Metrohm TitrIC pro III User Manual

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Delivery

1.

- deliver

-Optional

Installati

2.

. 815 Rob

. Titrando

. Conduct

. 850 Prof

. Dosino h

3.

Cable co

Tubing c

4.

. External

. Installati

. Overvie

5.

Miscella

5.

. Membra

. Stirrer ....

. Length o

. Electrod

6.

Software

ts:

ackage ........

d with TitrIC

accessories:

n ..................

tic USB Sam

2.905.0010) .

meter (2.856

ssional IC A

lder (6.2057.

nections ......

nnections .....

ell$ ..............

n of the 50 m

of all the tub

eous .............

e Pumps of t

.....................

the aspiratio

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.....................

ro III packag

.....................

ple Processo

.....................

.0010) ...........

Cat – MCS (

210) .............

.....................

L Dosing Uni

ing connectio

.....................

e 815 ..........

.....................

n tips in the e

.....................

: ..................

.....................

XL (2T/2P) ..

.....................

.850.3030) ..

.....................

....................

s .................

.....................

ternal cell ....

.....................

.... 3

.... 4

.... 5

.... 6

.... 7

6.

. Installati

. Configur

.1. Devices .

.2. Solution .

.3. Swing H

.4. Lift positi

.5. Needle ri

Fig

.: TitrIC pro III

ystem setup

.6. Methods

. Configur

.1. Devices .

.2. Solution .

.3. Electrod

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tion of MagI

.....................

ad configura

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nse position ..

.....................

tion of tiamo

.....................

s ...................

are ...............

Net .............

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..................

.....................

Page 1

.... 7

.... 8

.... 9

f 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

6.3.4. Methods .................................................................... 9

6.4. Setup of RS232 communication between MagIC Net

and tiamo

TM

.............................................................. 9

7. Complete Analysis with TitrIC ................................. 10

9. TitrIC pro – Combo Kit Dilution ............................... 11

9.1 Delivery package .................................................... 11

9.2 Installation .............................................................. 11

9.3 Dosino .................................................................... 11

9.4 Transfer Tubing ...................................................... 11

9.5 External Dilution Vessel .......................................... 11

9.6 Analysis .................................................................. 11

9. TitrIC pro – Combo Kit Partial Loop ........................ 13

9.1 Delivery package .................................................... 13

9.2 Installation .............................................................. 13

9.3 Rinsing station ........................................................ 13

9.4 MiPT Dosino ........................................................... 13

9.5 Analysis .................................................................. 13

Page 2 of 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

1. Delivery package

- delivered with TitrIC pro III package:

No. Article no. Article designation

IC

1 2.850.3030 850 Professional IC AnCat – MCS

2 2.850.9010 IC Conductivity Detector

Sample processor

1 2.815.0110 815 Robotic USB Sample Processor

XL (2T/2P)

2 2.786.0040 Swing Head

1 6.1462.040 Robotic Arm with transfer head for

786 Swing Head, right swinging

1 6.1462.080 Robotic Arm DIS-COVER

1 6.2833.020 Needle holder 1/8 in. With tubing

connection M6

1 6.1835.050 PEEK sample aspiration tube (1.58

mm ID)

1 6.2629.000 Screw nut to needle holder IC

Conductometry

1 2.856.0010 856 Conductivity Module

1 6.0915.100 Five-ring conductivity measuring

cell, c = 0.7 cm-1, with Pt 1000

1 6.2151.000 Cable USB A - mini-DIN 8P (R)

1 6.2763.000 Flow through cell for 60915100

p and m value titration (pH measurement)

1 2.905.0010 905 Titrando

1 6.0277.300 iAquatrode plus with Pt 1000

1 6.2151.000 Cable USB A – mini-DIN 8P

1 6.2307.230 Buffer solutions pH 4, 7 and 9

1 6.2325.000 Phit kit

Liquid Handling

2 2.800.0010 800 Dosino

1 6.3032.220 807 Dosing Unit, glass, 20 mL

1 6.3032.250 807 Dosing Unit, glass, 50 mL

1 6.2057.210 Holder Dosino for IC Instruments

1 6.1608.030 Glass bottle GL45 1L (round)

1 6.1808.280 Adapter Dosino Port 4 / M6

1 6.1618.020 Thread adapter S 40 to GL45

2 6.2744.080 Coupling M6-UNF 10/32 (Dosing

Unit – IC screw)

1 6.2744.070 Pressure screw made of PEEK,

short, 5x

1 6.1808.010 Coupling piece 2 x M6 outer threads

1 6.1808.060 T Connector M6

Connection tubings

1 6.1805.510 Connection tubing FEP, L = 60 cm,

2 x M8 thread

1 6.1805.110 Connection tubing FEP, L = 80 cm,

2 x M6 thread

1 6.1805.030 Connection tubing FEP, L = 150 cm,

2 x M6 thread

External cell

1 2.802.0020 802 Rod Stirrer

1 6.2001.070 Stand support for 804

1 6.1414.060 Titration vessel lid micro ECO

1 6.1415.250 Titration vessel / 50-150 mL

5 6.2730.030 Stopper with nipple and O-ring

1 6.2730.080 Screw nipple M16/NS14

1 6.2730.020 Septum stopper

3 6.2730.060 Screw nipple for electrodes

1 6.1543.170 Aspiration tip M8

1 6.2709.090 Stopper (12 mm)

1 6.1543.210 3-way stopper with antidiffusion

valve

Software

1 6.6056.231 Tiamo 2.3 light CD: 1 Licence

1 6.6059.232 MagIC Net 2.3 Professional CD: 1

Licence

RS232 Communcation MagIC - Tiamo

1 6.2134.040 Connecting cable RS-232 to IMP-PC

(DBp)

2 6.2148.050 USB/RS-232 Converter for 900

Touch Control / Ti-Touch

-Optional accessories:

1 6.2041.xxx Sample rack made of PVC

1 6.1432.xxx Sample beaker

1 6.2324.000 Conductivity standard (100 µS/cm)

1 6.2301.060 Conductivity standard (12.88 mS)

1 6.2307.230 Buffer solutions 3 x 10 x 30mL of pH

4 / 7 / 9

1 6.2065.000 Stacking frame for 846 Dosing

Interface, 856 Conductivity Module,867 pH Module

1 6.2041.800 Sample rack 100* 75 ml

1 6.2041.810 Sample rack 34* 150 ml

1 6.2041.820 Sample rack 28* 250 ml

1 6.2041.840 Sample rack 59* 120 ml

Page 3 of 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

1 6.1432.210 Sample beaker 75 mL made of glass

(for 6.2041.800)

1 6.1432.320 Sample beaker 250 mL made of

glass (for 6.2041.820)

1 6.1453.250 Sample beaker 250 mL made of

polypropylene (for 6.2041.820)

1 6.1459.300 Sample beaker 120 mL made of

polypropylene (250 pieces) (for

6.2041.840)

1 6.1006.510

Metrosep A Supp 5 - 100/4.0

1 6.1006.520 Metrosep A Supp 5 - 150/4.0

1 6.1006.500 Metrosep A Supp 4/5 Guard/4.0

1

6.1030.410 Metrosep A Supp 15 – 100/4.0

6.1030.420 Metrosep A Supp 15 – 150/4.0

1 6.1030.500 Metrosep A Supp 15 Guard/4.0

1 6.1050.410 Metrosep C 4 – 100/4.0

1 6.1050.420 Metrosep C 4 – 150/4.0

1 6.1050.500 Metrosep C 4 Guard/4.0

1 2.849.1030 849 Level Control for Inline Eluent

Preparation

2. Installation

The following is a detailed description of the TitrIC pro III installation.

We strongly recommend that the individual steps are carried out in the order given below!

2.1. 815 Robotic USB Sample Processor XL (2T/2P)

The sample processor is placed at the side at which it is most easily accessible. Please note that the following procedure refers exclusively to the version in which the sample processor is located at the left-hand side of the IC system.

 On the left-hand side of the 815 Robotic USB Sample

Processor XL, attach the stand support (6.2001.070) for the external titration vessel.

 Mount both Swing Heads (2.786.0040) onto the 815

(see installation instructions).

 Do not screw the robotic arm (6.1462.040) nor the

robotic arm DIS-COVER (6.1462.080) onto the Swing Head!

 The Sample Rack supplied is screwed onto the 815.

 In the vicinity of the 815 the two canisters (standard

equipment of 815) are placed on the floor: One 10 L canister is used as a waste container, the second one as a reservoir for deionized (DI) water used for rinsing the external cell.

 From the smaller opening of the canisters containing DI

water, an M8 PTFE tubing connection of suitable length is led to the connection box made of white plastic of membrane pump 1 / tower 1 and connected.

 From the front opening of the waste canister an M8

PTFE tubing connection of suitable length is led directly to membrane pump 1 / tower 2 (black plastic) and connected.

A more detailed description is given in the instructions for use of the 815 Robotic USB Sample Processor XL.

2.2. Titrando (2.905.0010)

Directly to the right of the 815 Robotic USB Sample Processor, place the Titrando with a bottle of titration solution (0.1 mol/L HCl will be connected to the 20 mL Dosing Unit and 800 Dosino).

2.3. Conductometer (2.856.0010)

The 856 Conductometer is placed directly at the left of the Titrando. For detailed information about the usage check the Instructions of Use of the 856.

Before measurement it is recommended to carry out the calibration of the cell constant in the flow-through cell of this

Page 4 of 14

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Page 5

f 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

tower 1 of the 815 with the M8-PTFE-tubing connection (6.1805.510, 60 cm).

This opening is not used. It can be closed with a stopper (6.2709.090)

After the screw nipple (6.2730.080) has been screwed into opening 9, the 802 Rod Stirrer (2.802.0020) is pushed through it and connected to the tower 1 stirrer connection of the 815 Robotic USB Sample Processor.

4.2. Installation of the 50 mL Dosing Unit

6.5620.000

Luer: Port 4

Port 3

6.1805.030

Port 1

M6: Port 2

6.2744.080

6.2744.070

6.1803.020

6.1805.110

Fig.: Connections on the bottom of the 50 mL Dosing Unit

 Port 1 is used for transferring the sample to the

external titration vessel using FEP-tubing 6.1805.110 (80 cm, supplied by the 815 Sample Processor)

 Port 2 is used for aspirating the sample via conductivity

flow through cell which is connected to the titration arm. The FEP-tubing 6.1805.110 is used here (80 cm, again supplied by the 815 Sample Processor).

 Port 3 is used by for sample transfer to the IC system.

The transition from M6 to the IC screw size (1/16 in.) is achieved with the 6.2744.080 adapter. A PTFE-capillary (0.75 mm ID) is used to aspirate the sample from the T piece at the swing arm through the anion injection valve into the 50 mL Dosino. At the T piece the adapter M6 thread to UNF 10/32 (6.2744.080) is used.

 Port 4 requires a coupling between Luer and M6

(6.1808.280): This port is used for emptying the Dosing Unit into the waste canister. Herefore the FEP-tubing (6.1805.030) with 150 cm length is used.

 Once the tubing connections have been made, the

Dosing Unit is attached to the Dosino holder (6.2057.210) with the thread adapter 6.1618.020.

4.3. Overview of all the tubing connections

The three 60 cm FEP-tubing connections

(6.1850.060, supplied with the 815) are used to connect the membrane pump 1 / tower 1 of the 815 and the three rinsing nozzles (6.2740.020, supplied with 815) to the openings 1,3, and 5 of the external cell (see chapter 4.1).

The 60 cm M8-PTFE-tubing connection

(6.1805.510) is used to connect the membrane pump 1 / tower 2 of the 815 and the M8-PTFEaspiration tip (6.1543.170) to the opening 7 of the external cell (see chapter 4.1).

The Robotic Arm (6.1462.040) is equipped with a

PEEK aspiration tube (6.1835.050). The aspiration tube can be mounted using the screw nut (6.2629.000) and the needle holder (1/8 in with tubing connection M6, 6.2833.020). The coupling piece with two outer M6 connections (6.1808.010) is used to connect the needle to the T Connector M6 (6.1808.060).

The two 80-cm-FEP-tubing connections

(6.1850.110) supplied with the 815 are used to connect the T piece (6.1808.060) at the robotic arm with the flow-through cell (6.2763.000) for the conductivity measurement and the flow-through cell with the 50 mL Dosino at Port 2. The third 80cm-FEP-tubing (6.1850.110) supplied separately is used to connect the 50 mL Dosino Port 1 to the external titration vessel at the left of the 815.

The 40-cm-FEP-tubing connection (6.1805.100,

supplied with the Dosing Unit) is used to connect port 1 of the 20 mL Dosing Unit (0.1 mol/L HCl) with the 3-way stopper in the external cell (opening 6 in chapter 4.1)

The 150-cm-FEP-tubing connection (6.1805.030)

is used to connect port 4 of the 50 mL Dosing Unit to the 10 L PE waste canister (6.1621.000, supplied with the 815).

Suitable lengths of the 0.97 mm PTFE capillary

(6.1803.020, supplied with the 850) are used to connect port 3 of the 50 mL Dosing Unit (using the screws 6.2744.080 and 6.2744.070) and the injection valves of the 850 Professional IC instrument. The injection valves are connected in series and finally connected to the T-piece (6.1808.060) at the robotic arm (using the screws

6.2744.080 and 6.2744.070). In this setup and

Page 6 of 14

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The M8 as the base of ensure that

The 3-way



should reac

5.4. Electr



The pH ele

6.0277.300 connected

905) to the

1.

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If the electr be returned (6.2323.00



The electro electrolyte

Conductivit



cable is con the 856 Co into the flo through cell support (6.

cell

the following

nted: T-piece

ection valve

us

rane Pumps

pump at tow

of the extern

d to empty th

brane pum

or leading

xternal ves

2 is connect

f membrane

ector of the

les to rinse t

brane pump

tirrer is inse

d connected

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of the aspi

tration vessel

iration tip in o the titration v the external

topper with a

h the middle

odes

trode (iAquat is inserted in

ith the 854 i 05 Titrando

de is not use to its holder ).

e has to be f

olution (6.23

cell (6.0915.

nected to the

ductometer.

-through cell

itself is mou

001.070).

sequential ar

– anion injec

50 mL Dosi

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d for some ti

nd kept in th

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8.020).

100): The me opening mar

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6.2763.000).

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properly.

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Pt 1000; The cable is ded with the

measuring in

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MagIC Net

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Fi

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ation of the

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Depending carried out:

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6.3. Confi

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Fig

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F

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Fig

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Edit/Ne

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information

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Port 1

Port 3

Port 2

Port 4

table of the 20

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25 cm

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Page 9

f 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

RS232 cable (6.2134.040) directly between the two ports. If the PC does not have the built-in RS232 ports please connect two USB/RS232 Converters (6.2148.050) to two USB ports. You can e.g. use the USB hubs of the IC instrument, but it is recommendable to use the USB hubs of your computer, as they are more powerful. Then connect the two converters using the RS232 cable (6.2134.040). In the Device Manager of your Windows operating system check which two RS232 ports you are using.

Open the MagIC Net software. On the left click on

Configuration’, then in the devices window select

‘ ‘Edit/New/Miscellaneous’ and choose the RS 232 device. Keep the proposed Device name and enter a random serial number. Go to the RS232 subsection and choose one of the used RS232 ports. Click on ‘ Close the window with

Connect’ and confirm with <Ok>.

<Ok>

Repeat the same steps in the tiamo

TM

software and choose

the second RS232 port.

7. Complete Analysis with TitrIC

As an example a short description of a complete analysis with TitrIC pro III is described here.

The whole procedure is controlled by the MagIC Net

TM

software which is the master software. In tiamo method

TitrIC pro III is selected as a single determination.

, the

Start the determination in an autorepeat mode. To set it into autorepeat go to the Run window, right-mouse-click and select ‘

Properties Run window’. Under Process select

‘Autorepeat determination’. Close the window with <Ok>.

TM

Start the determination. Now tiamo

is waiting for the start

signal from MagIC Net via RS232.

In the MagIC Net software select the method

TitrIC pro III.

Enter the required sample position, sample identification etc. into MagIC Net. For value 1 choose according to the list below:

 Value 1 = 1 a complete analysis including titration and

ion chromatography

 Value 1 = 2 only an ion chromatography analysis (e.g.

a calibration)

 Value 1 = 3 only a titration analysis

Start the determination in MagIC Net. All sample liquid handling is done by MagIC Net. At the right moment MagIC

TM

Net communicates to tiamo

via RS232 to do the titration analysis. Results are transferred back to MagIC Net and the rinsing steps of the titration equipment by MagIC Net initialized.

All data goes into the MagIC Net database and therefore one report can be generated.

Page 10 of 14

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9.

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N

t:



TitrIC pro III

method. De following wi

Value 1 = 1 ion chroma Value 1 = 2 a calibratio Value 1 = 3



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

TitrIC pro III

method is u sensor. It h

tiamoTM m



TitrIC pro III

method is u HCl solutio combinatio

determinati

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e following

tia

moTM:



TitrIC pro II It does the results to M TitrIC pro II

he external indow manu

ngle is ~117

e 815 Robotic

naly

is

et files) met

dilution:

pending on th

l be carried o

complete a

ography.

only an ion

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only a titrati

is used in c

amoTM.

dilution cond

ed for calibr

s to be used

thod

diution titer d

ed to deter used in tiam with the tia

n of HCl

methods (.

: This metho

omplete titra

gIC Net. It i

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ilution vesse

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tion:

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Page 11

f 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

In tiamoTM it is typically used as a single determination in autorepeat mode. In other words, it is always ready to do a titration as soon MagIC requires it. To set it into autorepeat go to the Run window, right-mouse-click and

Properties Run window. Under Process select

select

Autorepeat determination. Close the window with <ok>.



TitrIC pro III_pH calibration manual: Here the iAquatrode

is taken out of the titration vessel and placed into the

TM

buffer solutions. Start this method only from tiamo



TitrIC pro III_titer determination of HCl: This method is

!

used for the titer determination. It has to be used in combination with the MagIC Net method

III_titer determination of HCl

TitrIC pro III_conductivity calibration: This method is



.

TitrIC pro

used for calibration of the conductivity sensor. It has to be used in combination with the MagIC Net method

TitrIC pro III_calibration conductivity.

Import: Click on

TM

tiamo

Import…

), then select under File / Method manager… / Edit /

Import the methods related to TitrIC pro III with the

Method at the left (in MagIC Net and

Dilution kit from the MagIC Net CD. You will find the methods in the folder example/TitrIC of the CD

.

Note!

Alterations of these methods should only be carried out by a person at the administrator level and who is thoroughly familiar with tiamoTM and MagIC Net

With the TitrIC pro – Combo Kit Dilution following analysis can be carried out using the TitrIC pro III_dilution methods

TM

in MagIC respectively tiamo

:

The whole procedure is controlled by the MagIC Net software which is the master software. In tiamoTM the method TitrIC pro III is selected as a single determination. Start the determination in autorepeat mode. To set it into autorepeat go to the Run window, right-mouse-click and select

Autorepeat determination. Close the window with <ok>. Start

the determination. Now tiamo

Properties Run window. Under Process select

TM

is waiting for the start

signal from MagIC Net via RS232.

In the MagIC Net software select the method

III_dilution

. Enter the required sample position, sample

TitrIC pro

identification etc. into MagIC Net. For value 1 choose according to the list below:

 Value 1 = 1 complete analysis including titration and

ion chromatography.

 Value 1 = 2 only an ion chromatography analysis (e.g.

a calibration)

 Value 1 = 3 only a titration analysis

With Value 1 = 1 a complete analysis is carried out. Depending on the entered dilution factor the following will be done:

Dilution Factor = 1:

Depending on the measured conductivity an appropriate dilution factor is automatically applied by MagIC Net. The calculation factor is calculated according to Time Program No. 2. The finally used dilution factor is the integer of the conductivity divided by 250.

Dilution Factor >1:

If a dilution factor is known it can be directly entered into the sample table. It will be diluted accordingly. The conductivity measurement has no influence on the dilution in this case.

E.g. With Value 1 = 2 an ion chromatographic analysis will be carried out with the entered dilution factor. No dilution factor will be calculated as no conductivity measurement will take place.

Page 12 of 14

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pillary of 2

as well as ection valve

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ith TitrIC p

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for the angl

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USB Sample P

L is conne n the anion i is further co

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2 mL Dosing (6.1829.010

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ment for MiP

partial loop k

lose the outl

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hen the rac

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with the ma

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e of ~116.5°,

°. Define th e positions 1 he angle 11 e 111° (exte

of the rin

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ted both to

jection valv nected to th .5 mm i.d.

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e following (.

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

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Depending

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(6.1608.070

onnected to

ent.

naly

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met files) m

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n the value

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nted directly

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ethod is the s

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on the 2 L

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vided for M

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ollowing will

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t IC

gIC

d.

e

carried out:

Value 1 = 1 ion chroma Value 1 = 2 a calibratio Value 1 = 3



This metho method in t has to be p standard +1 into the sa



TitrIC pro III

is used for to be used i

TitrIC pro III



TitrIC pro III

is used to d solution us with the tia

of HCl

complete a

ography.

only an ion

)

only a titrati

is used in c

amoTM. For c

sitioned at th

. The calibrat

ple table is a

MiPT conduc

alibration of t

n combinatio

calibration c

MiPT titer det

termine the

d in tiamo. It

oTM method

.

alysis includi

hromatogra

n analysis

mbination wi alibration the e rack positio ion injection

lways 4 µL.

ivity calibrati

he conductivi

with the tia

nductivity

ermination of

.

iter of the 0.1

has to be use

TitrIC pro III_t

g titration an

hy analysis (

h

TitrIC pro III

cation standa n for the anio olume entere

n:

This meth

y sensor. It h

oTM method

Cl:

This met

mol/L HCl

d in combinat

ter determina

.g.

rd

d

s

od

ion

Th

e following

tia

moTM:



TitrIC pro III

It does the results to M

TitrIC pro III

methods (.

This method

omplete titra

gIC Net. It i

MiPT

method

met files)

is the standa ion analysis used in com in MagIC Ne

re provided

d method us nd sends the

ination with

.

for

d.

TM

t is typically u

In tiamo in autorepe to do a titra autorepeat select

utorepeat



TitrIC pro III

is taken out buffer soluti



TitrIC pro III

used for th

ion as soon

Prop

titer determi

t mode. In ot

o to the Run

rties Run win

etermination

pH calibratio

of the titratio

ns. Start thi

titer determin

sed as a sing

her words, it i

agIC require

window, righ

ow

. Under P

.

Close the wi

manual:

vessel and

method only

ation of HCl:

ation. It has

le determinati

always rea it. To set it i

-mouse-click ocess select

dow with

Her

the iAquatr laced into th from tiamo

his method i

o be used in

<o

T

on

y

to

and

>

.

de

!

Page 13

f 14

Application Bulletin 355

Installation Instructions for TitrIC pro III

combination with the MagIC Net method TitrIC pro

III_titer determination of HCl

.

 TitrIC pro III_conductivity calibration: This method is

used for calibration of the conductivity sensor. It has to be used in combination with the MagIC Net method

TitrIC pro III_calibration conductivity.

Import: Click on

TM

tiamo

Import

), then select under File / Method manager… / Edit /

… Import the methods related to TitrIC pro III with the

Method at the left (in MagIC Net and

MiPT kit from the MagIC Net CD. You will find the methods in the folder example/TitrIC of the CD.

Note!

Alterations of these methods should only be carried out by a person at the administrator level and who is thoroughly

TM

familiar with tiamo

and MagIC Net

With the TitrIC pro – Combo Kit Partial Loop setup the following analysis can be carried out using the TitrIC pro III_MiPT methods in MagIC respectively tiamoTM:

The whole procedure is controlled by the MagIC Net

TM

software which is the master software. In tiamo

the method TitrIC pro III is selected as a single determination. Start the determination in autorepeat mode. To set it into autorepeat go to the Run window, right-mouse-click and select

Autorepeat determination. Close the window with <ok>. Start

the determination. Now tiamo

Properties Run window. Under Process select

TM

is waiting for the start

signal from MagIC Net via RS232.

In the MagIC Net software select the method

. Enter the required sample position, sample

III_MiPT

TitrIC pro

identification etc. into MagIC Net. The Sample volume is used for the anions injection volume. The cation injection volume has to be entered into the value 2.

For value 1 choose according to the list below:

 Value 1 = 1 complete analysis including titration and

ion chromatography.

 Value 1 = 2 only an ion chromatography analysis (e.g.

a calibration)

 Value 1 = 3 only a titration analysis

Page 14 of 14

Metrohm TitrIC pro III User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual