, relative. Volume for absolute start volume. Factor for calculation of relative start volume: factor * smpl size. Dosing rate for start volume. Waiting time, e.g. after start volume. Selection of the dosing unit. Measuring input for pH and U. Titration temperature.

0...4...9

0...10.0...999.9 µL

0...0.10...9.999 mL

0.01...150 mL/min, max.

pH, U:0.5..50..999 mV/min, OFF

0...26...9999 s, OFF

abs., rel., OFF

0...999.99 mL

0...±999 999

0.01...150 mL/min, max.

0...999 999 s

internal D0, external D1/D2

1, 2, diff.

-170.0...25.0...500.0 °C

>stop conditions stop V: stop V factor

stop pH

stop EP

filling rate

Type of stop volume: absolute or relative. Volume for absolute stop volume. Factor for calculation of relative stop volume: factor * smpl size. Stop at measured value pH, U, I.

Stop after a number of EP's have been found. Filling rate after the titration.

abs., rel., OFF

0...99.99...9999.99 mL

0...±999 999

pH: 0.00...±20.00, OFF

U: 0...±2000 mV, OFF

1...9, OFF

0.01...150 mL/min, max.

>statistics status: mean n= res.tab: delete n=

Status of statistics calculation. Number n of single values for statistics. Result table for statistics calculation. Delete data from sample number n.

ON, OFF

2...20

original, delete n, delete all

1...20

>evaluation EPC

EP recognition:

fix EP1 at pH

pK/HNP:

Endpoint criterion.

Type of EP recognition: all EP's, only greatest EP, only last EP, only EP's in windows, no evaluation. If ”window” is selected, lower and upper limits of windows are inquired. Interpolation of volume at given pH, U, or I, resp. Up to 9 fix EP's. Evaluation of pK or half neutralization potential (HNP).

DET 0...5...200

MET pH: 0.10...0.50...9.99

U: 1...30...999 mV

all, greatest, last, window, OFF

pH: 0.00...±20.00, OFF

U: 0...±2000 mV, OFF

ON, OFF

>preselections

Preselections for the sequence see DOS, page 19.

Page 17

2.3 Mode SET, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.3 Mode SET, parameters

Display Meaning Input range

>SET1 EP at pH

dynamics

max.rate min.rate stop crit: stop drift t(delay)

stop time

Individual parameters for EP1. Preset EP1 at pH, U, or I, resp.

Distance from EP where constant dosing stops and controlling begins. Maximum dosing rate. Minimum dosing rate. Type of stop criteria. Titration stops if stop drift is reached. Stop if there is no dosing during t(delay). If t(delay) is ”INF”: stop after a time.

pH: 0.00...±20.00, OFF

(0...±2000 mV, 0.0...±200.0 µA)

pH: 0.01...20.00, OFF

(1...2000 mV, 0.1...200.0 µA)

0.01...10...150 mL/min, max.

0.01...25.0...9999 µL/min

drift, time

1...20...999 µL/min

0...10...999 s, INF

0...999 999 s, OFF

>SET2 Parameters for EP2. Identical as SET1.

>titration parameters titr.direction:

pause 1 start V: start V factor

dos.rate pause 2 extr.time dos.element meas.input: temperature time interval

General titration parameters. +:Titration to higher pH, voltage, or current. Auto: Direction is set automatically. Waiting time before start volume. Type of start volume: absolute or relative. Volume for absolute start volume. Factor for calculation of relative start volume: factor * smpl size. Dosing rate for start volume. Waiting time after start volume. Extraction time. Selection of the dosing unit. Measuring input for pH and U. Titration temperature. Time interval for measured value acquisition.

+, -, auto

0...999 999 s

abs., rel., OFF

0...999.99 mL

0...±999 999

0.01...150 mL/min, max.

0...999 999 s

internal D0, external D1/D2

1, 2, diff.

