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© BTG

Operation Manual Mütek

TM

PCD-05, September 2017

49

V. Measuring

5.13.3 Service Settings

Information

With the following settings the instruments calibration
will be changed, this has a direct influence to the mea-
surement results. This setting should be changed only
from a skilled user.

Pump volume:

The pump volume can be changed between 4.5 and

5.5.

Analog input (potential):

1. Select either cell 1 or cell 2 depending which cell you

want to calibrate

2. Clean measuring cell manually
3. Fill in 10 ml 0.001 N PES Na
4. Insert measuring cell and hook piston
5. Press "Start" in the "Analog In (potential)" field
6. Wait until it becomes stable, value in the brackets

should be below 100 then press "Stop"

Mastercode:

Specific adjustment can be done, only if a code from

BTG Instruments is provided.

5.14 Help

Information

Under the tab "Help" the following can be found:
• Training and instruction movies.
• Operation Manual.

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Summary of Contents for Mutek PCD-05 Smart

Page 1: ...Operation Manual MütekTM PCD 05 Smart Light Particle Charge Detector ...

Page 2: ...turing BTG shall have no liability for any error or damages of any kind resulting from the use of this document All rights reserved No part of this document may be copied photocopied published reproduced translated or converted into electronic or machine readable form without written permission of BTG Instruments AB Original Instructions BTG Instruments AB 2017 ...

Page 3: ... 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 Applications 15 2 3 Designation of the PCD 05 16 2 3 1 Type plates PCD 05 16 2 3 1 1 Type plate PCD 05 Base Unit 16 2 3 1 2 Type plate PCD 05 Travel Titrator 16 2 3 1 3 Type plate PCD 05 Smart Display 16 2 3 1 4 Typ...

Page 4: ... external titrator 27 4 6 3 Startup of PCD 05 Smart 28 4 6 3 1 Connect smart display 28 4 6 3 2 Connect Travel titrator module 28 4 6 3 3 Checking setting titrant parameters 30 4 6 4 Rinsing the dosing tubes 30 V Measuring 5 1 Safety rules 31 5 2 Personnel requirements 31 5 3 Limitations 31 5 4 Overview of Smart display Mütek PCD 05 Smart Light 32 5 4 1 Screens Mütek PCD 05 Standard 32 5 4 2 Overv...

Page 5: ...41 5 10 4 Result handling Mütek PCD 05 42 5 10 4 1 Transfer result data to USB stick 42 5 11 Measuring with the Mütek PCD 05 Smart using a Wi Fi device 43 5 11 1 Setup the measurement 43 5 11 2 Start measurement 43 5 11 3 Data handling Mütek PCD 05 Smart 43 5 12 Methods 44 5 12 1 Method settings 44 5 12 1 1 Setting of standard methods 45 5 12 1 2 Method Mode 45 5 12 1 3 Method screen Addition 46 5...

Page 6: ...ll 53 7 2 3 Standard titration 54 7 2 4 Checking the streaming potential 55 7 2 4 1 Electrostatic charging of the measuring cell 55 7 2 5 Functional testing of the pH electrode 55 7 3 Proper handling of the pH electrode 56 7 4 Yearly LAB Check inspection 56 VIII Shutting down the system storage and disposal 8 1 Safety instructions 57 8 2 Personnel requirements 57 8 3 Shutting down the system 57 8 ...

Page 7: ... rules Users are obliged to immediately eliminate any faults that may affect operational safety Warranty and liability This instrument was built and tested in accordance with EU Guidelines 2014 30 EC and 2014 35 EC It com plied with all safety regulations at the time it left the fac tory To maintain this condition and ensure safe operation the user must observe the safety instructions and warning ...

Page 8: ...i cal changes to this document 1 2 Intended applications of the PCD 05 The Mütek PCD 05 shall be used exclusively for the purposes defined in this operation manual and in the technical description and shall only be operated in con junction with external instruments and components recommended or approved by BTG Instruments AB The Mütek PCD 05 Particle Charge Detector shall solely be used for charge...

Page 9: ...that documentation on general and local accident pre vention and environmental protection standards is near at hand and strictly adhered to Keep all safety instructions and warnings on the Mütek PCD 05 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 Mütek PCD 05 and t...

Page 10: ...ing or postal delivery of the instrument To exclude transport damage never put any additi onal items in the trolley To avoid transport damage to the precision contact 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 com partment in the trolley At outdoor temperatures below 15 C 59 F let the unit adjust to ambi...

Page 11: ...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 elec trokinetic effect can be identified via Electrophoresis Electroosmosis Sedimentation potential Streaming potential Streaming potential If a liquid is forced along a particle surface under pres sure it will shear off the counter ions of th...

Page 12: ...an 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 displa cement piston 5 oscillates in the measuring cell 4 and creates an intensive liquid flow which entrains the free counter ions thus separating them from the adsor bed sample material At the built in electrodes 3 th...

Page 13: ...iltrate of an anionic fiber suspension is pipetted into the measuring cell of the Mütek PCD 05 and titra ted with a 0 001 N Poly Dadmac solution until the point of zero charge is reached In the example 5 ml cationic polyelectrolyte Poly Dadmac 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 s...

Page 14: ...5 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 measuring cell This is why the curve progression should not be taken as a basis for the discussion of result...

Page 15: ...s Fig 2 5 Heterogeneous stock systems 2 2 Applications Papermaking Improved machine running by controlling anionic trash Improved retention control Enhanced chemical performance Stable paper quality Effluent treatment Optimized chemicals by controlled flocculant dosa ges Increased dry content of sludges through improved dewatering Exact identification of the demulsification point of emulsions and ...

Page 16: ...he titrator adapter Fig 2 10 Type plate PCD 05 Titrator Adapter 2 3 2 Service sticker PCD 05 You will find a service sticker on the wall of the instru ment It shows the date of the last functional inspection of the Mütek PCD 05 together with a recommended date for the next service Fig 2 11 Service sticker 82569200 BTG Instruments AB Industrigatan 1 3 66129 Säffle SWEDEN N1619 TYPE NO REV I U 24 V ...

Page 17: ...potential mV pH Results Anionic cationic demand ml Charge quantity µeq l pH Isoelectric point IEP Sample volume Measuring cell 10 60 ml Outputs Streaming potential 2500 mV Titrant consumption on the display of Mütek PCD 05 pH on the display of Mütek PCD 05 with pH measurement option USB interfaces of Mütek PCD 05 to store end result and parameter to an USB memory Wi Fi Connection to a Wi Fi device...

Page 18: ...anual Qty Item 1 Precision pipette 2 10 ml 1 Plastic transportation box 1 pH set pH electrode buffer solution 4 01 buffer solution 7 00 buffer solution 9 21 1 Titrator adapter module 1 BTG Lab Software full version Consumables Qty Item 1 Base unit PCD 05 1 Smart display 1 Measuring cell 1 Displacement piston 1 External power supply 1 Power cable 1 Piston brush 1 Poly Dadmac bottle 0 001N 250 ml 1 ...

Page 19: ... or Light version 3 1 Description of PCD 05 Smart Light Fig 3 1 Front view PCD 05 Smart Designations 1 Titrant tubes 2 Titrant feed tube insert 3 Rinsing backflush tube insert 4 Titrant tube holder 5 Anionic and cationic titrant bottle 6 Measuring cell 7 Guide for measuring cell 8 Contact pins 9 Displacement piston 10 Smart display 11 Latch for smart display 1 2 3 4 5 6 11 10 9 7 8 ...

Page 20: ...ayout and functions Fig 3 2 Front view PCD 05 Light Designations 1 Latch for Travel titrator module option 2 Titrant tube holder 3 Displacement piston 4 Measuring cell 5 Guide for measuring cell 6 Contact pins 7 Latch for smart display 8 Smart display 1 2 3 4 5 6 7 8 ...

Page 21: ...e 82569200 BTG Instruments AB Industrigatan 1 3 66129 Säffle SWEDEN N1619 TYPE NO REV I U I U 24 V DC Contains FCC ID Z64 WL 18DBOD Hereby BTG Instruments AB declares that the radio equipment type PCD 05 is in compliance with Directive 2014 53 EU The full text of the EU declaration of conformity is available at the with Directive 2014 53 EU The full text of the EU declaration of conformity is avai...

Page 22: ...but also the pH of a sample In combination with a Travel Titrator module or an exter nal Titrator the instrument can determine the isoelectric point of a sample via the pH electrode Install the pH electrode in the measuring cell on the wall opposite the titrant tubes that is at a maximum distance from the tube tips Fig 3 6 Measuring cell and pH electrode Designations 1 Electrode cable with A2 conn...

Page 23: ...table and flat surface The room where the Mütek PCD 05 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 directly 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 eit ...

Page 24: ...purpose fill 10 ml of the solvent de ionized water or a water alcohol mixture 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 minimum amount of a cationic titrant is added I...

Page 25: ...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 Polyelectrolytes BTG Instruments AB recommends the use of Pes Na and Poly Dadmac as standard reagents since their charge densities are practically pH independent Pes Na Pes Na sodium polyethylene sulfonate is an anionic polyelectrolyte serving as a ...

Page 26: ...lution are highly inflam mable Warning Please follow the safety instructions in chapter 1 5 General safety directions page 9 The cleaning solution for manual cleaning of the measu ring cell of the Mütek PCD 05 is available from BTG Instruments AB or can be produced from 50 parts sodium bromide NaBr and 50 parts acetone plus 125 parts water Prepare the above proportions Fill water into a suitable v...

Page 27: ... the cable at the backside of the instrument see 2 Fig 3 3 Fig 4 2 Connection of Smart display 4 6 2 Connect with an external titrator The Mütek PCD 05 can be operated with an external automatic titrator Use the titrator adapter module to connect the Mütek PCD 05 to the external titrator Fig 4 3 PCD 05 combined with an external titrator external automatic titrator external titrator adapter ...

Page 28: ...nt solutions Fig 4 6 Inserting titrant solutions Designations 1 Travel titrator module 2 Anionic alkaline titrant bottle 3 Cationic acid titrant bottle 4 RINSE insert dosing tube for backflush of titrant solution 5 FEED insert feeding tube Before screw in shake the titrant bottles Shake the titrant bottles each time the instru ment has been left unused Screw in titrant bottles 2 3 from below into ...

Page 29: ...t the other side of the feeding tube into the tit rant bottle Therefore insert the tubes end into the FEED insert until the tube reaches the bottom of the tit rant bottle When not using the screw in titrant bottles but others external bottles insert the feeding tube end into external bottle until the tube reaches the bottom Insert dosing tubes The other side of the dosing tubes should be placed in...

Page 30: ...try Press Cancel to cancel the entry no changes will be stored 4 6 4 Rinsing the dosing tubes Hint Rinse the dosing tubes in order to assure that they are bubble free before starting the measurement Procedure with Smart display Turn on the Mütek PCD 05 Smart After initialization press Rinse Both tubes will be rinsed with 10 ml After 10 ml it will stop automatically or it can be stopped anytime in ...

Page 31: ...ssibility to synchronize each other s actions Web application will not show if someone else is opera ting with the instrument and how instrument is acting depending on actions received from another user For example if one user starts titration another user will not be able to see how its results are being built up titration curve Our recommendation is that one user at the time should operate with ...

Page 32: ...nsfer to USB Information Transfer ﬁnished 1 PCD 05 Smart SN 82365947 V2 2 11 Cell 1 Method 3 Rinse Transfer to USB Measure PCD 05 Smart 0 22 SN 90300259 V2 5 Cell 1 Method 1 OK DEMAND 4 71 ml Startpotential 11 75 mV Equivalent 471 eq l μ pH Resuslts PCD 05 Smart 0 22 SN 90300259 V2 5 Cell 1 Method 1 Home Rinsing both tubes with 10ml PCD 05 Smart 0 22 SN 90300259 V2 5 Cell 1 Method 1 Home START STA...

Page 33: ... BTG Operation Manual MütekTM PCD 05 September 2017 33 V Measuring 5 4 2 Overview of web application main screens The following screens are examples from a connected Smartphone ...

Page 34: ...er For best user experience we recommend Chrome 55 or Safari 10 1 Turn on the PCD 05 Smart 2 Turn on the Wi Fi function of the mobile device to use smartphone tablet or laptop 3 Search for Wi Fi network a list of available networks should appear an example is shown below 4 Choose network SSID BTG Lab a device depen ding 10 digits number the full SSID can be seen at the type plate of the Smart disp...

Page 35: ...mation about e g the charge conditions of solids In each case quantitative sampling must be ensured to obtain reproducible values 5 7 1 Filtration To separate larger solid particles from a sample a whi teband 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 c...

Page 36: ... 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 residual 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...

Page 37: ...tioned if the displacement piston can be hooked in the bayo net catch easily and without canting Assure that the marking facing the front Fig 5 2 Measuring cell and displacement piston If applicable install pH electrode in the measuring cell see Fig 5 6 Insert pH electrode page 39 Hint Position the pH electrode such as to prevent titrant from directly dripping onto it Hint The pH electrode must im...

Page 38: ...mble the MütekTM PCD 05 Light according to chapter 4 6 1 Start up of PCD 05 Light page 27 Switch on thePCD 05 Light Choose Measure The measure screen appears Fig 5 5 Measuring screen with optional pH measure ment The following values and functions are available Fill in measuring sample and install the measuring cell according to chapter 5 8 Fill sample into the measuring cell page 37 With pH optio...

Page 39: ...ng potential and pH signal optional will be send to the titrator Information For more detailed information about the titration setting parameters and data storage please refer to the manual of your external titration system 5 9 2 1 Start measurement Start the potential measurement according to see 5 9 1 1 Start measurement page 38 5 9 2 2 Start titration Select oppositely charged titrant on your t...

Page 40: ...D 05 Smart display The following functions are available The following values and functions are available Rinse Both tubes will be rinsed with 10 ml Measure Change to Measure screen Transfer to USB Final results and parameters will be transferred through USB port PCD 05 Smart SN 82365947 V2 2 11 Cell 1 Method 3 Rinse Transfer to USB Measure mV Indicates the current streaming poten tial The value i...

Page 41: ...g 5 8 Methods Information To create reprogram your own method enter the Method tab on the Wi Fi device 5 10 3 Start titration Press Titrant on the smart display The titration is performed automatically by using the pump selected in the method screen see 5 12 1 Method settings page 44 The Mütek PCD 05 stops as soon as the ter mination criteria is reached Information Since the displacement piston co...

Page 42: ...a transfer to USB plug an USB stick on the back side panel of the instrument From the main window press Transfer to USB All results and parameters will be transferred to a plugged USB stick up to 100 Information The data transfer of a full result memory 100 can take a few minutes The following values may be transferred Serial number Date Time Sample name Start potential mV Demand ml Equivalent µeq...

Page 43: ... titration curve choose the tab Results The titration stops as soon as the termination crite ria is reached Information Since the displacement piston continuous its oscillating movement the steaming potential and pH signal optio nal may change This is a normal effect without any influence on measurement results Press Stop Titration to stop the measurement 5 11 3 Data handling Mütek PCD 05 Smart Al...

Page 44: ...x Field Description Counter Samplename ID of the sample StartPot Streaming potential in mV at the start of a measurement Demand Demand of titrant which is dosed in ml when termination criteria is rea ched pH EP measurement pH value at the start point of a mea surement IEP measurement pH value when the mV termination criteria is reached Method 1 Method 900 and 2 Method 901 are preset as default met...

Page 45: ... within a time window the MütekTM PCD 05 continues with the next dispensing step dE mV dt s Time window dt in which the variation of the mV signal is below dE t min s t max s This display gives the minimum and maximum wait times between two dispensing steps Addition amount has to be preset dynamic or continuos in the addition screen see chapter 5 12 1 3 page 46 Termination mV EP 0 mV Pump Automati...

Page 46: ...mV From this point on a dynamic titration addition will take place according to the control parameters dV max dV min and dE set The settings for the time interval between two addition steps which are adjusted under the field Mode fixed or adapt are independent from the control band They are applied during the complete titration The value for the control band is valid for both cationic and anionic ...

Page 47: ... use touch the appropriate field acid pH 4 01 or alkaline pH 9 21 Software version Shows the software version of the base unit Serial number Serial number of the PCD 05 Titration unit Select ml or µeq l measurement results will be displayed accor dingly Settling time Alternative to start a titration manually it is possible to enter fix waiting time before titration starts automatically For example...

