Metrohm MVA-20 User Manual

Application Bulletin 402/1 e

Installation ins truction for MVA-20: 894 Profession al CVS fully automat ed for CVS determinations

The «MVA-20» is a fully automated system for the determination of suppressor and brightener in plating solutions in small sample series.
PC controlled operation.
Manual operations:
o Filling of the sample vials on the Autosampler
with suppressor standard solution, plating bath samples and rinsing solution.
Automatic addition of 4 solutions: VMS, brightener concentrate, suppressor conc entrat e and suppressor standard or plating bath sample.
Automatic rinsing of the measuring vessel.
Method change during the determination series is
possible.
Applications:
o Analysis of suppressor concentration in plating
baths with CVS.
o Analysis of brightener concentration in plating
baths with CVS.

Content

1. Instruments and accessories .......................................... 2
2. System setup .................................................................. 2
2.1. Electrical connections ............................................ 2
2.2. Tubing connections for rinsing and draining of the
measuring vessel ................................................... 3
2.3. Tubing connections for automatic dosing of
standard solutions and auxiliary solutions .............. 4
3. viva «Configuration» ....................................................... 5
3.1. Devices – 894 Profesional CVS ............................. 5
3.2. Sensors/Electrodes ................................................ 5
3.3. Dosing units ........................................................... 5
3.4. Solutions ................................................................ 6
3.5. Devices – 919 IC Autosampler plus for CVS ......... 6
4. viva «Method» ................................................................ 8
4.1. Method run ............................................................. 8
4.2. Evaluation .............................................................. 9
5. Operation...................................................................... 10
5.1. Suppre ssor determi nation series ......................... 10
5.2. Brightener determination series ........................... 11
6. Remarks ....................................................................... 12
6.1. Single additiv e set up ............................................ 12
6.2. Combination of applications ................................. 12
6.3. Storing dosing units ............................................. 12
Fig. 1: MVA-20
Page 1 of 12
6.4. Storing electrodes ................................................ 12
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.
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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
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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
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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
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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.
VMS 894/D1 50mL VMS Brightener concentrate 894/D2 2mL Brightener
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».
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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 the command PUMP PERISTALTIC
PUMP
ON.
Fig. 10: Method snippet TRACK PERISTALTIC PUMP
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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 PUMP RINSE und PUPM PUMP DRAIN 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 MOVE RINSING
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 MOVE RINSING 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
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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 SAMPLE has 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 ADD SAMPLE DT.
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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
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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
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