Metrohm VoltIC pro I User Manual

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No.
Article no.
Article designation
IC
1
2.850.3040
850 Professional IC AnCat - MSM­HC - MCS
2
2.850.9010
IC Conductivity Detector
1
6.6059.232
MagIC Net™ 2.3 Professional CD ­1 License
VA 1 2.797.0010
797 VA Computrace
1
2.843.0140
843 Pump Station
2
2.800.0010
800 Dosino
1
6.2148.010
Remote box MSB
1
6.2141.290
Cable 843 - 838
1
6.2055.100
Double flask holder
2
6.1608.050
Glass bottle GL45 100 mL
2
6.1618.060
Thread adaptor GL45/GL45
2
6.1819.010
PTFE tube
2
6.3032.120
2 mL Dosing Unit 807 glass
Sample processor & Liquid handling
1
2.858.0020
858 Professional Sample Processor Pump
1
6.1826.020
PVC pump tubing (blue/blue)
1
6.1602.150
Bottle neck attachment / GL 45 – 3 × UNF 10/32
1
6.1608.070
Eluent bottle / 2 L / GL 45
2
2.800.0010
800 Dosino
2
6.3032.210
10 mL Dosing Unit 807 glass
1
6.2057.040
Dosino holder for 838
1
6.2846.000
ZrO2 needle 1/8 in for IC/VA 151 mm
2
6.2148.050
USB RS converter for 900
1
6.2134.100
Cable RS232 (DB9)-IBM PC (DB9) 5 m
1
6.2841.100
Rinsing station for IC
1
6.2041.450
Sample Rack 56x11 mL+56x50 mL: VA 1 6.2747.010
Sample tubes 50 mL 25x
Application Bulletin 356
Installation instruction for «VoltIC pro I»
The «VoltIC pro I» combines a Professional AnCat IC system with an automated VA system and shared sample handling. «VoltIC pro I» is an all-in-one solution for the fully automated analysis of anions, cations and heavy metals.
1. Scope of delivery
Fig.: VoltIC pro I system
Table of contents
1. Scope of delivery ...................................................... 1
2. Installation ................................................................ 2
2.1 Electrical connections ............................................... 2
2.2 850 Professional IC .................................................. 3
2.3 797 VA Computrace ................................................. 5
2.4 858 Professional Sample Processor ......................... 6
2.5 Connection of devices .............................................. 7
3 Software ................................................................... 8
3.1 Installation of an Serial port (RS) printer ................... 8
3.2 Installation of MagIC NetTM ..................................... 11
3.3 Configuration of MagIC NetTM ................................. 11
3.4 Installation of 797 VA Computrace software ........... 13
3.5 Configuration of 797 VA Computrace software ....... 13
3.6 Starting a determination ......................................... 14
4 Exemplary measurement ........................................ 15
5 Appendix ................................................................ 17
5.1 Time Program ......................................................... 17
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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1
6.2743.057
Sample tubes 11 mL 200x
1
6.2743.077
Stopper with perforation 200x
1
6.1808.280
Adapter Dosino Port 4 / M6
1
6.1805.530
FEP tube connection M6 200
1
6.1831.070
PEEK Cap. 1/16 In/0.75 mm 70 cm
1
6.1803.150
PTFE capillary 1/16 In/0.25 mm 1 m
1
6.1822.410
PEEK connection capillary
1
6.5620.000
Connecting set to Dosing Unit: port 4 1 6.1608.030
Bottle Colourless Glass 1 L / GL 45
1
6.2744.034
Coupling nozzle – UNF 10/32, 2 pieces
1
6.2744.070
Pressure screw short, 5 pieces
3
6.2744.080
Coupling Outer M6/UNF
1
6.1803.030
PTFE capillary 0.5 mm i.d. / 3m
Optional
1
6.6059.208
MagIC Net™ 2.x Progessional Upgrade Multi - 3 licenses
1
6.1006.520
Metrosep A Supp 5 - 150/4.0
1
6.1006.500
Metrosep A Supp 4/5 Guard/4.0
1
6.1050.410
Metrosep C 4 - 100/4.0
1
6.1050.500
Metrosep C 4 Guard/4.0
2. Installation
We strongly recommend that the individual steps are carried out in the order given below.
