Operation Manual PCD-04 (Travel) - INVEN Technology ... Screens sub level PCD-04/ Setup menu . . . . . . . . 36 5.3.3 Screens main level PCD-04 Travel . . . . . . . . . . . . 37 5.3.4

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Copyright© 2010 BTG Instruments GmbHAll 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, March 2010Printed in Germany

List of contents

Chapter Paragraph Title Page

List of contents

MütekTM PCD-04 (Travel) Operation Manual 3© BTG Instruments GmbH, March 2010

I. Basic safety instructions

1.1 Manufacturer’s liability . . . . . . . . . . . . . . . . . . . . . . . 71.2 Intended applications . . . . . . . . . . . . . . . . . . . . . . . 81.3 Illegitimate use . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81.4 Qualification of personnel . . . . . . . . . . . . . . . . . . . . 81.5 General safety directions. . . . . . . . . . . . . . . . . . . . . 91.6 Informal safety directions . . . . . . . . . . . . . . . . . . . . 91.7 Spare parts and expendables . . . . . . . . . . . . . . . . . 91.8 Symbols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91.9 Packaging & transport . . . . . . . . . . . . . . . . . . . . . . . 10

II. Product description 2.1 Theoretical background. . . . . . . . . . . . . . . . . . . . . . 112.1.1 Measuring principle . . . . . . . . . . . . . . . . . . . . . . . . . 122.1.2 Calculation of charges. . . . . . . . . . . . . . . . . . . . . . . 132.1.3 Determination of the isoelectric point . . . . . . . . . . . 142.1.4 Titrations curves . . . . . . . . . . . . . . . . . . . . . . . . . . . 142.1.4.1 Colloidally dissolved particles . . . . . . . . . . . . . . . . . 142.1.4.2 Solid particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152.1.4.3 Heterogeneous stock systems . . . . . . . . . . . . . . . . 152.2 System applications . . . . . . . . . . . . . . . . . . . . . . . . 152.3 Designation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162.3.1 Type plate PCD-04 (Travel). . . . . . . . . . . . . . . . . . . 162.3.1.1 Type plate titration module . . . . . . . . . . . . . . . . . . . 162.3.2 Service sticker PCD-04 (Travel) . . . . . . . . . . . . . . . 162.4 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172.5 Scope of delivery. . . . . . . . . . . . . . . . . . . . . . . . . . . 182.5.1 PCD-04 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182.5.2 PCD-04 Travel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

III. Layout and functions 3.1 Description of PCD-04 (Travel) . . . . . . . . . . . . . . . . 193.1.1 Measuring cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 213.1.2 pH set (optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

IV. Installation 4.1 Safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 234.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 234.3 Preparations onsite . . . . . . . . . . . . . . . . . . . . . . . . . 234.4 Installation environment . . . . . . . . . . . . . . . . . . . . . 234.4.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 234.4.2 External power pack . . . . . . . . . . . . . . . . . . . . . . . . 234.4.3 Sample specification . . . . . . . . . . . . . . . . . . . . . . . . 244.5 Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254.5.1 Titrants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254.5.2 Acids/ bases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254.5.3 Cleaning solution. . . . . . . . . . . . . . . . . . . . . . . . . . . 264.6 Startup of PCD-04 . . . . . . . . . . . . . . . . . . . . . . . . . . 274.6.1 Manual operation. . . . . . . . . . . . . . . . . . . . . . . . . . . 27

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4 MütekTM PCD-04 (Travel) Operation Manual© BTG Instruments GmbH, March 2010

4.6.2 Operation with an external titrator . . . . . . . . . . . . . 284.6.2.1 Preparing dosing hoses . . . . . . . . . . . . . . . . . . . . . 284.7 Startup of PCD-04 Travel . . . . . . . . . . . . . . . . . . . . 294.7.1 Using SD card . . . . . . . . . . . . . . . . . . . . . . . . . . . . 294.7.1.1 Insert SD card. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 294.7.1.2 Remove SD card . . . . . . . . . . . . . . . . . . . . . . . . . . 294.7.2 Preparing dosing hoses . . . . . . . . . . . . . . . . . . . . . 294.7.3 Inserting titrant cartridges . . . . . . . . . . . . . . . . . . . . 304.7.4 Rinsing the dosing hoses . . . . . . . . . . . . . . . . . . . . 314.7.5 Operation with external titrator . . . . . . . . . . . . . . . . 324.8 pH calibration (optional) . . . . . . . . . . . . . . . . . . . . . 33

V. Measuring 5.1 Safety rules. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 355.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 355.3 Overview touchpanel screens . . . . . . . . . . . . . . . . 355.3.1 Screens main level PCD-04 . . . . . . . . . . . . . . . . . . 355.3.2 Screens sub level PCD-04/ Setup menu . . . . . . . . 365.3.3 Screens main level PCD-04 Travel . . . . . . . . . . . . 375.3.4 Screens sub level PCD-04 Travel/ Setup menu . . . 385.3.5 Screens sub level PCD-04 Travel/ Titrator menu . . 395.3.6 Screens sub level pH calibration (optional) . . . . . . 405.4 Preparing the instrument . . . . . . . . . . . . . . . . . . . . 415.5 Sample preparation . . . . . . . . . . . . . . . . . . . . . . . . 415.5.1 Filtration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415.5.2 Centrifugation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415.5.3 Screening . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415.5.4 Back titration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 425.5.4.1 Example for back titration . . . . . . . . . . . . . . . . . . . . 425.6 Measuring with the PCD-04 (Travel) . . . . . . . . . . . 435.6.1 PCD-04 Standard . . . . . . . . . . . . . . . . . . . . . . . . . . 445.6.1.1 Start measurement . . . . . . . . . . . . . . . . . . . . . . . . . 445.6.2 PCD-04 Travel . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445.6.2.1 Titration with Travel titration module. . . . . . . . . . . . 455.6.3 Display/ save results. . . . . . . . . . . . . . . . . . . . . . . . 475.6.4 Editing measured values . . . . . . . . . . . . . . . . . . . . 485.6.4.1 Editing measured values via SD card. . . . . . . . . . . 485.6.4.2 Editing measured values via USB interface . . . . . . 485.7 Settings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 495.7.1 Setting titration method. . . . . . . . . . . . . . . . . . . . . . 495.7.2 Setting the date . . . . . . . . . . . . . . . . . . . . . . . . . . . 505.7.3 Setting the time. . . . . . . . . . . . . . . . . . . . . . . . . . . . 505.7.4 Calibrating the touchpanel . . . . . . . . . . . . . . . . . . . 515.7.4.1 Touchpanel reset . . . . . . . . . . . . . . . . . . . . . . . . . . 51

VI. Diagnostics and troubleshooting

6.1 Safety rules. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 536.3 Table of system faults. . . . . . . . . . . . . . . . . . . . . . . 53

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6.3.1 Error messages on the PCD-04 Travel . . . . . . . . . . 536.3.2 Basic faults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

VII. Maintenance 7.1 Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 577.1.1 Cleaning the instrument . . . . . . . . . . . . . . . . . . . . . 577.1.2 Cleaning the measuring cell . . . . . . . . . . . . . . . . . . 577.2 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 577.2.1 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 577.2.2 Functional testing . . . . . . . . . . . . . . . . . . . . . . . . . . 577.2.2.1 Basic test of PCD-04 (Travel) without measuring

cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 577.2.3 Standard titration . . . . . . . . . . . . . . . . . . . . . . . . . . . 587.2.4 Checking the streaming potential . . . . . . . . . . . . . . 597.2.4.1 Electrostatic charging of the measuring cell . . . . . . 597.2.4.2 Functional testing of the pH electrode. . . . . . . . . . . 59

VIII. Shutting down the system, storage and disposal

8.1 Safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 618.2 Personnel requirements . . . . . . . . . . . . . . . . . . . . . 618.3 Shutting down the system . . . . . . . . . . . . . . . . . . . . 618.4 Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 618.5 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 618.5.1 Official Regulations . . . . . . . . . . . . . . . . . . . . . . . . . 61

IX. Parts list 9.1 Spare parts list . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639.2 Consumables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . 64