-170.0...25.0...500.0 °C

1...2...999 999 s

>stop conditions stop V: stop V factor

filling rate

Type of stop volume: absolute or relative. Volume for absolute stop volume. Factor for calculation of relative stop volume: factor * smpl size. Filling rate after titration.

abs., rel., OFF

0...99.99...9999.99 mL

0...±999 999

0.01...150 mL/min, max.

>statistics Statistics calculation see at DET, page 14.

>preselections conditioning: display drift: drift corr: drift value req.ident: req.smpl size: limit smpl size: activate pulse:

Automatic conditioning of titration vessel Display of drift during conditioning. Type of drift correction. Value for manual drift correction. Request of identifications after start. Request of sample size after start. Limit control of sample size. Pulse output on I/O line L6.

ON, OFF

auto, man., OFF

0.0...99.9 µL/min

id1, id1 & 2, all, OFF

value, unit, all, OFF

ON, OFF

first, all, cond., OFF

Page 18

2.4 Mode KFT, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.4 Mode KFT, parameters

Display Meaning Input range

>control parameters EP at ...

dynamics

max.rate min.volume incr. stop crit: stop drift t(delay) stop time

Controlling parameters for KFT. Endpoint for Ipol. Endpoint for Upol Distance from EP where constant dosing stops and controlling begins. Maximum dosing rate. Minimum volume increment Type of stop criteria. Titration stops if stop drift is reached. Stop if there is no dosing during t(delay). If t(delay) is ”INF”: stop time.

U: -2000 ... 250...2000 mV

I: -200.0... 25.0...200.0 µA

U: 1...100...2000 mV

I: 0.1...10...200.0 µA

0.01...150 mL/min, max.

0.1...9.9 µL, min

drift, time

1...20...999 µL/min

0...10...999 s, INF

0...999 999 s, OFF

>titration parameters titr.direction:

pause 1 start V: start V factor

dos.rate pause 2 extr.time dos.element I(pol) U(pol) electrode test: temperature time interval

General titration parameters. +: Titration to higher voltage or current. auto: Direction is set automatically. Waiting time before start volume. Type of start volume: absolute or relative. Volume for absolute start volume. Factor for calculation of relative start volume: factor * smpl size. Dosing rate for start volume. Waiting time after start volume. Extraction time. Selection of the dosing unit. Polarization current for Ipol or voltage for Upol in 10 mV-intervals. Performing of electrode test Titration temperature. Time interval for measured value acquisition.

+, -, auto

0...999 999 s

abs., rel., OFF

0...999.99 mL

0...±999 999

0.01...150 mL/min, max.

0...999 999 s

internal D0, external D1/D2

-127...50...127 µA or.

-1270...400...1270 mV

ON, OFF

-170.0...25.0...500.0 °C

1...2...999 999 s

>stop conditions stop V: stop V factor

filling rate

Type of stop volume: absolute or relative. Volume for absolute stop volume. Factor for calculation of relative stop volume: factor * smpl size. Filling rate after the titration.

abs., rel., OFF

0...99.99...9999.99 mL

0...±999 999

0.01...150 mL/min, max.

>statistics Statistics calculation see at DET, page 14.

>preselections conditioning: display drift: drift corr: drift value req.ident: req.smpl size: limit smpl size: oven:

activate pulse:

Automatic conditioning of titration vessel. Display of drift during conditioning. Type of drift correction. Value for manual drift correction. Request of identifications after start. Request of sample size after start. Limit control of sample size. RS-COM of Titrino where Oven is connected. Pulse output on I/O line L6.

ON, OFF

auto, man., OFF

0.0...99.9 mL/min

id1, id1 & 2, all, OFF

value, unit, all, OFF

ON, OFF

COM1, COM2, OFF

first, all, cond., OFF

Page 19

2.5 Mode STAT, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.5 Mode STAT, parameters

Display Meaning Input range

>control parameters EP at pH

dynamics

max.rate min.rate

Endpoint, control point: This value is kept constant. Distance from EP where constant dosing stops and controlling begins. Maximum dosing rate Minimum dosing rate

pH: 0.00...±20.00, OFF

(0...±2000 mV, 0.0...±200.0 µA)

pH: 0.01...1...20.00, OFF

(1..60..2000 mV, 0.1.6..200.0µA)

0.01...10...150 mL/min, max.