2.1 Electrical connections
In order to install the VoltIC pro I you have to establish following connections mentioned below:
858 to 850: Connect «controller» output of 858 to USB
serial port of 850
800 Dosino (10 mL) to 858: Connect by MSB (Port 2)  800 Dosino (10 mL) to 858: Connect by MSB (Port 3)  2 x 800 Dosinos (2 mL) to 797 VA Computrace:
Connect by MSB (Port 1, Port 2)
797 VA Computrace to 843 Pump Station: Connect by
remote cable 6.2141.280
843 Pump Station to Remote box: Connect by remote
cable 6.2141.290
Remote box to 858: Connect to MSB 1  850 to computer: Connect 850 to USB serial port of PC  797 VA Computrace to computer: Connect USB serial
port of 797 VA Computrace to USB serial port of PC
Null modem cable: Attach the two USB RS converters
(6.2148.050) to the available USB ports of the 858 and connect both using the RS232 cable (6.2134.100)
Application Bulletin 356
Installation instruction for «VoltIC pro I»
Page 3 of 18
Fig.: Electrical connection diagram for the VoltIC pro I system
2.2 850 Professional IC
In order to install the Professional IC you have to perform the following steps: Remove rollers and handle, place the detector blocks in the instrument and connect the detector cables, remove transport locking screws, connect the leak sensor cable, connect the drainage tubing, and set up the eluent bottles. Please refer to the 850 Professional IC manual for a detailed description (chapters 2.6 and 2.8).
1. Connection to the eluent bottle for anion determination
2. Capillary to anion separation column
3. MSM inlet capillary – labeled with Eluent
4. MSM outlet capillary – labeled with Detector, which can be connected to the MCS or directly to the detector.
The MCS air aspiration capillary is connected to the CO2-absorber cartridge.
5. Capillary from MCS to anion detector, long PEEK pressure screws (6.2744.090) are used for the MCS connection
6. Detector outlet capillary to waste
7. Regeneration solution aspiration capillaries (PTFE, 0.97 mm ID), connected to two bottles with ultrapure water and 50 mmol/L sulfuric acid respectively via peristaltic pump tubing with orange/yellow stoppers (6.1826.320)
8. MSM regeneration solution outlet capillaries – labeled with Waste – to waste
9. Connection to the Eluent bottle for cation determination
10. Capillary to cation separation column
11. Capillary from cation separation column to cation detector
12. Detector outlet capillary to waste
13. Sample inlet capillary (PTFE, 90 cm, d=0.25 mm), connected to the anion valve (position 1)
14. Optional sample degasser Capillary connection (PTFE, 40 cm, d=0.5 mm) between
anion valve (position 2) and cation valve (position 1)
15. Connection capillary anion channel valve to cation channel valve
16. Capillary to the waste
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Prepare and degas two eluents suitable for the anion and cation columns you want to use (see column manuals). For Metrosep A Supp 5 a solution of 3.2 mmol/L Na2CO3 / 1.0 mmol/L NaHCO3 is adequate. For Metrosep C 4 a solution of 1.7 mmol/L HNO3 / 0.7 mmol/L dipicolinic acid (DPA, 2,6­Pyridinedicarboxylic acid) is adequate.
Provide regeneration solutions for the MSM Suppressor (ultrapure water and 100 mmol/L sulfuric acid).
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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2.3 797 VA Computrace
Following steps have to be done to install the MVA-3 system:
a) Establish the following tubing connections between the system components
b) Establish the tubing connections for 800 Dosinos for the addition of solutions:
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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c) Establish the tubing connections at the measuring
head of the 797 VA Computrace:
2.4 858 Professional Sample Processor
For a detailed description, please refer to the 858 Professional Sample Processor manual. In general, you will have to do the following: Plug in the Swing Head connection cable, and plug in the power supply cable. The sample processor initializes and lifts its Swing Head, once it is connected to the IC device and the MSB connection is recognized. Afterwards, it is possible to mount the retaining plate (manual chapters 3.2 - 3.4).
Mount the Dosino holder (6.2057.040) on the side of the tower and attach a 10 mL Dosing Unit (6.3032.210) and a 800 Dosino (2.800.0010) to it.
A rinsing station is mandatory for this setup. The rinsing station is mounted onto the sample processor,
which is easiest when the rack is temporarily removed. The exact position can be adjusted by directing the needle into the rinsing station with the manual control (in the window manual). The inner compartment approximately relates to a swing head angle of ~116°, the outer one approximately relates to ~110°. Memorize your angle settings.