Page 48: ... Wait until the displayed mV value has stabilized and select OK Depending on your preselection one of the follo wing screens will come up Rinse the electrode with deionized water again Then immerse the pH electrode in a buffer solution with pH 4 01 for acid range or pH 9 21 for alkaline range and select Start Wait until the displayed value has stabilized and select OK This brings up the following ...

Page 49: ... 5 Analog input potential 1 Select either cell 1 or cell 2 depending which cell you want to calibrate 2 Clean measuring cell manually 3 Fill in 10 ml 0 001 N PES Na 4 Insert measuring cell and hook piston 5 Press Start in the Analog In potential field 6 Wait until it becomes stable value in the brackets should be below 100 then press Stop Mastercode Specific adjustment can be done only if a code f...

Page 50: ...50 Operation Manual MütekTM PCD 05 September 2017 BTG V Measuring ...

Page 51: ...detected Maximum titrant volume of 20 ml reached Maximum titration steps of 2200 steps reached pH end point is reached before 0 mV is reached Verify correct position of anionic and cationic titrant Sample concentration too high dilute sample Verify that titrant tubes are immer sed in sample Rinse titrant tubes thoroughly to remove air bubbles Increment too low adjust method Slope out of range The ...

Page 52: ... 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 attained 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 ...

Page 53: ... 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 Not cleaning the measuring cell after each measure ment will lead to measuring errors and prevent reprodu cibility of results To avoid deposits in the measuring cell and on the replacement piston fill the freshly ...

Page 54: ... Smart page 34 Under the tab Titrator select 5 ml or 10 ml Pes Na by using the toggle button Information If you select 5 ml Pes Na fill 5 ml de ionized water into the measuring cell Press Start Pes Na will be dosed into the measuring cell After Pes Na is dosed the screen Measure comes up Sample name will be Standard automatically After 30 seconds the titration will start The result of the standard...

Page 55: ...everal 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 53 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 05 receives a signal from the measuring cell ...

Page 56: ...ning of every working day with the unit The buffer solutions supplied are meant as single use solutions In order to assure reproducible results always use new stable buffer solutions 7 4 Yearly LAB Check inspection To guarantee reliable measurement from the start every Mütek laboratory instrument undergoes thoro ugh testing before leaving the factory BTG s maintenance program LAB Check keeps your ...

Page 57: ...e instrument Disconnect the instrument from the mains If applicable disconnect the Mütek PCD 05 from the titrator Clean the measuring cell see chapter 7 1 2 Clea ning the measuring cell page 53 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 6 from drying up Fill the cap of the pH electrode with 3 M KCl solution and keep th...

Page 58: ...58 Operation Manual MütekTM PCD 05 September 2017 BTG VIII Shutting down the system storage and disposal ...

Page 59: ...pette 2 10 ml P00X18772 7 Plastic tips for precision pipette 2 10 ml P00X18773 8 Seal for precision pipette P00X18776 9 pH electrode plexiglass shaft ceramic diaphragm gel filling holder H00X09115 10 pH electrode glass shaft glass section diaphragm gel filling holder H00X09133 11 Suction tube for PCD 05 Travel titrator module P00X20427 12 Dosing tube for PCD 05 Travel titrator module P00X20272 Ite...

Page 60: ...0 001 N 250 ml Ready to use titrant for MütekTM PCD 05 H00X20398 6 Pes Na bottle 0 0001 N 250 ml Ready to use titrant for MütekTM PCD 05 H00X20400 7 Pes Na 0 001 N 1000 ml Ready to use titrant for MütekTM PCD 05 H00X10216 8 PVSK bottle 0 001 N 250 ml Ready to use titrant for MütekTM PCD 05 H00X20403 9 PVSK bottle 0 0001 N 250 ml Ready to use titrant for MütekTM PCD 05 H00X20404 10 Set of 2 empty b...

Page 61: ......

Page 62: ...BTG Instruments AB P O Box 602 SE 661 29 Säffle Sweden Phone 46 533 426 00 www btg com ...

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