6.5. Waste containe r ................................................... 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
Systems
CVS
1
6.2141.300
Remote cable
1
6.5339.0X0
CVS electrode kit
1. Instruments and
accessories
Quantity Article number
1 2.894.1210
2 2.800.0010 800 Dosino
1 2.843.0240
1 2.919.0120
1 6.5339.500
1 6.6065.10X viva 1.0
894 Professional CVS
semiautomated
843 Membrane Pump
Station for Professional CVS
919 IC Autosampler plus for
Equipment with 2 Dosing
Units for VA/CVS
2. System setup
2.1. Electrical connections
Fig. 2: Electrical connections
Please note! The cable 6.2141.300 has to be connected to
«Remote 2» of the 843 Pump Station.
Page 2 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
2.2. Tubing connections for rinsing and draining of the
measuring vessel
Fig. 3: Tubing connections for rinsing and draining of the measuring
vessel
Fig. 4: Detailed view of the measuring head
Page 3 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
2.3. Tubing connections for automatic dosing of
standard solutions and auxiliary solutions
Fig. 5: Tubing connections for automatic dosing of standard
solutions and auxiliary solutions
Fig. 7: Detailed view of the measuring head
Fig. 6: Detailed view how to mount the T-connector
Page 4 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
8.103.8010xx
viva Tutorial CVS
referred to as Tutorial
Auxiliary electrode
Auxiliary electrode
RDE
RDE
Reference electrode
Reference electrode
3. viva «Configuration»
In addition to this application bulletin it is recommended to
have the following document availabl e.
Fig. 8: Detailed view for the tubing connections of the dosing unit
waste port
3.1. Devices – 894 Profesional CVS
The 894 Professional CVS is automatically recognized by
the viva software. When an instrument is connected for the
first time it needs to be entered in the viva «Configuration».
The corresponding dialogue will pop up automatically.
Device name* 894_1
* as used in the example method
For a step by step description please see the Tutorial
chapter «4.1.1 Configuring the instrument».
3.2. Sensors/Electrodes
With the software a set of electrodes is preinstalled in the
viva «Configuration». The following three electrodes have to
be present if the measuring command in the method is used
as specified in the viva method templates.
Sensor name Sensor type
In the following chapters it will be
3.3. Dosing units
An 807 Dosing Unit attached to an 800 Dosino, which is
connected to the 894 Professional CVS, is automatically
recognized by the viva software. When the Dosing Unit is
connected for the first time it needs to be entered in the viva
«Configuration». The corresponding dialogue will pop up
automatically. For a step by step description please see the
Tutorial chapter «5.1.3 Configuring dosing units».
3.3.1. Dosing unit at 800 Dosino (1)
Dosing Unit name as used in the viva method templates.
800 Dosino (MSB 1) 894/D1 50mL VMS
Parameters for preparation
Dosing port Prep/empty Dosing port 2
Page 5 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
Port
Length
Diameter
Dosing port 1
Port 1
138 cm
2 mm
Dosing port 2
Port 3
0 cm
2 mm
800 Dosino (MSB 2)
894/D2 2mL Brightener
800 Dosino (MSB 3)
894/D3 2mL Suppressor
Dosing rate Fill port
Maximum
mL/L
Dosing rate special port
Maximum
mL/L
Port
Length
Diameter
Rotating direction
automatic
800 Dosino (MSB 4)
894/D4 2mL Std or sample
Dosing rate Fill port
4.0
mL/L
Dosing rate special port
maximum
mL/L
Fill port
Port 2
201 cm
1 mm
Special port
Port 4
0 cm
2 mm
Rotating direction
automatic
Solution name
Dosing Unit
Suppressor concentrate
894/D3 2mL Suppressor
Std or sample
894/D4 2mL Std or sample
Device name*
919 IC Autosampler plus 1
Axial distance
189.0
mm
Dosing rate port 1 Maximum mL/L
Dosing rate port 2 Maximum mL/L
Dosing rate Fill port Maximum mL/L
Dosing rate special port Maximum mL/L
Tubing parameters
Fill port Port 2 25 cm 2 mm
Special port Port 4 0 cm 2 mm
Valve disk
Rotating direction automatic
3.3.2. Dosing unit at 800 Dosino (2) and 800 Dosino (3)
Dosing Unit name as used in the viva method templates.
Parameters for preparation
Dosing port Prep/empty Dosing port 2
Dosing rate port 1 2.0 mL/L
Dosing rate port 2 Maximum mL/L
Tubing parameters
Dosing port 1 Port 1 80 cm 0.3 mm
Dosing port 2 Port 3 0 cm 2 mm
Fill port Port 2 55 cm 2 mm
Special port Port 4 0 cm 2 mm
Valve disk
Tubing parameters
Port Length Diameter
Dosing port 1 Port 1 80 cm 0.3 mm
Dosing port 2 Port 3 0 cm 2 mm
Valve disk
3.4. Solutions
Solutions that should automatically be dosed have to be
defined in the viva «Configuration» and need to be
assigned to the Dosing Unit which is used for the dosing.
The following table shows the solution names and assigned
Dosing Units as used in the viva method templates.
SOLUTION TYPE for «VMS» and «Suppressor concentrate»
has to be AUXILIARY SOLUTION, for «Brightener concentrate»
and «Std or sample» it is S
TANDARD SOLUTION.
For a step by step description please see the Tutorial
chapter «5.1.4 Define solutions».
3.5. Devices – 919 IC Autosampler plus for CVS
The «919 IC Autosampler plus for CVS» is automatically
recognized by the viva software. When an instrument is
connected for the first time it needs to be entered in the viva
«Configuration». The corresponding dialogue will pop up
automatically.
3.3.3. Dosing unit at 800 Dosino (4)
Dosing Unit name as used in the viva method templates.
Parameters for preparation
Dosing port Prep/empty Dosing port 2
Dosing rate port 1 2.0 mL/L
Dosing rate port 2 maximum mL/L
Page 6 of 12
* as used in the example method
For a step by step description, using the example of an 858
Professional Sample Processor, please see the Tutorial
chapter «6.1.1 Configuring the instrument».
3.5.1. Tower
Tower parameters
Max. stroke path 133 mm
Min. beaker radius Off
Lift rate 25 mm/s mm/s
Application Bulletin 402/1 e
Installation instruction for MVA-20
Beaker radius samples
off
mm
Beaker sensor
off Rack offset
0
°
Special position
0
mm
Work position
Not available
Not used
3.5.2. Rack
Rack name 6.2041.490
Shift rate 20 °/s
3.5.3. Rack data
Rack parameters
Lift positions – Tower 1
Work position
User
mm
defined, see
3.5.4
Rinse position 0 mm
Shift position 0 mm
Lift positions – Tower 2
Rinse position Not available
Shift position Not available
Special position Not available
Special beakers
3.5.4. Needle adjustment
The work position of the pipetting needle 6.1835.050 has to
be adjusted in a way that the lower end of the needle is
positioned max. 1 mm above the bottom of the sample vial.
This is essential to guarantee a complete transfer of the
sample from the sample vial on the rack of the 919 IC
Autosampler plus into the measuring vessel of the 894
Professional CVS.
Fig. 9: Needle adjustment
0.5 … 1 mm
Procedure to adjust the needle position in viva
1. Insert an empty sample vial to one of the sample
positions on the rack (position 1 to 28).
2. Click on the Manual symbol.
3. Select Tower 1 (Sample changers – 919 IC
Autosampler plus 1).
4. Open tab «Move».
5. Enter the position of the empty sample vial in the field
«Target position».
6. Click Start to move the needle to the chosen rack
position.
7. Enter 125 mm in the field «Target position» in the
section «Lift position».
Page 7 of 12
8. Click Start to lower the needle to the chosen target
position. For the exact position ing of the needle as
shown in «Fig. 9», use the arrow up and down buttons
to adjust the needle position stepwise.
9. Once the needle is properly adjusted select the tab
«Assign position».
Application Bulletin 402/1 e
Installation instruction for MVA-20
10. The new value can be seen in the section «Lift position
– Current position».
11. Select the option «Work position for Tower» in the
section Lift position.
12. Click on «Assign» in the section Lift position .
13. Leave the Manual control with a click on the «Close»
button.
4. viva «Method»
4.1. Method run
viva software includes three method templates for CVS
analysis with an automated system.
• Brightener determination (CVS, MLAT), automated
• Conditioning (Cu VMS), automated
• Suppressor determination (CVS, DT), automated
The templates already establish t h e bas ic s eq u e nc es fo r the
different applications, the use of 800 Dosinos for automatic
dosing as well as the calculation of the result and the
application of a sample changer and pumps to process a
sample series. However certain commands and settings
have to be adapted to the used hardware and the
requirements of the specific application.
For a step by step description please see the Tutorial
chapter «6.2 Methods for the automated determination».
The following commands have to be adapted:
4.1.1. Measuring commands
Such as
•Assign the 894 Professional CVS instrument to be used
on the tab «General/Hardware».
•Adapt the measuring parameters on the tabs «Pre-
treatment», «Sweep», «Post-treatment» and
«Potentiostat» according to the requirements of the
application. These parameters can be found in separate
application documentation.
4.1.2. Dosing commands
Such as:
•Define the volume of solution that should be dosed
when this command is due.
Such as:
•Define the volume of solution that should be dosed
when this command is due.
•Assign the Dosing Unit that should be used to run this
command.
Such as:
•On the tab «General/Hardware» assign the 894
Professional CVS instrument to which the 800 Dosino is
connected.
4.1.3. Automation commands
Such as:
•Assign the 919 IC Autosampler plus that should be
used to run this command.
4.1.4. Transferring sample
This only applies for the brightener determination by MLAT!
To guarantee a complete transfer of the sample from the
sample vial on the rack of the 919 IC Autosampler plus into
the measuring vessel of the 894 Professional CVS the
peristaltic pump time has to be adjusted in the TRACK
PERISTALTIC PUMP in thecommand PUMP–PERISTALTIC
PUMP
ON.
Fig. 10: Method snippet TRACK–PERISTALTIC PUMP
–
Page 8 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
Cell volume
50 mL
100 mL
4.1.5. Rinsing measuring vessel
After each sample the measuring vessel need to be rinsed
with deionized water. The rinsing and draining times depend
on the total volume used in the determination.
If the method templates are used, the rinsing and draining
times are defined in the corresponding PUMP
commands in
the TRACK–RINSE and TRACK–DRAIN. The number of
rinsing cycles is defined in the command LOOP–LOOP
RINSING in the TRACK–RINSING CYCLES.
Fig. 11: Method snippet TRACK–RINSING CYCLE
Examples for rinsing and draining times:
Number of rinsing cycles 2 2
Draining time [s] 35 50
Rinsing time [s] 9 18
Please note! The device assigned to the commands PUMP
–PUMPRINSE und PUPM–PUMPDRAIN need to be the
919 IC Autosampler plus, since the 843 Pump Station is
connected to and controlled from the sample changer.
4.1.6. Rinsing transfer tubing
This only applies for the brightener determination by MLAT!
After each sample the transfer tubing from the 919 IC
Autosampler plus to the measuring vessel of the 894
Professional CVS need to be rinsed with deionized water.
The rinsing solution is placed in a vial on the rack of the 919
IC Autosampler plus. The position of the rinsing solution
relative to the sample position is defined in the TRACK
TO RINSING POSITION
POSITION
.
in the command MOVE–MOVERINSING
–GO
Fig. 12 Method snippet TRACK–GO TO RINSING POSITION
To change the relative position of the rinsing solution the
formula editor has to be used on the parameter «Number»
in the section «Target» i n th e comman d MOVERINSING POSITION.
Fig. 13 Formula editor to change the rinsing position
The transfer time for the rinsing solution corresponds to the
sample transfer time defined in the TRACK–PERISTALTIC
PUMP
in the command PUMP–PERISTALTIC PUMP ON.
4.2. Evaluation
Settings regarding evaluation and documentation of the
determination are located in the «Evaluation» part of the
method. The templates already include all necessary
settings to determine brightener or suppressor concentration
in an acid copper bath. If modifications however should be
necessary, here is where important parameters are found:
–MOVE
Page 9 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
4.2.1. Substances
In the «Substances» part settings for peak recognition and
baseline parameters are defined.
4.2.2. Standards
In the «Standards» part the concentration of the used
standard solution is defined.
4.2.3. Calibration
In the «Calibration» part the calibration method, such as DT
or MLAT, is defined as well as the regression type.
4.2.4. Results
In the «Results» part on the tab «Results» the substance is
selected for which the concentration should be calculated
and displayed.
5. Operation
5.1. Suppressor determination series
5.1.1. Manual operation
•Dosing Unit «894/D1 50mL VMS» connected to Dosino
1 has to be prepared with VMS.
•Suppressor standard solutions and plating bath
samples are placed on position 1 to 27 of the sample
rack using the sample vials for 50 mL (6.2747.010).
•On the position after the last sample a vial with
deionized water is placed to rinse Dosino 4 after the
end of the suppressor sample seri e s.
Fig. 14: Example positions of solutions on the sample rack
6.2041.490 for suppressor determination
5.1.2. Workplace
•In the «Run» window on the tab «Determination series»
create a sample table
Fig. 15: Example sample table for suppressor determination
•To run a calibration with a standard solution select
sample type S
TANDARD. For a determination the sample
type SAMPLEhas to be selected.
•No «Sample amount» needs to be defined in the
sample table, since addition volumes for the standard
and the sample are defined in the method commands
ADD
STD and ADDSAMPLEDT.