Fig.: Rinsing station parts
A tubing is fixed at the bottom of the rinsing station to drain the waste water. A bottle of ultrapure water is needed as reservoir for the rinsing solution. The rinsing solution is transported by one channel of the peristaltic pump of the sample processor.
Mount the rinsing station on the sample processor. Connect ultrapure water reservoir with the peristaltic pump
(via pump tubing (6.1826.360) and PEEK screws / tubing olives) using a PTFE capillary (part of 6.1803.030). Then connect the peristaltic pump (via pump tubing and PEEK Screws / tubing olives) to the inner compartment of the rinsing station also using a PTFE capillary (part of
6.1803.030).
The outer compartment of the rinsing station is connected to the waste container.
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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2.5 Connection of devices
The 858 Professional Sample Processor, the 850 Professional IC AnCat system and the 797 VA Computrace are connected with each other via the 800 Dosino with a 10 mL Dosing Unit mounted on the 858 Professional Sample Processor.
Connect the sample needle to Port 3 of the 10 mL Dosing Unit at the 800 Dosino using a PEEK capillary (70 cm, d=0.75 mm, 6.1831.070). The 850 Professional IC AnCat system is connected to the Dosing Unit at Port 1 using a PTFE capillary (90 cm, d=0.25 mm, part of 6.1803.150). The sample inlet capillary (PEEK, 90 cm, d=0.5 mm, part of
6.1822.410) of the 797 VA Computrace is connected to the
Dosing Unit at Port 2. Port 4 of the Dosing Unit is equipped with an adapter (6.1808.280) and a FEP tube (6.1805.530) and connected to the waste.
The second 10 mL Dosing Unit with an 800 Dosino is connected to one capillary of the fourfold micro tip and is used to dilute the sample for the VA measurement automatically (solution j).
Fig.: Capillary connections to and from rinsing station
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Fig.: schematic configuration of the VoltIC pro I system a) PEEK, 70 cm, d=0.75 mm, 6.1831.070 / b) PTFE, 90 cm, d=0.25 mm, part of 6.1803.150 / c) PEEK, 90 cm, d=0.50 mm, part of 6.1822.410 /
d) FEP tube, 6.1805.530 / e) Fourfold micro tip, 6.1824.000 / f) FEP tube, 6.1805.530 / g) PTFE, 40 cm, d=0.50 mm, part of 6.1803.030 / h) Heavy metal multistandard solution / i) buffer solution pH 4.6 / j) ultrapure water / k) rinsing solution for VA / l) anion eluent / m) cation eluent / n) rinsing solution for rinsing station
3 Software
3.1 Installation of an Serial port (RS) printer
The data generated in the VA Computrace software is being transferred to MagIC Net via a generic text printer. The following steps describes how a generic text printer is being installed under Windows 7.
Check the newly created COM-ports in your system after connecting the null modem cable and USB RS adapters (refer 2.1): Start Control Panel Device Manager
Under Ports (COM&LPT) the newly created USB serial ports are visible (e.g. COM14 and COM15):
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Check and – if necessary – adjust the «Port Settings» to the following parameters of both COM ports under «Properties» by double-clicking on each COM port:
Create a generic text printer under: «Start» «Devices and Printers» «Add a Printer»
Add a local printer by using the first newly created COM port (e.g. COM 14) and select the «Generic / Text only» printer driver. Use the current version of the driver. Rename the printer to «RS Printer».
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Do not share this printer, do not print a test page and finish the printer wizard.
Configure the newly created «RS Printer» go to «Start» «Devices and Printers», right-click on the «RS printer» and select «Printer properties»
Check the selected COM-port and the settings under «Ports» and «Configure Port…»
Check the settings under «Advanced»:
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Enter «stopp» in the field «End Print Job» under «Printer Commands»
3.2 Installation of MagIC NetTM
All programs must be shut down first. Install MagIC NetTM (MagIC NetTM CD). All the standard directories proposed by the program should be accepted. Restart windows.
Connected USB devices are automatically recognized when MagIC Net is started. The Microsoft Installation Wizard is accepted and executed. After confirmation of the automatically generated request, the devices are stored in the configuration. The devices are predefined as «850 Professional IC 1» and «858 Professional Sample Processor 1». Name them accordingly, if other names appear in your configuration (e.g. due to changed setting on your computer).