0.01...25.0...9999 µL/min

>titration parameters start V: start V factor dos.rate pause start time start pH

start rate time interval titr.direction:

dos.element meas.input: temperature

General titration parameters. Type of start volume: absolute or relative. Volume for absolute start volume. Factor of relative start volume. Dosing rate for start volume. Waiting time, after start volume. Start time for data acquisition. Start measured value for data acquisition.

Start rate for data acquisition. Time interval for data acquisition. +: Titration to higher pH, U or I. auto: Direction is set automatically. Selection of dosing unit. Measuring input for pH and U. Temperature.

abs., rel., OFF

0...999.99 mL

0...±999 999

0.01...150 mL/min, max.

0...999 999 s

pH: 0.00...±20.00, OFF

(0...±2000 mV, 0.0...±200.0 µA)

0.01...150 mL/min, OFF

1...2...999 999 s

+, -, auto

internal D0, external D1/D2

1, 2, diff.

-170.0...25.0...500.0 °C

>stop conditions stop time: stop time factor t(delta) t(delay) stop V: stop V factor stop rate filling rate

Type of stop time: absolute or relative. Time for absolute stop time. Factor for calculation of relative stop time. Time after EP is once reached. Time after last dosing step. Type of stop volume: absolute or relative. Volume for absolute stop volume. Factor of relative stop volume. Stop when the dosing rate is smaller than.. Filling rate.

abs., rel., delta, delay, OFF

0...999 999 s

0...±999 999

0...999 999 s

abs., rel., OFF

0...99.99...9999.99 mL

0...±999 999

0.01...150 mL/min, OFF

0.01...150 mL/min, max.

>statistics Statistics calculation see at DET, page 14.

>evaluation low lim. up lim.

fix V1

fix time 1

Evaluation of dosing rates within programmed time windows (→ C8X). Max. 9 windows. Interpolation of volumes at fixed times (→ C5X). Up to 9 fix V's. Interpolation of times at fixed volume rations of the end volume (→ C6X). Up to 9 fix times.

0...999 999 s, OFF

0.01...1, OFF

Page 20

2.5 Mode STAT, parameters

799 GPT Titrino: Titration, dosing and measuring modes

Display Meaning Input range

>monitoring meas.val: low lim.pH up lim.pH action:

rate:

temperature:

assign output L10:

violated limit: output L10: assign output L1X:

Monitoring of measured values. Limits for measured values.

Action, if a limit is exceeded. End: Abort. Wait: Dosing interrupted, until measured value is within limits again, then continue. Monitoring of rate (same actions as above). Monitoring of temperature (same actions as above). Assignment of output L10 to monitored quantity. Assignment of output to violated limit. Set a signal when limits are violated. For lines L11, L12, and L13 as for L10.

ON, OFF

pH: 0.00...±20.00

(0...±2000 mV, 0.0...±200.0 µA)

end, hold, wait, none

ON, OFF

meas, temp, rate, all, none

any, upper, lower

active, pulse

>preselections

req.ident: req.smpl size: limit smpl size: display rate:

activate pulse:

Request of identifications after start. Request of sample size after start. Limit control of sample size. Display of rate.

Pulse output on I/O line L6.

id1, id1 & 2, all, OFF

Value, unit, all, OFF

ON, OFF

Page 21

2.6 Mode DOS, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.6 Mode DOS, parameters

Display Meaning Input range

>dosing parameters dispensing type:

volume disp.crit: rate disp.time pause time interval dos.element temperature

Volume, time or rate. Inquiry of 2 values. 3rd value is calculated . 1st criterion i.e. volume. Selection of 2nd criterion. 2nd value, i.e. rate or dispensing time. Waiting time before start. Time interval for data acquisition. Selection of the dosing unit Temperature.

volume, time, rate

0...10...99 999.99 mL

time, rate

0.001...150 mL/min, max.

