Application Bulletin 318 e. Installation Instructions of TitrIC 4

Transcription

1 The TitrIC 4 System is used for the fully automatic analysis of water samples using direct measurement, titration and ion chromatography. The following parameters are determined in a very short time: temperature, conductivity, ph, acid capacity, calcium, magnesium, total hardness and, in parallel, the concentrations of the individual anions. Further Metrohm instruments can be incorporated in the existing system at any time and used to measure additional parameters. Analytical sequence 1. Conductivity is measured in the sample vessel on the sample processor. 2. First sample transfer to the 881 Compact IC pro. 3. The IC anion determination is started automatically. 4. Second sample transfer to the external titration cell of the 815 Robotic USB Sample Processor XL. 5. Temperature, ph and acid capacity (p and m values) calcium, magnesium and total hardness are determined. The whole procedure is controlled by the TitrIC software: The user enters the sample position and sample identification, IC system and tiamo TM method, after which TitrIC transfers all the relevant information to tiamo TM and MagIC Net. When the measurement has been concluded, TitrIC automatically generates a joint report containing all results. This report can be printed out or exported as an Excel file.

2 Page 2/16 Table of contents 1 Delivery package Installation Robotic USB Sample Processor XL Conductometer ( ) Titrando ( ) Dosino holder ( ) Compact IC pro Anion MCS ( ) Cable connections Tubing connections External cell Installation of the 50 ml Dosing Unit Overview of all the tubing connections Miscellaneous Stirrer Electrodes Software Installation of the software Configuration of tiamo TM Devices Swing Head configuration Special beaker definition Lift positions Solutions Electrodes Methods Configuration of the export template Configuration of MagIC Net Configuration of TitrIC... 16

3 Page 3/16 1 Delivery package - delivered with TitrIC 4 package: Number Article no. Article designation IC Compact IC pro Anion - MCS Sample processor Robotic USB Sample Processor XL with 2 pumps Swing Head Titration head Conductometry Conductometer Five-ring conductivity measuring cell, c = 0.7 cm -1, with integrated Pt Cable USB A mini-din 8 pins Titrations / ph measurement Titrando (incl. 854 iconnect, 2 meas. interfaces) Aquatrode; combined ph glass electrode (with temperature measurement) Polymer membrane electrode Ca Cable USB A - mini-din 8P Electrode cable with 2 x plug B (4 mm, 1m) Electrode cable 1 m, F Pufferlösung ph=4 (500 ml) Pufferlösung ph=7 (500 ml) Pufferlösung ph=9 (500 ml) Phit kit Liquid Handling Dosino Dosing Unit, glass, 50 ml Dosing Unit, glass, 20 ml Dosing Unit, glass, 10 ml Dosino holder Glass bottle GL45 1L (round) Connecting set for Dosing Unit: Dosino port Coupling M6-UNF 10/32 (Dosing Unit IC screw) Pressure screw made of PEEK, short Aspiration tip 1.5 / 240 mm External cell Rod Stirrer Stand support for Titration vessel lid micro Titration vessel Stopper with nipple and O-ring way stopper with antidiffusion valve Screw nipple Septum stopper Screw nipple for electrodes Connection tubings Connection tubing FEP, L = 60 cm, 2 x M6 thread, i.d. = 2 mm Connection tubing FEP, L = 150 cm, 2 x M6 thread, i.d.= 2 mm PTFE capillary, L = 5 m, i.d.= 0.97 mm Software Tiamo TM 2.1 full MagIC Net 2.0 Compact CD: 1 Licencse TitrIC 2.0

4 Page 4/16 - optional accessories: xxx Sample rack made of PVC xxx Sample beaker made of glass xxx Anion column Metrosep A Supp xxx Guard column Metrosep A Supp xxx Cation column Metrosep C xxx Guard column Metrosep C Storage solution Electrolyte solution (3 mol/l KCl) Conductivity standard (100 µs/cm) Conductivity standard (12.88 ms) /110/120 Buffer solutions 500 ml, ph 4 / 7 / Stacking frame for 846 Dosing Interface, 856 Conductivity Module,867 ph Module

5 Page 5/16 2 Installation The following is a detailed description of the TitrIC 4 System's installation. We strongly recommend that the individual steps are carried out in the order given below! Robotic USB Sample Processor XL The sample processor is placed at the side at which it is most easily accessible. Please note that the following procedure refers exclusively to the version in which the sample processor is located at the lefthand side of the system. On the right-hand side of the 815 Robotic USB Sample Processor XL, attach the stand support ( ) without the horizontal brace to the tower of the 815 (hexagon screw beneath membrane pump 1). The brace will be installed later. Do not screw the swing arm ( ) onto the Swing Head! The Sample Rack supplied is screwed onto the 815. In the vicinity of the 815 the two canisters (standard equipment of 815) are placed on the floor: One 10 L canister is used as a waste container, the second as a reservoir for deionized (DI) water used for rinsing the external cell. From the smaller opening of the canisters containing DI water, an M8 PTFE tubing connection of suitable length is led to the connection box made of white plastic of membrane pump 1 and connected. From the front opening of the waste canister an M8 PTFE tubing connection of suitable length is led directly to membrane pump 2 (black plastic) and connected. A more detailed description is given in the Instructions for Use of the 815 Robotic USB Sample Processor XL Conductometer ( ) The 856 Conductometer is placed directly at the right of the sample processor. For detailed information about the usage check the Instructions of Use of the 856. It is recommended to carry out the calibration of the cell constant in tiamo TM before measurements. For further information consult the installation instructions of the 856 Conductometer. 2.3 Titrando ( ) Directly to the right of the 856 Conductometer, place the Titrando with the titration solution (0.05 mol/l EDTA, at the front, with 10 ml Dosing Unit and 800 Dosino) and the auxiliary complexing solution (0.2 mol/l TRIS / 0.1 M Acetylacetone, at the rear, with 20 ml Dosing Unit and 800 Dosino). 2.4 Dosino holder ( ) The Dosino holder ( ) is placed at the back of the Titrando and the 856 Conductometer; the 50 ml ( ) Dosing Unit is screwed and the 20 ml ( ) Dosing Unit is placed with its 0.1 mol/l HCl titration solution onto this holder at a later stage. 2.5 Compact IC pro Anion MCS ( ) Place the 881 Compact IC pro for anions ( ) to the right of the bottle holder. The instrument can already be installed. Please consult the Instructions for Use for the Compact IC pro instrument.

6 Page 6/16 3 Cable connections First all the power cables are connected to the instruments. Both the instruments and the PC remain switched off. Cable USB A - mini-din 8P ( ) from 856 Conductometer to PC, do not connect! USB cable ( ) from Compact IC pro IC to PC. USB cable ( ) from PC to 905 Controller, do not connect! MSB cable from Dosino 800, 50 ml (Liquid Handling) to 905 MSB 1, do not connect! MSB cable from Dosino 800, 20 ml (0.1M HCl) to 905 MSB 2, do not connect! MSB cable from Dosino 800, 10 ml (EDTA solution) to 905 MSB 3, do not connect! MSB cable from Dosino 800, 20 ml (Auxiliary complexing solution) to 905 MSB 4, do not connect! USB cable ( ) from controller of 815 to USB of 905.