3.3 Configuration of MagIC NetTM
In the window configuration, the 850 Professional IC, the 858 Professional Sample Processor and the columns Metrosep A Supp 5 - 150/4.0 and Metrosep C 4 - 100/4.0 are visible. Add and define the eluents and the suppressor solutions.
The settings for the rack require a «work position» fitting to the respective rack (e.g. 125 mm for rack 6.2041.450).
Click «Apply» and «OK».
Also define an «External 1» position to access the rinsing station for rinsing the needle. The needle position is in the inner compartment which corresponds to an angle of ~116° and a work position of 120 mm. The exact angle depends on your installation (see chapter 2.4).
For the outer compartment, an external position 2 can be defined with an angle of ~110° and a work position of 60 mm. The external position 2 could be used as drain position (e.g. to expel sample directly to the waste), however, it is not carried out during the time program of method VoltIC pro I.
Application Bulletin 356
Installation instruction for «VoltIC pro I»
Page 12 of 18
For the data transfer from the VA Computrace software to MagIC Net an RS 232 device must be added to the device list as follows:
Go to the Configuration window in MagIC Net and select «New» from the «Edit» button in the Device window. Select the «RS 232 Device» from the «Miscellaneous» list:
Rename the device «797 RS232 Printer». Enter «1» in the field «serial number».
Make the following settings under «RS 232»: (Attention: the second newly generated COM port by the
null modem cable has to be selected as «COM Port», e.g. COM 15 !)
Enter «stopp» in the field «Terminator for receive».
In the window method, import the method for VoltIC pro I from the installation CD: Go to File method manager and choose your method group. Afterwards, click on edit import and choose the pathway on the installation CD (MagICnet\examples\methods\VoltICpro.imet).
The method carries out a parallel determination of cations and anions. Immediately after starting the anion determination, the cation determination (of the same sample) is initialized. Samples could be taken from the same vial, or from two vials with one of them containing the acidified sample solution for cation determination. Both measurements are recorded in the same data file. In order to measure samples from two different vial please select method «VoltICpro_mod.imet» from the same folder.
In the window method, open the VoltICpro method and assign the following equipment: Assign the column
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Metrosep A Supp 5 - 150/4.0 to the analysis anion, assign the column Metrosep C 4 - 100/4.0 to the analysis cation, assign the two eluents to their respective IC pump, match the two suppressor solutions to the IC peristaltic pump, and define the rack of the connected sample processor. Adjust the temperature of the column oven to 30°C. Save the method.
In order to start the equilibration, go to the window work place, load your method, and press «Start HW». Before inserting the columns, flush the system for about 10 minutes and get rid of air bubbles (by using the purge valve and syringe), then insert and rinse the precolumns for 10 minutes, and only afterwards put the analytical columns into the flow (see also 850 manual).
3.4 Installation of 797 VA Computrace software
Install the software. All the standard directories proposed by the program should be accepted. Restart windows.
Connected USB devices are automatically recognized when VA Computrace software is started.
3.5 Configuration of 797 VA Computrace software
Make the following general settings in the main window under «Settings» «General Settings»s” and click «OK»:
Load method «Det of Zn Cd Pb Cu_IC_VA.mth», modify or create a new method.
Click on «Dosinos» in the «Working Method Specifications» window and make following settings:
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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3.6 Starting a determination
The hyphenated analysis of IC and VA follows the cycle described below:
All sample information (sample ID, dilution factor, etc…) is
programmed in MagIC NetTM. MagIC NetTM triggers VA Computrace software by remote
signal. VA Computrace software will feeds back information to
MagIC NetTM after preparing the measuring cell (before sample transfer) and after VA analysis has been finished and the cell has been prepared for the next analysis.
Please follow the steps below for system startup:
Close all applications  Turn on all instruments (843 Pump Station should be
switched on after the 797 VA Computrace, otherwise pumps start pumping)
Start MagIC NetTM and check if all hardware
components have been recognized and available in the configuration window.
Load method «VoltICpro.imet» in MagIC NetTM  Start VA Computrace and check if hardware
components have been recognized
Load «Det of Zn Cd Pb Cu_IC_VA.mth» in VA
Computrace software
Under «Settings» «General Settings»
«Automation» activate «Remote Start» and «End of Sample» and click «OK» (This must be done with every restart of VA Computrace software as these settings are not saved!)
