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Copyright 2012 BTG Instruments GmbH
All rights reserved. No part of this manual may be copied, photocopied,
published, reproduced, translated or converted into electronic or machine-
readable form without the prior written approval of BTG Instruments GmbH.

Subject to technical modifications.


BTG Instruments GmbH, September 2012
Printed in Germany
List of contents

List of contents

Chapter Paragraph Title Page

I. Basic safety 1.1 Manufacturers liability . . . . . . . . . . . . . . . . . . . . . . . 7


instructions 1.2 Intended applications . . . . . . . . . . . . . . . . . . . . . . . 8
1.3 Illegitimate use . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
1.4 Qualification of personnel . . . . . . . . . . . . . . . . . . . . 8
1.5 General safety directions. . . . . . . . . . . . . . . . . . . . . 9
1.6 Informal safety directions . . . . . . . . . . . . . . . . . . . . 9
1.7 Spare parts and expendables . . . . . . . . . . . . . . . . . 9
1.8 Symbols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.9 Packaging & transport . . . . . . . . . . . . . . . . . . . . . . . 10

II. Product description 2.1 Theoretical background . . . . . . . . . . . . . . . . . . . . . . 11


2.1.1 Measuring principle . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.1.2 Calculation of charges . . . . . . . . . . . . . . . . . . . . . . . 13
2.1.3 Determination of the isoelectric point . . . . . . . . . . . 14
2.1.4 Titrations curves . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.4.1 Colloidally dissolved particles . . . . . . . . . . . . . . . . . 14
2.1.4.2 Solid particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.1.4.3 Heterogeneous stock systems . . . . . . . . . . . . . . . . 15
2.2 System applications . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3 Designation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.3.1 Type plate PCD-04 (Travel). . . . . . . . . . . . . . . . . . . 16
2.3.1.1 Type plate titration module . . . . . . . . . . . . . . . . . . . 16
2.3.2 Service sticker PCD-04 (Travel) . . . . . . . . . . . . . . . 16
2.4 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.5 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
2.5.1 PCD-04 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
2.5.2 PCD-04 Travel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

III. Layout and functions 3.1 Description of PCD-04 (Travel) . . . . . . . . . . . . . . . . 19


3.1.1 Measuring cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
3.1.2 pH set (optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

IV. Installation 4.1 Safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23


4.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 23
4.3 Preparations onsite . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.4 Installation environment . . . . . . . . . . . . . . . . . . . . . 23
4.4.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.4.2 External power pack . . . . . . . . . . . . . . . . . . . . . . . . 23
4.4.3 Sample specification . . . . . . . . . . . . . . . . . . . . . . . . 24
4.5 Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.5.1 Titrants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.5.2 Acids/ bases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.5.3 Cleaning solution . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.6 Startup of PCD-04 . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.6.1 Manual operation. . . . . . . . . . . . . . . . . . . . . . . . . . . 27

MtekTM PCD-04 (Travel) Operation Manual 3


BTG Instruments GmbH, September 2012
List of contents

Chapter Paragraph Title Page

4.6.2 Operation with an external titrator . . . . . . . . . . . . . 28


4.6.2.1 Preparing dosing hoses . . . . . . . . . . . . . . . . . . . . . 28
4.7 Startup of PCD-04 Travel . . . . . . . . . . . . . . . . . . . . 29
4.7.1 Using SD card . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.7.1.1 Insert SD card. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.7.1.2 Remove SD card . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.7.2 Preparing dosing hoses . . . . . . . . . . . . . . . . . . . . . 29
4.7.3 Inserting titrant bottles . . . . . . . . . . . . . . . . . . . . . . 30
4.7.4 Rinsing the dosing hoses . . . . . . . . . . . . . . . . . . . . 31
4.7.5 Operation with external titrator . . . . . . . . . . . . . . . . 32
4.8 pH calibration (optional) . . . . . . . . . . . . . . . . . . . . . 33

V. Measuring 5.1 Safety rules. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35


5.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 35
5.3 Overview touchpanel screens . . . . . . . . . . . . . . . . 35
5.3.1 Screens main level PCD-04 . . . . . . . . . . . . . . . . . . 35
5.3.2 Screens sub level PCD-04/ Setup menu . . . . . . . . 36
5.3.3 Screens main level PCD-04 Travel . . . . . . . . . . . . 37
5.3.4 Screens sub level PCD-04 Travel/ Setup menu . . . 38
5.3.5 Screens sub level PCD-04 Travel/ Titrator menu . . 39
5.3.6 Screens sub level pH calibration (optional) . . . . . . 40
5.4 Preparing the instrument . . . . . . . . . . . . . . . . . . . . 41
5.5 Sample preparation . . . . . . . . . . . . . . . . . . . . . . . . 41
5.5.1 Filtration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.5.2 Centrifugation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.5.3 Screening . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.5.4 Back titration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
5.5.4.1 Example for back titration . . . . . . . . . . . . . . . . . . . . 42
5.6 Measuring with the PCD-04 (Travel) . . . . . . . . . . . 43
5.6.1 PCD-04 Standard . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.6.1.1 Start measurement . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.6.2 PCD-04 Travel . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.6.2.1 Titration with Travel titration module. . . . . . . . . . . . 45
5.6.3 Display/ save results. . . . . . . . . . . . . . . . . . . . . . . . 47
5.6.4 Editing measured values . . . . . . . . . . . . . . . . . . . . 48
5.6.4.1 Editing measured values via SD card. . . . . . . . . . . 48
5.6.4.2 Editing measured values via USB interface . . . . . . 48
5.7 Settings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
5.7.1 Setting titration method. . . . . . . . . . . . . . . . . . . . . . 49
5.7.2 Setting the date . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
5.7.3 Setting the time. . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
5.7.4 Calibrating the touchpanel . . . . . . . . . . . . . . . . . . . 51

VI. Diagnostics and 6.1 Safety rules. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53


troubleshooting 6.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 53
6.3 Table of system faults. . . . . . . . . . . . . . . . . . . . . . . 53
6.3.1 Error messages on the PCD-04 Travel . . . . . . . . . 53

4 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
List of contents

Chapter Paragraph Title Page

6.3.2 Basic faults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

VII. Maintenance 7.1 Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55


7.1.1 Cleaning the instrument . . . . . . . . . . . . . . . . . . . . . 55
7.1.2 Cleaning the measuring cell . . . . . . . . . . . . . . . . . . 55
7.2 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
7.2.1 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 55
7.2.2 Functional testing . . . . . . . . . . . . . . . . . . . . . . . . . . 55
7.2.2.1 Basic test of PCD-04 (Travel) without
measuring cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
7.2.3 Standard titration . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
7.2.4 Checking the streaming potential . . . . . . . . . . . . . . 57
7.2.4.1 Electrostatic charging of the measuring cell . . . . . . 57
7.2.4.2 Functional testing of the pH electrode . . . . . . . . . . . 57
7.3 Yearly LAB Check inspection . . . . . . . . . . . . . . . 57

VIII. Shutting down the 8.1 Safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59


system, storage and 8.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 59
disposal 8.3 Shutting down the system . . . . . . . . . . . . . . . . . . . . 59
8.4 Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
8.5 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
8.5.1 Official Regulations . . . . . . . . . . . . . . . . . . . . . . . . . 59

IX. Parts list 9.1 Spare parts list . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61


9.2 Consumables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
9.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

MtekTM PCD-04 (Travel) Operation Manual 5


BTG Instruments GmbH, September 2012
List of contents

Chapter Paragraph Title Page

6 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
I. Basic safety instructions

I. Basic safety instructions

1.1 Manufacturers liability


Instructions in the operation manual Users are obliged to immediately eliminate any faults
- All users of the Mtek PCD-04 (Travel) have to that may affect operational safety.
observe this operation manual and to strictly
Warranty and liability
adhere to the basic safety instructions and safety
rules in order to ensure safe handling and relia- This instrument was built and tested in accordance
ble operation of the MtekTM PCD-04 (Travel) with EU Guidelines 89/336/EEC and 73/23/EEC. It
- This operation manual contains the most import- complied with all safety regulations at the time it left
ant safety directions to ensure the operational the factory. To maintain this condition and ensure
safety of the Mtek PCD-04 (Travel) safe operation, the user must observe the safety ins-
- In addition, all applicable accident prevention tructions and warning notes contained in this op-era-
regulations have to be met for the specific loca- tion manual. It is the responsibility of the owner and
tion where the device is set up user to make sure that all safety devices and require-
ments concerning the operating environment of the
Obligations of the user
instrument are adequately provided for.
The warranty and the service quality guarantee shall
Basically, the General Terms and Conditions of BTG
only be valid if the following conditions are met:
Instruments GmbH will apply. These will be made
- The Mtek PCD-04 (Travel) may only be ope- available to the operator of the Mtek PCD-04
rated by persons who are proven to have been (Travel) at the latest on the day the sales contract is
thoroughly trained and authorized by BTG Instru-
concluded.
ments GmbH
- The user has to observe all instructions by BTG BTG Instruments GmbH shall not be liable for any
Instruments GmbH regarding operation and warranty or liability claims for personal injury or pro-
maintenance of the Mtek PCD-04 (Travel) perty damage that may be consequential to one or
- Storage and maintenance of the instrument shall several of the following causes:
be in accordance with the instructions given by - Non-legitimated use of the Mtek PCD-04
BTG Instruments GmbH (Travel)
- Use of any parts other than the original spare - Opening of the instrument on the rear or at the
parts and expendables of BTG Instruments bottom plate of the system
GmbH will cause instant termination of warranty, - Inexpert installation/ assembly, commissioning,
availability and guarantee claims operation and servicing of the Mtek PCD-04
- Any faults which may affect operational safety of (Travel)
the system have to be eliminated immediately - Operation of the Mtek PCD-04 (Travel)
- When the system is obviously damaged or parts although its safety devices and protection facili-
inside the system are loose or the system does ties are defective, inexpertly mounted or malfun-
not work, the Mtek PCD-04 (Travel) has to be ctioning
shut down. - Failure of the user/ operator to adhere to the ins-
tructions given in this operation manual regar-
Hazards involved in handling the MtekTM PCD-04 ding transport, storage, assembly,
(Travel) Particle Charge Detector commissioning, operation and maintenance of
The Mtek PCD-04 (Travel) has been built to the Mtek PCD-04 (Travel)
reflect state-of-the-art techniques and to meet recog- - Modifications made to the Mtek PCD-04 (Tra-
nized safety rules. However, its operation may entail vel) without prior approval of BTG Instruments
the risk of accidents for users or third parties or of GmbH
damage to the Mtek PCD-04 (Travel) or to other - Inadequate routine checks of parts/assemblies
property. The Mtek PCD-04 (Travel) shall only be of the Mtek PCD-04 (Travel) which are sub-
used: ject to wear
- For the intended applications outlined in this - Inexpert repairs
operation manual - Catastrophes caused by the effects of foreign
- When it is in a condition meeting all safety rules objects or by Acts of God

MtekTM PCD-04 (Travel) Operation Manual 7


BTG Instruments GmbH, September 2012
I. Basic safety instructions

Trouble-free and safe operation of the instrument is 1.2 Intended applications


only possible subject to correct transport, storage,
installation and assembly and to careful handling and The Mtek PCD-04 (Travel) shall be used exclusi-
maintenance. vely for the purposes defined in this operation man-
If the Mtek PCD-04 (Travel) is sent in for repair, ual and in the technical description and shall only be
the whole system has to be returned, including mea- operated in conjunction with external instruments
suring cell and displacement piston. and components recommended or approved by BTG
Instruments GmbH.
The guarantee for the Mtek PCD-04 (Travel) is
one year starting as of the date of delivery. The Mtek PCD-04 (Travel) Particle Charge
Detector shall solely be used for charge identification
Regarding defects covered by the guarantee, BTG
of aqueous samples and for determining their iso-
Instruments GmbH shall not be liable for any dam-
electric point. The instrument is exclusively intended
ages exceeding the cost price.
for indoor use.
The guarantee shall only extend to parts found
Since any other or further-reaching application is
defective by BTG Instruments GmbH. The company
considered illegitimate by BTG Instruments GmbH,
is entitled to decide whether such parts are to be
the company shall not be held liable for damages
exchanged or repaired provided the parts have been
resulting from such use.
returned in time to the nearest authorized retailer of
BTG Instruments GmbH.
This guarantee does not extend to parts that have To comply with the intended applications as defined
been repaired or modified by the user/ operator above, the user/ operator is required
without the prior written approval of an authorized - To follow all the instructions in this operation
retailer of BTG Instruments GmbH. manual and
BTG Instruments GmbH neither assumes any obliga- - To perform all inspection and maintenance tasks
tion in connection with the sale of the instrument nor as specified
has it instructed any other person to undertake such
obligation. 1.3 Illegitimate use
Caution Illegitimate use (misuse) is defined as follows:
Any changes or modifications not expressly appro- - Any usage other than the allowed usage defined
ved by the party responsible for compliance could above or extending beyond the defined usage
void the users authority to operate the equipment. - Failure to follow the instructions given in this
operation manual
Disclaimer of liability - Failure to observe the safety directions
BTG Instruments GmbH has checked the contents of - Failure to remedy immediately - i.e. before conti-
the printed manual for consistency with the hardware nuing operation of the instrument - any defect
& software described. However, since deviations which might endanger its operational safety and
cannot be entirely excluded, BTG Instruments GmbH reliability.
does not accept responsibility for absolute consis- - Any unauthorized modification to the instrument
tency. The contents of this manual are regularly revi-
sed and any corrections that may be necessary will 1.4 Qualification of personnel
be included in later issues.
The instrument may be commissioned and operated
only by qualified personnel. Qualified personnel as
BTG Instruments GmbH reserves the right to make
defined in the safety instructions of this operation
technical changes to this document.
manual are persons trained and instructed by BTG
Instruments GmbH.

8 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
I. Basic safety instructions

1.5 General safety directions 1.8 Symbols


For all installation, operation, maintenance and The following symbols and notices are used in this
repair work performed on the Mtek PCD-04 (Tra- operation manual to designate hazards or to provide
vel) Particle Charge Detector, it is essential that the special information:
directions given below be followed:
Information
- Installation and operation have to be performed
by trained personnel "Information" includes tips for operators and provides
- Maintenance work described in this manual shall useful information.
exclusively be carried out by trained staff It helps you make optimum use of all functions of the
- Maintenance and repair work not described in Mtek PCD-04 (Travel).
this manual shall only be performed by BTG In-
struments GmbH or by personnel trained by an Hint
authorized service agent of BTG Instruments "Hint" refers to expert handling and operation of the
GmbH Mtek PCD-04 (Travel).
- When working on electrical and electronic parts, Non-adherence to these hints may lead to operatio-
be sure to power off the instrument at the main nal failures of the Mtek PCD-04 (Travel) or to
switch and to disconnect the power plug
trouble in its environment.
- When replacing defective parts, make sure to
use only original spare parts and expendables Caution
- When handling hazardous materials, please "Caution" refers to a potentially dangerous situation.
observe the directions for protective equipment, Failure to observe this information may result in slight
industrial hygiene and proper disposal
personal injury or in damage to equipment.

1.6 Informal safety directions Warning


"Warning" refers to the risk of accidents.
Take care to keep this operation manual handy at all
Failure to observe this information may result in
times on the Mtek PCD-04 (Travel). In addition,
severe damage to health or even in life-threatening
make sure that documentation on general and local
injuries.
accident prevention and environmental protection
standards is near at hand and strictly adhered to.

Keep all safety instructions and warnings on the


Mtek PCD-04 (Travel) in a legible condition and
replace, if necessary.

1.7 Spare parts and expendables


Be sure to use exclusively original spare parts and
expendables to ensure operational safety of the
Mtek PCD-04 (Travel) and to safeguard your gua-
rantee claims. Please order these items from your
local authorized representative of BTG Instruments
GmbH.

MtekTM PCD-04 (Travel) Operation Manual 9


BTG Instruments GmbH, September 2012
I. Basic safety instructions

1.9 Packaging & transport


The Mtek PCD-04 (Travel) Particle Charge
Detector is a compact and sturdy unit for which an
aluminium trolley is available to enable measure-
ments on site.
The Mtek PCD-04 Travel can be transported with
installed titrant bottles.

Information
It is recommended ordering the aluminium trolley to
avoid transport damage.

Hint
The aluminium trolley is unsuitable for rail forwarding
or postal delivery of the instrument.
- To exclude transport damage, never put any
additional items in the trolley
- To avoid transport damage to the precision cont-
act pins, do not keep any small components in
the measuring chamber. Before transport, take
the measuring cell off its guide and place it in its
compartment in the trolley.
- At outdoor temperatures below +15 C [59F], let
the unit adjust to ambient temperature after
transport before putting it into operation
Hint
If the Mtek PCD-04 Travel is exposed to tempera-
tures below 0C, the titrants might freezing causing
damage to the bottles and tubes. Therefore do not
leave the instrument in the trunk of your car at cold
weather.

10 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
II. Product description

II. Product description

2.1 Theoretical background


Whether a suspension of particles or a true solution Streaming potential
of large molecules, most materials dispersed in water If a liquid is forced along a particle surface under
carry an electric charge. pressure, it will shear off the counter-ions of the dif-
In such an aqueous system charges at solid/ liquid or fuse layer and an electric field is built up. The resul-
liquid/ liquid interfaces play a crucial role. ting electric current is picked up by two electrodes
They cause reaction mechanism of the type found in and is either indicated by a streaming current signal
dispersions, suspensions or emulsions. or converted to a potential. The Mtek PCD-04
Measuring the streaming potential gives information (Travel) Particle Charge Detector displays the poten-
about interactions of the components in water and is tial in mV. The sign of the measured value indicates
used to assess the stability of a system. whether the sample carries a positive (cationic) or
negative (anionic) charge. The streaming potential is
Double layer a relative value and depends on various influential
Once a particle is dispersed in water it develops a factors, such as
charge at the particle surface which affects the distri-
bution of the dissolved ions in the water. This results - Dimensions of the measuring cell
in an increased concentration of ions of opposite - Cleanliness of the cell
charge to that of the particle close to its surface. Clo- - Conductivity
sest to the surface a stationary layer of counter-ions - Chemical properties of the sample
forms; further away a diffuse layer surrounds the par- - Molecular weight
ticle. Thus each particle carries an electrical double
- Particle size
layer. Such a double layer can only be formed by
- pH
particles at least 1 nm in size, the so-called colloids.
- Viscosity
Electrokinetic effect - Temperature
A relative movement of a liquid to a dispersed mate-
rial generates an electrokinetic effect. If an electric To quantify the charges of a sample, a titration with
field or a pressure is applied, the solid particles are an oppositely charged titrant (polyelectrolyte) has to
caused to move relative to the liquid electrolyte or be performed up to the point where a streaming
vice versa. Depending on which of the phases is potential of 0 mV is reached.
moving, the electrokinetic effect can be identified via
There is a correlation between streaming potential
- Electrophoresis and zeta potential, which latter has been identified by
- Electroosmosis electrophoresis. In actual practice, however, a com-
- Sedimentation potential parison of the two potentials is seldom possible and if
- Streaming potential at all, only under defined ideal conditions.

MtekTM PCD-04 (Travel) Operation Manual 11


BTG Instruments GmbH, September 2012
II. Product description

2.1.1 Measuring principle


Streaming potential measurements with the Mtek
PCD-04 (Travel) are based on the principle shown
schematically in Fig. 2-1. The central element is a 6
plastic measuring cell (4) with a fitted displacement 1
piston (5).
5
If an aqueous sample is filled into the measuring cell,
colloidally dissolved molecules will adsorb at the pla-
stic surface of the displacement piston and on the
cell walls under the action of van-der-Waal forces.
The micro-sized counter-ions remain comparatively 4
free to move.
2
A defined narrow gap is provided between cell wall
and displacement piston. Driven by a motor (6), the
displacement piston (5) oscillates in the measuring 3
cell (4) and creates an intensive liquid flow which Fig. 2-1 Schematic of test setup
entrains the free counter-ions, thus separating them
from the adsorbed sample material.
Designations
At the built-in electrodes (3), the counter-ions induce 1 Display 4 Plastic measuring cell
a current which is evaluated digitally (2) before it is 2 Electronic 5 Displacement piston
shown on the display (1) as streaming potential with 3 Electrodes 6 Motor
the appropriate sign.

12 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
II. Product description

2.1.2 Calculation of charges

Polyelectrolyte titration If the charge level is to be identified for an active sub-


For quantitative charge measurements of the stance (starch, wet strength agent) or for solids (pig-
sample, a polyelectrolyte titration has to be conduc- ment slurry), the mass of the product should
ted which uses the streaming potential to identify the additionally be included in the calculation to obtain
point of zero charge (0 mV). the so-called specific charge density.
To this end, add an oppositely charged polyelect-
rolyte of known charge level to the sample as a tit- Calculation of the specific charge density
rant.
The specific charge density q [eq/g] is calculated by
the following formula:
The titrant charges neutralize existing charges of the
sample. Titration is stopped as soon as the point of V*c
zero charge (0 mV) is reached. q=
m
The titrant consumption obtained in ml forms the
basis for further calculations.
V: Consumed titrant volume [l]
Provided equal samples are titrated under identical c: Titrant concentration [eq/l]
conditions, the consumed titrant volumes can be m: Solids of sample or its active substance [g]
directly compared. Normally, however, the charge q: Specific charge density [eq/g]
level present in aqueous samples is expressed in
terms of the anionic or cationic demand in eq/l.
Example:
Calculation of cationic/ anionic demand A 10 ml sample of a 0.1% Ti02 suspension contains
The cationic or anionic demand [eq/l] of a sample is 0.01 g solids at m = 0.01 g.
calculated by the following formula: The consumption of cationic polyelectrolyte up to the
point of zero charge is 2.5 ml for a titrant concentra-
C1 * V1 tion of 0.001 N.
C2 =
V2 The specific charge density is the following:

C1: Concentration of titrant in [N] or [eq/l] 0.0025 [l] * 0.001 [eq/l]


C2: Concentration of the titrated sample in [eq/l] q= = 250 * 10-6 [eq/g]
V1: Titrant consumption in [l] 0.01 [g]
V2: Sample volume to be titrated in [l]
250*10-6 eq/g or 0.250 meq/g or 250 eq/g
Example:
10 ml filtrate of an anionic fiber suspension is pipet- By multiplying the specific charge density in eq/g by
ted into the measuring cell of the Mtek PCD-04 the Faraday's constant F = 96485 C/eq, the total
(Travel) and titrated with a 0.001 N Poly-Dadmac
charge in C/g will be obtained.
solution until the point of zero charge is reached. In
the example, 5 ml cationic polyelectrolyte (Poly-Dad-
mac) is required.

The cationic demand of the sample is the following:

0.001 eq/l * 0.005 l


C2 = = 0.0005 eq/l
0.01 l

0.0005 eq/l or 0.5 meq/l or 500 eq/l

MtekTM PCD-04 (Travel) Operation Manual 13


BTG Instruments GmbH, September 2012
II. Product description

2.1.3 Determination of the isoelectric point 2.1.4 Titrations curves

Acid/ base titration Information


Apart from charge measurements, the Mtek PCD- The Mtek PCD-04 Travel continuously generates
04 lends itself to identifying the isoelectric point (IEP) a titration curve while performing a sample titration.
of dispersions. Otherwise titration curves can only be obtained if the
Mtek PCD-04 (Travel) is operated together with
The IEP is the pH-dependent point of zero charge of an external titrator, the associated software and a
a particle. printer.
Titration curves are basically difficult to interpret,
because the curve progression does not exclusively
By adding a titrant (acid/ base) drop by drop, the
reflect the sample material, but rather the adsorption
samples pH is shifted until the isoelectric point (stre-
behaviour of the sample at the surface of the measu-
aming potential = 0 mV) is reached.
ring cell. This is why the curve progression should
not be taken as a basis for the discussion of results.
Cationic samples are titrated with a base and anionic Instead, under certain conditions, the curves provide
samples with an acid up to the point of 0 mV. information about the nature of the sample under
test. The titration curves shown in the following may
roughly be associated with different stock systems:
Hint
The isoelectric point can only be identified if the 2.1.4.1 Colloidally dissolved particles
Mtek PCD-04 (Travel) is used in combination with
Titration curve obtained for a colloidally dissolved
an external titrator. sample.
At the onset of titration, the streaming potential
remains essentially unchanged, since the non-adsor-
bed colloids are neutralized and do not therefore
contribute toward the generation of a streaming
IEP potential.
Later on, the streaming potential undergoes a sharp
drop, which is indicative of the fact that adsorbed
charge carriers are neutralized at the cell wall and
piston.

Fig. 2-2 Schematic of isoelectric point

Fig. 2-3 Colloidally dissolved particles

14 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
II. Product description

2.1.4.2 Solid particles 2.2 System applications


Titration curve for an aqueous suspension of par-
Papermaking
ticles.
Here the titration curve is nearly linear, because all - Improved machine running by controlling anionic
solid particles contribute toward the creation of a trash
streaming potential. - Improved retention control
- Enhanced chemical performance
- Stable paper quality
Effluent treatment
- Optimized chemicals by controlled flocculant
dosages
- Increased dry content of sludges through impro-
ved dewatering
- Exact identification of the demulsification point of
emulsions and cooling lubricants
- Optimized selection of flocculants
Filler/ pigment processing
- Determination of the optimum dispersed condi-
tion and of dispersant dosages
- Selective flocculation of particles after identifica-
tion of the isoelectric point

Fig. 2-4 Suspended solids Other applications


An identification of charges is also very important for
producers from the beverage and food industry and
2.1.4.3 Heterogeneous stock systems
in the ceramics, dyes, cosmetics and pharmaceuti-
Titration curve of heterogeneous systems (colloids, cals sectors. In all these areas the Mtek PCD-04
dissolved material, solid particles, fibres etc.). (Travel) is finding increasing application.
After dropping sharply at the beginning, the curve
flattens out toward the end of titration.
The buffer effect around the point of zero charge may
be caused by the fact that titrant is included in the fib-
res.

Fig. 2-5 Heterogeneous stock systems

MtekTM PCD-04 (Travel) Operation Manual 15


BTG Instruments GmbH, September 2012
II. Product description

2.3 Designation
Hint 2.3.2 Service sticker PCD-04 (Travel)
Check if a legible type plate (below) is provided on You will find a service sticker on the right side wall of
the rear panel of the device. Please replace if il- the instrument. It shows the date of the last functional
legible or missing. inspection of the Mtek PCD-04 (Travel) together
with a recommended date for the next service.
2.3.1 Type plate PCD-04 (Travel)
The following type plate Fig. 2-6 is provided on the
rear panel of the instrument:

BTG Instruments GmbH


Herrsching / Germany
S/N: 440-0102
TEL:(+49) 8152 9312-0 Typ: PCD-04
FAX:(+49) 8152 9312-900 U: 24 VDC
www.btg.com

. I: 1.88 A
MADE IN GERMANY

Fig. 2-8 Service sticker

Fig. 2-6 Type plate PCD-04 (Travel) with FCC label

2.3.1.1 Type plate titration module


The integrated titration module of the Mtek PCD-
04 Travel is labelled with the additional type plate
Fig. 2-7. It is located on the rear panel of the titration
module:

BTG Instruments GmbH


Herrsching / Germany
S/N: 441-0103
TEL:(+49) 8152 9312-0 Typ: PCD-04
FAX:(+49) 8152 9312-900 TRAVEL UNIT
www.btg.com

.
MADE IN GERMANY

Fig. 2-7 Type plate titration module PCD-04 Travel


with FCC label

16 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
II. Product description

2.4 Technical data

Dimensions - MtekTM PCD-04: 160 mm wide x 215 mm deep x 340 mm high


- MtekTM PCD-04 Travel: 160 mm wide x 225 mm deep x 370 mm high

Weight - MtekTM PCD-04: approx. 6.5 kg


- MtekTM PCD-04 Travel: approx. 8.7 kg

Power supply - External power pack


Input: 100-240 VAC; 1.5 A; 50-60 Hz

Service conditions - Ambient temperature: +15C up to +40C


- Storage/ transport temperature: +5C up to +40C

Measured variables - Streaming potential in mV


- pH

Results - Anionic & cationic demand


- Charge density
- pH

Sample volume - 10-60 ml

Outputs - Streaming potential (+/- 2500 mV)


- Consumption of titrant on the touchpanel of Mtek PCD-04 Travel
- pH on the touchpanel of Mtek PCD-04 (Travel) with pH measure-
ment option
- USB interface of Mtek PCD-04 Travel
- SD card of Mtek PCD-04 Travel

Operating modes - MtekTM PCD-04


Manual: Hand pipette
Automatic: External MtekTM PCD-T3 Titrator

- MtekTM PCD-04 Travel


Automatic: Integrated titration module or
external MtekTM PCD-T3 Titrator

Reproducibility - Rel. standard deviation SD(x):


(results obtained by titration of Pes-Na against Poly-Dadmac)
- < 0.3% (MtekTM PCD-04 Travel)
- < 0.1% (MtekTM PCD-04 combined with MtekTM PCD-T3 Titrator)

Detection limit Up to 1 ppm depending on sample specification

Standards - MtekTM PCD-04 DIN EN 61326, DIN EN 61010


- MtekTM PCD-04 Travel DIN EN 301489-1
DIN EN 301489-3
DIN EN 60950
DIN EN 300330

Safety Protection class I

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BTG Instruments GmbH, September 2012
II. Product description

2.5 Scope of delivery

2.5.1 PCD-04 2.5.2 PCD-04 Travel

Standard delivery Standard delivery

Qty Item Qty Item


1 MtekTM PCD-04 1 MtekTM PCD-04 Travel
1 Measuring cell 1 Measuring cell
1 Displacement piston 1 Displacement piston
1 External power pack incl. power cable 1 External power pack incl. power cable
1 Piston brush 1 Piston brush
1 Cationic titrant bottle 2 Cationic titrant bottle
1 Anionic titrant bottle 2 Anionic titrant bottle
1 Screen for filtrating fibre suspensions 1 Screen for filtrating fibre suspensions
1 Instructions for use of standard polyelec- 1 SD card
trolytes
1 Instructions for use of standard polyelec-
1 Test printout of standard titration trolytes
1 Operation manual 1 Test printout of standard titration
1 Recommended test procedure 1 Operation manual
1 Recommended test procedure

Optional Optional
Qty Item Qty Item
1 Precision pipette, 2-10 ml 1 Precision pipette, 2-10 ml
1 Aluminium trolley 1 Aluminium trolley
1 pH set for MtekTM PCD-04 1 pH set for MtekTM PCD-04
- pH electrode - pH electrode
- 2 x buffer 4.01 single dose solution - 2 x buffer 4.01 single dose solution
- 2 x buffer 7.00 single dose solution - 2 x buffer 7.00 single dose solution
- 2 x buffer 9.21 single dose solution - 2 x buffer 9.21 single dose solution
- Beaker for pH electrode 10 ml - Beaker for pH electrode 10 ml
2 Refillable titrant bottles

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BTG Instruments GmbH, September 2012
III. Layout and functions

III. Layout and functions

3.1 Description of PCD-04 (Travel)


The Mtek PCD-04 Particle Charge Detector is
available as a standard version (PCD-04) or with 16
integrated titration module (PCD-04 Travel). 15
14

13

12

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

Fig. 3-1 Front view PCD-04 Fig. 3-2 Front view PCD-04 Travel

Designations
1 Dosing hose holder 9 Measuring chamber
2 Displacement piston 10 Latch for touchpanel
3 Measuring cell 11 Touchpanel
4 Guide for measuring cell 12 Bottle holder (hinged)
5 Beaker for pH electrode (optional) 13 Latch for titrant bottle
6 Holder for beaker 14 Anionic titrant bottle
7 Connection for pH electrode 15 Cationic titrant bottle
8 Contact pins 16 Dosing hoses

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BTG Instruments GmbH, September 2012
III. Layout and functions

7 8

4
6 3

2
1

Fig. 3-3 Rear panel PCD-04/ PCD-04 Travel

Deignations
1 Connection to external power pack 5 SD card slot
2 ON/ OFF switch 6 USB interface
3 Output pH 7 Service sticker
4 Output streaming potential 8 Type plate

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BTG Instruments GmbH, September 2012
III. Layout and functions

3.1.1 Measuring cell 3.1.2 pH set (optional)


Standard delivery of the Mtek PCD-04 (Travel) When equipped with the optionally available pH set,
includes a precision measuring cell and a displace- the Mtek PCD-04 (Travel) identifies not only the
ment piston. Fitted in the measuring cell are two pla- charge level but also the pH of a sample. In combina-
tinum electrodes for identifying the streaming tion with a Mtek PCD-T3 Titrator, the instrument
potential. determines the isoelectric point of a sample via the
pH electrode.
Install the pH electrode in the measuring cell on the
wall opposite the dosing hoses, i.e. at a maximum
distance from the hose tips.

2
3
Fig. 3-4 Measuring cell and displacement piston 4

Fig. 3-5 Measuring cell and pH electrode

Designations
1 Electrode cable with A2 connector
2 Plexiglass shaft
3 Clip
4 Ceramic diaphragm
5 Electrode cap

The pH electrode should immerse in the sample


solution. If necessary, sample volume for isoelectric
point measurements could be increased by adding
water. Do not use water to dilute the sample for pH
measurements! Use more sample material or mea-
sure the pH outside of the measuring cell.

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III. Layout and functions

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BTG Instruments GmbH, September 2012
IV. Installation

IV. Installation

This chapter covers the installation of the Mtek 4.4.2 External power pack
PCD-04 (Travel) Particle Charge Detector and the
necessary preparations. In the course of installation, Hint
all required settings have to be made. Before starting the instrument, check if the local
mains voltage is identical to that indicated on the
4.1 Safety rules type plate.
The Mtek PCD-04 (Travel) is equipped with an
Please adhere to the applicable safety rules during external power pack in the form of a PFM controller
preparatory work and when commissioning the which connects to all power voltages within the range
system. indicated on it.
Information
4.2 Personnel requirements
If the touchpanel no longer responds to your touch,
The Mtek PCD-04 (Travel) may only be installed do a panel reset as follows:
by qualified and skilled personnel. Turn off the Mtek PCD-04 (Travel).
Touch the touchpanel with your finger at an opti-
4.3 Preparations onsite onal point.
Turn on the Mtek PCD-04 (Travel) again and
Prior to installation of the Mtek PCD-04 (Travel), keep your finger on the touchpanel until "Calibra-
all preparations mentioned in chapter 4.4 "Installation tion screen" is displayed (after approx. 5 s).
environment", page 23 must be made and the ambi- Recalibrate the touchpanel.
ent conditions met.
Allow the Mtek PCD-04 (Travel) to adapt to ambi-
Input voltage: 100 - 240 VAC
ent temperature before commissioning.
Frequency: 50 - 60 Hz
In the room where the device is set up, electrical
4.4 Installation environment installations must conform to current regulations
Be sure to connect the power pack to an appro-
4.4.1 Installation site ved earthed socket
Do not undo any earthing contacts
Hint
The guarantee by BTG Instruments GmbH expi-
To warrant safe and reliable operation of the res if the device is used with an inappropriate
Mtek PCD-04 (Travel), check on the following voltage or if it is not connected to the external
conditions before commissioning the instrument: power pack that comes with the instrument

Ambient temperature: +15C up to +40C


Place the device on a stable and flat surface
The room where the Mtek PCD-04 (Travel) is
set up must be clean and dry
Do not operate the device while it is exposed to
direct sunlight
Never use the instrument when it is or was direc-
tly exposed to water
Never use the device in explosion prone rooms
Never use the instrument if it is or was exposed
to aggressive chemical substances
If you notice the presence of condensed water
either during transport or after storage, allow
approx. two hours before turning on the instru-
ment

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BTG Instruments GmbH, September 2012
IV. Installation

4.4.3 Sample specification

General Particle sizes


Basically, nearly every aqueous sample - including Solid particle sizes in a sample should not exceed
original concentrations - can be measured. The mea- 500 m. The minimum detectable limit value is 1 nm.
surability of a sample may be verified by the Mtek
PCD-04 (Travel) Particle Charge Detector. To this Viscosity
end, fill a sample into the measuring cell, install the Suitable for measurement are all samples with a vis-
cell together with the displacement piston in the cosity below 6000 mPa*s. Viscosities exceeding this
Mtek PCD-04 (Travel) and turn on the motor. value impede the oscillating movement of the dis-
Measurement may be started as soon as the motor placement piston in the measuring cell. This restric-
runs smoothly and silently and the signal keeps com- tion is still aggravated by the flocculation effect
paratively stable (at approx. 50 mV). typically occurring toward the end of titration.

The limit values indicated in this chapter are not Accordingly, samples with a viscosity exceeding
absolute values, but are merely indicative of sample 6000 mPa*s should conveniently be diluted with de-
characteristics that might lead to measuring pro- ionized water.
blems.
If highly viscous samples are to be titrated, mixing
If there are doubts about whether or not a substance the titrant with the sample takes longer than with low-
can be measured, conduct a test measurement and, viscosity samples.
if necessary, condition the sample accordingly.
Molecular weight
Solvents
The minimum molecular weight of polyelectrolytes to
Charge measurement is possible after functional be tested should be at approx. 300 g/mol, since with
groups are dissociated. Since this dissociation can smaller molecules, their adsorption on the cell wall by
only take place in aqueous solutions, the substance van-der-Waal forces is no longer ensured. Ions pre-
to be tested must be available in this form or be dis- sent in a sample due to dissolved inorganic salts are
persed in water. below the detection limit.

If required, the substance to be tested may be dissol- At the upper end of the scale, there is no limiting
ved in lower alcohols (methanol, ethanol, isopro- molecular weight of colloidally dissolved substances.
panol) before it is diluted with de-ionized water for
subsequent titration.

The proportion of organic solvents depends on the


sample and should be determined in pretests. To
begin with, a blank reading should be obtained for
the solvent concerned. For this purpose, fill 10 ml of
the solvent (de-ionized water or a water/ alcohol mix-
ture) into the measuring cell and titrate up to the
point of zero charge.

Even if the cell is filled with de-ionized water only, the


streaming potential will not be at 0 mV as might be
expected, but will show a comparatively high anionic
signal. This signal drops to zero as soon as a mini-
mum amount of a cationic titrant is added.
If de-ionized water is titrated, approx. 0.02 ml Poly-
Dadmac is normally required.

The blank value thus obtained is to be deducted from


the results of all further titrations.

24 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
IV. Installation

Conductivity 4.5 Solutions


The conductivity of a sample decisively impacts the
streaming potential: the higher the conductivity, the 4.5.1 Titrants
lower the electrical resistance in the sample will be
Titrants must always carry the opposite charge of the
and the more the streaming potential will decrease
without, however, influencing the titration results. sample.
The sample concentration (dilution) should optimally
be selected to keep the titrant consumption between
0.2 and 10 ml.
Polyelectrolytes
BTG Instruments GmbH recommends the use of
Pes-Na and Poly-Dadmac as standard reagents,
since their charge densities are practically pH-inde-
pendent.
Pes-Na
Pes-Na (polyethene sodium sulfonate) is an anionic
polyelectrolyte serving as a calibrating substance to
determine the content of other titrants.
Poly-Dadmac
Poly-Dadmac (polydimethyl diallyl ammonium chlo-
ride) is a cationic polyelectrolyte.
For technical reasons, the activity of Poly-Dadmac is
Fig. 4-1 Conductivity vs. streaming potential subject to minor variation between individual
batches. Before using a fresh solution, apply Pes-Na
to conduct a factor determination.
In Fig. 4-1, various different NaCl proportions were
added to Pes-Na 0.001 N and the samples were titra- Consumption of Poly-Dadmac 0.001 N is usually bet-
ted with Poly-Dadmac 0.001 N. ween 9.75 and 10.25 ml for 10 ml Pes-Na 0.001 N.

Hint Other polyelectrolytes


If conductivities are excessively high (20 mS/cm - 50 The following additional titrants are in frequent use
mS/cm), the streaming potential may fluctuate be- today:
tween anionic and cationic so than an endpoint
detection and thus titration is no longer possible. In Cationic:
these cases, reduce the conductivity by diluting the - Methyl glycol chitosan (MGCh) 'Hymin'
sample with de-ionized water. Anionic:
Information - Potassium polyvinyl sulphate (PVSK)
Samples that do not meet the above specifications - Sodium dodecyl sulfate (SDS)
may be prepared as outlined in chapter 5.5 "Sample Information
preparation", page 35.
For the Mtek PCD-04 (Travel), BTG Instruments
GmbH supplies titrant bottles containing Poly-Dad-
mac, Pes-Na and PVSK in the concentrations 0.001
N and 0.0001 N.

4.5.2 Acids/ bases


Use diluted acids as titrants for anionic samples, and
diluted bases for cationic samples.
Hydrochloric acid, sulphuric acid and sodium hydro-
xide solution have proven useful in this context and
are normally applied in concentrations of 0.1 - 0.01
mol/l.

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BTG Instruments GmbH, September 2012
IV. Installation

4.5.3 Cleaning solution

Warning
Acetone and the cleaning solution are highly
inflammable.

Warning
Please follow the safety instructions in chapter 1.5
"General safety directions", page 9.

The cleaning solution for manual cleaning of the


measuring cell of the Mtek PCD-04 (Travel) is
produced from 50 parts sodium bromide (NaBr) and
50 parts acetone plus 125 parts water.
Prepare the above proportions.
Fill water into a suitable vessel.
Add sodium bromide and dissolve.
Hint
Take care that sodium bromide dissolves completely.
Add acetone and mix gently.
Information
Selection of an optimum detergent depends on the
sample concerned.

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IV. Installation

4.6 Startup of PCD-04


The Mtek PCD-04 measures the streaming The titrant consumption is visible on the measuring
potential of an aqueous sample. To detect its charge pipette. Based on consumption, the charge level is
level a titration is performed until reaching a stream- quantitatively calculated especially in the case of a
ing potential of 0 mV. Titration may be performed polyelectrolyte titration.
manually or better with help of an automatic titrator.
If you conduct an acid/ base titration with the
4.6.1 Manual operation Mtek PCD-04, the pH display indicates the iso-
For manual operation of the Mtek PCD-04 Parti- electric point (at 0 mV streaming potential).
cle Charge Detector, use a measuring pipette to
Information
transfer titrant drop by drop into the measuring cell.
The endpoint, i.e. the point of zero charge, is rea- Manual titration with a measuring pipette should
ched when the streaming potential is at 0 mV. solely be carried out for pretests.

Fig. 4-2 Manual operation

Designation
1 Measuring pipette

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BTG Instruments GmbH, September 2012
IV. Installation

4.6.2 Operation with an external titrator 4.6.2.1 Preparing dosing hoses


The figure below shows the Mtek PCD-04 Install the dosing hoses from the external titrator in
together with a Mtek PCD-T3 automatic titrator. their rest position as illustrated below.

MtekTM PCD-T3

Dosing hose holder

Fig. 4-5 Dosing hoses in rest position (front view)

MtekTM PCD-04
Information
Before starting measurement, rinse the dosing hoses
Fig. 4-3 PCD-04 combined with PCD-T3 as specified in the operation manual of the Mtek
PCD-T3 Titrator.
To work with the external titrator, the Mtek
PCD-04 has to transmit the streaming potential and,
in the case of an acid/ base titration, the pH to the
titrator.
The required cabling is illustrated in the figure below:

Streaming
pH potential

Fig. 4-4 Cabling PCD-04 with PCD-T3

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IV. Installation

4.7 Startup of PCD-04 Travel


The Mtek PCD-04 Travel measures the stream- 4.7.1.2 Remove SD card
ing potential of an aqueous sample. To detect its Switch off the MtekTM PCD-04 Travel using the
charge level a titration is performed until reaching a
power switch on the back side of the unit.
streaming potential of 0 mV. Titration may be perfor-
med either with the integrated titration module or with Remove the SD card from the memory card slot
an external titrator. see Fig. 4-6 (push-to-pull mechanism).
Hint
4.7.1 Using SD card
You may not remove or exchange the SD card, when
The Mtek PCD-04 Travel displays up to 100 the MtekTM PCD-04 Travel:
results on its touchpanel. Much more data can be
stored on the provided memory card (SD card).
- Is switched on
Information - Is in the write mode: "Writing on SD card!"
The SD card must be installed before switching on - Is in the read mode: "Loading data from SD
the Mtek PCD-04 Travel, otherwise all data will card!"
be lost on power-off.
Switch on the MtekTM PCD-04 Travel for further
Information usage.
The SD card delivered with the Mtek PCD-04 Tra-
vel is a SAN DISK. Do not use other SD cards. 4.7.2 Preparing dosing hoses
When working with integrated titration module, install
4.7.1.1 Insert SD card the dosing hoses as shown below:
Switch off the MtekTM PCD-04 Travel using the
power switch on the back side of the unit.
Insert the SD card in the memory card slot on the
Mtek PCD-04 Travel as shown below:

Fig. 4-7 Dosing hoses shown installed (rear view)

Insert the dosing hoses in rest position in their holder


(see Fig. 4-8).

Fig. 4-6 SD card

Switch on the MtekTM PCD-04 Travel for further Dosing hose holder
usage.

Fig. 4-8 Dosing hoses in rest position (front view)

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BTG Instruments GmbH, September 2012
IV. Installation

4.7.3 Inserting titrant bottles Shake the titrant by folding the bottle holder up
and down several times.
With the Mtek PCD-04 Travel, screw in the titrant
bottles in their holder as shown in Fig. 4-9. - Shake the titrant each time the instrument
has been left unused for several days
Hint Fold up the bottle holder until it clicks into place.
Be sure to install the bottles in the correct position as
indicated by the + and - signs. Caution
Never unscrew the bottles with the bottle holder in
Caution folded-up position, since this would allow the liquid to
Never use acids or bases in the titration module. drain.

Checking & setting titrant parameters


1 When the titrant bottles have been installed, the tit-
rant parameters have to be entered manually.
Procedure
Turn on the Mtek PCD-04 Travel.
In the main menu select "Titrator".
This will bring up the following screen:

3
4

Fig. 4-9 Inserting titrant bottles The two output fields (white boxes) show the follo-
wing titrant parameters:
- Name: titrant used
Designations
- Best Before: use-by-date
1 Latch
- Factor: correction factor
2 Bottle holder
- Normality: concentration
3 Cationic titrant bottle
4 Anionic titrant bottle
Exit the screen by touching "MENU".
Touch one of the output fields to set the titrant
Press latch (1) to unlock and fold down bottle
parameters manually.
holder (2).
Screw in titrant bottles (3 & 4) from below into the
bottle holder as shown in Fig. 4-9.
Hint
Screw in the bottles with the labels facing to the
front and the triangle on the bottle coinciding with
the triangle on the instrument.

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BTG Instruments GmbH, September 2012
IV. Installation

- Depending on which field has been touched, 4.7.4 Rinsing the dosing hoses
one of the following displays will come up:
Hint
Before starting measurement, check if the dosing
hoses are filled bubble-free.
Procedure
Turn on the Mtek PCD-04 Travel.
In the main menu select "Titrator".
- This brings up the following screen:

- You may rinse the two titrant bottles in 1 ml


steps from 1 - 10 ml.
To select the desired rinsing volume, touch the
associated field.
Press "Start" to trigger the rinsing cycle.
Hint
Before starting the rinsing function, please check the
liquid level of the titrant bottles.
After touching a field you may make entries as
desired:
- Name: 7-letter-name
- Best before: use-by date
- Factor: correction factor, default = 1
- Normality: any from 0.01 - 0.0001
Press "OK" in order to save your entries and exit
the screen.
To exit the screen without saving, press
"MENU" or "ESC".

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IV. Installation

4.7.5 Operation with external titrator


The figure below shows the Mtek PCD-04 Travel To control the external titrator, the Mtek PCD-04
together with an external titrator Mtek PCD-T3. Travel has to transmit the streaming potential - and in
Before turning on the Mtek PCD-04 Travel, fold the case of an acid/ base titration, the pH - to the tit-
down the bottle holder. This deactivates the integra- rator. The required cabling is illustrated in the figure
ted titration module so that the Mtek PCD-04 Tra- below.
vel will function like a Mtek PCD-04.

MtekTM PCD-T3

Streaming
potential
pH

Fig. 4-11 Cabling of PCD-04 Travel and PCD-T3

MtekTM PCD-04 Travel

Fig. 4-10 PCD-04 Travel with PCD-T3

Information
Before starting measurement, rinse the dosing hoses
as outlined in the operation manual of the Mtek
PCD-T3 Titrator.

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IV. Installation

4.8 pH calibration (optional)


Hint - This will open one of the following screen dis-
plays:
If the Mtek PCD-04 (Travel) is connected to an
external titrator Mtek PCD-T3, the calibration of
the pH electrode has to be repeated on the titrator.
Hint
If you use the Mtek PCD-04 Travel with integra-
ted titration module, the pH electrode only serves for
identifying the pH of the sample.

For calibration, use two commercial buffer solutions,


one of them with pH 7.0 and the other with pH 4.01
or pH 9.21.
Information
The buffers used for calibration should correspond to
the pH range of the samples.

Procedure
In the main menu, select "Setup".
In the Setup menu touch "Calibrate pH" and the
screen shown below will appear.
Depending on the range of the second buffer
solution you wish to use, touch the appropriate
field (acid pH 4.01 or alkaline pH 9.21).

Immerse the pH electrode in the pH 7.00 buffer


solution and select "Start".

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BTG Instruments GmbH, September 2012
IV. Installation

Wait until the displayed mV value has stabilized - This brings up one of the following screen dis-
before you select "OK". plays:
- Depending on your preselection, one of the
following screens will come up:

Confirm calibration by pressing "OK".


Then immerse the pH electrode in a buffer solu- Repeat calibration if the slope is beyond the
tion with pH 4.01 or pH 9.21 and press "Start". range of -50 and -65 mV/pH.
Wait until the displayed value has stabilized and
select "OK".

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V. Measuring

V. Measuring

5.1 Safety rules


Be sure to follow the chapter I. "Basic safety instructi-
ons", page 7, before commissioning the Mtek
PCD-04 (Travel).

5.2 Personnel requirements


Only qualified and skilled personnel are allowed to
operate the Mtek PCD-04 (Travel).

5.3 Overview touchpanel screens


Information
The touchpanel is equipped with a screen saver
which automatically appears after 20 min. To deacti-
vate the screen saver just touch the screen.

Information
The pH display shown on the following screens is
only available to users who have ordered the option
"pH Set" with the instrument.

5.3.1 Screens main level PCD-04

Start screen

Measure screen Main menu Setup menu

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BTG Instruments GmbH, September 2012
V. Measuring

5.3.2 Screens sub level PCD-04/ Setup menu

for servicing only

Setup menu

Measure screen Master code keypad

Date keypad
Menu for pH calibration

Time keypad

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V. Measuring

5.3.3 Screens main level PCD-04 Travel

Start screen

Keyboard for sample name Measure screen

Result list Main menu Diagram screen

Titrator menu Setup menu Method menu

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V. Measuring

5.3.4 Screens sub level PCD-04 Travel/ Setup menu

for servicing only

Setup menu

Measure screen Master code keypad

Date keypad
Menu for pH calibration

Time keypad

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V. Measuring

5.3.5 Screens sub level PCD-04 Travel/ Titrator menu

Titrant screen Titrant screen

MtekTM PCD-04 (Travel) Operation Manual 39


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V. Measuring

5.3.6 Screens sub level pH calibration (optional)

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V. Measuring

5.4 Preparing the instrument


Start the Mtek PCD-04 (Travel) (see 4.6 5.5.2 Centrifugation
"Startup of PCD-04", page 27). The centrifugation period must be identical for all
Clean the measuring cell and the displacement samples.
piston (see 7.1.2 "Cleaning the measuring cell",
page 55). 5.5.3 Screening
In the majority of cases, it will be sufficient to sepa-
5.5 Sample preparation rate long fibres and larger particles by means of a
nylon screen.
For stock systems including both colloidally dissolved
material and solid particles, different ways of sample
preparation will give different data on the charge con- Quick and reproducible sampling is achieved by
ditions prevailing in a sample (see 4.4.3 "Sample immersing a Mtek filtration beaker with screen in
specification", page 24). the sample and removing the supernatant liquid with
Generally speaking, results are only directly com- a measuring pipette.
parable if the samples are prepared in an identical
manner. Test results obtained for samples of the
same kind but which were treated by different
methods may yield additional information about,
e.g., the charge conditions of solids.
1
In each case, quantitative sampling must be ensured
to obtain reproducible values.

5.5.1 Filtration
To separate larger solid particles from a sample, a
whiteband filter is normally used. However, this may
falsify results because polyelectrolytes tend to be
adsorbed at the filter paper. We therefore strongly
3
advise against using paper filters.

The use of ceramic filters by comparison is normally


problem-free.

Fig. 5-1 Screening of samples

Designations
1 Rising measurable sample
2 Original sample, e.g. thick stock, coated broke
3 Filtration beaker with 300 m screen

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V. Measuring

5.5.4 Back titration Calculation of charge density q:


This method of sample preparation suggests itself in (V2 - V1) * c
the following cases:
q=
m
- Due to their structure, the samples cannot be
transferred to the cell directly which would V2 - V1: The difference between the charges of
enable quantitative determination of the charge the fresh Poly-Dadmac and the reacted
level of larger particles Poly-Dadmac indicates the charge
- The reaction of the substance to be tested with amount neutralized in the sample.
the titrant is too slow for direct titration
c: Concentration of the titrant,
5.5.4.1 Example for back titration here 0.001 eq/l
Sample
m: 2 g of the original sample were used for
The total charge of an anionic solid sample is to be
determined. In view of the high solids content or titration. (20 g were filled up to 100 g of
excessive particle sizes, direct measurement in the which 10 g were used for titration.)
measuring cell is not feasible. Instead, back titration
is recommended. (0.01068 - 0.00483) [l] * 0.001 [eq/l]
q=
Procedure 2 [g]
Take 20 g of the anionic sample to be measured and
fill up to 100 g with Poly-Dadmac 0.001 N. Stir this q = 2.925 * 10-6 [eq/g]
mixture for approx. 2 hours with a magnetic stirrer.
During this period, the cationic Poly-Dadmac will
neutralize all anionic charges of the sample. Since Result: The charge of the sample under test is
there is an excess amount of Poly-Dadmac, a resi- 2.925 eq/g.
dual cationic charge will remain in the sample.

After the reaction period, remove the solids from the


mixture by screening. Pipette 10 ml of the solution
into the measuring cell and titrate up to the point of
zero charge with Pes-Na 0.001 N.

Result V1: Consumed Pes-Na 4.83 ml

In addition, titrate 10 ml of fresh Poly-Dadmac solu-


tion with Pes-Na up to the point of zero charge.

Result V2: Consumed Pes-Na 10.68 ml

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V. Measuring

5.6 Measuring with the PCD-04 (Travel)


Preparation Hint
Fill a sample into the measuring cell. The pH electrode should immerse in the sample
solution. If necessary, sample volume for isoelec-
tric point measurements could be increased by
adding water. Do not use water to dilute the
sample for pH measurements! Use more sample
material or measure the pH outside of the measu-
ring cell.
To measure pH with the Mtek PCD-04 Travel
it is best to determine the pH value outside the
measuring cell, e.g. in a small beaker. Start the
pH measurement before you start the automatic
titration.

Install the dosing hoses as illustrated below.


Fig. 5-2 Measuring cell and displacement piston - The hose tips should be immersed in the
solution
Information
Since both electrodes inside the measuring cell
must be covered with liquid, the sample volume
should be at least 10 ml. To precisely dose the
sample volume for charge calculation, weigh in
the sample or use a measuring pipette.

Information Dosing hose holder


Good reproducibility of results is only achieved if
the sample is appropriately homogenized for
quantitative sampling.
Insert the displacement piston in the measuring
cell. Fig. 5-3 Dosing hoses installed ready for titration
In the Mtek PCD-04 (Travel), move the mea-
suring cell along the guide up to the stop.
Lift displacement piston upward and turn clock-
wise to lock it in the bayonet catch.
- The measuring cell is correctly positioned if
the displacement piston can be hooked in the
bayonet catch easily and without canting
If applicable, install pH electrode in the measu-
ring cell (see 3.1.2 "pH set (optional)", page 21).
Hint
Position the pH electrode such as to prevent tit-
rant from directly dripping onto it.

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V. Measuring

5.6.1 PCD-04 Standard 5.6.2 PCD-04 Travel


Switch on Mtek PCD-04.
TM
Switch on MtekTM PCD-04 Travel.
- Following screen appears: - Following screen appears:

Fig. 5-4 Measuring screen PCD-04 or PCD-04 Fig. 5-5 Measuring screen PCD-04 Travel
Travel with no active titration module and with activated titration module and
with option pH measurement with option pH measurement

The following values and functions are available: The following values and functions are available:
Potential Indicates the current streaming poten- Potential Indicates the current streaming poten-
tial. The value is reduced in steps tial. The value is reduced in steps
when adding titrant. when adding titrant.
On/ Off toggle button for indication of On/ Off toggle button for indication of
streaming potential. streaming potential.
pH Indicates the current pH, if the pH Titrant Shows the current titrant consumption.
measurement option has been cho- When the streaming potential has
sen. gone through the point of zero charge,
titration is finished and the consumed
Start/ Stop toggle button for pH mea-
amount of titrant is displayed.
surement.
Start/ Stop toggle button
5.6.1.1 Start measurement - "Start" starts titration
Press the button "On" on the left side of the mV - "Stop" stops titration in case of fai-
display "Potential". lure
- This will cause the displacement piston to pH Indicates the current pH, if the pH
oscillate and the streaming potential to be dis- measurement option has been cho-
played in mV sen.
Wait for approximately 30 seconds until the sig-
nal has stabilized. Start/ Stop toggle button for pH mea-
Use a pipette to dose oppositely charged titrant surement.
until point of zero charge 0 mV is reached (see Sample Pressing the "Sample Name" button
4.6.1 "Manual operation", page 27). Name brings up keyboard for insert of
Note down dosage amount ml and pH value at sample name.
point of zero charge as your measuring result.
Information
Result is not stored.

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V. Measuring

5.6.2.1 Titration with Travel titration module

Information Touch "OK" to go back to the "Measure screen".


When using an external titrator, please consult the Touch "MENU" in order to return to main
menu and select "Setup" to enter the setup menu
associated operation manual. The following proce-
(see menu tree 5.3.3).
dure refers to the use of Mtek PCD-04 Travel with
Select a titration method (1 = standard method).
activated titration module.
- Touch on the method number to change it
To start sample measurement:
Enter the samples name
Select a method
Switch on the potential measurement
Start addition of titrant

All steps are described as follows:


Starting from the measure screen, enter sample
name by touching the field (see Fig. 5-5) to the
right side of "Sample Name".
- The system suggests the last given sample
name
- This brings up the keyboard screen:

Fig. 5-6 Setup menu

- This brings up the keyboard screen for typing


in a method number 1-9

Information
To create/reprogramm your own method enter the
method menu from the main menu screen (see
5.7.1 "Setting titration method", page 35).
Touch "MEASURE" in order to return to the
measure menu.

Type the desired sample name which will simul-


taneously be entered in the results list.

Specifically, the following functions are available:


Switches between capital and small
letters

ESC Cancels the last entry and returns you


to the Measure screen
Deletes the last character

Confirmation and exit from entry


mode Touch "On" to the left side of the mV display
"Potential".
Information - This will cause the displacement piston to
You may enter or modify a sample name until you oscillate and the streaming potential to be dis-
actually start addition of titrant. played in mV

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BTG Instruments GmbH, September 2012
V. Measuring

Wait for approximately 30 seconds until the sig-


nal has stabilized. - The Mtek PCD-04 Travel stops as soon
Touch "Start" to the left side of the ml display as 0 mV is reached
"Titrant".

- The titration is performed automatically by Information


using an oppositely charged titrant Since the displacement piston continues its os-
cillating movement, the streaming potential may
change. This is a normal effect without any influ-
ence on measurement results.
Press "Off" (to the left of the "Potential" field) to
stop the displacement piston from oscillating.

- A titration curve is generated continuously


To look at the titration curve choose "Diagram" in
the "Measure screen".

Press "MEASURE" to go back to the "Mea-


sure screen".

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V. Measuring

5.6.3 Display/ save results

Information The following functions are available:


The following procedure refers to the use of Mtek Button for scrolling in the results list
PCD-04 Travel with activated titration module. up and down, line by line.
Using MtekTM PCD-04 standard, all results (ml-titrant
consumption and end pH-value) have to be note
down.
Information Button for skimming through the
When using an external titrator, please consult the results list by page up and down.
associated operation manual. Several titrators are
equipped with printer interface which will allow prin-
ting out the results.

Shown on the screen is a listing of all measurement


results up to a total of 100. If you insert an SD card in
the slot on the rear panel of the Mtek PCD-04
Travel before switching on the instrument, the results
listing remains saved on the card after the instrument
is turned off.

To see the results list, proceed as follows:

In the main menu, choose "Results".


- This opens the following screen:

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V. Measuring

5.6.4 Editing measured values

5.6.4.1 Editing measured values via SD card 5.6.4.2 Editing measured values via USB inter-
face

Hint Hint
Measured values can only be edited when working Measured values can only be edited when working
with the Mtek PCD-04 Travel with integrated titra- with the Mtek PCD-04 Travel with integrated titra-
tion module. tion module.

The following values may be edited: The following values may be edited:
- Serial number - Serial number
- Date - Date
- Time - Time
- Factor anionic - Factor anionic
- Factor cationic - Factor cationic
- Sample name - Sample name
- Potential - Potential
- Consumption - Consumption
- Equivalent - Equivalent
- pH - pH

In order to manipulate the measurement values on Hint


your computer, please use a card reader or install
the card in the SD slot of your computer. Measured To manipulate on your computer the measured
values are edited in MS Excel format. values edited at the USB interface, you have to
install a USB driver. Please consult a BTG service
Information technician in this context.
The Excel columns are separated by commas.

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V. Measuring

5.7 Settings

5.7.1 Setting titration method Following functions are available:


To set/change parameters of a titration method pro- Method 1:Method 900 is preset as default
ceed as follows: method. Methods 2-9 are available
Select the Method menu from the main menu for userdefined programming.
screen.
Increment Titration interval
Enter the pass word "4711".
here: 1 unit every 3 seconds
- This will bring up the following screen:
dE(set) presets mV-threshold for changing
from maximum increment dV(max) to
minimum increment dV(min) dosage.
here: if the potential value varies
more than 8 mV with one increment
dosage, the increment amount will
change from
dV(max)= 0,100 ml to
dV(min)= 0,010 ml.
dV(min) Minimum increment amount in ml,
changeable by arrows left/right
dV(max) Maximum increment amount in ml,
changeable by arrows left/right
Pump "Automatic" selects the oppositely
Information charged titrant solution automatically
The Method menu is used to programm specific according to mV-sign (+/-).
methods. Selecting a method for measuring the right "Left" pumps from the left titrant
method number has to be set in the Setup menu (see installed.
Fig. 5-6 "Setup menu", page 35). "Right" pumps from the right titrant
installed.

ESC Aborts method programming.

Termination and storing of created


method.

Information
For fix incremental dosage (non-dynamic titration),
set amount dV(min) = dV(max).

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V. Measuring

5.7.2 Setting the date 5.7.3 Setting the time


To set the date, proceed as follows: To set the time, proceed as follows:
In the Setup menu, select "Date". In the Setup menu, select "Time".
- This will bring up the following screen: - This will bring up the following screen:

Following functions are available: The following functions are available:

Modifies the date format: Use buttons 0 to 9 to enter the time


DD.MM.YY
DD.MM.YY as an uninterrupted 4-digit value
- DD.MM.YY
- MM/DD/YY (no break character in between).

Use buttons 0 to 9 to enter the date Deletes the value entered last.
as an uninterrupted 6-digit value
(no break character in between). Exits time entry mode without
ESC
Deletes the value entered last. accepting the current time and
returns you to Setup menu.

Exits date entry mode without Exits time entry mode and saves
ESC
ESC
accepting the current date and the entered time. Returns to Setup
returns you to Setup menu. menu.

Exits date entry mode and saves


the entered date. Returns you to
Setup menu.

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V. Measuring

5.7.4 Calibrating the touchpanel


You may calibrate the touchpanel to suit your perso-
nal finger touch. This will facilitate the use of the
touchpanel e.g. by right- or left-handers.

To calibrate the touchpanel, proceed as follows:


Hint
To calibrate, touch the cross with your finger. If
you touch another point, the touchpanel will be
deactivated and can only be reactivated by the
following procedure (see below).
Turn off the Mtek PCD-04 (Travel).
Touch the touchpanel with your finger at an opti-
onal point.
Turn on the Mtek PCD-04 (Travel) again and
keep your finger on the touchpanel until "Calibra-
tion screen" is displayed (after approx. 5 s).

Touch the small cross.


- This will move the cross to another position
Touch the cross repeatedly until calibration is
automatically finished.
If the prompt "Save Calibration?" appears, select
"Yes".
- The system returns you to the measure
screen

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V. Measuring

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VI. Diagnostics and troubleshooting

VI. Diagnostics and troubleshooting

6.1 Safety rules 6.2 Personnel requirements


If errors occur that are not listed in the table below, Troubleshooting may only be performed by qualified
disconnect the Mtek PCD-04 (Travel) and tag it and skilled personnel.
as "defective". Contact BTG Instruments GmbH to
ensure quick corrective action.

6.3 Table of system faults

6.3.1 Error messages on the PCD-04 Travel

Error message Cause Corrective action


Information: - No SD card inserted Switch off Mtek PCD-04 Travel
No SD card and install SD card.
- Without a SD card installed, no
data will be stored
Warning: - Maximum titrant volume of 20 Verify correct position of anionic
No endpoint detected ml reached and cationic titrant.
Sample concentration too high,
dilute sample.
Verify that dosing hoses are
immersed in sample.
Rinse dosing hoses thoroughly to
remove air bubbles.
Anionic polyelectrolyte: - 14 days left until use-by date Prepare exchange of anionic tit-
Best before: Date rant bottle.

Cationic polyelectrolyte: - 14 days left until use-by date Prepare exchange of cationic tit-
Best before: Date rant bottle.

Anionic polyelectrolyte: - Use-by date expired Replace anionic titrant bottle.


Use-by date expired!
Cationic polyelectrolyte: - Use-by date expired Replace cationic titrant bottle.
Use-by date expired!

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VI. Diagnostics and troubleshooting

6.3.2 Basic faults


The following basic faults may be experienced with the Mtek PCD-04 (Travel) also when used in combination
with an external titrator:

Problem Cause Solution


Bad or no touch response of - Touchpanel calibration out of Turn off the Mtek PCD-04
the touchpanel range (Travel) and touch the touchpanel
with your finger at an optional
point.
Turn on the Mtek PCD-04
(Travel) again and keep your fin-
ger on the touchpanel until "Cali-
bration screen" is displayed (after
approx. 5 s).
Re-calibrate the touchpanel.
Heavy fluctuations of strea- - Excessive conductivity of the Dilute sample.
ming potential after sample sample
is filled in
- Insufficient sample volume in mea- Weigh in once again or use
suring cell pipette.
- High solids in the sample Dilute the sample or centrifuge/
screen it to remove coarse par-
ticles.
Potential reverses after - Very slow reaction between titrant Titrate more slowly or perform
reaching the endpoint and sample back titration.
If necessary, check sample prepa-
ration for homogeneity.
At the start of titration, - Wrong titrant Select titrant with opposite charge
potential increases instead to that of sample.
of decreasing
- Adsorption equilibrium not attained Proceed slowly with titration.
- Sample concentration too high or Dilute sample.
titrant concentration too low
Potential remains essenti- - Sample concentration very high Dilute sample or use a higher
ally unchanged during titra- strength titrant.
tion
- Wet contacts on Mtek PCD-04 Dry contact pins with a soft cloth.
(Travel)
- Wet electrodes on the outside of Dry electrodes with a soft cloth.
the measuring cell
- Measuring cell contaminated Thoroughly clean measuring cell
and displacement piston.
Sign of displayed potential - Sample charge is pH dependent Check on pH dependence of
not in conformity with sample.
sample specification
- Excessive viscosity Dilute sample.
- Measuring cell contaminated Thoroughly clean measuring cell
and displacement piston.
pH electrode cannot be cali- - pH electrode contaminated or Clean pH electrode, if necessary
brated defective replace it.

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VII. Maintenance

VII. Maintenance

7.1 Cleaning 7.2 Maintenance

7.1.1 Cleaning the instrument 7.2.1 Personnel requirements


Use a soft and lint-free cloth to wipe the outer sur- Maintenance shall exclusively be carried out by qua-
faces of the instrument. Take care not to scratch the lified and skilled personnel.
touchpanel. If contamination persists, moisten the
cloth with soap water. A special cleaning procedure 7.2.2 Functional testing
is required for the measuring cell.
To avoid measuring errors caused by faulty opera-
tion of the instrument or contamination of the measu-
7.1.2 Cleaning the measuring cell
ring cell, functional testing can be performed by
Clean the measuring cell with water and cleaning different methods.
solution only.
After each measuring cycle, go through the following 7.2.2.1 Basic test of PCD-04 (Travel) without
cleaning routine: measuring cell
Turn on power switch (see Fig. 3-3, page 20).
Switch on displacement piston drive.
- A streaming potential of 0 mV will be dis-
played on the touchpanel

Fig. 7-1 Measuring cell and displacement piston

Empty the measuring cell.


Rinse it with water.
Use a brush and cleaning solution (see chapter
4.5.3 "Cleaning solution", page 26) to clean mea-
suring cell and displacement piston.
Rinse both with de-ionized water.
Empty the measuring cell.
Use a clean paper cloth to dry the outside of the
measuring cell - but NOT the inside of the cell or
the displacement piston.
Hint
Failure to clean the measuring cell after each measu-
rement will lead to measuring errors and prevent
reproducibility of results.
To avoid deposits in the measuring cell and on the
replacement piston, fill the freshly cleaned cell with
water and leave overnight.

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VII. Maintenance

7.2.3 Standard titration


- The result of the standard titration will be dis-
General played as follows:
Fill exactly 10 ml of the anionic standard Pes-Na
0.001 N into the the measuring cell and titrate with
Poly-Dadmac 0.001 N up to the point of zero charge.
If the Mtek PCD-04 (Travel) is combined with an
automatic titrator, the consumption of Poly-Dadmac
should be in the range of 9.75 - 10.25 ml.
With the Mtek PCD-04 Travel and activated titra-
tion module a standard titration can be performed
automatically, as described below. Accept the standard titration and start sample tit-
rations by pressing "YES" in the pop-up window.
Procedure If you consider the deviation from the target
In the main menu, touch "Titrator". value too high press "No".
Select 5 ml or 10 ml Pes-Na. - The system will ask for repeating the stan-
dard titration
Information
If you select 5 ml Pes-Na, fill 5 ml de-ionized
water into the measuring cell.
Touch "Start".

Clean the measuring cell thoroughly and


repeat the standard titraton by pressing
"Yes".
- This will cause a return to the Titrator
menu
- By pressing "No" the following screen will open:

- Pes-Na will be dosed into the measuring cell


- After 20 seconds and the titration will start By pressing "Yes" a new correction factor for
Poly-Dadmac will be calculated.
By pressing "No" you will keep on working
with the original correction factor of Poly-Dad-
mac.
Information
A standard titration verifies functionality of the
Mtek PCD-04 (Travel) and checks on the concen-
tation of the used titrants.

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VII. Maintenance

7.2.4 Checking the streaming potential 7.3 Yearly LAB Check inspection
If a freshly cleaned measuring cell is filled with 10 ml
To guarantee reliable measurement from the start,
of anionic standard Pes-Na 0.001 N repeatedly in
succession, the streaming potential measured every Mtek laboratory instrument undergoes tho-
should be roughly identical. Depending on the instru- rough testing before leaving the factory.
ment, the streaming potential is generally around BTGs maintenance program LAB Check keeps
-1600 mV 200 mV. your laboratory device in perfect working order year
after year. Feel free to call in your local service team
If the cell is used very frequently, this value will dimi-
nish over time due to wear. This does not affect titra- or send in your system for factory maintenance.
tion results. To keep track of the next inspection interval, the
However, if the streaming potential suddenly drops Mtek PCD-04 (Travel) indicates following remin-
by several 100 mV from one measurement to the der messages:
next, the measuring cell is probably soiled. To avoid - 2 weeks before the service interval is due, a ser-
measuring errors, clean the cell thoroughly (see vice reminder message will show up, when swit-
chapter 7.1.2 "Cleaning the measuring cell", page ching on the Mtek PCD-04 (Travel):
55).

7.2.4.1 Electrostatic charging of the measuring


cell
When the mV signal remains extremely stable during
the titration process and you are in doubt if the
Mtek PCD-04 (Travel) receives a signal from the
measuring cell, test the instrument functionality as
follows:
Switch on the motor and rub your hand quickly up - When the service date has already been rea-
and down on the outside of the cell. This causes the ched or been exceeded, following message will
signal to bounce. If no such reaction is observed appear, when switching on the Mtek PCD-04
although the motor is running, there is probably an (Travel):
electronics failure. In this case please contact the
Service Department of BTG Instruments GmbH or
your local agent of BTG Instruments GmbH.

7.2.4.2 Functional testing of the pH electrode


Before starting a test series, measure a buffer solu-
tion by means of the pH electrode which should res-
pond within 10-30 seconds. If it does not, clean and
re-calibrate the electrode. If the fault persists, replace
the pH electrode.

MtekTM PCD-04 (Travel) Operation Manual 57


BTG Instruments GmbH, September 2012
VII. Maintenance

58 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
VIII. Shutting down the system, storage and disposal

VIII. Shutting down the system, storage and disposal

8.1 Safety rules 8.4 Storage


Please adhere to the applicable safety rules when Store the Mtek PCD-04 (Travel) in a suitably pro-
shutting down the system. tected place. Do not keep outdoors.

8.2 Personnel requirements 8.5 Disposal


The system shall only be shut down by qualified and
8.5.1 Official Regulations
skilled personnel.
Be sure to meet the current local regulations gover-
ning the disposal of the Mtek PCD-04 (Travel).
8.3 Shutting down the system
To place the Mtek PCD-04 (Travel) out of opera-
tion, proceed as follows:
Turn off the instrument.
Disconnect the instrument from the mains.
If applicable, disconnect the Mtek PCD-04
(Travel) from the titrator.
Clean the measuring cell (see "Cleaning the
measuring cell", page 55).
Hint
The titrant bottles of the MtekTM PCD-04 Travel can
be left installed. This will also avoid drying out of the
diaphragm pumps.

If you use a pH electrode:


Clean the pH electrode with a 3 M KCl solution.
Prevent the diaphragm of the pH electrode (4,
Fig. 3-5) from drying up. Fill the cap of the pH
electrode with 3 M KCl solution and keep the
electrode in this cap in times of disuse.

MtekTM PCD-04 (Travel) Operation Manual 59


BTG Instruments GmbH, September 2012
VIII. Shutting down the system, storage and disposal

60 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
IX. Parts list

IX. Parts list

9.1 Spare parts list

Item Description Part No.


1 Aluminium trolley X20129
2 Measuring cell for MtekTM PCD-04 (Travel) X20240
3 Displacement piston for MtekTM PCD-04 (Travel) X20239
4 Connection cable between MtekTM PCD-04 (Travel) and titrator (BNC/BNC) X02484
for streaming potential and pH transmission
5 External power pack X20266
6 Piston brush for cleaning the measuring cells, d = 20 mm X10158
7 MtekTM filtration beaker with screen, 300 m mesh X18977
8 Precision pipette 2-10 ml X18772
9 Plastic tips for precision pipette 2-10 ml X18773
10 SD card X20055
11 pH electrode, plexiglass shaft, ceramic diaphragm, gel filling, holder X09115
12 Beaker for pH electrode, 10 ml X20241

9.2 Consumables

Item Description Remarks Part No.


1 Poly-Dadmac bottle 0.001 N, 250 ml Ready-to-use titrant for X20399
MtekTM PCD-04 (Travel)
2 Poly-Dadmac bottle 0.001 N, 4x250 ml Ready-to-use titrant for X20406
MtekTM PCD-04 (Travel)
3 Poly-Dadmac bottle 0.0001 N, 250 ml Ready-to-use titrant for X20401
MtekTM PCD-04 (Travel)
4 Poly-Dadmac 0.001 N, 1000 ml Ready-to-use titrant for X10217
MtekTM PCD-04
5 Pes-Na bottle 0.001 N, 250 ml Ready-to-use titrant for X20398
MtekTM PCD-04 (Travel)
6 Pes-Na bottle 0.0001 N, 250 ml Ready-to-use titrant for X20400
MtekTM PCD-04 (Travel)
7 Pes-Na 0.001 N, 1000 ml Ready-to-use titrant for X10216
MtekTM PCD-04
8 PVSK bottle 0.001 N, 250 ml Ready-to-use titrant for X20403
MtekTM PCD-04 (Travel)

MtekTM PCD-04 (Travel) Operation Manual 61


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IX. Parts list

9 PVSK bottle 0.0001 N, 250 ml Ready-to-use titrant for X20404


MtekTM PCD-04 (Travel)
10 2 empty bottles (to be filled with titrants of one labelled anionic, one cationic X20402
the user), 250 ml
11 2 empty bottles (to be filled with titrants of both labelled cationic X20405
the user), 250 ml
12 Buffer solution pH 4.01 X17592
13 Buffer solution pH 7.00 X17593
14 Buffer solution pH 9.21 X17594
15 Acetone commercial quality
16 Sodium bromide (NaBr) commercial quality
17 3 M KCl solution commercial quality
18 Cleaning solution for manual cleaning to be prepared (see 4.5.3 "Cleaning
solution")

9.3 Safety measures

Item* PPE Safety measures after contact Disposal Hazard


(Personal Protec-
tive Equipment)

5/6/7/8/ Goggles Rinse thoroughly with plenty of water after skin Incineration n.a.
9 or eye contact
1/2/3/4 Gloves, Rinse thoroughly with plenty of water after skin Controlled land- n.a.
goggles or eye contact fill or incineration
14/17 Gloves, Rinse with water after skin contact. In case of Special waste Highly inflam-
goggles eye contact rinse with water immediately and meable
consult an eye specialist
15 Gloves, Rinse thoroughly with plenty of water after skin Special waste n.a.
goggles or eye contact
16 Gloves, Rinse with water after skin contact. In case of Special waste Highly inflam-
goggles eye contact rinse with water immediately and meable
consult an eye specialist
*The consecutive numbers in the "Item" column refer
to handling of the expendables listed in chapter 9.2.
Chapter 9.3 shows an excerpt from the Material Saf-
ety Data Sheets (MSDS).

62 MtekTM PCD-04 (Travel) Operation Manual


BTG Instruments GmbH, September 2012
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^~=NM d~ c~W HQV=UNRO=VPNOJVMM KK

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