7 Page 7/16 4 Tubing connections 4.1 External cell The numbers given here (, ) and «opening 1,...» refer to the drawing below. In the next step the external cell is prepared. The following components are inserted in the titration vessel lid ( ): The small stoppers (with the black rubber ring) are screwed loosely into openings 1, 2, 3, 5 and 7 and fixed in position when the buret tips, etc. are inserted. The large stopper will be screwed into opening 9, the septum stopper ( ) without the upper part into opening 6 and the screw nipples ( ) into openings 4, 6 and 8. The titration vessel lid is attached to the stand support ( ) using opening 10. It is fixed at the required height with the clamping ring and the horizontal brace of the stand support is mounted on the 815 with the socket head screw. Numbers and connections on the titration vessel lid ( ) The M8 PTFE aspiration tip ( , supplied with 815) is inserted in opening 1 and connected to membrane pump 2 of the 815 with the M8-PTFE-tubing ( ). The rinsing nozzle ( , supplied with 815) is inserted into opening 2, which is connected to membrane pump 1 of the 815 with the FEP-tubing ( , supp. with 815). The buret tip ( , supplied with 807) is inserted through opening 3 and will be connected to the connection set ( , see next page), port 4 of the 50 ml Dosing Unit (LQH) with the 60 cm FEP-tubing connection ( , supplied with 815). This is where the ph electrode will later be inserted. The rinsing nozzle ( , supplied with 815) is inserted into opening 5, which is connected to membrane pump 1 of the 815 with the FEP-tubing connection ( ). The septum stopper ( ) (without upper screw and septum) and the screw nipple ( ) are pushed/screwed into opening 6. Then the 3-way stopper ( ) is inserted. The 3 connectors are connected to port 1 of the three Dosing Units 10 ml (EDTA), 20 ml (Auxiliary complexing solution) and 20 ml (0.1 mol/l HCl) with three 40 cm FEP-tubing connections ( , supplied with 807 Dosing Units). The rinsing nozzle ( , supplied with 815) is inserted into opening 7, which is connected to membrane pump 1 of the 815 with the FEP-tubing connection ( ). This is where the Ca-ISE ( ) will be inserted. This is where the 802 Rod Stirrer will be inserted.

8 Page 8/ Installation of the 50 ml Dosing Unit Luer: Port Port Port M6: Port Connections on the bottoms of the 50 ml Dosing Unit Port 1 is used for emptying the Dosing Unit into the waste canister. Port 2 is used by the 50 ml Dosing Unit for aspirating the sample via the titration arm. Port 3 is used for sample transfer to the IC system. The transition from M6 to the IC screw size (1/16 in.) is achieved with the adapter. Port 4 is used for the 50 ml Dosing Unit. This requires a coupling between Luer and M6: The PEEK connection ( ) is attached to the Luer connection on the bottom of the Dosing Unit. The 60 cm M6 FEP-tubing can be directly connected to the Luer/M6 adapter to realize «liquid handling» to the external cell. Once the tubing connections have been made, the Dosing Units are attached to the Dosino holder ( ) with the screw attachment and the distance ring of the Connecting Set for Dosing Unit ( ).

9 Page 9/ Overview of all the tubing connections The three 60-cm-FEP-tubing connections ( , supplied with 815) are used to connect membrane pump 1 of the 815 and the three rinsing nozzles ( , supplied with 815) to openings 2, 5 and 7 of the external cell (see page 7). The 60-cm-M8-PTFE-tubing connection ( , supplied with 815) is used to connect membrane pump 2 of the 815 and the M8 PTFE aspiration tip ( , supplied with 815) to opening 1 of the external cell (see page 7). The aspiration tip ( ) is attached by a stopper ( ) to the titration head ( ). The 80-cm-FEP-tubing connection ( , supplied with 815) is used to connect the aspiration tip ( ) at the titration head ( ) and port 2 of the 50 ml Dosing Unit. The three 40-cm-FEP-tubing connection ( , supplied with 807) are used to connect port 1 of the 10 ml (EDTA) and the two 20 ml Dosing Units (HCl / Auxiliary complexing solution) with the three connectors of the 3-way stopper at opening 6 of the external cell (see page 7). The 60-cm-FEP-tubing connection ( ) is used to connect port 4 of the 50 ml Dosing Unit and the buret tip ( , supplied with 807) in opening 3 of the external cell (see page 7). A suitable length of the 0.97 mm PTFE capillary ( , supplied with 881) is used to connect port 3 of the 50 ml Dosing Units (using the screws and ) and the injection valve of the 881 Compact IC pro. The four 150-cm-FEP-tubing connections ( ) are connected to port 1 of the 50 ml Dosing Units, as well as port 3 of the two 20 ml and the 10 ml Dosing Units; all four tubing connections are then connected to the 10 L PE waste canister ( ).

10 Page 10/16 5 Miscellaneous 5.1 Stirrer The 802 Rod Stirrer is inserted through opening 9 of the external cell (see page 7) and connected to the tower of the 815. The propeller ( ) is pushed on from below. Length of the aspiration tips in the external cell Clamp the titration vessel ( ) to the titration vessel lid ( ). The M8 aspiration tip in opening 1 must reach right to the base of the titration vessel as this is the only way to ensure that the external cell is cleaned properly. The buret tips of the 3-way stopper in opening 6 and the buret tip of opening 3 should reach the middle of the titration vessel. The three tubings of the 3-way stopper have to be mounted with antidiffusion micro valves to ensure a precise titration. 5.2 Electrodes The ph electrode (Aquatrode Plus with Pt 1000; ) is inserted into opening 4. The cable is connected to the Titrando at Input 2. The plug of the gray cable is connected to the opening marked Ind.. The red plugs with the adapters and are inserted in the openings marked Temp. If the electrode is not used for some time then it should be returned to its holder and kept in the storage solution ( ). The Ca-ISE (Polymer membrane electrode Ca, ) is connected to the electrode cable ( ) and inserted into opening 8. The cable is connected to the Titrando at Input 1. The plug of the gray cable is connected to the opening marked Ind.. To have a reference electrode for the Ca-ISE one can short-circuit the reference channel of the Ca-ISE with the one of the Aquatrode. Thereto connect Ref. of Input 1 with Ref. of Input 2 with the electrode cable 2x plug B ( ). Conductivity cell ( ): The measuring cell cable is led through the guide chain of the 815 and the plug is inserted into the opening marked Cond. Cell of the 856 Conductometer. Later (as soon as the titration head has been mounted) the measuring cell with the SGJ sleeve ( ) will be inserted in the SGJ 14 opening of the titration head. 6 Software 6.1 Installation of the software tiamo TM 2.1 installation (tiamo TM CD): All the standard directories proposed by the program should be accepted. MagIC Net 2.0 installation (MagIC Net CD): All the standard directories proposed by the program should be accepted. Restart windows. TitrIC 2.0 installation (TitrIC CD): TitrIC 2.0 must only be installed after tiamo TM 2.1 and MagIC Net 2.0 have already been installed. After installation the standard TitrIC directory can be found under C:\Program files\ Metrohm\TitrIC, the TitrIC.exe file under C:\Program files\metrohm\tiamo\bin. The TitrIC database and reports are found on C:\Documents and Settings\All Users\ApplicationData\TitrIC. All programs should be closed!

11 Page 11/ Configuration of tiamo TM The controller cable ( ), which is already connected to the 905, is now connected to an USB interface on the PC. Wait a few seconds. The driver installation for 905 and 815 follows. It s not necessary to start windows update, click on automatic installation of the software for both. The controller cable ( ), which is already connected to the 856 conductivity module, is now connected to an USB interface on the PC tiamo TM 2.1 is started Devices Connected USB devices are automatically recognized when tiamo TM is started. After confirmation of the automatically generated request the devices are stored in the configuration. Keep the proposed device names Swing Head configuration Under Configuration at the top left, double-click on 815_1 under Devices, click on the entry Tower 1, set the Axial distance to mm and in the middle of the window under Swing Head click on Configuration and Yes and then enter the following values: Configuration of the Swing Head for Titration head Confirm the entries twice with <OK> and then mark 815_1 under Devices and click on Edit / Initialize. Wait until the initialization has been finished. The titration head ( ) can now be mounted on the Swing Head Special beaker definition Under Configuration mark 815_1, select Edit / Properties / Rack / Rack data / Special beaker, Special beaker 1, click on Edit and define the position to be used for rinsing as Rack position. The last position on the rack is normally used as the rinsing position. A sample vessel containing DI water should always stand in this position. Confirm by clicking on <OK> twice Lift positions Under Configuration / Tools / Manual operation click on 815 Sample Changer / Tower 1 in the left-hand column and use the entries Move and Assign position (See 815 Instructions for Use, page 47) to define suitable values (click on <Assign> each time) for: Shift position for changing the rack position (approx. 53 mm) Work position for aspirating of the sample (approx. 173 mm) Special position for dipping for the conductivity measurement (approx. 130 mm) For the special position, you must define the work position again, then at the right beside Work position click on Tower and select Special position 1. Confirm these settings with a click on close.