1...100...999 999 s

0...999 999 s

1...10...999 999 s

internal D0, external D1/D2

-170.0...25.0...500.0 °C

>stop conditions stop V: stop V factor filling rate

Type of stop volume: absolute or relative. Volume for absolute stop volume. Factor of relative stop volume: Filling rate.

abs., rel., OFF

0...99.99..99 999.99 mL

0...±999 999

0.01...150 mL/min, max.

>statistics Statistics calculation see at DET, page 14.

>monitoring meas.mode: meas.input: low lim.pH up lim.pH action:

temperature: low lim. up lim. action: assign output L10:

violated limit: output L10: assign output L1X:

Measured quantity for monitoring. Meas. input for pH and U. Limits for measured values.

Action, if a limit is exceeded. End: Abort. Wait: Dosing interrupted, until measured value is within limits again, then continue. Monitoring of temperature. Limits for temperature.

Action, if a limit is exceeded . Assignment of output L10 to monitored quantity. Assignment of output to violated limit. Set a signal when limits are violated. For lines L11, L12, and L13 as for L10.

pH, U, I(pol), U(pol), OFF

1, 2, diff

pH: 0.00...±20.00

(0...±2000 mV, 0.0...±200.0 µA)

end, hold, wait, none

ON, OFF

-170.0...500.0 °C

end, hold, wait, none

meas, temp, all, none

any, upper, lower

active, pulse

>preselections req.ident: req.smpl size: limit smpl size: activate pulse:

Request of identifications after start. Request of sample size after start. Limit control of sample size. Pulse output on I/O line L6.

id1, id1 & 2, all, OFF

value, unit, all, OFF

ON, OFF

Page 22

2.7 Mode DOC, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.7 Mode DOC, parameters

Display Meaning Input range

>dosing parameters begin at

end at

sweep time dynamics

max.rate min.rate direction:

start V: start V factor dos.rate pause time interval dos.element meas.input: temperature

Begin of measured value sweep.

End of measured value sweep.

Time required for sweep. Distance from EP where constant dosing starts. OFF means no constant dosing. Maximum dosing rate. Minimum dosing rate. Direction of sweep. +: Titration to higher pH, voltage, or current. Auto: Direction is set automatically. Type of start volume: absolute or relative. Volume for absolute start volume. Factor for of relative start volume: Dosing rate for start volume. Waiting time, after start volume. Time interval for data acquisition Selection of dosing unit. Meas. input for pH and U. Temperature.

pH: 0.00...±20.00, init

(0...±2000 mV, 0.0...±200.0 µA)

pH: 0.00...±20.00, OFF

(0...±2000 mV, 0.0...±200.0 µA)

0...300...999 999 s

pH: 0.01...0.25...20.00, OFF

(1...15...2000 mV, 0.1...6...200

µA)

0.01...150 mL/min, max.

0.01...5...9999 µL/min

+, -, auto

abs., rel., OFF

0...999.99 mL

0...±999 999

0.01...150 mL/min, max.

0...999 999 s

1...10...999 999 s

internal D0, external D1/D2

1, 2, diff.

-170.0...25.0...500.0 °C

>stop conditions stop V: stop V factor filling rate

Type of stop volume: absolute or relative. Volume for absolute stop volume. Factor of relative stop volume. Filling rate.

abs., rel., OFF

0...99.99...9999.99 mL

0...±999 999

0.01...150 mL/min, max.

>statistics Statistics calculation see at DET, page 14.

>monitoring meas.val: temperature:

Monitoring see at STAT, page 18. Monitoring of measured value. Monitoring of temperature.

>preselections req.ident: req.smpl size: Limit smpl size: display rate: activate pulse:

Request of identifications after start. Request of sample size after start. Display of rate. Limit control of sample size. Pulse output on I/O line L6.

id1, id1 & 2, all, OFF

value, unit, all, OFF

ON, OFF

Page 23

2.8 Mode MEAS and CAL, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.8 Mode MEAS and CAL, parameters

MEAS

Display Meaning Input range

>measuring parameters signal drift

equilibr.time meas.input: temperature time interval

Drift for measured value acquisition.

Waiting time for meas. value acquisition. Measuring input for pH and U. Measuring temperature. Time interval for measured value acquisition.

pH, U: 0.5..999 mV/min, OFF

T: 0.5...999 °C/min, OFF

0...9999 s, OFF

1, 2, diff.

-170.0...25.0...500.0 °C

1...2...999 999s

>statistics Statistics calculation see at DET, page 14.

>preselections req.ident: req.smpl size: Limit smpl size: activate pulse:

Request of identifications after start. Request of sample size after start. Limit control of sample size. Pulse output on I/O line L6.

id1, id1 & 2, all, OFF

value, unit, all, OFF

ON, OFF

CAL

Display Meaning Input range

>cal. parameters meas.input: cal.temp. buffer 1 pH signal drift equilibr.time electr.id sample changer cal: activate pulse:

Measuring input. Calibration temperature. pH-value for buffer 1. up to 9 buffer.

Drift for measured value acquisition. Waiting time for meas. value acquisition. Electrode identification. Calibration with Sample Changer. Pulse output on I/O line L6.

1, 2, diff.

-20.0...25.0...120.0 °C

0...±20.00

0.5..2...999 mV/min, OFF

0...110...999 s, OFF

up to 8 ASCII characters

ON, OFF

all, first, OFF

>statistics Statistics calculation see at DET, page 14.

Page 24

2.9 Mode TIP, parameters

799 GPT Titrino: Titration, dosing and measuring modes

2.9 Mode TIP, parameters

With TIP, methods and other functions can be linked to a titration sequence. Press the key <DEF> to define the titration sequence.

Display Meaning Input range

>sequence method:

pause L4 output: L6 output: info

prep stirrer:

Method from the internal method memory or from the card. Waiting time. Can be aborted with <QUIT>. Set a signal when on I/O line L4. Set a signal when on I/O line L6. The sequence will be held and an info appears in the display. Preparation of the dosing unit. Switching the stirrer ON/OFF.

method name

0...999 999 s, inf.

active, inactive, pulse, OFF

up to 16 characters

internal D0, external D1/D2

ON, OFF

>statistics Statistics calculation see at DET, page 14.

>preselections req.ident: req.smpl size: limit smpl size: meas.mode:

meas.input: temperature

Request of identifications after start. Request of sample size after start. Limit control of sample size. Selection of the measured quantity for <MEAS/HOLD>. Measuring input for pH and U. Temperature for the compensation of the pH values.

id1, id1 & 2, all, OFF

value, unit, all, OFF

ON, OFF

pH, U, I(pol), U(pol), T, OFF

1, 2, diff.

-170.0...500.0 °C

Page 25

2.10 Calculations

799 GPT Titrino: Titration, dosing and measuring modes

2.10 Calculations

The results are calculated with the formulas given in the method. For the calculation, the raw values, determined in the method (EP's and C variables), are available. The results and the raw values can be assigned for further calculations, e.g. for statistics or as common variables.

Formula input and assignments, key <DEF>

Display Meaning Input range

>formula RS? RS1=EP1*C01/C00

RS1 text RS1 decimal places RS1 unit:

RS1 limit control: RS1 low lim. RS1 up.lim. RS1 L13 output:

Input of formula. Enter result number. Enter formula by means of 3

functions of keyboard. Text for result output. Number of decimal places for result output. Select result unit.

Limit control of the result. Lower limit for RS1. Upper limit for RS1 Output on line L13 if the result is out of limits.