List of contents






1.1 Manufacturer’s liabilityInstructions in the operation manual- All users of the Mütek™ PCD-04 (Travel) have to

observe this operation manual and to strictly adhere to the basic safety instructions and safety rules in order to ensure safe handling and reli-able operation of the MütekTM PCD-04 (Travel)

- This operation manual contains the most impor-tant safety directions to ensure the operational safety of the Mütek™ PCD-04 (Travel)

- In addition, all applicable accident prevention regulations have to be met for the specific loca-tion where the device is set up

Obligations of the userThe warranty and the service quality guarantee shall only be valid if the following conditions are met:- The Mütek™ PCD-04 (Travel) may only be ope-

rated by persons who are proven to have been thoroughly trained and authorized by BTG Instru-ments GmbH

- The user has to observe all instructions by BTG Instruments GmbH regarding operation and maintenance of the Mütek™ PCD-04 (Travel)

- Storage and maintenance of the instrument shall be in accordance with the instructions given by BTG Instruments GmbH

- Use of any parts other than the original spare parts and expendables of BTG Instruments GmbH will cause instant termination of warranty, availability and guarantee claims

- Any faults which may affect operational safety of the system have to be eliminated immediately

- When the system is obviously damaged or parts inside the system are loose or the system does not work, the Mütek™ PCD-04 (Travel) has to be shut down.

Hazards involved in handling the MütekTM PCD-04 (Travel) Particle Charge DetectorThe Mütek™ PCD-04 (Travel) has been built to reflect state-of-the-art techniques and to meet recog-nized safety rules. However, its operation may entail the risk of accidents for users or third parties or of damage to the Mütek™ PCD-04 (Travel) or to other property. The Mütek™ PCD-04 (Travel) shall only be used:- For the intended applications outlined in this

operation manual- When it is in a condition meeting all safety rules

Users are obliged to immediately eliminate any faults that may affect operational safety.

Warranty and liabilityThis instrument was built and tested in accordance with EU Guidelines 89/336/EEC and 73/23/EEC. It complied with all safety regulations at the time it left the factory. To maintain this condition and ensure safe operation, the user must observe the safety instructions and warning notes contained in this op-eration manual. It is the responsibility of the owner and user to make sure that all safety devices and requirements concerning the operating environment of the instrument are adequately provided for.Basically, the General Terms and Conditions of BTG Instruments GmbH will apply. These will be made available to the operator of the Mütek™ PCD-04 (Travel) at the latest on the day the sales contract is concluded.BTG Instruments GmbH shall not be liable for any warranty or liability claims for personal injury or pro-perty damage that may be consequential to one or several of the following causes:- Non-legitimated use of the Mütek™ PCD-04

(Travel)- Opening of the instrument on the rear or at the

bottom plate of the system- Inexpert installation/ assembly, commissioning,

operation and servicing of the Mütek™ PCD-04 (Travel)

- Operation of the Mütek™ PCD-04 (Travel) alt-hough its safety devices and protection facilities are defective, inexpertly mounted or malfunctio-ning

- Failure of the user/ operator to adhere to the instructions given in this operation manual regar-ding transport, storage, assembly, commissio-ning, operation and maintenance of the Mütek™ PCD-04 (Travel)

- Modifications made to the Mütek™ PCD-04 (Tra-vel) without prior approval of BTG Instruments GmbH

- Inadequate routine checks of parts/assemblies of the Mütek™ PCD-04 (Travel) which are sub-ject to wear

- Inexpert repairs- Catastrophes caused by the effects of foreign

objects or by Acts of God



Trouble-free and safe operation of the instrument is only possible subject to correct transport, storage, installation and assembly and to careful handling and maintenance.If the Mütek™ PCD-04 (Travel) is sent in for repair, the whole system has to be returned, including measuring cell and displacement piston. The guarantee for the Mütek™ PCD-04 (Travel) is one year starting as of the date of delivery. Regarding defects covered by the guarantee, BTG Instruments GmbH shall not be liable for any dam-ages exceeding the cost price.The guarantee shall only extend to parts found defective by BTG Instruments GmbH. The company is entitled to decide whether such parts are to be exchanged or repaired provided the parts have been returned in time to the nearest authorized retailer of BTG Instruments GmbH. This guarantee does not extend to parts that have been repaired or modified by the user/ operator wit-hout the prior written approval of an authorized retai-ler of BTG Instruments GmbH.BTG Instruments GmbH neither assumes any obliga-tion in connection with the sale of the instrument nor has it instructed any other person to undertake such obligation.

CautionAny changes or modifications not expressly appro-ved by the party responsible for compliance could void the user’s authority to operate the equipment.

Disclaimer of liabilityBTG Instruments GmbH has checked the contents of the printed manual for consistency with the hardware & software described. However, since deviations cannot be entirely excluded, BTG Instruments GmbH does not accept responsibility for absolute consis-tency. The contents of this manual are regularly revised and any corrections that may be necessary will be included in later issues.

BTG Instruments GmbH reserves the right to make technical changes to this document.

1.2 Intended applicationsThe Mütek™ PCD-04 (Travel) shall be used exclusi-vely for the purposes defined in this operation man-ual and in the technical description and shall only be operated in conjunction with external instruments and components recommended or approved by BTG Instruments GmbH.The Mütek™ PCD-04 (Travel) Particle Charge Detector shall solely be used for charge identification of aqueous samples and for determining their isoe-lectric point. The instrument is exclusively intended for indoor use.Since any other or further-reaching application is considered illegitimate by BTG Instruments GmbH, the company shall not be held liable for damages resulting from such use.

To comply with the intended applications as defined above, the user/ operator is required- To follow all the instructions in this operation

manual and- To perform all inspection and maintenance tasks

as specified

1.3 Illegitimate useIllegitimate use (misuse) is defined as follows:- Any usage other than the allowed usage defined

above or extending beyond the defined usage- Failure to follow the instructions given in this

operation manual- Failure to observe the safety directions- Failure to remedy immediately - i.e. before conti-

nuing operation of the instrument - any defect which might endanger its operational safety and reliability.

- Any unauthorized modification to the instrument

1.4 Qualification of personnelThe instrument may be commissioned and operated only by qualified personnel. Qualified personnel as defined in the safety instructions of this operation manual are persons trained and instructed by BTG Instruments GmbH.



1.5 General safety directionsFor all installation, operation, maintenance and repair work performed on the Mütek™ PCD-04 (Tra-vel) Particle Charge Detector, it is essential that the directions given below be followed:- Installation and operation have to be performed

by trained personnel- Maintenance work described in this manual shall

exclusively be carried out by trained staff- Maintenance and repair work not described in

this manual shall only be performed by BTG In-struments GmbH or by personnel trained by an authorized service agent of BTG Instruments GmbH

- When working on electrical and electronic parts, be sure to power off the instrument at the main switch and to disconnect the power plug

- When replacing defective parts, make sure to use only original spare parts and expendables

- When handling hazardous materials, please observe the directions for protective equipment, industrial hygiene and proper disposal

1.6 Informal safety directionsTake care to keep this operation manual handy at all times on the Mütek™ PCD-04 (Travel). In addition, make sure that documentation on general and local accident prevention and environmental protection standards is near at hand and strictly adhered to.

Keep all safety instructions and warnings on the Mütek™ PCD-04 (Travel) in a legible condition and replace, if necessary.

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

1.8 SymbolsThe following symbols and notices are used in this operation manual to designate hazards or to provide special information:

Information"Information" includes tips for operators and provides useful information. It helps you make optimum use of all functions of the Mütek™ PCD-04 (Travel).

Hint"Hint" refers to expert handling and operation of the Mütek™ PCD-04 (Travel).Non-adherence to these hints may lead to operatio-nal failures of the Mütek™ PCD-04 (Travel) or to trouble in its environment.

Caution"Caution" refers to a potentially dangerous situation. Failure to observe this information may result in slight personal injury or in damage to equipment.

Warning"Warning" refers to the risk of accidents.Failure to observe this information may result in severe damage to health or even in life-threatening injuries.



1.9 Packaging & transportThe Mütek™ 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 Mütek™ PCD-04 Travel can be transported with installed titrant cartridges.

InformationIt is recommended ordering the aluminium trolley to avoid transport damage.

HintThe 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 con-

tact 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 [59°F], let the unit adjust to ambient temperature after transport before putting it into operation

HintIf the Mütek™ PCD-04 Travel is exposed to tempera-tures below 0°C, the titrants might freezing causing damage to the cartridges and tubes. Therefore do not leave the instrument in the trunk of your car at cold weather.


II. Product description


2.1 Theoretical backgroundWhether a suspension of particles or a true solution of large molecules, most materials dispersed in water carry an electric charge.In such an aqueous system charges at solid/ liquid or liquid/ liquid interfaces play a crucial role.They cause reaction mechanism of the type found in dispersions, suspensions or emulsions.Measuring the streaming potential gives information about interactions of the components in water and is used to assess the stability of a system.

Double layerOnce a particle is dispersed in water it develops a charge at the particle surface which affects the distri-bution of the dissolved ions in the water. This results in an increased concentration of ions of opposite charge to that of the particle close to its surface. Clo-sest to the surface a stationary layer of counter-ions forms; further away a diffuse layer surrounds the par-ticle. Thus each particle carries an electrical double layer. Such a double layer can only be formed by particles at least 1 nm in size, the so-called colloids.

Electrokinetic effectA relative movement of a liquid to a dispersed mate-rial generates an electrokinetic effect. If an electric field or a pressure is applied, the solid particles are caused to move relative to the liquid electrolyte or vice versa. Depending on which of the phases is moving, the electrokinetic effect can be identified via

- Electrophoresis- Electroosmosis- Sedimentation potential- Streaming potential

Streaming potentialIf a liquid is forced along a particle surface under pressure, it will shear off the counter-ions of the dif-fuse layer and an electric field is built up. The resul-ting electric current is picked up by two electrodes and is either indicated by a streaming current signal or converted to a potential. The Mütek™ PCD-04 (Travel) Particle Charge Detector displays the poten-tial in ±mV. The sign of the measured value indicates whether the sample carries a positive (cationic) or negative (anionic) charge. The streaming potential is a relative value and depends on various influential factors, such as

- Dimensions of the measuring cell- Cleanliness of the cell- Conductivity- Chemical properties of the sample- Molecular weight- Particle size- pH- Viscosity- Temperature

To quantify the charges of a sample, a titration with an oppositely charged titrant (polyelectrolyte) has to be performed up to the point where a streaming potential of 0 mV is reached.

There is a correlation between streaming potential and zeta potential, which latter has been identified by electrophoresis. In actual practice, however, a com-parison of the two potentials is seldom possible and if at all, only under defined ideal conditions.



2.1.1 Measuring principleStreaming potential measurements with the Mütek™ PCD-04 (Travel) are based on the principle shown schematically in Fig. 2-1. The central element is a plastic measuring cell (4) with a fitted displacement piston (5).

If an aqueous sample is filled into the measuring cell, colloidally dissolved molecules will adsorb at the plastic 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 free to move.

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 cell (4) and creates an intensive liquid flow which ent-rains the free counter-ions, thus separating them from the adsorbed sample material.

At the built-in electrodes (3), the counter-ions induce a current which is evaluated digitally (2) before it is shown on the display (1) as streaming potential with the appropriate sign.

Fig. 2-1 Schematic of test setup

Designations1 Display 4 Plastic measuring cell2 Electronic 5 Displacement piston3 Electrodes 6 Motor

1

2

4

5

6

3



2.1.2 Calculation of charges

Polyelectrolyte titrationFor quantitative charge measurements of the sample, a polyelectrolyte titration has to be conduc-ted which uses the streaming potential to identify the point of zero charge (0 mV). To this end, add an oppositely charged polyelectro-lyte of known charge level to the sample as a titrant.

The titrant charges neutralize existing charges of the sample. Titration is stopped as soon as the point of zero charge (0 mV) is reached.

The titrant consumption obtained in ml forms the basis for further calculations.

Provided equal samples are titrated under identical conditions, the consumed titrant volumes can be directly compared. Normally, however, the charge level present in aqueous samples is expressed in terms of the anionic or cationic demand in eq/l.

Calculation of cationic/ anionic demandThe cationic or anionic demand [eq/l] of a sample is calculated by the following formula:

C1: Concentration of titrant in [N] or [eq/l]C2: Concentration of the titrated sample in [eq/l]V1: Titrant consumption in [l]V2: Sample volume to be titrated in [l]

Example:10 ml filtrate of an anionic fiber suspension is pipet-ted into the measuring cell of the Mütek™ PCD-04 (Travel) and titrated with a 0.001 N Poly-Dadmac 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:

0.0005 eq/l or 0.5 meq/l or 500 µeq/l

If the charge level is to be identified for an active sub-stance (starch, wet strength agent) or for solids (pig-ment slurry), the mass of the product should additionally be included in the calculation to obtain the so-called specific charge density.

Calculation of the specific charge densityThe specific charge density q [eq/g] is calculated by the following formula:

V: Consumed titrant volume [l]c: Titrant concentration [eq/l]m: Solids of sample or its active substance [g]q: Specific charge density [eq/g]

Example:A 10 ml sample of a 0.1% Ti02 suspension contains 0.01 g solids at m = 0.01 g.The consumption of cationic polyelectrolyte up to the point of zero charge is 2.5 ml for a titrant concentra-tion of 0.001 N.

The specific charge density is the following:

250*10-6 eq/g or 0.250 meq/g or 250 µeq/g

By multiplying the specific charge density in eq/g by the Faraday's constant F = 96485 C/eq, the total charge in C/g will be obtained.

C1 * V1C2 =

V2

0.001 eq/l * 0.005 lC2 = = 0.0005 eq/l

0.01 l

V * cq =

m

0.0025 [l] * 0.001 [eq/l]= 250 * 10-6 [eq/g]

0.01 [g]q =



2.1.3 Determination of the isoelectric point

Acid/ base titrationApart from charge measurements, the Mütek™ PCD-04 lends itself to identifying the isoelectric point (IEP) of dispersions.

The IEP is the pH-dependent point of zero charge of a particle.

By adding a titrant (acid/ base) drop by drop, the sample’s pH is shifted until the isoelectric point (stre-aming potential = 0 mV) is reached.

Cationic samples are titrated with a base and anionic samples with an acid up to the point of 0 mV.

HintThe isoelectric point can only be identified if the Mütek™ PCD-04 (Travel) is used in combination with an external titrator.

Fig. 2-2 Schematic of isoelectric point

2.1.4 Titrations curves

InformationThe Mütek™ PCD-04 Travel continuously generates a titration curve while performing a sample titration. Otherwise titration curves can only be obtained if the Mütek™ PCD-04 (Travel) is operated together with an external titrator, the associated software and a printer.Titration curves are basically difficult to interpret, because the curve progression does not exclusively reflect the sample material, but rather the adsorption behaviour of the sample at the surface of the measu-ring cell. This is why the curve progression should not be taken as a basis for the discussion of results. Instead, under certain conditions, the curves provide information about the nature of the sample under test. The titration curves shown in the following may roughly be associated with different stock systems:

2.1.4.1 Colloidally dissolved particlesTitration curve obtained for a colloidally dissolved 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 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. 2-3 Colloidally dissolved particles

IEP



2.1.4.2 Solid particlesTitration curve for an aqueous suspension of partic-les.Here the titration curve is nearly linear, because all solid particles contribute toward the creation of a streaming potential.

Fig. 2-4 Suspended solids

2.1.4.3 Heterogeneous stock systemsTitration curve of heterogeneous systems (colloids, dissolved material, solid particles, fibres etc.).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

2.2 System applicationsPapermaking- Improved machine running by controlling anionic

trash - 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

Other applicationsAn identification of charges is also very important for producers from the beverage and food industry and in the ceramics, dyes, cosmetics and pharmaceuti-cals sectors. In all these areas the Mütek™ PCD-04 (Travel) is finding increasing application.



2.3 Designation

HintCheck if a legible type plate (below) is provided on the rear panel of the device. Please replace if il-legible or missing.

2.3.1 Type plate PCD-04 (Travel)The following type plate Fig. 2-6 is provided on the rear panel of the instrument:

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

2.3.1.1 Type plate titration moduleThe integrated titration module of the Mütek™ PCD-04 Travel is labelled with the additional type plate Fig. 2-7. It is located on the rear panel of the titration module:

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

2.3.2 Service sticker PCD-04 (Travel)You will find a service sticker on the right side wall of the instrument. It shows the date of the last functional inspection of the Mütek™ PCD-04 (Travel) together with a recommended date for the next service.

Fig. 2-8 Service sticker



2.4 Technical data

Dimensions - MütekTM PCD-04: 160 mm wide x 215 mm deep x 340 mm high- MütekTM PCD-04 Travel: 160 mm wide x 225 mm deep x 370 mm high

Weight - MütekTM PCD-04: approx. 6.5 kg- MütekTM PCD-04 Travel: approx. 8.7 kg

Power supply - External power packInput: 100-240 VAC; 1.5 A; 50-60 Hz

Service conditions - Ambient temperature: +15°C up to +40°C- Storage/ transport temperature: +5°C up to +40°C

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 Mütek™ PCD-04 Travel- pH on the touchpanel of Mütek™ PCD-04 (Travel) with pH measure-

ment option- USB interface of Mütek™ PCD-04 Travel- SD card of Mütek™ PCD-04 Travel

Operating modes - MütekTM PCD-04Manual: Hand pipetteAutomatic: External MütekTM PCD-T3 Titrator

- MütekTM PCD-04 TravelAutomatic: Integrated titration module or

external MütekTM PCD-T3 Titrator

Reproducibility - Rel. standard deviation SD(x): (results obtained by titration of Pes-Na against Poly-Dadmac)

- < 0.3% (MütekTM PCD-04 Travel)- < 0.1% (MütekTM PCD-04 combined with MütekTM PCD-T3 Titrator)

Detection limit Up to 1 ppm depending on sample specification

Standards - MütekTM PCD-04 DIN EN 61326, DIN EN 61010- MütekTM PCD-04 Travel DIN EN 301489-1

DIN EN 301489-3DIN EN 60950DIN EN 300330

Safety Protection class I



2.5 Scope of delivery

2.5.1 PCD-04

Standard delivery

Optional

2.5.2 PCD-04 Travel

Standard delivery

Optional

Qty Item

1 MütekTM PCD-04

1 Measuring cell

1 Displacement piston

1 External power pack incl. power cable

1 Piston brush

1 Cationic titrant cartridge

1 Anionic titrant cartridge

1 Screen for filtrating fibre suspensions

1 Instructions for use of standard polyelec-trolytes

1 Test printout of standard titration

1 Operation manual

1 Recommended test procedure

Qty Item

1 Precision pipette, 2-10 ml

1 Aluminium trolley

1 pH set for MütekTM PCD-04- pH electrode- 2 x buffer 4.01 single dose solution- 2 x buffer 7.00 single dose solution- 2 x buffer 9.21 single dose solution- Beaker for pH electrode 10 ml

Qty Item

1 MütekTM PCD-04 Travel

1 Measuring cell

1 Displacement piston

1 External power pack incl. power cable

1 Piston brush

2 Cationic titrant cartridge

2 Anionic titrant cartridge

1 Screen for filtrating fibre suspensions

1 SD card

1 Instructions for use of standard polyelec-trolytes

1 Test printout of standard titration

1 Operation manual

1 Recommended test procedure

Qty Item

1 Precision pipette, 2-10 ml

1 Aluminium trolley

1 pH set for MütekTM PCD-04- pH electrode- 2 x buffer 4.01 single dose solution- 2 x buffer 7.00 single dose solution- 2 x buffer 9.21 single dose solution- Beaker for pH electrode 10 ml

2 Refillable titrant cartridges


III. Layout and functions


3.1 Description of PCD-04 (Travel)The Mütek™ PCD-04 Particle Charge Detector is available as a standard version (PCD-04) or with integrated titration module (PCD-04 Travel).

Fig. 3-1 Front view PCD-04

Designations1 Dosing hose holder2 Displacement piston3 Measuring cell4 Guide for measuring cell5 Beaker for pH electrode (optional)6 Holder for beaker7 Connection for pH electrode8 Contact pins

Fig. 3-2 Front view PCD-04 Travel

9 Measuring chamber10 Latch for touchpanel11 Touchpanel12 Cartridge holder (hinged)13 Latch for titrant cartridge14 Anionic titrant cartridge15 Cationic titrant cartridge16 Dosing hoses

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2

3

45

6

7

89

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11

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2

3

45

6

7

89

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11

12

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

Deignations1 Connection to external power pack2 ON/ OFF switch3 Output pH4 Output streaming potential

5 SD card slot6 USB interface7 Service sticker8 Type plate

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3

4

5

6

87



3.1.1 Measuring cellStandard delivery of the Mütek™ PCD-04 (Travel) includes a precision measuring cell and a displace-ment piston. Fitted in the measuring cell are two pla-tinum electrodes for identifying the streaming potential.

Fig. 3-4 Measuring cell and displacement piston

3.1.2 pH set (optional)When equipped with the optionally available pH set, the Mütek™ PCD-04 (Travel) identifies not only the charge level but also the pH of a sample. In combina-tion with a Mütek™ PCD-T3 Titrator, the instrument 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.

Fig. 3-5 Measuring cell and pH electrode

Designations1 Electrode cable with A2 connector2 Plexiglass shaft3 Clip4 Ceramic diaphragm5 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 measure the pH outside of the measuring cell.

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5




IV. Installation

IV. Installation

This chapter covers the installation of the Mütek™ PCD-04 (Travel) Particle Charge Detector and the necessary preparations. In the course of installation, all required settings have to be made.

4.1 Safety rulesPlease adhere to the applicable safety rules during preparatory work and when commissioning the system.

4.2 Personnel requirementsThe Mütek™ PCD-04 (Travel) may only be installed by qualified and skilled personnel.

4.3 Preparations onsitePrior to installation of the Mütek™ PCD-04 (Travel), all preparations mentioned in chapter 4.4 "Installation environment", page 23 must be made and the ambi-ent conditions met.Allow the Mütek™ PCD-04 (Travel) to adapt to ambi-ent temperature before commissioning.

4.4 Installation environment

4.4.1 Installation site

HintTo warrant safe and reliable operation of the Mütek™ PCD-04 (Travel), check on the following conditions before commissioning the instrument:

Ambient temperature: +15°C up to +40°CPlace the device on a stable and flat surfaceThe room where the Mütek™ PCD-04 (Travel) is set up must be clean and dryDo not operate the device while it is exposed to direct sunlightNever use the instrument when it is or was directly exposed to waterNever use the device in explosion prone roomsNever use the instrument if it is or was exposed to aggressive chemical substancesIf you notice the presence of condensed water either during transport or after storage, allow approx. two hours before turning on the instru-ment

4.4.2 External power pack

HintBefore starting the instrument, check if the local mains voltage is identical to that indicated on the type plate.The Mütek™ PCD-04 (Travel) is equipped with an external power pack in the form of a PFM controller which connects to all power voltages within the range indicated on it.

Input voltage: 100 - 240 VACFrequency: 50 - 60 HzIn the room where the device is set up, electrical installations must conform to current regulationsBe sure to connect the power pack to an appro-ved earthed socketDo not undo any earthing contactsThe guarantee by BTG Instruments GmbH expi-res if the device is used with an inappropriate voltage or if it is not connected to the external power pack that comes with the instrument


IV. Installation

4.4.3 Sample specification

GeneralBasically, nearly every aqueous sample - including original concentrations - can be measured. The measurability of a sample may be verified by the Mütek™ PCD-04 (Travel) Particle Charge Detector. To this end, fill a sample into the measuring cell, install the cell together with the displacement piston in the Mütek™ PCD-04 (Travel) and turn on the motor. Measurement may be started as soon as the motor runs smoothly and silently and the signal keeps comparatively stable (at approx. ±50 mV).

The limit values indicated in this chapter are not absolute values, but are merely indicative of sample characteristics that might lead to measuring pro-blems.

If there are doubts about whether or not a substance can be measured, conduct a test measurement and, if necessary, condition the sample accordingly.

SolventsCharge measurement is possible after functional groups are dissociated. Since this dissociation can only take place in aqueous solutions, the substance to be tested must be available in this form or be dispersed in water.

If required, the substance to be tested may be dissol-ved in lower alcohols (methanol, ethanol, isopro-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.

Particle sizesSolid particle sizes in a sample should not exceed 500 µm. The minimum detectable limit value is 1 nm.

ViscositySuitable for measurement are all samples with a vis-cosity below 6000 mPa*s. Viscosities exceeding this value impede the oscillating movement of the displa-cement piston in the measuring cell. This restriction is still aggravated by the flocculation effect typically occurring toward the end of titration.

Accordingly, samples with a viscosity exceeding 6000 mPa*s should conveniently be diluted with de-ionized water.

If highly viscous samples are to be titrated, mixing the titrant with the sample takes longer than with low-viscosity samples.

Molecular weightThe minimum molecular weight of polyelectrolytes to be tested should be at approx. 300 g/mol, since with smaller molecules, their adsorption on the cell wall by van-der-Waal forces is no longer ensured. Ions pre-sent in a sample due to dissolved inorganic salts are below the detection limit.

At the upper end of the scale, there is no limiting molecular weight of colloidally dissolved substances.


IV. Installation

ConductivityThe conductivity of a sample decisively impacts the streaming potential: the higher the conductivity, the lower the electrical resistance in the sample will be and the more the streaming potential will decrease without, however, influencing the titration results.

Fig. 4-1 Conductivity vs. streaming potential

In Fig. 4-1, various different NaCl proportions were added to Pes-Na 0.001 N and the samples were titra-ted with Poly-Dadmac 0.001 N.

HintIf conductivities are excessively high (20 mS/cm - 50 mS/cm), the streaming potential may fluctuate be-tween anionic and cationic so than an endpoint detection and thus titration is no longer possible. In these cases, reduce the conductivity by diluting the sample with de-ionized water.

InformationSamples that do not meet the above specifications may be prepared as outlined in chapter 5.5 "Sample preparation", page 41.

4.5 Solutions

4.5.1 TitrantsTitrants must always carry the opposite charge of the sample.The sample concentration (dilution) should optimally be selected to keep the titrant consumption between 0.2 and 10 ml.

PolyelectrolytesBTG Instruments GmbH recommends the use of Pes-Na and Poly-Dadmac as standard reagents, since their charge densities are practically pH-inde-pendent.

Pes-NaPes-Na (polyethene sodium sulfonate) is an anionic polyelectrolyte serving as a calibrating substance to determine the content of other titrants.

Poly-DadmacPoly-Dadmac (polydimethyl diallyl ammonium chlo-ride) is a cationic polyelectrolyte.For technical reasons, the activity of Poly-Dadmac is subject to minor variation between individual bat-ches. Before using a fresh solution, apply Pes-Na to conduct a factor determination. Consumption of Poly-Dadmac 0.001 N is usually bet-ween 9.75 and 10.25 ml for 10 ml Pes-Na 0.001 N.

Other polyelectrolytesThe following additional titrants are in frequent use today:

Cationic: - Methyl glycol chitosan (MGCh) 'Hymin'

Anionic:- Potassium polyvinyl sulphate (PVSK)- Sodium dodecyl sulfate (SDS)

InformationFor the Mütek™ PCD-04 (Travel), BTG Instruments GmbH supplies titrant cartridges containing Poly-Dadmac, Pes-Na and PVSK in the concentrations 0.001 N and 0.0001 N.

4.5.2 Acids/ basesUse 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.


IV. Installation

4.5.3 Cleaning solution

WarningAcetone and the cleaning solution are highly inflammable.

WarningPlease 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 Mütek™ 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.

HintTake care that sodium bromide dissolves completely.• Add acetone and mix gently.

InformationSelection of an optimum detergent depends on the sample concerned.


IV. Installation

4.6 Startup of PCD-04 The Mütek™ PCD-04 measures the streaming potential of an aqueous sample. To detect its charge level a titration is performed until reaching a strea-ming potential of 0 mV. Titration may be performed manually or better with help of an automatic titrator.

4.6.1 Manual operationFor manual operation of the Mütek™ PCD-04 Par-ticle Charge Detector, use a measuring pipette to transfer titrant drop by drop into the measuring cell. The endpoint, i.e. the point of zero charge, is rea-ched when the streaming potential is at 0 mV.

Fig. 4-2 Manual operation

Designation1 Measuring pipette

The titrant consumption is visible on the measuring pipette. Based on consumption, the charge level is quantitatively calculated especially in the case of a polyelectrolyte titration.

If you conduct an acid/ base titration with the Mütek™ PCD-04, the pH display indicates the isoelectric point (at 0 mV streaming potential).

InformationManual titration with a measuring pipette should solely be carried out for pretests.

1


IV. Installation

4.6.2 Operation with an external titratorThe figure below shows the Mütek™ PCD-04 toge-ther with a Mütek™ PCD-T3 automatic titrator.

Fig. 4-3 PCD-04 combined with PCD-T3

To work with the external titrator, the Mütek™ 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:

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

4.6.2.1 Preparing dosing hosesInstall the dosing hoses from the external titrator in their rest position as illustrated below.

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

InformationBefore starting measurement, rinse the dosing hoses as specified in the operation manual of the Mütek™ PCD-T3 Titrator.

MütekTM PCD-T3

MütekTM PCD-04

Streaming potentialpH

Dosing hose holder


IV. Installation

4.7 Startup of PCD-04 TravelThe Mütek™ PCD-04 Travel measures the strea-ming potential of an aqueous sample. To detect its charge level a titration is performed until reaching a streaming potential of 0 mV. Titration may be perfor-med either with the integrated titration module or with an external titrator.

4.7.1 Using SD cardThe Mütek™ PCD-04 Travel displays up to 100 results on its touchpanel. Much more data can be stored on the provided memory card (SD card).

InformationThe SD card must be installed before switching on the Mütek™ PCD-04 Travel, otherwise all data will be lost on power-off.

InformationThe SD card delivered with the Mütek™ PCD-04 Tra-vel is a SAN DISK. Do not use other SD cards.

4.7.1.1 Insert SD card• Switch off the MütekTM 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

Mütek™ PCD-04 Travel as shown below:

Fig. 4-6 SD card

• Switch on the MütekTM PCD-04 Travel for further usage.

4.7.1.2 Remove SD card• Switch off the MütekTM PCD-04 Travel using the

power switch on the back side of the unit.• Remove the SD card from the memory card slot

see Fig. 4-6 (push-to-pull mechanism).

HintYou may not remove or exchange the SD card, when the MütekTM PCD-04 Travel:

- Is switched on- Is in the write mode: "Writing on SD card!"- Is in the read mode: "Loading data from SD

card!"

• Switch on the MütekTM PCD-04 Travel for further usage.

4.7.2 Preparing dosing hosesWhen working with integrated titration module, install the dosing hoses 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. 4-8 Dosing hoses in rest position (front view)

Dosing hose holder


IV. Installation

4.7.3 Inserting titrant cartridgesWith the Mütek™ PCD-04 Travel, screw in the titrant cartridges in their holder as shown in Fig. 4-9.

HintBe sure to install the cartridges in the correct position as indicated by the + and - signs.

CautionNever use acids or bases in the titration module.

Fig. 4-9 Inserting titrant cartridges

Designations1 Latch2 Cartridge holder3 Cationic titrant cartridge4 Anionic titrant cartridge

• Press latch (1) to unlock and fold down cartridge holder (2).

• Screw in titrant cartridges (3 & 4) from below into the cartridge holder as shown in Fig. 4-9.

HintScrew in the cartridges with the labels facing to the front and the triangle on the cartridge coinci-ding with the triangle on the instrument. This

enables identification of the cartridge by the instrument.

• Shake the titrant by folding the cartridge holder up and down several times.- Shake the titrant each time the instrument

has been left unused for several days• Fold up the cartridge holder until it clicks into

place.

CautionNever unscrew the cartridges with the cartridge hol-der in folded-up position, since this would allow the liquid to drain.

Checking & setting titrant parametersWhen the ready-to-use Mütek™ titrant cartridges have been installed, the instrument will automatically display the titrant parameters in the associated boxes.

Procedure• Turn on the Mütek™ PCD-04 Travel.• In the main menu select "Titrator".This will bring up the following screen:

The two output fields (white boxes) show the follo-wing titrant parameters:

- Name: titrant used- Best Before: use-by-date- Level: residual amount- Normality: concentration- Factor: correction factor

• Exit the screen by touching "MENU".

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IV. Installation

InformationIf you need to use other titrants than the ready-to-use ones, special empty cartridges have to be ordered which can be filled with your titrant. Parameters of these titrants have to be entered manually.Use of refillable cartridges:• Touch one of the output fields to set the titrant

parameters manually.- Depending on which field has been touched,

one of the following displays will come up:

• After touching a field you may make entries as desired:- Name: 7-letter-name- Best before: use-by date- Level: volume 0 - 250 ml- 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".

4.7.4 Rinsing the dosing hoses

HintBefore starting measurement, check if the dosing hoses are filled bubble-free.

Procedure• Turn on the Mütek™ PCD-04 Travel.• In the main menu select "Titrator".

- This brings up the following screen:

- You may rinse the two titrant cartridges 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.

HintBefore starting the rinsing function, please check the liquid level of the titrant cartridges.


IV. Installation

4.7.5 Operation with external titratorThe figure below shows the Mütek™ PCD-04 Travel together with an external titrator Mütek™ PCD-T3. Before turning on the Mütek™ PCD-04 Travel, fold down the cartridge holder. This deactivates the inte-grated titration module so that the Mütek™ PCD-04 Travel will function like a Mütek™ PCD-04.

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

InformationBefore starting measurement, rinse the dosing hoses as outlined in the operation manual of the Mütek™ PCD-T3 Titrator.

To control the external titrator, the Mütek™ PCD-04 Travel has to transmit the streaming potential - and in the case of an acid/base titration, the pH - to the titra-tor. The required cabling is illustrated in the figure below.

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

MütekTM PCD-T3

MütekTM PCD-04 Travel

Streaming potentialpH


IV. Installation

4.8 pH calibration (optional)

HintIf the Mütek™ PCD-04 (Travel) is connected to an external titrator Mütek™ PCD-T3, the calibration of the pH electrode has to be repeated on the titrator.

HintIf you use the Mütek™ 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.

InformationThe 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).

- This will open one of the following screen dis-plays:

• Immerse the pH electrode in the pH 7.00 buffer solution and select "Start".


IV. Installation

• Wait until the displayed mV value has stabilized before you select "OK".- Depending on your preselection, one of the

following screens will come up:•

• Then immerse the pH electrode in a buffer solu-tion with pH 4.01 or pH 9.21 and press "Start".

• Wait until the displayed value has stabilized and select "OK".

- This brings up one of the following screen dis-plays:

• Confirm calibration by pressing "OK".• Repeat calibration if the slope is beyond the

range of -50 and -65 mV/pH.


V. Measuring

V. Measuring

5.1 Safety rulesBe sure to follow the chapter I. "Basic safety instruc-tions", page 7, before commissioning the Mütek™ PCD-04 (Travel).

5.2 Personnel requirementsOnly qualified and skilled personnel are allowed to operate the Mütek™ PCD-04 (Travel).

5.3 Overview touchpanel screens

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

InformationThe 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

Measure screen

Start screen

Main menu Setup menu


V. Measuring

5.3.2 Screens sub level PCD-04/ Setup menu

for servicing only

Master code keypad

Date keypad

Time keypad

Calibration screen

Menu for pH calibration

Setup menu

Measure screen


V. Measuring

5.3.3 Screens main level PCD-04 Travel

Measure screen

Result list

Keyboard for sample name

Start screen

Setup menu

Main menu Diagram screen

Method menuTitrator menu


V. Measuring

5.3.4 Screens sub level PCD-04 Travel/ Setup menu

for servicing only

Master code keypadMeasure screen

Date keypad

Time keypad

Calibration screen

Menu for pH calibration

Setup menu


V. Measuring

5.3.5 Screens sub level PCD-04 Travel/ Titrator menu

Titrant screen Titrant screen


V. Measuring

5.3.6 Screens sub level pH calibration (optional)


V. Measuring

5.4 Preparing the instrument• Start the Mütek™ PCD-04 (Travel) (see 4.6

"Startup of PCD-04", page 27).• Clean the measuring cell and the displacement

piston (see 7.1.2 "Cleaning the measuring cell", page 57).

5.5 Sample preparationFor stock systems including both colloidally dissolved material and solid particles, different ways of sample preparation will give different data on the charge con-ditions prevailing in a sample (see 4.4.3 "Sample specification", page 24). Generally speaking, results are only directly com-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.

In each case, quantitative sampling must be ensured to obtain reproducible values.

5.5.1 FiltrationTo 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 advise against using paper filters.

The use of ceramic filters by comparison is normally problem-free.

5.5.2 CentrifugationThe centrifugation period must be identical for all samples.

5.5.3 ScreeningIn the majority of cases, it will be sufficient to sepa-rate long fibres and larger particles by means of a nylon screen.

Quick and reproducible sampling is achieved by immersing a Mütek™ filtration beaker with screen in the sample and removing the supernatant liquid with a measuring pipette.

Fig. 5-1 Screening of samples

Designations1 Rising measurable sample2 Original sample, e.g. thick stock, coated broke3 Filtration beaker with 300 µm screen

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V. Measuring

5.5.4 Back titrationThis method of sample preparation suggests itself in the following cases:

- Due to their structure, the samples cannot be transferred to the cell directly which would enable quantitative determination of the charge level of larger particles

- The reaction of the substance to be tested with the titrant is too slow for direct titration

5.5.4.1 Example for back titration

SampleThe total charge of an anionic solid sample is to be determined. In view of the high solids content or excessive particle sizes, direct measurement in the measuring cell is not feasible. Instead, back titration is recommended.

ProcedureTake 20 g of the anionic sample to be measured and fill up to 100 g with Poly-Dadmac 0.001 N. Stir this 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 there is an excess amount of Poly-Dadmac, a resi-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

Calculation of charge density q:

V2 - V1: The difference between the charges ofthe fresh Poly-Dadmac and the reacted Poly-Dadmac indicates the chargeamount neutralized in the sample.

c: Concentration of the titrant, here 0.001 eq/l

m: 2 g of the original sample were used fortitration. (20 g were filled up to 100 g ofwhich 10 g were used for titration.)

Result: The charge of the sample under test is 2.925 µeq/g.

(V2 - V1) * c

mq =

(0.01068 - 0.00483) [l] * 0.001 [eq/l]q =

2 [g]

q = 2.925 * 10-6 [eq/g]


V. Measuring

5.6 Measuring with the PCD-04 (Travel)Preparation• Fill a sample into the measuring cell.


InformationSince 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.

InformationGood reproducibility of results is only achieved if the sample is appropriately homogenized for quantitative sampling.

• Insert the displacement piston in the measuring cell.

• In the Mütek™ PCD-04 (Travel), move the measuring 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).

HintPosition the pH electrode such as to prevent titrant from directly dripping onto it.

HintThe 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 Mütek™ 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.- The hose tips should be immersed in the

solution

Fig. 5-3 Dosing hoses installed ready for titration

Dosing hose holder


V. Measuring

5.6.1 PCD-04 Standard• Switch on MütekTM PCD-04.

- Following screen appears:

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

with option pH measurement

The following values and functions are available:

5.6.1.1 Start measurement• Press the button "On" on the left side of the mV

display "Potential".- This will cause the displacement piston to

oscillate and the streaming potential to be dis-played in mV

• Wait for approximately 30 seconds until the sig-nal has stabilized.

• Use a pipette to dose oppositely charged titrant until point of zero charge 0 mV is reached (see 4.6.1 "Manual operation", page 27).

• Note down dosage amount ml and pH value at point of zero charge as your measuring result.

InformationResult is not stored.

5.6.2 PCD-04 Travel• Switch on MütekTM PCD-04 Travel.

- Following screen appears:

Fig. 5-5 Measuring screen PCD-04 Travel with activated titration module and with option pH measurement

The following values and functions are available:

Potential Indicates the current streaming poten-tial. The value is reduced in steps when adding titrant.

On/ Off toggle button for indication of streaming potential.

pH Indicates the current pH, if the pH measurement option has been cho-sen.

Start/ Stop toggle button for pH measurement.

Potential Indicates the current streaming poten-tial. The value is reduced in steps when adding titrant.

On/ Off toggle button for indication of streaming potential.

Titrant Shows the current titrant consumption. When the streaming potential has gone through the point of zero charge, titration is finished and the consumed amount of titrant is displayed.

Start/ Stop toggle button- "Start" starts titration- "Stop" stops titration in case of fai-

lure

pH Indicates the current pH, if the pH measurement option has been cho-sen.

Start/ Stop toggle button for pH measurement.

Sample Name

Pressing the "Sample Name" button brings up keyboard for insert of sample name.


V. Measuring

5.6.2.1 Titration with Travel titration module

InformationWhen using an external titrator, please consult the associated operation manual. The following proce-dure refers to the use of Mütek™ PCD-04 Travel with activated titration module.

To start sample measurement:• Enter the sample’s 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:

• Type the desired sample name which will simul-taneously be entered in the results list.

Specifically, the following functions are available:

InformationYou may enter or modify a sample name until you actually start addition of titrant.

• Touch "OK" to go back to the "Measure screen".• Touch "MENU" in order to return to main

menu and select "Setup" to enter the setup menu (see menu tree 5.3.3).

• Select a titration method (1 = standard method).- Touch on the method number to change it

Fig. 5-6 Setup menu

- This brings up the keyboard screen for typing in a method number 1-9

InformationTo create/reprogramm your own method enter the method menu from the main menu screen (see 5.7.1 "Setting titration method", page 49).

• Touch "MEASURE" in order to return to the measure menu.

• Touch "On" to the left side of the mV display "Potential".- This will cause the displacement piston to

oscillate and the streaming potential to be dis-played in mV

Switches between capital and small letters

Cancels the last entry and returns you to the Measure screen

Deletes the last character

Confirmation and exit from entry mode


V. Measuring

• Wait for approximately 30 seconds until the sig-nal has stabilized.

• Touch "Start" to the left side of the ml display "Titrant".

- The titration is performed automatically by using an oppositely charged titrant

- 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 "Measure screen".

- The Mütek™ PCD-04 Travel stops as soon as 0 mV is reached

InformationSince the displacement piston continues its oscillating 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.


V. Measuring

5.6.3 Display/ save results

InformationThe following procedure refers to the use of Mütek™ PCD-04 Travel with activated titration module.Using MütekTM PCD-04 standard, all results (ml-titrant consumption and end pH-value) have to be note down.

InformationWhen using an external titrator, please consult the 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 Mütek™ 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:

The following functions are available:

Button for scrolling in the results list up and down, line by line.

Button for skimming through the results list by page up and down.


V. Measuring

5.6.4 Editing measured values

5.6.4.1 Editing measured values via SD card

HintMeasured values can only be edited when working with the Mütek™ PCD-04 Travel with integrated titra-tion module.

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

In order to manipulate the measurement values on your computer, please use a card reader or install the card in the SD slot of your computer. Measured values are edited in MS Excel format.

InformationThe Excel columns are separated by commas.

5.6.4.2 Editing measured values via USB inter-face

HintMeasured values can only be edited when working with the Mütek™ PCD-04 Travel with integrated titra-tion module.

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

HintTo manipulate on your computer the measured values edited at the USB interface, you have to install a USB driver. Please consult a BTG service technician in this context.


V. Measuring

5.7 Settings

5.7.1 Setting titration methodTo set/change parameters of a titration method pro-ceed as follows:• Select the Method menu from the main menu

screen.• Enter the pass word "4711".

- This will bring up the following screen:

InformationThe Method menu is used to programm specific methods. Selecting a method for measuring the right method number has to be set in the Setup menu (see Fig. 5-6 "Setup menu", page 45).

Following functions are available:

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

Method 1:Method 900 is preset as default method. Methods 2-9 are available for userdefined programming.

Increment Titration interval here: 1 unit every 3 seconds

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 todV(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 charged titrant solution automatically according to mV-sign (+/-)."Left" pumps from the left titrant installed."Right" pumps from the right titrant installed.

Aborts method programming.

Termination and storing of created method.


V. Measuring

5.7.2 Setting the dateTo set the date, proceed as follows:• In the Setup menu, select "Date".


Following functions are available:

5.7.3 Setting the timeTo set the time, proceed as follows:• In the Setup menu, select "Time".


The following functions are available:

Modifies the date format:- DD.MM.YY- MM/DD/YY

Use buttons 0 to 9 to enter the date as an uninterrupted 6-digit value (no break character in between).

Deletes the value entered last.

Exits date entry mode without accepting the current date and returns you to Setup menu.

Exits date entry mode and saves the entered date. Returns you to Setup menu.

Use buttons 0 to 9 to enter the time as an uninterrupted 4-digit value (no break character in between).

Deletes the value entered last.

Exits time entry mode without accepting the current time and returns you to Setup menu.

Exits time entry mode and saves the entered time. Returns to Setup menu.


V. Measuring

5.7.4 Calibrating the touchpanelYou 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:

HintTo calibrate, touch the cross with your finger. If you touch another point, the touchpanel will be deactivated and can only be reactivated by a panel reset (see below).

• In the Setup menu, choose "Calibrate Touchpa-nel".- This will open the following display:

• 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

5.7.4.1 Touchpanel resetIf the touchpanel no longer responds to your touch after calibration, do a panel reset as follows:

• Turn off the Mütek™ PCD-04 (Travel).• Touch the touchpanel with your finger at an opti-

onal point.• Turn on the Mütek™ PCD-04 (Travel) again and

keep your finger on the touchpanel until "Calibra-tion screen" is displayed (after approx. 5 s).

• Re-calibrate the touchpanel.


V. Measuring




6.1 Safety rulesIf errors occur that are not listed in the table below, disconnect the Mütek™ PCD-04 (Travel) and tag it as "defective". Contact BTG Instruments GmbH to ensure quick corrective action.

6.2 Personnel requirementsTroubleshooting may only be performed by qualified and skilled personnel.

6.3 Table of system faults

6.3.1 Error messages on the PCD-04 Travel

Error message Cause Corrective action

Warning:RFID: Not available

- No communication with titration module

• Contact a BTG Service Techni-cian.

Information: No SD card

- No SD card inserted • Switch off PCD-04 Travel and install SD card.- Without a SD card installed, no

data will be stored

Warning:No endpoint detected

- Maximum titrant volume of 20 ml reached

• Verify correct position of anionic 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.

Warning:No anionic titrant available

- No anionic titrant identified • Adjust position of titrant cartridge so that the arrow on the cartridge coincides with that on the instru-ment.

• Switch off the instrument and fold down the cartridge holder. Then insert an anionic titrant cartridge.

Information:Anionic titrant less than 50 ml, 40 ml, 30 ml, 20 ml

- Anionic titrant less than 50 ml, 40 ml, 30 ml, 20 ml

• Prepare exchange of anionic titrant cartridge.

Warning:Anionic titrant is empty

- Anionic titrant solution less than 10 ml or empty

• Replace empty cartridge by new anionic titrant cartridge.



Warning:No cationic titrant available

- No cationic titrant identified • Adjust position of titrant cartridge to make the arrow on the cartridge coincide with that on the instru-ment.

• Switch off the instrument, fold down the cartridge holder and screw in a new cationic titrant cart-ridge.

Information:Cationic titrant less than 50 ml, 40 ml, 30 ml, 20 ml

- Cationic titrant less than 50 ml, 40 ml, 30 ml, 20 ml

• Prepare exchange of cationic titrant cartridge.

Warning:Cationic titrant is empty

- Cationic titrant solution less than 10 ml or empty

• Replace empty cationic cartridge by a new one.

Anionic polyelectrolyte:Best before: Date

- 14 days left until use-by date • Prepare exchange of anionic titrant cartridge.

Cationic polyelectrolyte:Best before: Date

- 14 days left until use-by date • Prepare exchange of cationic titrant cartridge.

Anionic polyelectrolyte:Use-by date expired!

- Use-by date expired • Replace anionic titrant cartridge.

Cationic polyelectrolyte:Use-by date expired!

- Use-by date expired • Replace cationic titrant cartridge.

Error message Cause Corrective action



6.3.2 Basic faultsThe following basic faults may be experienced with the Mütek™ PCD-04 (Travel) also when used in combination with an external titrator:

Problem Cause Solution

Heavy fluctuations of strea-ming potential after sample is filled in

- Excessive conductivity of the sample

• Dilute sample.

- Insufficient sample volume in measuring cell

• Weigh in once again or use pipette.

- High solids in the sample • Dilute the sample or centrifuge/screen it to remove coarse partic-les.

Potential reverses after reaching the endpoint

- Very slow reaction between titrant and sample

• Titrate more slowly or perform back titration.

• If necessary, check sample prepa-ration for homogeneity.

At the start of titration, potential increases instead of decreasing

- Wrong titrant • Select titrant with opposite charge to that of sample.

- Adsorption equilibrium not attai-ned

• Proceed slowly with titration.

- Sample concentration too high or titrant concentration too low

• Dilute sample.

Potential remains essenti-ally unchanged during titra-tion

- Sample concentration very high • Dilute sample or use a higher strength titrant.

- Wet contacts on Mütek™ PCD-04 (Travel)

• Dry contact pins with a soft cloth.

- Wet electrodes on the outside of the measuring cell

• Dry electrodes with a soft cloth.

- Measuring cell contaminated • Thoroughly clean measuring cell and displacement piston.

Sign of displayed potential not in conformity with sample specification

- Sample charge is pH dependent • Check on pH dependence of sample.

- Excessive viscosity • Dilute sample.

- Measuring cell contaminated • Thoroughly clean measuring cell and displacement piston.

pH electrode cannot be cali-brated

- pH electrode contaminated or defective

• Clean pH electrode, if necessary replace it.




VII. Maintenance

VII. Maintenance

7.1 Cleaning

7.1.1 Cleaning the instrumentUse a soft and lint-free cloth to wipe the outer sur-faces of the instrument. Take care not to scratch the touchpanel. If contamination persists, moisten the cloth with soap water. A special cleaning procedure is required for the measuring cell.

7.1.2 Cleaning the measuring cellClean the measuring cell with water and cleaning solution only. After each measuring cycle, go through the following cleaning routine:


• 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 measuring 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.

HintFailure 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.

7.2 Maintenance

7.2.1 Personnel requirementsMaintenance shall exclusively be carried out by qua-lified and skilled personnel.

7.2.2 Functional testingTo avoid measuring errors caused by faulty opera-tion of the instrument or contamination of the measu-ring cell, functional testing can be performed by different methods.

7.2.2.1 Basic test of PCD-04 (Travel) without 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


VII. Maintenance

7.2.3 Standard titration

GeneralFill 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 Mütek™ 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 Mütek™ PCD-04 Travel and activated titra-tion module a standard titration can be performed automatically, as described below.

Procedure• In the main menu, touch "Titrator".• Select 5 ml or 10 ml Pes-Na.

InformationIf you select 5 ml Pes-Na, fill 5 ml de-ionized water into the measuring cell.

• Touch "Start".

- Pes-Na will be dosed into the measuring cell- After 20 seconds and the titration will start

- The result of the standard titration will be dis-played as follows:

• Accept the standard titration and start sample tit-rations by pressing "YES" in the pop-up window.• If you consider the deviation from the target

value too high press "No".- The system will ask for repeating the stan-

dard titration

• 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:

• 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.

InformationA standard titration verifies functionality of the Mütek™ PCD-04 (Travel) and checks on the concen-tation of the used titrants.


VII. Maintenance

7.2.4 Checking the streaming potentialIf a freshly cleaned measuring cell is filled with 10 ml of anionic standard Pes-Na 0.001 N repeatedly in succession, the streaming potential measured should be roughly identical. Depending on the instru-ment, the streaming potential is generally around -1600 mV ±200 mV. If the cell is used very frequently, this value will dimi-nish over time due to wear. This does not affect titra-tion results.However, if the streaming potential suddenly drops by several 100 mV from one measurement to the next, the measuring cell is probably soiled. To avoid measuring errors, clean the cell thoroughly (see chapter 7.1.2 "Cleaning the measuring cell", page 57).

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 Mütek™ 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 and down on the outside of the cell. This causes the signal to bounce. If no such reaction is observed alt-hough the motor is running, there is probably an 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 electrodeBefore starting a test series, measure a buffer solu-tion by means of the pH electrode which should respond within 10-30 seconds. If it does not, clean and re-calibrate the electrode. If the fault persists, replace the pH electrode.


VII. Maintenance




8.1 Safety rulesPlease adhere to the applicable safety rules when shutting down the system.

8.2 Personnel requirementsThe system shall only be shut down by qualified and skilled personnel.

8.3 Shutting down the systemTo place the Mütek™ PCD-04 (Travel) out of opera-tion, proceed as follows:• Turn off the instrument.• Disconnect the instrument from the mains.• If applicable, disconnect the Mütek™ PCD-04

(Travel) from the titrator.• Clean the measuring cell (see "Cleaning the

measuring cell", page 57).

HintThe titrant cartridges of the MütekTM 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.

8.4 StorageStore the Mütek™ PCD-04 (Travel) in a suitably pro-tected place. Do not keep outdoors.

8.5 Disposal

8.5.1 Official RegulationsBe sure to meet the current local regulations gover-ning the disposal of the Mütek™ PCD-04 (Travel).




IX. Parts list

IX. Parts list

9.1 Spare parts list

9.2 Consumables

Item Description Part No.

1 Aluminium trolley X20129

2 Measuring cell for MütekTM PCD-04 (Travel) X20240

3 Displacement piston for MütekTM PCD-04 (Travel) X20239

4 Connection cable between MütekTM PCD-04 (Travel) and titrator (BNC/BNC) for streaming potential and pH transmission

X02484

5 External power pack X20266

6 Piston brush for cleaning the measuring cells, d = 20 mm X10158

7 MütekTM filtration beaker with screen, 300 µm 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

Item Description Remarks Part No.

1 Poly-Dadmac cartridge 0.001 N, 250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20133

2 Poly-Dadmac cartridge 0.001 N, 4x250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20264

3 Poly-Dadmac cartridge 0.0001 N, 250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20135

4 Poly-Dadmac 0.001 N, 1000 ml Ready-to-use titrant for MütekTM PCD-04

X10217

5 Pes-Na cartridge 0.001 N, 250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20132

6 Pes-Na cartridge 0.0001 N, 250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20134

7 Pes-Na 0.001 N, 1000 ml Ready-to-use titrant for MütekTM PCD-04

X10216

8 PVSK cartridge 0.001 N, 250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20138


IX. Parts list

9.3 Safety measures

*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 Safety Data Sheets (MSDS).

9 PVSK cartridge 0.0001 N, 250 ml Ready-to-use titrant for MütekTM PCD-04 (Travel)

X20139

10 2 empty cartridges (to be filled with titrants of the user), 250 ml

one labelled anionic, one cationic X20136

11 Buffer solution pH 4.01 X17592



14 Acetone commercial quality

15 Sodium bromide (NaBr) commercial quality

16 3 M KCl solution commercial quality

17 Cleaning solution for manual cleaning to be prepared (see 4.5.3 "Cleaning solution")

Item* PPE (Personal Protec-tive Equipment)

Safety measures after contact Disposal Hazard

5/6/7/8/9

Goggles Rinse thoroughly with plenty of water after skin or eye contact

Incineration n.a.

1/2/3/4 Gloves,goggles

Rinse thoroughly with plenty of water after skin or eye contact

Controlled land-fill or incineration

n.a.

14/17 Gloves,goggles

Rinse with water after skin contact. In case of eye contact rinse with water immediately and consult an eye specialist

Special waste Highly inflam-meable

15 Gloves,goggles

Rinse thoroughly with plenty of water after skin or eye contact

Special waste n.a.

16 Gloves,goggles

Rinse with water after skin contact. In case of eye contact rinse with water immediately and consult an eye specialist

Special waste Highly inflam-meable

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Documents

Operation Manual PCD-04 (Travel) - INVEN Technology ... Screens sub level PCD-04/ Setup menu . . . . . . . . 36 5.3.3 Screens main level PCD-04 Travel . . . . . . . . . . . . 37 5.3.4