Metrohm 894 User Manual

Application Bulletin 401/1 e

Installation ins truction for 894 Professional CVS semiautomated: 894 Profession al CVS with 800 Dosinos for automatic dosing

The «894 Professional CVS semiautomated» is a system for the semiautomatic deter minat i on of suppres sor in plat ing solutions. With the additional accessory kit «Equipment with 2 Dosing Units for VA/CVS» also brightener can be determined.
PC controlled operation.
Automatic addition of 2 solutions: VMS, suppressor
standard or plating bath sample.
With «Equipment with 2 Dosing Units for VA/CVS» automatic addition of 4 solutions: VMS, brightener concentrate, suppressor co nc entrat e and suppressor standard or plating bath sample.
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 automatic dosing of
standard solutions and auxiliar y solution s .............. 3
3. viva «Configuration» ....................................................... 4
3.1. Devices .................................................................. 4
3.2. Sensors/Electrodes ................................................ 4
3.3. Dosing units ........................................................... 4
3.4. Solutions ................................................................ 5
4. viva «Method» ................................................................ 5
4.1. Method run ............................................................. 5
4.2. Evaluation .............................................................. 6
5. Operation........................................................................ 6
5.1. Suppressor determination ...................................... 6
5.2. Brightener determination ........................................ 7
Fig. 1: 894 Professional CVS semiautomated with optional equipment with 2 Dosing Units for VA/CVS
6. Remarks ......................................................................... 7
6.1. Storing dosing units ............................................... 7
6.2. Storing electrodes .................................................. 7
6.3. Waste bottle ........................................................... 7
Page 1 of 7
Application Bulletin 401/1 e
Installation instruction for 894 Professional CVS semiautomated
1
6.6065.10X
viva 1.0
Optional:
2
2.800.0010
800 Dosino

1. Instruments and accessories

Quantity Article number 1 2.894.1210
1 6.5339.0X0 CVS electrode kit
1 6.5339.500
894 Professional CVS semiautomated
Equipment with 2 Dosing Units for VA/CVS

2. System setup

2.1. Electrical connections

Fig. 2: Electrical connections 894 Professional CVS semiautomated
Fig. 3 Electrical connections 894 Professional CVS semiautomated with optional equipment with 2 Dosing Units for VA/CVS
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Application Bulletin 401/1 e
Installation instruction for 894 Professional CVS semiautomated
2.2. Tubing connections for automatic dosing of
standard solutions and auxiliary solutions
Fig. 4: Tubing connections for automatic dosing of VMS and suppressor standard or plating bath sample
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Fig. 5: Tubing connections for automatic dosing of VMS, suppressor concentrate, brightener concentrate and suppressor standard or plating bath sample
Application Bulletin 401/1 e
Installation instruction for 894 Professional CVS semiautomated
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.

3.1. Devices

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
Fig. 6: Detailed view of the measuring head
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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
Application Bulletin 401/1 e
Installation instruction for 894 Professional CVS semiautomated
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
800 Dosino (MSB 4)
894/D4 2mL Std or sample
2.0
Dosing rate Fill port
Maximum
mL/L
Dosing rate special port
Maximum
mL/L
Port
Length
Diameter
Rotating direction
automatic
Solution name
Dosing Unit
Suppressor concentrate
894/D3 2mL Suppressor
Std or sample
894/D4 2mL Std or sample
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
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
For a step by step description please see the Tutorial chapter «5.1.4 Define solutions».
TANDARD SOLUTION.
Rotating direction automatic
3.3.2. Dosing unit at 800 Dosino (2), 800 Dosino (3) and
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 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
mL/L

4. viva «Method»

viva software includes three method templates for CVS analysis with a semiautomated system.
Brightener determination (CVS, MLAT), semiautomated
Conditioning (Cu VMS), semiautomated
Suppressor determination (CVS, DT), semiautomated
The templates already establish the basic sequences for the different applications and the use of 800 Dosinos for automatic dosing as well as the calculation of the result. 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 «5.2 Methods for the semiautomated determination».
The following commands have to be adapted:

4.1. Method run

4.1.1. Measuring commands
Such as

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.
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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.
Application Bulletin 401/1 e
Installation instruction for 894 Professional CVS semiautomated
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.
On the tab «Database» the database is defined where determinations should be stored. By default viva database is used.
On the tab «Report» a report template for an automatic printout can be defined. By default no printout is defined.

5. Operation

5.1. Suppressor determination

5.1.1. Manual operation
Dosing Unit «894/D1 50mL VMS» connected to Dosino 1 has to be prepared with VMS.
Dosing Unit «894/D4 2mL Std or sample» connected to Dosino 4 has to be prepared with suppressor standard solution if a calibration is recorded or with plating bath sample for the determination.
5.1.2. Workplace

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:
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.
Select sample type S
TANDARD to run a calibration in the
«Run» window of the «Workplace». For a determination sample type S
AMPLE has to be selected.
No «Sample amount» needs to be defined in the «Run» window on the «Workplace», since addition volumes for the standard and the sample are defined in the method commands ADD
STD and ADD SAMPLE DT.
5.1.3. Course of events
The execution of calibration or determination by dilution titration is controlled by the 894 Professional CVS and viva.
Dosino 1 automatically doses the VMS and Dosino 4 is used for the automatic addition of suppressor standard or plating bath sample.
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.
Page 6 of 7
Application Bulletin 401/1 e
Installation instruction for 894 Professional CVS semiautomated

5.2. Brightener determination

5.2.1. Manual operation
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 Suppressor» con nec ted to Dosino 3 has to be prepared with suppressor concentrate.
The correct «Sample amount» has to be pipetted into the measuring vessel when requested.
5.2.2. Workplace
Select sample type S «Workplace» to run a determination.
Define the volume of sample used for the determination under «Sample amount» in the «Run» window of the «Workplace».
AMPLE in the «Run» window of the
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.

6.2. 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 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.

6.3. Waste bottle

The waste bottle must not be closed completely. For pressure balancing in the waste bottle, keep at least one opening unsealed. Overpressure would lead to a malfunction of the 800 Dosinos.
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.
The intercept solution is automatically prepared at the beginning of each determination, by dosing VMS from Dosino 1 and suppressor concentrate from Dosino 3.
After the determination of the intercept value, a window will pop up prompting to add the sample on top of the intercept solution. The ex act s ampl e volu me has to be pipetted manually through the pipetting opening of the 894 Professional CVS.
Standard addition is carried out automatically with brightener concentrate from Dosino 2.

6. Remarks

6.1. Storing dosing units

When the dosing units are not used (during the night, over the weekend) the dosing cylinder has to be rinsed with
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