Page 10 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
5.1.3. Course of events
•The execution of calibration and determination by
dilution titration is controlled by the 894 Professional
CVS and viva.
a) T he measurin g vessel is em pti ed using the 843
Pump Station.
b) Dosing Unit «894/D4 2mL Std or sample»
connected to Dosino 4 is automatically rinsed and
prepared with suppressor standard or sample from
the vial on the rack of the sample changer.
c) The measuring vessel is rinsed using the 843
Pump Station.
d) Dosino 1 automatically adds the VMS and Dosino
4 is used for the automatic addition of suppressor
standard or plating bath sample.
e) At the end of each determination the measuring
vessel, is automatically emptied and rinsed using
the 843 Pump Station.
Next sample starts again from a).
• Recalibration within a determination series is possible.
• At the end of a determination series Dosino 4 is
automatically prepared with rinsing solution.
5.2. Brightener determination series
5.2.1. Manual operation
Fig. 16: Example positions of solutions on the sample rack
6.2041.490 for brightener determination
5.2.2. Workplace
•Dosing Unit «894/D1 50mL VMS» connected to Dosino
1 has to be prepared with VMS.
•Dosing Unit «894/D2 2mL Brightener» connected to
Dosino 2 has to be prepared with brightener
concentrate.
•Dosing Unit «894/D3 2mL Suppres sor» con nec ted to
Dosino 3 has to be prepared with suppressor
concentrate.
•Plating bath samples are placed on position 1 to 14 of
the sample rack using the sample vials for 50 mL
(6.2747.010). The exact sample volume needed for the
determination has to be pipetted into the vial.
•Rinsing solutions are placed on position 15 to 28 of the
sample rack using the sample vials for 50 mL
(6.2747.010). Usually the same volume of deionized
water is used for rinsing like it was used for the sample.
The rinsing solution has to be placed diagonally
opposite the sample on the second half of the circle
(Sample position + 14).
•In the «Run» window on the tab «Determination series»
create a sample table
Fig. 17: Example sample table for brightener determination
• As sample type SAMPLE has to be selected.
• For «Sample amount» the volume pipetted into the vial
has to be entered.
5.2.3. Course of events
•The execution of the determination by modified linear
approximation technique is controlled by the 894
Professional CVS and viva.
a) T he measurin g vessel is em pti ed using the 843
Pump Station.
b) The intercept solution is automatically prepared at
the beginning of each determination, by dosing
Page 11 of 12
Application Bulletin 402/1 e
Installation instruction for MVA-20
VMS from Dosino 1 and suppressor concentrate
from Dosino 3.
c) After the determination of the intercept value, the
plating bath sample is transferred from the sample
rack to the measuring vessel by means of the builtin peristaltic pump of the 919 IC Autosampler plus.
The sample is added on top of the intercept
solution.
d) Standard addition is carried out automatically with
brightener concentrate from Dosino 2.
e) At the end of each determination the measuring
vessel is emptied using the 843 Pump Station.
f) The transfer tubing from the sample changer to the
measuring vessel is rinsed with the rinsing solution
placed on the rack of the sample changer.
g) After the transfer tubing is rinsed the measuring
vessel is automatically emptied and rinsed using
the 843 Pump Station.
Next sample starts again from a).
6. Remarks
stored separately in a vial filled with deionized water (KCl
solution, in case KCl is used as bridge electrolyte), so that
the reference electrode immerses at least to the rim of the
electrolyte vessel.
6.5. Waste container
The waste container must not be closed completely. For
pressure balancing in the waste container, keep at least one
opening unsealed. Overpressure would lead to a
malfunction of the drain pump.
6.1. Single additive setup
If the system is only used for suppressor or brightener
determination the unused port at the T connector
(6.2744.290) has to be closed with a threaded stopper
(6.2744.060).
6.2. Combination of applications
The determination of suppressor by dilution titration (DT)
and the determination of brightener by modified linear
approximation technique (MLAT) can also be combined in
one series.
6.3. Storing dosing units
When the dosing units are not used (during the night, over
the weekend) the dosing cylinder has to be rinsed with
water. Otherwise elemental copper can be formed or
additives can precipitate between the valve disk and the
distributor disk or in the tubings. A blockage can damage
the 800 Dosino. Emptying the cylinder and filling it with
water is sufficient to prevent a blockage.
6.4. Storing electrodes
When the electrodes are not used (during the night, over the
weekend) the electrodes should be thoroughly rinsed.
Working and auxiliary electrode can either be stored in
deionized water or dry. The reference electrode should be
Page 12 of 12
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