Prepare both systems:
Ion chromatograph
o Equilibrate the system («Start HW») o Check for stable system pressure (+/- 0.1
MPa) on both channels; remove air bubbles manually if necessary
o Check for stable baselines (anion channel:
~0.9 µS/cm, cation channel: ~680 µS/cm for
the mentioned eluents, refer 2.2) VA o Check working electrode and reference
electrode; refill if necessary o Check nitrogen pressure, performance of
working electrode (create new drops) o Perform electrode check
Start the VA method (VA will wait for trigger signal from
MagIC NetTM)
Enter the amount of standards and standard
concentrations in MagIC NetTM
Enter sample table in MagIC NetTM
For quantitative analysis, samples subjected to cation analysis are normally acidified, whereas anion analysis is normally carried out with unmodified samples. Method «VoltICpro.imet» includes only one sample for anion, cation and heavy metal analysis. Method «VoltICpro_mod.imet» includes 2 sample vials on the rack for each sample (an unmodified one for anion determination and an acidified one for cation and heavy metal determination). According to the method «VoltICpro_mod.imet» the position of the vial for anion determination should be defined in the column «sample position» and the position of the vial for cation and heavy metal determination is the subsequent one.
Both methods «VoltICpro.imet» and «VoltICpro_mod.imet» include variable sample volume for VA analysis (0.2 mL – 10 mL). The desired sample volume is entered as «Value 1» (see sample table below).
As the VA Computrace software calculates with a fixed sample volume of 10 mL, the difference to 10 mL is dosed by the optional Dosino (ultrapure water) directly into the VA vessel.
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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Correlation coefficient
Relative standard deviation [%]
Lithium
0.999984
0.761
Sodium
0.999947
1.347
Ammonium
0.999939
1.371
Potassium
0.999776
2.904
Calcium
0.999864
1.813
Magnesium
0.999973
0.890
Correlation coefficient
Relative standard deviation [%]
Fluoride
0.999954
1.594
Chloride
0.999988
0.786
Nitrite
0.999992
0.650
Bromide
0.999993
0.584
Nitrate
0.999993
0.587
Phosphate
0.999997
0.408
Sulfate
0.999992
0.616
The recalculation to the actual sample volume used (Value
1) takes place after the VA analysis in MagIC NetTM. Therefore, your sample table might look like the following
one:
Fig.: Sample table excerpt showing the use of «VoltICpro.imet»
For evaluation and after recording the first chromatogram, check the retention times of your compounds. Since they depend on the performance of your column, you may have to adjust them in your method.
4 Exemplary measurement
An exemplary measurement was performed, including the ions fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfate, lithium, sodium, ammonium, potassium, calcium, and magnesium (1000 µg/L each), zinc, cadmium, lead and copper. Anions and cations were measured from separate sample vials with the sample for cation measurement being acidified with 50 µL nitric acid (2 mol/L) per 50 mL sample. The two following chromatograms were recorded in parallel.
For the calibration, the average peak areas of 3 injections were evaluated. Within the concentration range of 20 – 1000 µg/L, a quadratic curve type was used for evaluation of anions, and a linear curve type was used for evaluation of cations. Correlation coefficients and standard deviations are listed in the following table. The calibration curves for chloride and sodium are shown as examples.
Fig.: Statistical data of a six-point cation calibration from 20 µg/L to 1000 µg/L
Fig.: Standard chromatogram cations, 1000 µg/L
Fig.: Standard chromatogram anions, 1000 µg/L
Fig.: Statistical data of a six-point anion calibration from 20 µg/L to 1000 µg/L
Fig.: Chloride calibration curve from 20 µg/L to 1000 µg/L
Application Bulletin 356
Installation instruction for «VoltIC pro I»
Page 16 of 18
Fig.: Sodium calibration curve from 20 µg/L to 1000 µg/L
Fig.: Example of a combined report for IC and VA results in the MagIC Net database
Fig.: Example voltammogramm of Zn, Cd, Pb and Cu determination
Fig.: Standard addition graphs of Zn, Cd, Pb and Cu determination (sample: table water, Add 1)
Application Bulletin 356
Installation instruction for «VoltIC pro I»
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5 Appendix
5.1 Time Program
Time program «VoltICpro.imet»
Application Bulletin 356
Installation instruction for «VoltIC pro I»
Page 18 of 18
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