Enter values of calculation variables with <C-FMLA>.

1...9

RS1 or up to 8 ASCII characters

0...2...5

%, ppm, g/L, mg/mL, mg/pc,

mol/L, mmol/L, g, mg, mL, s,

mL/min, no unit or up to 6 ASCII

characters

ON, OFF

0.0...999 999

OFF, active, pulse

>silo calculations

C24= C25= match id:

Allocations for silo calculation, see page 96 of the Instructions for Use. Enter values to be stored in the silo memory. Indication which id's must coincide for the statistical evaluation in the silo memory.

RSX, EPX, CXX

id1, id1 & 2, all, OFF

>common variables C30=

Allocations of common variables C30...C39. Assign RSX, EPX, CXX, or MNX.

RSX, MNX, EPX, CXX

>report

report COM1:

report COM2:

Selection of report blocks for data output at COM1.

Depends on the selected mode. If you wish several reports, use ”;” as separator. As for COM1.

full, short, mplist, curve, derive,

comb, meas crv, temp crv, scalc

full, scalc srt, calc, param, calib,

>mean MN1=

Allocations for statistics. Assign RSX, EPX, or CXX.

RSX, EPX, CXX

>temporary variables C70=

Allocations of temporary variables for calculations under TIP.

RSX, EPX, CXX

Page 26

2.10 Calculations

799 GPT Titrino: Titration, dosing and measuring modes

Meaning of the calculation variables

C variables are

• determined by the method (C24...C27, C4X, C5X, C6X, C7X, C8X)

• entered as sample specific data (C00, C21...C23)

• given as fixed constants in the methods (C01...C19)

Variable Meaning

C00 C01...C19

C21...C23 C24, C25 C26, C27 C30...C39 C40 C41 C42 C43 C44 C45 C46 C47 C48 C49 C51...C59 C61...C69 C70...C79 C80 C81...C89

Sample size, key <SMPL DATA>. Method specific calculation values, such as molecular mass, factors, key <CFMLA>. Sample specific calculation values, such as dilution factors, key <SMPL DATA>. Variables for storing determination results in the silo memory. Means from silo calculations. Common variables, e.g. for titer. Initial measured value of the sample, last measured value for MEAS. End volume. Determination time. Volume drift for KFT and SET with conditioning. Temperature. Dispensed start volume. Asymmetry pH (pH calibration). Electrode slope (pH calibration). Volume at the point of the curve with maximum voltage. Volume at the point of the curve with minimum voltage. Fix EP for DET and MET or fix V for STAT. pK/HNP values for DET and MET or fix times for STAT. Temporary variables for calculations in TIP. Mean rate for STAT: Overall rate, evaluated over all points of the measuring list. Rates, evaluated in preset time windows for STAT.

Sample data, key <SMPL DATA>

• Sample identifications or sample specific calculation values C21...C23

• Sample size C00

For working with the silo memory, see page 27.

Display Meaning Input range

id#1 or C21 id#2 or C22 id#3 or C23 smpl size smpl unit:

Inquiries with silo = OFF (LED ”silo” is OFF):

Sample identification. Can be used as

sample specific calculation values.

Sample size Unit of sample size

up to 8 ASCII characters

or 0...±999 999

-999 999...1...999 999

g, mg, mL, µL, pc, no unit or up

to 5 ASCII characters

}

Page 27

3.1 Method memory

799 GPT Titrino: Other functions

3 Other functions

This chapter gives you a survey over other functions of the Titrino. If you are looking for more information to the different quantities, you will find the display text as a keyword in the index of the Instructions for Use.

3.1 Method memory

Methods can be stored in the internal method memory or on the memory card. These method memories are organized as follows:

Memory Card

Directory 7

Directory 6

Directory 5

Directory 4

Directory 3

Directory 2

Directory 1

current directory of the

Memory Card

Reload

internal method mem-

ory

Metrohm 799 GPT Titrino User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual