Measure

what is measurable
and make measurable
that which is not.
Galileo Galilei (1564-1642)

Instructions and Safety Information

Dosing System

for Litesizer 500

(Original Instruction)
Disclaimer
This document may contain errors and omissions. If you discover any such errors or if you would like to see
more information in this document, please contact us at our address below. Anton Paar assumes no liability
for any errors or omissions in this document.

Changes, copyright, trademarks etc.

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as such. They are the property of their respective owner.

Further information
Published and printed by Anton Paar GmbH, Austria
Copyright © 2020 Anton Paar GmbH, Graz, Austria
Address of the instrument producer: Anton Paar GmbH
Anton-Paar-Str. 20
A-8054 Graz / Austria – Europe
Tel: +43 (0) 316 257-0
Fax: +43 (0) 316 257-257
E-Mail: [email protected]
Web: www.anton-paar.com

Date: January 2020

Document number: D51IB009EN-F

Instructions and Safety Information

Dosing System

for Litesizer 500

(Original Instruction)
 D51IB009EN-FContents

D51IB009EN-FContents
1 About the Instruction Manual ................................................................................................................ 7
2 Safety Instructions for the Dosing System .......................................................................................... 8
2.1 General Safety Instructions............................................................................................................... 8
2.2 Special Safety Instructions................................................................................................................ 9
2.2.1 Electrical Safety Instructions..................................................................................................... 9
2.2.2 Working with Corrosive Liquids ................................................................................................ 9
2.2.3 Safety Symbols inside the FM 10 ........................................................................................... 10
2.2.4 Transport ................................................................................................................................ 10
3 Dosing System - An Overview ............................................................................................................. 11
3.1 Intended Use of the Instrument....................................................................................................... 11
3.2 Main Components........................................................................................................................... 11
3.3 Functional Principle......................................................................................................................... 12
4 Checking the Supplied Parts ............................................................................................................... 13
5 Installing the Dosing System............................................................................................................... 17
5.1 Installation Requirements ............................................................................................................... 17
5.1.1 Environmental Requirements ................................................................................................. 17
5.1.2 Computer Requirements......................................................................................................... 17
5.2 Assembling the Components .......................................................................................................... 17
5.2.1 Combining Dosinos and Dosing Units .................................................................................... 17
5.2.2 Installing the Magnetic Stirrer with Electrode Stand and pH Module...................................... 18
5.2.3 Installing Reagent Bottles and Titration Vessel ...................................................................... 19
5.2.4 Installing the pH Electrode...................................................................................................... 20
5.2.5 Installing the FM 10 Flow Module and Checking the Pinch Valve Function ........................... 20
5.3 Connecting the Dosing System....................................................................................................... 22
5.3.1 Fluid Connections ................................................................................................................... 22
5.3.2 Electrical Connections ............................................................................................................ 26
5.4 Installing the rod stirrer ................................................................................................................... 27
6 Operating the Dosing System.............................................................................................................. 29
6.1 Software Installation and Update .................................................................................................... 29
6.1.1 Kalliope ................................................................................................................................... 29
6.1.2 Metrohm Instrument Drivers ................................................................................................... 29
6.1.3 Installing the Dosing System in Kalliope................................................................................. 29
6.2 Dosing System Menu...................................................................................................................... 29
6.2.1 Dosing System Submenu ....................................................................................................... 30
6.2.2 Workflows Submenu............................................................................................................... 30
6.2.3 Actions Submenu.................................................................................................................... 31
6.2.4 pH Calibration Submenu......................................................................................................... 32
6.3 Setting Up a Measurement ............................................................................................................. 32
6.4 Performing the Measurement ......................................................................................................... 34
6.5 Cleaning the Dosing System........................................................................................................... 35
7 Upkeep and Cleaning ........................................................................................................................... 37
7.1 General Considerations .................................................................................................................. 37
7.2 Monthly Cleaning Procedure........................................................................................................... 37
7.3 Cleaning and Maintenance of the Individual Components.............................................................. 37
7.3.1 pH Electrode ........................................................................................................................... 37
7.3.2 pH Module and Stirrer............................................................................................................. 37
7.3.3 Dosinos................................................................................................................................... 38
7.3.4 Dosing Units ........................................................................................................................... 38
7.3.5 Cleaning the FM 10 Flow Module ........................................................................................... 38
7.3.6 Cleaning the Omega Cuvettes................................................................................................ 38
7.4 Software Administration .................................................................................................................. 39
7.5 Wetted Parts ................................................................................................................................... 39
7.6 Storing and Transporting the Instrument ........................................................................................ 40

4 D51IB009EN-F
 D51IB009EN-FContents

8 Maintenance and Repair....................................................................................................................... 41

8.1 Repair Performed by an Authorized Anton Paar Representative ................................................... 41
Appendix A: Technical Data ................................................................................................................... 42
Appendix B: Specification Sheet............................................................................................................ 43

D51IB009EN-F 5
D51IB009EN-FContents

6 D51IB009EN-F
 1 About the Instruction Manual

1 About the Instruction Manual

This instruction manual informs you about the instal-
lation and the safe handling and use of the product.
Pay special attention to the safety instructions and CAUTION
warnings in the manual and on the product.
Laser radiation
The instruction manual is a part of the product. Keep The Litesizer 500 is equipped with a laser of the
this instruction manual for the complete working life laser class 3B. The laser can only be operated in
of the product and make sure it is easily accessible the instrument’s protective casing and therefore
to all people involved with the product. If you receive conforms to the laser class 1. Follow your
any additions or revisions to this instruction manual national safety regulations.
from Anton Paar GmbH, these must be treated as
part of the instruction manual.
Wear protective gloves
Conventions for safety messages Wear protective gloves when handling
the Dosing System.
The following conventions for safety messages are
used in this instruction manual: Wear safety goggles
Wear safety goggles when handling
the Dosing System.
WARNING Use protective clothing
Description of risk. Use protective clothing when handling
Warning indicates a hazardous situation which, if the Dosing System.
not avoided, could result in death or serious
injury. TIP: Tip gives extra information about the situation
at hand.

CAUTION Typographical conventions

The following typographical conventions are used in
Description of risk.
this instruction manual:
Caution indicates a hazardous situation which, if
not avoided, could result in minor or moderate Table 1-1: Typographical Conventions
injury.
Convention Description

NOTICE <key> The names of keys and buttons

Description of risk. are written inside angle brackets.
Notice indicates a situation which, if not avoided,
"Menu Menu paths are written in bold,
could result in damage to property.
Level 1 > inside straight quotation marks.
Menu The menu levels are connected
Level 2" using a closing angle bracket.
CAUTION
Software screenshots
Hot surface
This symbol calls attention to the fact that the The screenshots depicted in this manual are repre-
respective surface can get very hot. Do not sentative only. They may not reflect the latest ver-
touch this surface without adequate protective sion of the Kalliope software.
measures.