12 Page 12/ Solutions The solutions to be used must, as usual, be defined in tiamo TM. Connect the Dosino of the 50 ml Dosing Unit to MSB 1 of the 905, the Dosino of the 20 ml Dosing Unit (HCl) to MSB 2 of the 905, the Dosino of the 10 ml Dosing Unit (EDTA) to MSB 3 of the 905 and the Dosino of the 20 ml Dosing Unit (Auxiliary complexing solution) to MSB 4 of the 905. The user is automatically requested to save the solutions click on <Yes>. In order to ensure compatibility with the methods provided, they must be named as described below. At the left click on Configuration, then at the top right under Titrants / Solutions double-click on the appropriate (empty) entries and enter the following under Solution name and Concentration: Configuration table for titrants / solutions Now the tubing lengths and ports are defined for each Dosing Unit under Edit / Properties / Dosing unit as follows: Anion HCl EDTA Auxiliary complexing sol Port Length Port Length Port Length Port Length Dosing Port Prep/ Empty Special Port - Dosing Port 1 - Dosing Port 1 - Dosing Port 1 - Dosing Port 1 Port 4 60 cm Port 1 40 cm Port 1 40 cm Port 1 40 cm Dosing Port 2 Port 3 0 cm Port 3 0 cm Port 3 0 cm Port 3 0 cm Fill Port Port 2 80 cm Port 2 25cm Port 2 25 cm Port 2 25 cm Special Port Port 1 0 cm Port 4 0 cm Port 4 0 cm Port 4 0 cm Configuration table of the four Dosing Units Electrodes ph electrode: Under Configuration/Sensors click on Edit / New / ph electrode and enter under Sensor name Aquatrode Plus, type in the desired sensor information (e.g. serial number) and click on <Ok>. Ca-ISE: Under Configuration/Sensors double click on the entry ISE electrode and type in the desired sensor information (e.g. serial number) and click on <Ok>. Conductivity sensor: Under Configuration / Sensors click on Edit / New / other sensor and enter under Sensor name Conductivity sensor type in the desired sensor information and click on <Ok> Methods The following methods are provided for tiamo TM : TitrIC 4 - complete run: With this method all the available parameters are measured and the IC measurement is initiated.

13 Page 13/16 TitrIC 4 - preparation of titration equipment: This method is used for preparing all titration instruments, i.e., rinsing the tubing connections of the Dosing Units with reagents or deionized water and rinsing the external cell. Start this method only from tiamo TM not from TitrIC! TitrIC 4 - IC calibration: This method is used for calibrating the IC measurement with standard solutions without the titration part of a typical TitrIC measurement; this means that a lot of standard solution can be saved. TitrIC 4 semi automated ph calibration: With this method the ph electrode is calibrated semiautomatically; the buffer solutions are flushed into the titration vessel. Start this method only from tiamo TM not from TitrIC! TitrIC 4 - ph calibration: Here the Aquatrode is taken out of the titration vessel and placed into the buffer solutions. Start this method only from tiamo TM! TitrIC 4 - titer determination of EDTA: This method is used for the titer determination. Start this method only from tiamo TM! TitrIC 4 - titer determination of HCl: This method is used for the titer determination. Start this method only from tiamo TM! TitrIC Calibrate 856 conductivity module This method is used for calibration of the conductivity module. Start this method only from tiamo TM! Import: Click on Method at the left, then select under File / Method manager / Edit / Import in the following directory on the CD you will find all methods: \Methods\Titration. Note! Alterations of these methods should only be carried out by a person at the administrator level and who is thoroughly familiar with tiamo TM. Never forget that in TitrIC this new method must be selected in the sample table under Methods tiamo Configuration of the export template Export template: tiamo TM must transfer its results to TitrIC in a particular way, which means that the export template must be generated exactly in the following form: Under Database / Tools/ Templates / Export templates / New enter the following: Configuration of the export template in TitrIC The target directory for the report is as following: Windows 2000, Windows XP: C:\Dokumente und Einstellungen\All Users\Application Data\Titric\reports Vista, Windows 7: C:\ProgramData\Titric\reports In Windows Vista and Windows 7 hidden folders need to be made visible in the explorer to get access. Then click on Select fields and enter the following:

14 Page 14/16 Input window for the export template The entry Start counter is obtained at the left by clicking on Determination / Identification, ID1.Name and ID1.value are obtained at the left by clicking on Sample / Identifications, RS0x by clicking on Results / RS0xxx. By clicking on the upper double arrow in the center, the entries can be moved to the right. Of course another number of results than nine is possible. Shut down tiamo TM 2.1! 6.3 Configuration of MagIC Net Start MagIC Net 2.0 Configuration of the export template Export template: MagIC Net must transfer its results to TitrIC in a particular way, which means that the export template must be generated exactly in the following form: Under Database / Tools / Templates / Export templates / New enter the following: Configuration of the export template in MagIC Net

15 Page 15/16 The target directory for the report is as following: Windows 2000, Windows XP: Vista, Windows 7: C:\Dokumente und Einstellungen\All Users\Application Data\Titric\reports C:\ProgramData\Titric\reports In Windows Vista and Windows 7 hidden folders need to be made visible in the explorer to get access. Then click on Select fields and enter the following: Input window for the export template The entry Start counter is obtained at the left by clicking on Determination/Identification, Info 1 is obtained at the left by clicking on Sample / Identifications and Ident by clicking on Sample / Sample Data. Results are obtained at the left by clicking on Results. By clicking on the upper double arrow in the center, the entries can be moved to the right. Of course another number of results is possible. On the CD under \Methods\IC the TitrIC software contains predefined IC methods. Import the TitrIC 4 method into MagIC Net. Herefore, go to the Method section on the left and follow the path File/Method manager to choose Edit and Import. The suppressor step is not made at the start of the measurement in the usual way, but with <Fill> directly after the end of the chromatogram. This means that after long pauses between measurements the suppression may no longer function. This is why after longer pauses you should carry out a suppressor step manually and ensure that the injection valve is in the <Fill> position. Depending on the application and column it may be necessary to adapt the time program in the IC system: <Inject> should always be carried out right at the start of the time program, <Fill> right at the end. In this way you can start to measure with a stable baseline immediately after the sample loop has been filled by the Dosinos. If a calibration is carried out later and the new calibration data are to be applied to a sample that has already been measured, then please refer to the online help of the TitrIC software under Database / Recalculate / Recalculate for the results of several samples. Shut down MagIC Net 2.0

16 Page 16/ Configuration of TitrIC TitrIC is started (MagIC Net and tiamo TM are started automatically after each other) All paths have already been entered as defaults and the system is ready for work. If other paths are used instead of the default paths, then this must be altered in the corresponding dialog under Workplace / Settings /. TitrIC starts MagIC Net first and after the tiamo TM software is started. If TitrIC is shut down then tiamo TM and MagIC Net will also be shut down. MagIC Net will ask you if you want to shut down all devices. Always shut down TitrIC as the first program! For further information please consult the TitrIC online help (? / Show Help) or contact your local Metrohm agency. You can also report your problems to the following support titric@metrohm.com. Always start and shut down TitrIC first!