D51IB009EN-F 7
2 Safety Instructions for the Dosing System

2 Safety Instructions for the Dosing System

• Read this instruction manual before using the Installation and use
Dosing System.
• The Dosing System is not an explosion-proof
• Follow all hints and instructions contained in this instrument and therefore must not be operated
instruction manual to ensure the correct use and in areas with risk of explosion.
safe functioning of the Dosing System.
• The installation procedure should only be car-
• The Dosing System is delivered with 4 addi- ried out by authorized personnel who are famil-
tional instruction manuals corresponding to 4 iar with the installation instructions.
sub-components manufactured by the company
• Do not use any accessories or spare parts other
Metrohm. Make sure to read these instruction
than those supplied or approved by Anton Paar
manuals before operating the system. These
GmbH.
parts are:
• Make sure that all operators have been trained
- Dosino (Metrohm Mat. No. 800)
to use the instrument safely and correctly before
- Stirrer (Metrohm Mat. No. 801)
starting to operate it.
- Dosing Unit (Metrohm Mat. No. 807)
- pH Module (Metrohm Mat. No. 867) • In case of damage or malfunction, do not con-
tinue operating the Dosing System.
• Some of the safety considerations relating to the
use of the Dosing System together with the Lite- • Do not operate the instrument under conditions
sizer, in particular those relating to the measure- which could result in damage to goods and/or
ment module FM 10, are detailed in the Litesizer injuries and loss of life.
Series Reference Guide (Doc. No. D51IB010).
• Ensure the sufficient supervision of the Dosing
Make sure to read this instruction manual before
System during operation.
operating the system.
• Make sure that the Dosing System instruction Maintenance and service
manual (present document), the Litesizer Refer-
• The results delivered by the Dosing System not
ence Guide (Doc. No. D51IB010) as well as the
only depend on the correct functioning of the
4 Metrohm instruction manuals listed above are
instrument, but also on various other factors.
easily accessible to all persons working with this
We therefore recommend you have the results
device.
checked (e.g. plausibility tested) by skilled per-
sonnel before consequential actions are taken
2.1 General Safety Instructions based on the results.
• Service and repair procedures may only be car-
Liability ried out by authorized personnel or by Anton
Paar GmbH.
• This instruction manual does not claim to
address all safety issues associated with the Disposal
use of the instrument and samples. It is your
responsibility to establish health and safety • Concerning the disposal of the Dosing System,
practices and determine the applicability of reg- observe the legal requirements in your country.
ulatory limitations.
Returns
• Anton Paar GmbH only warrants the proper
functioning of the Dosing System if no adjust- • Do not return instruments which are contami-
ments have been made to the mechanics, elec- nated by radioactive materials, infectious agents
tronics, and firmware. or other harmful substances that cause health
hazards.
• Only use the Dosing System for the purpose
described in this instruction manual. Anton Paar Precautions for highly inflammable samples
GmbH is not liable for damages caused by
incorrect use of the Dosing System.

8 D51IB009EN-F
 2 Safety Instructions for the Dosing System

and cleaning agents

• Observe and adhere to your national safety reg-
ulations for handling the measured samples WARNING
(e.g. use of safety goggles, gloves, respiratory Electrical risk
protection etc.). Never open the housing of the Dosing System’s
• Before a measurement, check the instrument’s sub-components. It could damage the system
wetted parts for chemical resistance to the sam- and poses a risk of serious injury by electrocu-
ples and cleaning agents used. tion.

• Keep potential sources of ignition, like sparks or

open flames, at a safe distance from the device. NOTICE
• Place the device and all samples in a fume cup- Electronic components are sensitive to electro-
board of adequate capacity. The fume cupboard static charges and can be damaged by dis-
must be approved for flammable vapors. charges. Always disconnect the mains cable
before connecting or disconnecting the different
• Ensure that the setup location is sufficiently ven- electrical sub-components of the system.
tilated. The environment of the device must be
kept free of flammable gases and vapors.
• Take care that the liquids (samples and cleaning 2.2.2 Working with Corrosive Liquids
agents) that you use are chemically compatible
when they come in contact with each other.
They must not react exothermically or produce
harmful substances. WARNING
• Only store the minimum required amount of Strong acids and bases
sample, cleaning agents and other inflammable Strong acids and bases are corrosive liquids that
materials near the Dosing System. can cause serious injury and material damage.
Check all fluid connections for leaks regularly.
• Do not spill sample/cleaning agents or leave
Observe your national safety regulations regard-
their containers uncovered. Immediately remove
ing the handling and disposal of acids and
spilled sample/cleaning agents.
bases.
• Connect the Dosing System to the mains via a
safety switch located at a safe distance from the
instrument. In an emergency, turn off the power Wear protective gloves
using this switch instead of the power switch on Wear protective gloves when handling
the Dosing System. the Dosing System.
• Supply a fire extinguisher. Wear safety goggles
Wear safety goggles when handling
the Dosing System.
2.2 Special Safety Instructions
Use protective clothing
Use protective clothing when handling
2.2.1 Electrical Safety Instructions the Dosing System.

The electrical safety when working with the Dosing • The device is intended to be operated with
System is ensured as part of the international stan- aqueous samples only.
dard IEC 61010.
• Take care that the hoses are properly connected
before you start a measurement or a cleaning
procedure.
• Additionally, check the tightness of the hose
connections:
- During operation, by visually checking the
connections for leakage

D51IB009EN-F 9
2 Safety Instructions for the Dosing System

- Perform a monthly check of all fluid connec- 2.2.3 Safety Symbols inside the FM 10
tions.
• In the event of a leak, make provisions to pre-
vent contamination of the surroundings with
harmful substances, e.g.:
- Provide sufficient ventilation of the setup
location.
- Place the system in an adequate fume cup-
board.
- Place the system on a drip plate with ade-
quate drainage. 
• Use the delivered bottle holders as roll-over pro-
tection for the glass bottles.
• Use the delivered stacking frame to secure one
bottle holder on top of the pH module.
• Protect the waste container against tipping. We
recommend using a waste container that fits in
the remaining bottle holder space. 
• Do not disconnect the waste container during
operation of the measuring system.
• Check the filling level of the waste container Fig. 2-1: Safety sign inside the FM 10 flow module (1)
periodically, and empty the waste container and on the thermal insulation cover (2).
early enough.
• Make sure that spilled liquid cannot enter plug
connections or venting slots from the system’s CAUTION
electrical sub-components.
Hot surface
A "hot surface" safety symbol is located inside
the FM 10 flow module (see Fig. 2-1). Another
one is situated on the cuvette’s thermal insula-
tion cover. These surfaces can get very hot.
Do not touch them without adequate protective
measures. When measuring at high tempera-
tures (above 45 °C), the thermal insulation cover
and cuvette area should be allowed to cool down
before removing the cuvette.

2.2.4 Transport
To move or lift the titration unit:
• Empty the titration vessel, the transfer and addi-
tive bottles as well as all hoses.
• Disconnect all fluid and electrical connections.
• Move or lift all components separately. Never
attempt to move or lift the dosing system as a
whole since it is too unstable.
• Carry each component in front of you and keep
it close to your body.

10 D51IB009EN-F
 3 Dosing System - An Overview

3 Dosing System - An Overview

 








1 pH module 6 Dosino/dosing unit combo

2 Titration vessel 7 Dispersant bottle
3 Magnetic stirrer and electrode stand 8 Transfer Dosino
4 pH electrode 9 FM 10 Flow Module
5 Additive bottles (acid or base)
Fig. 3-1: Overview of the Dosing System connected to a FM 10 Flow Module.

3.1 Intended Use of the Instrument The Litesizer 500 has to be equipped with the flow
module FM 10 to be able to operate with the Dosing
System.
The Anton Paar Dosing System is an accessory
developed for Litesizer 500 particle analyzer. Note that the Dosing System is intended to work
with aqueous samples only.
The Dosing System automates the adjustment of
the sample’s pH. Thus, it enables the user to per-
form fast and accurate characterization of zeta
potential and particle size changes in response to
3.2 Main Components
pH.
A pH-measuring device is the central element of the
The Dosing System is composed of sub-compo- Dosing System. It is composed of an electronic pH
nents manufactured by Metrohm and assembled module (Fig. 3-1 ), which provides all electrical
according to an Anton Paar design. connections for the setup, a pH electrode (), an
electrode stand/magnetic stirrer unit () and a titra-
tion vessel ().

D51IB009EN-F 11
3 Dosing System - An Overview

Three glass bottles contain the 3 types of additives 2. An initialization procedure has to be performed
needed: an acid, a base, and a dispersant once a day, in which the transfer Dosino pumps
(Fig. 3-1  & ). All 3 bottles are topped with an liquid in the tubings, through the Omega cuvette
automatic buret (termed "dosing unit") combined (which is placed in the Litesizer) and into the
with an electronic dosing drive (termed "Dosino", titration vessel. Similarly, the acid and base
), which enable fluid circulation between the differ- Dosinos pump liquid into their respective tub-
ent components of the system. ings and into the titration vessel.
The Dosino/dosing unit combo topping the disper- 3. A short compensation routine is executed
sant bottle is single-handedly responsible for the before every measurement to compensate for
back-and-forth transfer of the sample between the dead volumes.
Litesizer and the titration vessel. Thus, it will be
This procedure ensures that the tubings are prop-
referred to as "transfer Dosino" in this instruction
erly filled, that no air bubbles are present in the
manual (Fig. 3-1 ).
system and that the dead volumes in the Dosino/
The liquid connections between the different ele- dosing unit combos are taken into account.
ments of the Dosing System can be summarized as
follows: Initial pH Measurement
• One connection is established between the dis- 1. The operator empties the titration vessel of the
persant bottle and the flow cuvette, which is initialization fluids and flushes both the titration
located in the flow module of the Litesizer. vessel and the hose ends leading to it with dis-
persant.
• The flow cuvette’s second fluid connection is to
the titration vessel. 2. The titration vessel is then filled with sample
(minimum volume: 5 ml).
• Both acid- and base-containing bottles have an
individual fluid connection to the titration vessel. 3. The initial pH of the sample is measured and
recorded by the pH module.
• A waste container is required to passively col-
lect the waste liquid and does not require a 4. The transfer Dosino then aspirates the sample
Dosino/dosing unit combo. This container is into the flow cuvette, where zeta potential and/or
connected to the dispersant bottle. particle size are measured by the Litesizer.
The Dosing System is steered by the same com-
pH Adjustment and pH Ramp Measurements
puter as the Litesizer and using the same software,
Kalliope. Computer communication is established To perform a pH ramp, the operator has to create a
by cable connection between the computer and the measurement profile in the software Kalliope using
rear panel of the pH module. the available templates. After the initial sample
parameters (pH, zeta potential, particle size...) have
been recorded, the pH ramp takes place as follows:
3.3 Functional Principle 1. The transfer Dosino pushes back the sample
into the titration vessel.
Initialization and Equilibration Step
2. The pH is adjusted in the titration vessel by add-
1. At the start of the measurement, the bottles con- ing acid or base to the sample until the next
taining dispersant, acid and base are filled, but required pH is reached.
the titration vessel is kept empty of sample.
3. The transfer Dosino aspirates the sample into
the cuvette again and ELS and/or DLS mea-
surements are performed.
4. Steps 1 to 3 are repeated for every pH value
required.

12 D51IB009EN-F
 4 Checking the Supplied Parts

4 Checking the Supplied Parts

The Dosing System was tested and packed care- 3. If a part is missing, contact your Anton Paar rep-
fully before shipment. However, damage may occur resentative.
during transport.
4. If a part is damaged, contact the transport com-
1. Keep the packaging material (box, foam piece, pany and your Anton Paar representative.
transport protection) for possible returns and
Table 4-1 lists the parts contained in your Dosing
further questions from the transport and insur-
System shipment.
ance company.
Table 4-2 lists the additional parts that are required
2. Check the delivery for completeness by compar-
to operate the Dosing System but have to be
ing the supplied parts to those noted in
ordered separately. Optional parts are listed in
table 4-1.
table 4-3.
Table 4-1: Supplied Parts

Symbol Pcs. Article Description Mat. No.

1 Dosing System for Litesizer 500 182462

Is composed of the following parts:

1 pH Module 867
Metrohm, Mat. No. 2.867.0010
For pH measurement. Provides all electrical connections for
the setup.

1 pH Electrode 182392
Metrohm, Mat. No. 6.0256.100
For the measurement of the pH, together with the pH module.

1 Magnetic Stirrer 801

Metrohm, Mat. No. 2.801.0040
Includes stirrer, electrode holder, support rod, 2 stirring bars
(16 mm and 25 mm) and mounting accessories.

3 Dosing Unit 807, 5 ml

Metrohm, Mat. No. 6.3032.150
Piston unit for use as bottle-top combo with Dosino 800.
Includes FEP tubing and anti-diffusion buret tip.

3 Dosino 800
Metrohm, Mat. No. 2.800.0010
Electronic dosing drive for use as bottle-top combo with Dos-
ing Unit 807. Includes cable and piston extractor.

D51IB009EN-F 13
4 Checking the Supplied Parts

Table 4-1: Supplied Parts

Symbol Pcs. Article Description Mat. No.

2 Bottle holder for Dosino

Metrohm, Mat. No. 6.2061.010

1 Stacking frame for pH module

Metrohm, Mat. No. 6.2065.000

3 Amber glass bottle 1000 mL 182391

Metrohm, Mat. No. 6.1608.023
For additives (acid and base) as well as dispersant.

1 Titration vessel 50 - 150 mL 182414

Metrohm, Mat. No. 6.1415.250

1 Titration vessel lid "Automation"

Metrohm, Mat. No. 6.1414.080

2 PEEK adapter 10/32 182415

Metrohm, Mat. No. 6.2744.110

2 PEEK adapter M6-UNF 182416

Metrohm, Mat. No. 6.2744.080

1 Electrode cable 1 m (G-head) 182412

Metrohm, Mat. No. 6.2104.020

1 Cable USB A – 8-pin mini-DIN 182413

Metrohm, Mat. No. 6.2151.000

1 C-Flex® hose (25 ft) 182495

C-Flex®, opaque white, 1/32" ID x 3/32" OD, Cole-Parmer
Mat. No. 06424-60

1 Hose barb adapters for Omega cuvette (25 units) 182492

Male Slip Luer to 1/16", Cole-Palmer Mat. No. 45504-22

14 D51IB009EN-F
 4 Checking the Supplied Parts

Table 4-1: Supplied Parts

Symbol Pcs. Article Description Mat. No.

1 pH Module 867 instruction manual

Metrohm Doc. No. 8.867.8003

1 Dosing Unit 807 instruction manual

Metrohm Doc. No. 8.807.8002

1 Magnetic Stirrer 801 instruction manual

Metrohm Doc. No. 8.801.8001

1 Dosino 800 instruction manual

Metrohm Doc. No. 8.800.8002

1 Dosing System instruction manual

Anton Paar Doc. No. D51IB009
Measure
what is measurable
and make measurable
that which is not.
Galileo Galilei (1564-1642)

,QVWUXFWLRQ0DQXDO

'RVLQJ6\VWHP
IRUWKH/LWHVL]HUΠSDUWLFOHDQDO\]HU

2ULJLQDO,QVWUXFWLRQ

Table 4-2: Additional Parts Required to Operate the Dosing System

Symbol Article Description Mat. No.

Litesizer 500 155761

FM 10 Flow Module 162931

Flow cuvette for ELS measurement 225288

Omega cuvette for zeta & size (Box of 10 cuvettes)
One box of Omega cuvettes is included in the Starter Kit of
the Litesizer 500.

D51IB009EN-F 15
4 Checking the Supplied Parts

Table 4-2: Additional Parts Required to Operate the Dosing System

Symbol Article Description Mat. No.

Kalliope software, version 1.8 or higher, one of the following:

166116
• Kalliope Professional (for 3 users)
170678
• Kalliope Professional Unlimited (unlimited no. of users)

Litesizer Reference Guide

Anton Paar Doc. No. D51IB010

Measure
what is measurable

This document is delivered as electronic copy (PDF) with

and make measurable
that which is not.
Galileo Galilei (1564-1642)

every Litesizer instrument.

,QVWUXFWLRQ0DQXDO

/LWHVL]HUŒ6HULHV,QVWUXPHQWV
/LWHVL]HUΠ /LWHVL]HUΠ

/LJKW6FDWWHULQJ,QVWUXPHQWV
IRU3DUWLFOH$QDO\VLV

Computer running Microsoft Windows OS Buy locally

See section 5.1.2 for minimum system requirements.

Waste container Buy locally

Table 4-3: Optional Parts

Symbol Article Description Mat. No.

Buffer for pH Electrode calibration, pH = 10.01 46271

Hamilton DuraCal, 500 mL

Buffer for pH Electrode calibration, pH = 7.00 12556

Hamilton DuraCal, 500 mL

Buffer for pH Electrode calibration, pH = 4.01 12554

Hamilton DuraCal, 500 mL

Rod stirrer 802 227811

The rod stirrer 802 together with Ti stand 804 provides an
addition to the magnetic stirrer of the dosing system.

Ti Stand 804 227810

Titration stand and controller for the rod stirrer 802. Together
with the rod stirrer 802 it provides an addition to the magnetic
stirrer for the dosing system.

Kalliope Professional Software Module 21 CFR Part 11 218627

• Software module for Kalliope to comply with the regulation
21 CFR Part 11 introduced by the US Food and Drug
Administration (FDA).
• Key features: electronic signature, audit trail, retrieval.

16 D51IB009EN-F
 5 Installing the Dosing System

5 Installing the Dosing System

5.1 Installation Requirements 5.2 Assembling the Components
Respect the Litesizer 500 installation requirements
described in the particle analyzer’s dedicated 5.2.1 Combining Dosinos and Dosing Units
instruction manual (Anton Paar document
D51IB001). Be aware that the minimum computer 1. Attach each of the 3 Metrohm Dosinos to a 5 mL
requirements for Litesizer instruments steering the Metrohm dosing unit as follows (Fig. 5-1):
Dosing System differ from those of Litesizer instru- a. Insert the guide pins of the Dosino
ments operating without accessory (see (Fig. 5-1 ) into the openings on the dosing
section 5.1.2 below). unit provided for this purpose. The green line
Read the Safety Instructions in Chapter 2 . marking of the Dosino () must come to rest
on the dotted white line marking (UNLOCK
Find all Technical Data in Appendix A - Technical position, ) of the dosing unit.
Data. b. Rotate the Dosino to the left until it stops.
The green line marking of the Dosino now
5.1.1 Environmental Requirements lies on the extended white line marking
(LOCK position, ) of the dosing unit.
The setup location and surroundings should meet
the requirements of a typical laboratory.
Allow the equipment to reach ambient temperature 
before installation. This is very important if the
equipment has been stored or transported at lower
temperatures. 
To ensure temperature stability and trouble-free
measurement never locate your instrument:

• next to a heating facility
• near an air conditioning, ventilation system or an 
open window

• in direct sunlight
Keep the instrument away from magnetic fields.

5.1.2 Computer Requirements

1 Green line marking
2 Guide pins
The minimum system requirements for computers
3 UNLOCK position
steering Litesizer instruments together with the
4 LOCK position
Dosing System are the following: 5 Status LED
• Dual core system (or better) Fig. 5-1: Mounting the Dosino onto the dosing unit
• Windows 7 - Service Pack 1 (or better)
NOTICE
• 5 GB HDD
After its combination with a dosing unit, the
• 6 GB RAM (Windows 7 - 64 Bit), or better Dosino’s Status LED (Fig. 5-1 ) must light up
when the control device is switched on. If this
does not occur, it means that the combo was not
mounted properly.

2. Mount the aspiration tubings on the 3 dosing onto the connector with inner thread ()on the
units. To this end, screw the tubing (Fig. 5-2 ) underside of the dosing unit.

D51IB009EN-F 17
5 Installing the Dosing System

5. If necessary, see the relevant Metrohm Instruc-

tion Manuals for more details.

5.2.2 Installing the Magnetic Stirrer with

 Electrode Stand and pH Module


1 Aspiration tubing
2 Port with inner thread (port 2 in Metrohm manual)
Fig. 5-2: Mounting the aspiration tubing onto a dosing
unit
3. Fill the 3 amber glass bottles respectively with
dispersant, acid and base.

WARNING
Strong acids and bases
Strong acids and bases can cause serious injury
and material damage. Wear adequate protection
when handling the reagents. Make sure acid and
base do not come in contact with each other.
Clean spilled material immediately.
Fig. 5-3: Typical pH module - magnetic stirrer combina-
4. Screw the Dosino – dosing unit combos onto tion with pH electrode and test vessel.
the filled amber glass bottles.
1. As described in Fig. 5-4-A, screw the support
stand (), which is delivered with the Stirrer
NOTICE 801, to the bottom of the pH Module 867 ()
Do not over-tighten the combos and do not use using the 4 supplied screws.
any mechanical mounting aids, as it could cause
malfunction. When using reagent bottles other 2. As described in Fig. 5-4-B, firmly screw the sup-
than those provided, make sure they have a port rod (, also delivered with the stirrer) to the
GL45 thread equipped with a decanting ring. support stand using the supplied hexagon screw
and key.

18 D51IB009EN-F
 5 Installing the Dosing System

5. Slide the titration vessel lid onto the support rod

A.
using the dedicated guide hole (Fig. 5-6).




1 Guide hole for the support rod
2 Opening for the pH electrode

B. Fig. 5-6: Titration vessel lid.


5.2.3 Installing Reagent Bottles and Titration
Vessel

1 pH module
2 Support stand
3 Support rod
Fig. 5-4: Mounting the stand plate and stand rod onto the
pH module Fig. 5-7: Bottle holder (left) and stacking frame (right)

3. Slide the magnetic stirrer onto the support rod Two bottle holders are delivered with the Dosing
and push it downwards (Fig. 5-5 A). System (Fig. 5-7, left).

4. Using the clamping screw (Fig. 5-5 B), fix the Place one bottle holder on top of the pH module
positioning height and/or the swing position of using the stacking frame (Fig. 5-7, right).
the magnetic stirrer. Place the second bottle holder next to the pH
module opposite the stirrer.
A. B.
We then recommend placing the acid and base
reagent bottles at the front of the setup (Fig. 5-8 ),
the dispersant bottle at the rear position on the pH
module () and the waste container at the remain-
ing rear position ().

Fig. 5-5: Fixing the magnetic stirrer on the support rod

D51IB009EN-F 19
5 Installing the Dosing System


 


  1 pH electrode
2 Electrode sleeve

3 Titration vessel
   4 Titration vessel lid
 5 Electrode storage
  vessel

1 Stirrer
2 pH module Fig. 5-9: Installed pH electrode. The figure depicts an
3 Stacking frame empty titration vessel, the electrode is therefore
4 Bottle holder 1 stored in its storage vessel.
5 Bottle holder 2
6 Acid or base bottle
7 Dispersant bottle 5.2.5 Installing the FM 10 Flow Module and
8 Waste container Checking the Pinch Valve Function
Fig. 5-8: Properly assembled Dosing System
The FM 10 flow module is equipped with a pinch
Finally, install the empty titration vessel on the stir-
valve which ensures measurement stability by
rer. Place a magnetic stirring bar inside the vessel
squeezing the hose that is fed through the lower
and press down the titration lid until the vessel is
hole of the FM 10 (see Fig. 5-11).
closed and held in place securely.
A proper function of the pinch valve is crucial to the
safe operation of the flow module. Therefore, the
5.2.4 Installing the pH Electrode user has to check the correct pinch valve function
once a day before a dosing/titration measurement is
Plug in the polyethylene sleeve (Fig. 5-9 , deliv- started:
ered with the pH electrode) into the dedicated open-
ing of the titration vessel lid (Fig. 5-6 ). Gently 1. Connect the FM 10 Flow Module to the Litesizer
insert the pH electrode through the sleeve. Make (see Fig. 5-10) and switch on the instrument.
sure that the tip of the electrode is immersed in the Refer to the Litesizer instruction manual if
sample but cannot be touched by the stirring bar. needed.
Important: When not in use, the electrode should
be stored in its storage vessel (Fig. 5-9 , part of
the electrode delivery) filled with 3 M KCl solution.
The electrode can also be stored in the storage
solution commercialized by its manufacturer
Metrohm (Mat. No. :6.2323.000).

Fig. 5-10: Connecting the FM 10 to the Litesizer

20 D51IB009EN-F
 5 Installing the Dosing System

2. When the Litesizer is ready for measurement, 4. Close the module lid. The pinch valve squeezes
open the module lid. This forces the pinch valve the hose and prevents it from moving. Check
to open for 2 minutes. If the pinch valve closes that this is the case by gently pulling the hose
after 2 minutes it can be reopened again by from outside the instrument.
closing and opening the module lid.
If the behavior is somehow different to that
3. Feed a C-Flex® hose through the lower hole of described above, contact Anton Paar for support.
the FM 10 (Fig. 5-11 ). The hose should be
Important: In case of sample spill or hose rupture,
able to move freely through the hole as long as
the flow module should be dried in an oven at 60 °C.
the pinch valve is open.
If the spilled liquid is thick and/or sticky, the hole in
the FM 10 where the pinch valve is located should
be flushed gently with deionized water (use a
syringe) before it is placed in the oven. The correct
function of the pinch valve must be checked imme-
diately after drying the FM 10. If the pinch valve is
not working properly, stop using the FM 10 and con-
tact Anton Paar for support.

1 Pinch valve location

Fig. 5-11: FM 10 Flow Module in open position with con-
nected Omega cuvette.

D51IB009EN-F 21
5 Installing the Dosing System

5.3 Connecting the Dosing System

5.3.1 Fluid Connections

 
 

 


 

Fig. 5-12: Sketch of the Dosing System fluid connections. Color code: yellow = sample; violet = dispersant;
red = base; orange = acid. The number tags (q) refer to the dosing unit port numbers according to Metrohm termi-
nology.
A sketch of all fluid connections is shown in 2. Attach an anti-diffusion tip (Fig. 5-13 ) to the
Fig. 5-12. The fluid connection system is steered by free end of each FEP tubing. The anti-diffusion
3 Dosinos/dosing unit combos. The transfer Dosino tip must then be fed into the titration vessel
is used to transfer the sample back and forth from through one of the small openings in the titration
the titration vessel to the Omega cuvette in the Lite- lid. Alternatively, a ball stopper (Fig. 5-13 )
sizer. Dosino 1 and 2 are the additive Dosinos and can be used to hold the tip through one of the
can alter the sample’s pH in the titration vessel by larger lid openings.
adding acid or base.
  
NOTICE
Waste container
The transfer Dosino must be connected to a
waste container via its port 3 (see Fig. 5-12).
This is necessary to prevent the dispersant from
leaking out of the apparatus during the cleaning
procedure.

Proceed as follows:
Fig. 5-13: FEP tubing (1), anti-diffusion tip (2) and ball
1. Connect port 1 of Dosino 1 and Dosino 2 with stopper (3). These parts are delivered with the Dosing
the FEP tubing (Fig. 5-13 ). Units.

3. Use another FEP tubing to connect port 3 of the ous notice).

transfer Dosino to a waste container (see previ-

22 D51IB009EN-F
 5 Installing the Dosing System

4. Attach 2 Luer-hose barb adapters to an Anton

Paar Omega cuvette (Fig. 5-14). The procedure
is identical for all Omega cuvette types.
5. Attach C-Flex® hoses to the hose barb adapters
of the Omega cuvette (Fig. 5-14). On hose 
should be 80 cm (± 5 cm) long while the other
should be 120 cm (± 5 cm) long.


Fig. 5-14: Anton Paar Omega cuvette (1) with Luer-hose

barb adapters (2) and C-Flex® tubing (3)

6. Use the wrench (Fig. 5-15 ) to tighten all
Metrohm fluid connections.

 


Fig. 5-16: Fluid connections from the Omega cuvette

through the opened (top panel) or closed (lower
 panel) FM 10 Flow Module. 1: to the titration vessel;
 2: to the transfer Dosino.
9. Screw the PEEK adapter 10/32 (Fig. 5-15 )
onto the PEEK adapter M6 (Fig. 5-15 ).
10.Connect the free end of the longer C-Flex® hose
Fig. 5-15: Fluid connection wrench (1), buret tip (2), (which is threaded into the lower module hole)
PEEK adapter 10/32 (3) and PEEK adapter M6 (4). to the thin opening of the PEEK adapter 10/32.

7. Place the Omega cuvette in the FM 10 Flow 11. Connect the large end of the PEEK adapter M6
Module and thread the shorter C-Flex® hose to port 1 of the transfer Dosino.
through the upper module hole (see 12.Take out the thin tube ending of a buret tip
Fig. 5-16 ). (Fig. 5-17 ) by firmly pulling it.
8. Thread the longer C-Flex® hose through the
lower hole (see Fig. 5-16 ). If the lower hole is
blocked by the pinch valve, make sure that the
Litesizer is ready for operation, then close and
open the module lid again (see section 5-9). The
opening of the lid will force the pinch valve to
open for two minutes.

D51IB009EN-F 23
5 Installing the Dosing System

 
Fig. 5-17: Buret tip (1) and modified buret tip (2) threaded
with the C-Flex® hose (3)
13.Cut the extremity of the shorter C-Flex® hose
(which is threaded into the upper module hole)
at a 45° angle using a knife or scissors, then
thread it through the buret tip body, as shown in
Fig. 5-17 .
14.Feed the modified buret tip through the titration
vessel lid and into the beaker. Again a ball stop-
per (Fig. 5-13 ) can be used to hold the tip
through one of the larger lid openings if neces-
sary.
15.Check that your setup matches that pictured in
Fig. 5-18 below.

24 D51IB009EN-F
 5 Installing the Dosing System

 


 

1 Titration vessel
2 Titration vessel lid
3 Acid or base Dosino
4 Acid or base Dosino connection to titration vessel
5 Anti-diffusion tips
6 Transfer Dosino
7 PEEK adapter
8 C-Flex® hose from transfer Dosino to FM 10
9 C-Flex® hose from FM 10 to Titration Vessel
10 Modified buret tip
Fig. 5-18: Fluid connections on a correctly assembled Dosing System

D51IB009EN-F 25
5 Installing the Dosing System

5.3.2 Electrical Connections

    pH Module 867 Magnetic stirrer 801


 
 




1 pH Electrode connector 8 Type plate
2 Reference electrode connector 9 Power socket
3 Temperature sensor connector 10 Metrohm Serial Bus (MSB) connectors 1 to 4
4 Polarizable electrode connector 11 MSB connector
5 iConnect electrode connector 12 Clamping screw
6 Controller connector 13 MSB connection cable
7 USB connector
Fig. 5-19: Rear panels of the Metrohm pH Module 867 (left) and of the Metrohm Magnetic Stirrer 801 (right).
The individual elements of the Dosing System have 5. Connect the pH electrode to the connector
to be connected either to the rear panel of the pH marked "Ind." on the pH module ().
module or to that of the magnetic stirrer.
6. Connect the black USB A/8-pin mini-DIN cable
1. Connect the transfer Dosino to the Metrohm between the 8-pin "Controller" connector at the
Serial Bus (MSB) connector marked "MSB 1" on rear of the pH module () and a free USB port
the rear panel of the pH module (Fig. 5-19 ). on the computer steering the Litesizer.
2. Connect the Dosino 1 (e.g., base) to the con- 7. Connect the power cable of the pH module
nector marked "MSB 2" on the rear panel of the between the module’s power socket () and the
pH module (). mains.
3. Connect the Dosino 2 (e.g., acid) to the connec- 8. Check that your setup matches that pictured in
tor marked "MSB" on the rear panel of the stirrer Fig. 5-20 below.
().
4. Connect the MSB connection cable of the stirrer NOTICE
() to the connector marked "MSB 3" on the Make sure the Dosinos are connected to the
rear panel of the pH module (). pH module and the stirrer as described above.
Using a different configuration will lead to a mal-
function of the Dosing System.

26 D51IB009EN-F
 5 Installing the Dosing System



 


1 Transfer Dosino 5 pH electrode

2 Dosino 1 (e.g., base) 6 Computer
3 Dosino 2 (e.g., acid) 7 Power
4 Stirrer
Fig. 5-20: Correct electrical connections on the rear panels of the stirrer and the pH module
As the Ti stand 804 uses the same MSB port as the
magnetic stirrer both stirrer types can not be used at
the same time, but must be connected manually
5.4 Installing the rod stirrer every time the stirrer type is changed. After connec-
tion of the hardware the rod stirrer can be used with
In case a rod stirrer is used instead of the magnetic Kalliope software in the same way as the magnetic
stirrer following equipment is needed in addition to stirrer, including different speed levels.
the initial Dosing Unit package:
• Rod stirrer 802 (Mat. No. 227811)
For proper handling it is recommended to place the
• Ti Stand 804 (Mat. No. 227810) titration vessel on the magnetic stirrer and to
arrange the hoses and pH electrode in the vessel lid
Please perform all steps to assemble the Dosing
as shown in figure Fig. 5-9. The rod stirrer 802
Unit described in chapters section 5.1, 5.2 and 5.3
should be placed in the center of the titration vessel.
before starting installing the rod stirrer. First, the rod
Please not that due to the length of the rod stirrer it
stirrer 802 has to be connected with the Ti Stand
is not possible to attach the titration vessel to the
804. Afterwards, the Ti Stand 804 has to be con-
vessel lid via the clamping ring.
nected to the MSB 3 port of the pH module via the
MSB connection cable (c.f. Fig. 5-19).

D51IB009EN-F 27
5 Installing the Dosing System

A minimum sample volume of 15 ml is required to

optimally perform dosing over volume measure-
ments with the rod stirrer (pH electrode not
immersed). In case of a dosing over pH measure-
ment (pH electrode required) a minimum sample
volume of 40 ml is recommended in order to ensure
that the tip of the electrode is immersed in the
sample but can not be touched by any part of the
stirrer.

28 D51IB009EN-F
 6 Operating the Dosing System

6 Operating the Dosing System

6.1 Software Installation and Update The Metrohm driver installation file "Metrohm USB
Update 1.65.exe" can be found in the sub-folders of
the Kalliope installation directory, usually under
6.1.1 Kalliope "C: > Program Files > Anton Paar > Kalliope >
driver > Metrohm".
Kalliope version 1.8 or newer is necessary to oper- Execute the program file and follow on-screen
ate the Dosing System. To check which version is instructions.
installed on your computer, go to Kalliope’s main
menu by clicking on the <Ka> icon on the top left-
hand corner of the screen, then select "About" 6.1.3 Installing the Dosing System in Kalli-
(Fig. 6-1). ope
Re-start Kalliope and go to its main menu by clicking
on the <Ka> icon on the top left-hand corner of the
screen. Next, go to the "Instrument" menu as
described in Fig. 6-2. In the "Device-dependent
features" submenu, select Litesizer 500 and
Dosing System using the drop-down menus.
A "Dosing System" menu should then appear in
Kalliope’s menu bar.

Fig. 6-1: Checking the Kalliope software version (circled

in green)
Should the version of Kalliope be lower than 1.8,
please download the latest software version from
the Anton Paar website (www.anton-paar.com, rec-
ommended search term "Kalliope").
Reminder: Please note that the minimum system
requirements for computers steering the Litesizer
Fig. 6-2: Installing the Dosing System feature
together with the Dosing System differ from those of
Litesizer instruments operating without accessory.
See section 5.1.2 for details.
6.2 Dosing System Menu
6.1.2 Metrohm Instrument Drivers Kalliope enables the operator to manually operate
the Dosing System via a dedicated menu. To
The Metrohm instrument drivers, which are neces- access this application menu select "Dosing Sys-
sary to steer the Dosinos, have to be installed man- tem" in Kalliope’s main menu.
ually by the user.

D51IB009EN-F 29
6 Operating the Dosing System

A screenshot of this menu is shown in Fig. 6-3 6.2.2 Workflows Submenu

below.
The "Workflows" submenu enables the user to
execute filling and cleaning routines which are nec-
6.2.1 Dosing System Submenu essary before or after measurement.
The status of the titration unit is shown in the "Dos-
"Prepare Dosinos":
ing System" section at the top of the screen.
This routine must be executed at least once a day
If "Offline" is displayed, the titration unit is not ready
(before the first measurement) or if the hoses are
and a manual operation of the titration unit is not
not free from air bubbles:
possible. This can happen if the pH module is not
powered up, if the USB connection to the PC is • All hoses connecting a dosing unit to the titration
missing or if the Metrohm instrument drivers have vessel are filled with the corresponding liquids.
not been installed. Refer to section 5.3 to check the The tubing from the transfer Dosino to the titra-
system’s connections and/or to section 6.1.2 to tion vessel (via the Omega cuvette) is filled with
install the drivers. dispersant and the tubings running from Dosi-
nos 1 and 2 to the titration vessel are filled with
If the titration unit is in the "Idle" state, the Dosing
the corresponding additives (acid or base).
System can be operated.
• As air bubbles very often get stuck in the cuvette
during the filling of the tubing, a dialog box will
pop up to alert the operator to remove the air
bubbles from the cuvette. To this end, open the
module lid and gently tap against the cuvette.

30 D51IB009EN-F
 6 Operating the Dosing System

Fig. 6-3: Dosing System menu: status and manual operation functions. The "Workflows" > "Prepare Dosinos" rou-
tine has to be executed daily before the Dosing System is put into operation.
"Empty Sample Unit":
NOTICE
Keep flow module lid open The tubing from the transfer Dosino to the titration
Do not close the flow module lid before the "Pre- vessel (via the Omega cuvette) is emptied.
pare Dosinos" routine is finished as it would
prompt the pinch valve to close. This in turn 6.2.3 Actions Submenu
would block the flow of the dispersant and force
the tubing at port 1 of the transfer Dosino to dis- "Stirrer":
connect itself.
This enables the manual activation of the stirrer.
Choose the stirrer speed from the drop-down menu
"Clean Dosinos":
("Slow", "Medium" or "Fast"). Press the <Start> and
<Stop> buttons to start and stop the stirring, respec-
This sequence is the opposite of the "Prepare
tively.
Dosinos" routine (all hoses are emptied). This rou-
tine must be performed at the end of the experi- "pH Measurement":
ment.
This action performs a continuous pH measurement
of the sample. Set the sample temperature and
"Clean Sample Unit":
press the <Start> and <Stop> buttons to start and
The tubing from the transfer Dosino to the titration stop the measurement. The pH value will appear in
vessel (via the Omega cuvette) is rinsed with the the dedicated field at the right-hand side of the
transfer liquid. <Stop> button.

D51IB009EN-F 31
6 Operating the Dosing System

6.2.4 pH Calibration Submenu In the "General" submenu:

• The Target temperature parameter corre-
A calibration of the pH electrode with buffer solu- sponds to the temperature of the buffer solution
tions can be performed using the "pH Calibration" (min. 10 °C, max. 40 °C).
submenu. We recommend performing this calibra-
tion once a week. • The equilibration time parameter defines the
time lapse before the pH measurement is
By clicking the <New> button at the bottom of the started (min. 0 s, max. 1 h). A value of min. 10 s
screen, a pH calibration measurement template is is recommended.
created (see Fig. 6-4).

Fig. 6-4: pH calibration submenu: measurement template

In the "Quality" submenu: When the parameters are set click the <Set calibra-
tion> button in the upper right corner of the screen
• Max. drift parameter: during pH equilibration,
to start the calibration.
the pH electrode registers voltage variations in
response to pH change. When this voltage vari-
ation drops below the defined Max. drift thresh-
old (min. 1 mV/min, max. 100 mV/min), the pH
6.3 Setting Up a Measurement
is considered stable and the measurement
1. Start Kalliope
stops. A value of 10 mV/min is recommended.
2. Wait until the Dosing System is in "Idle" state
• The Max. measurement time parameter
(see Fig. 6-3).
defines the maximum duration of a pH measure-
ment (min. 10 s, max. 30 min). If the pH drift 3. Before a dosing method is stared, ensure that
falls below the defined threshold (= Max. drift) all hoses connected to the titration vessel are
before this time is reached, the pH measure- filled with the corresponding liquids. This can be
ment ends earlier. A value of min. 1 min is rec- done by executing the "Prepare Dosinos" rou-
ommended. tine (see section •).
In the "Buffers" submenu, the operator has to set 4. Click on the "New Workbook" icon ( ) at the
up the number of buffers and the corresponding pH top left-hand side of the screen, then press the
values (between 0 and 14). Note that at least 3 buf- <+> button to access the measurement mode
fers are required. Additional buffers can be added screen (Fig. 6-5).
by clicking on the <+> button.

32 D51IB009EN-F
 6 Operating the Dosing System

5. Select one of the available dosing modes.The DLS / ELS parameters: Please refer to the Lite-
"Dosing over pH" allows both a zeta potential sizer instruction manual for help with the parameters
over pH and a particle size over pH curve. The relating to normal DLS and ELS measurements
"Dosing over volume" enables adding a ("Comment", "General", "Solvent", "Zeta Poten-
defined volume of liquid from the Dosino to the tial", "Particle Size").
sample without any pH feedback.
Temperature: Note that the sample temperature
6. Input your measurement parameters. Descrip- only refers to the sample temperature in the Omega
tions are listed in table 6-1. cuvette, as the Dosing System itself is not tem-
pered.

Fig. 6-5: Selecting the dosing measurement mode

Table 6-1: Setting Up a Measurement with the Dosing System: Input Parameters

"Submenu" / Parameter Description

"Comment" See Litesizer Reference Guide

"General" See Litesizer Reference Guide

"Solvent" See Litesizer Reference Guide

"Zeta Potential" See Litesizer Reference Guide

"Particle Size" See Litesizer Reference Guide

"Dosing configuration" Select if one or two additive Dosinos should be used for the measure-
ment and specify the pH (0 to 14) or concentration (1E-07 to 1 M) for
each one of them. Acid configuration means pH ≤ 7 and base configura-
tion is defined as pH ≥ 7.

"Dosing mode" Using the drop-down menu, the user can choose between two modes,
Region of interest or Target value:

Target value Possible with one and two additive Dosinos. If only one additive Dosino is
used with acid configuration, the target pH must be greater than the addi-
tive pH. If only one additive Dosino is used with base configuration, the
target pH must be lower than the additive pH. If only one additive Dosino
is used, the validation of the input parameters is only possible after the
initial sample pH is measured.

D51IB009EN-F 33
6 Operating the Dosing System

Table 6-1: Setting Up a Measurement with the Dosing System: Input Parameters

"Submenu" / Parameter Description

Region of interest Only possible if both additive Dosinos are used and if they are configured
as acid (pH ≤ 7) and base (pH ≥ 7). The lower and upper pH limit for the
region of interest must lie within the range predefined by the pH/concen-
tration values of the additive Dosinos.

Dosing direction Accessible only when Region of interest is selected. When the initial
sample pH is already within the region of interest, the user can select if
the dosing sequence should start with acidification (Acid first) or alkalini-
zation (Base first). If Automatic is chosen, the titration will first aim for
the pH range limit closest to the initial sample pH.

"Dosing steps" The desired pH interval between each dosing step can be set with the pH
step width parameter. The pH step value should be between 0.1 and 2.

"pH value determination" Settings for the measurement of the sample’s pH in the titration vessel.
Using the drop-down menu, the user can choose between 3 modes,
Automatic, Quick or Manual. The main parameters are:
• Equilibration time: defines the time lapse between the adding of an
additive and the start of the pH measurement.
• Max. measurement time: defines the maximum duration of a pH
measurement. If the voltage drift registered by the pH electrode falls
below the defined threshold of 10 mV/min before this time is reached,
the pH is considered stable and the measurement ends earlier.

Automatic Equilibration time is 10 s, Max. measurement time is 1 min.

Quick Equilibration time is 10 s, Max. measurement time is 20 s.

Manual The user can set the Equilibration time (min. 0 s, max. 30 min) and the
Max. measurement time (min. 10 s, max. 10 min) manually.

"After titration" Here the user can select if all the hoses should be emptied after the mea-
surement.

"Overflow protection" If the overflow protection is enabled, additional input parameters (beaker
volume = volume of titration vessel, initial sample volume) are needed.
Kalliope shows a warning if the beaker runs the risk to overflow. The
operator can confirm this warning and stop the measurement or confirm it
and proceed.

"Stirrer" Drop-down menu used to define stirrer speed (Slow, Medium or Fast).
The slow option should be favored when working with small sample vol-
umes.

6.4 Performing the Measurement A dialog box informs you to remove your sample if
you have already placed it in the titration vessel.
This is necessary because the titration unit performs
Clicking the <Start> button at the bottom right-hand
so-called compensation steps to ensure highest
side of the screen to start the measurement.
dosing accuracy and brings the transfer Dosino
piston into the correct position. During these com-
pensation steps, additives are ejected into the titra-
tion vessel.
Attention: During the compensation steps, we

34 D51IB009EN-F
 6 Operating the Dosing System

highly recommend filling the titration vessel with e.g. 3. The transfer Dosino pushes back the sample
distilled water in order to wash away the drops of into the titration vessel.
acid and/or base which form at the anti-diffusion
4. The sample pH is modified by adding acid or
buret tips. If these drops are not washed away, they
base to the titration vessel via the additive Dosi-
can alter the initial sample pH.
nos. The new sample pH is measured.
After these steps have been performed, a dialog box
5. Steps 2 to 4 are repeated until the target pH is
asks you to put your sample in the sample vessel.
reached.
Empty the titration vessel of all liquids, rinse it briefly
with distilled water, place your sample in the vessel
and confirm the dialog box. 6.5 Cleaning the Dosing System
As this is the first time the pH electrode comes into
When the experiment is finished:
contact with the sample, a delay of 30 s is imple-
mented for pH stabilization. 1. Perform the "Clean Dosinos" routine from the
"Dosing System" menu (see Fig. 6-3) to empty
The main steps of the titration sequence are
all hoses.
described in Fig. 6-6:
2. Empty and clean the titration vessel.
1. Initial state: The "Prepare Dosinos" routine
was executed via the Dosing System menu (see 3. Clean the pH electrode with distilled water and
section 6.2.2) and hence all hoses are filled with put it in its KCl-filled storage vessel (see
the corresponding liquids. The measurement section 5.2.4).
was started, the compensation steps were con-
4. Disconnect the Omega cuvette by taking the
ducted and the sample has then been poured in
barb adapters out, take it out of the instrument
the titration vessel. The initial sample pH is now
and clean it using distilled water and dry com-
measured.
pressed air as described in section 7.3.6.
2. The transfer Dosino aspirates the sample into
Important: Always perform the "Clean Dosino"
the Omega cuvette. After temperature equilibra-
routine before disconnecting any tubing, as it
tion, zeta potential and/or particle size are mea-
ensures that all hoses are empty and thus prevents
sured by the Litesizer.
sample and/or additive spills.

D51IB009EN-F 35
6 Operating the Dosing System

Fig. 6-6: Dosing System titration sequence. Color code: yellow = sample; violet = dispersant; red = additive (acid or
base). Sequence:  = Initial sample pH measurement in the titration vessel.  = Sample is aspirated by the trans-
fer Dosino into the Omega cuvette, where zeta potential and/or particle size are measured.  = Sample is pushed
back into the titration vessel.  = Sample pH is adjusted by the additive Dosino(s). The titration sequence then
consists in a repetition of steps ,  and  until the predefined pH limits are reached.

36 D51IB009EN-F
 7 Upkeep and Cleaning

7 Upkeep and Cleaning

7.1 General Considerations
• To assure a high and constant measurement WARNING
accuracy, operate and store the instrument Strong acids and bases
under the specified conditions and perform the Strong acids and bases can cause serious injury
recommended tasks regularly. as well as material damage. Wear adequate pro-
• Ensure that all environmental requirements from tection (gloves, goggles, protective clothing)
the installation chapter as well as the specifica- when cleaning the Dosing System.
tions chapter are always fulfilled.
• Always handle the instrument with care. Even
minor damage may cause serious measurement
7.3 Cleaning and Maintenance of the
errors. Individual Components
• Employ a regular optical check if there is no
contamination on the outside and inside the
instrument and perform an effective cleaning
7.3.1 pH Electrode
routine.
When not in use, the pH electrode should be stored
• Also make sure to follow the maintenance in its storage vessel filled with 3 M KCl (see
instructions provided with any third-party prod- section 5.2.4). The electrode can also be stored in
ucts. the storage solution commercialized by its manufac-
turer Metrohm (Mat. No. :6.2323.000).
• Please note that the automatic burets (Metrohm
807 dosing units), which are in contact with the The electrode should be calibrated regularly, once a
sample and the additives, require regular care week when the instrument is in use or every time the
on a monthly basis or more. Thus, we strongly Dosing System has been out of use for more than a
recommend that you get familiar with the essen- week. Refer to section 6.2.4 to perform the calibra-
tial maintenance steps of the dosing units. Read tion.
section 7.3.4 below for details.
• A full list of instrument parts wetted either by the 7.3.2 pH Module and Stirrer
sample or the additives is available in table 7-1
below. The Metrohm 867 pH Module and the Metrohm 801
Stirrer are robust instruments requiring little mainte-
nance. However, particular care must be taken to
7.2 Monthly Cleaning Procedure ensure that the plug connections at the back of the
instruments (see Fig. 5-19) do not get in contact
As strong acids and alkali are routinely used with the with corrosive liquids. Note that the power socket of
Dosing System, we recommend performing a the pH module is particularly sensitive to contamina-
monthly visual inspection of the system to identify tion.
potential leaks and spills. Spilled chemicals and sol-
vents must be removed with care using distilled
water and the components subsequently dried with
a lint-free cloth. CAUTION
Not that excessive contamination of the accessory Contamination of the power socket.
may result in functional disruption and a reduction of In the event of a contamination of the pH module
its lifetime. power socket with sample and/or additives,
immediately disconnect the instrument from the
mains. Failure to follow this notice might lead to
the destruction of the instrument’s electronics.

Please refer to the pH module and the stirrer’s Doc. No. 8.867.8003 and 8.801.8001) for more
respective instruction manuals (Metrohm maintenance and troubleshooting advice.

D51IB009EN-F 37
7 Upkeep and Cleaning

7.3.3 Dosinos 3. Ensuring that the discs do not adhere to one

another
The Metrohm 800 Dosinos, which are electronic These three steps are described in the 807 Dosing
dosing drives, are not in direct contact with samples Unit instruction manual (Metrohm
and additives and as such require little specific Doc. No. 8.807.8002) in sections 4.1.1 to 4.1.3.
maintenance. Perform monthly inspections to pre-
vent external damage from corrosive liquids. Also refer to section 5 of the above-mentioned
instruction manual for troubleshooting advice.

CAUTION 7.3.5 Cleaning the FM 10 Flow Module

Damage from corrosive liquids. In case of a spillage inside the cuvette module, use
Should the Dosing System be out of use for a lens cleaning cloth or an equivalent lint-free cloth.
more than a week, the Dosinos should be dis- Wet the lens cloth or lens tissue with water and
connected from the dosing units in order to pre- gently wipe out the module. Wet a further cloth with
vent corrosion. The dosing units should then be ethanol to remove any residual water, as well as any
rinsed and emptied (see section 7.3.4 below). water-insoluble residue.
The module’s electrical contacts (gold-plated, situ-
Refer to the Dosino’s instruction manual (Metrohm ated inside the cuvette module as well as on the
Doc. No. 8.800.8002) for more maintenance and module’s main connector) cant be wiped gently
troubleshooting advice. using an ethanol-soaked Q-tip.

7.3.4 Dosing Units NOTICE

Risk of damage to the FM-10 flow module
The Metrohm 807 Dosing Units are automatic Never use the following compounds to clean the
burets and, as such, are the only electronic compo- cuvette module:
nent of the Dosing System to be in contact with the
sample and/or the additives. • organic solvents (e.g. toluene, hexane, ace-
tone, chloroform)
If aggressive reagents are used with dosing units,
then the units should be rinsed with distilled water • strong acids or bases (e.g. nitric acid, sulfuric
and subsequently emptied. This is particularly acid, hydrochloric acid, caustic soda)
important if the dosing unit is not in use for more • strong mechanical action (steel brush)
than 2 days, because even water can corrode the
buret glass during prolonged periods of disuse.
Additionally, when the period of disuse is longer
7.3.6 Cleaning the Omega Cuvettes
than a week, the Dosinos must be disconnected
The cleaning procedure is the same for all Omega
from the dosing units and stored separately.
cuvette types:

NOTICE 1. Flush three times with purified water using a

syringe with the tip inserted into one of the sam-
• Dosing units require regular inspections and ple ports (see Fig. 7-1).
must be disassembled down to the cylinder
unit from time to time and cleaned.
• Monthly or even weekly inspections are nec-
essary when corrosive or high-concentration
reagents are used.

The following steps have to be performed for the

maintenance of the dosing units:
1. Cleaning of the dosing cylinder and the dosing
piston
2. Cleaning of the valve disc and distributor disc
Fig. 7-1: Flushing the Omega cuvette with purified water

38 D51IB009EN-F
 7 Upkeep and Cleaning

using a 1 mL syringe.
7.4 Software Administration
2. Flush with dry, clean compressed air until all
traces of moisture have disappeared. • Ensure that the computer connected to the
instrument meets the specified minimum
3. Store in a clean, dry place protected from dust.
requirements.

NOTICE • Install mandatory software and firmware

Risk of damage to the Omega cuvettes updates when provided by your local Anton
Never use organic solvents (e.g. toluene, Paar representative
hexane, acetone, chloroform) to clean an
Omega cuvette. Never use ultrasound to clean
an Omega cuvette. 7.5 Wetted Parts
The following materials are in contact with samples
and/or additives. Note that the wetted parts of the
cuvettes are listed in the Litesizer Series Reference
Guide (Doc. No. D51IB010).

Table 7-1: Sample & Additive Wetted Parts

Material Part

Glass • pH electrode
• Amber glass additive bottles

Borosilicate glass 3.3 (ISO 3585) • 807 Dosing unit: dosing cylinder
• Titration vessel

Polyethylene terephtalate, glycol-modified 807 Dosing unit: housing and centering tube
(PETG)

Polytetrafluoroethylene (PTFE) • 807 Dosing unit: dosing piston

• Stirring bars

Silicone carbide ceramic 807 Dosing unit: valve disc

Al2O3 ceramic 807 Dosing unit: distributor disc

Ethylene tetrafluoroethylene (ETFE) • 807 Dosing unit: distributor channels

• Anti-diffusion buret tip
• Buret tip

Fluorinated ethylene propylene (FEP) • 807 Dosing unit: M6 tubing

• Anti-diffusion buret tip
• Buret tip

Polyether ether ketone (PEEK) • PEEK adapter 10/32

• PEEK adapter M6

C-Flex® thermoplastic elastomer C-Flex® tubing

Polycarbonate Luer hose adapters

D51IB009EN-F 39
7 Upkeep and Cleaning

7.6 Storing and Transporting the • Empty the hoses, beakers, and measuring cell
before you move or lift the instrument.
Instrument • The instrument must be transported in the origi-
nal package and packed according to the sup-
• Store the instrument under clean conditions that
plier's instructions. During transport, the
fulfill the ambient conditions provided in the
instrument must not be exposed to intense
specifications chapter.
shocks or high forces.
• When not in use, the pH electrode should be
stored according to section 7.3.1.

40 D51IB009EN-F
 8 Maintenance and Repair

8 Maintenance and Repair

8.1 Repair Performed by an Authorized Following parts are generally excluded from the
warranty (wear and tear parts):
Anton Paar Representative • Hoses
In case your instrument needs repair, contact your • Adapters, connectors, fittings
local Anton Paar representative, who will take care
• Glass parts
of the necessary steps. If your instrument needs to
be returned, request an RMA (Return Material Au- • pH electrode
thorization Number). It must not be sent without the
• Piston parts
RMA and the filled “Safety Declaration for Instru-
ment Repairs”. Please make sure it is cleaned • Disc parts
before return.
• Cables
TIP : Find the contact data of your local Anton Paar
• Fuses
representative on the Anton Paar website (http://
www.anton-paar.com) under “Contact”.

D51IB009EN-F 41
Appendix A: Technical Data

Appendix A: Technical Data

pH Module For full technical specifications of the dosing units,
refer to the 807 Dosing Unit instruction manual
For full technical specifications of the pH module (Metrohm Doc. No. 8.807.8002), chapter 6,
refer to the 867 pH Module instruction manual pages 40 to 42.
(Metrohm Doc. No. 8.867.8003), chapter 7,
pages 34 to 38. pH Electrode
Stirrer The technical specifications of the pH electrode are
detailed in the table below:
For full technical specifications of the stirrer refer to
the 801 Stirrer instruction manual (Metrohm Table A-2: Technical specifications of the pH
Doc. No. 8.801.8001), chapter 4, pages 11 and 12. electrode

Dosinos Electrolyte flow rate < 2 µL/h

For full technical specifications of the Dosinos refer Diaphragm Fixed ground-
to the 800 Dosino instruction manual (Metrohm joint diaphragm
Doc. No. 8.800.8002), chapter 9, pages 37 and 38.
Min. immersion depth 1 mm
Dosing Units
Indicator electrode shape Flat membrane
The dosing units give the Dosing System its dosing
accuracy, which fulfills the requirements of the ISO/ pH range 0 - 13
EN/DIN standard 8655-3 "Volume measurement
Membrane resistance < 2000
instruments with pistons - Part 3: Piston
burets". This corresponds to the following permissi- Reference electrolyte type KCl 3 M
ble limit values:
Resistance 5 kΩ
Table A-1: Dosing Unit Accuracy According to
ISO 8655-3 Part 3 Shaft diameter 12 mm

Electrode slope > 0.97

Cylinder volume 5 mL

Max. systematic measurement ± 0.3 % Temperature range 0 - 60 °C

deviation (%) Electrode zero point ± 15 mV
Max. systematic measurement ± 15 µL Max. installation length 125 mm
deviation (vol.)
Reference system LL system
Max. permissible measurement ± 0.1 %
deviation (%) Shaft material Glass

Max. permissible measurement ± 5 µL Plug-in head Metrohm plug-in

deviation (vol.) head G

42 D51IB009EN-F
 Appendix B: Specification Sheet

Appendix B: Specification Sheet

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D51IB009EN-F 43