IC Equipment Thin-Layer cell Manual 8.110.
Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com IC Equipment Thin-Layer cell 6.5337.200 Manual 8.110.8020EN 06.
Teachware Metrohm AG CH-9100 Herisau teachware@metrohm.com This documentation is protected by copyright. All rights reserved. Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above. Documentation in additional languages can be found on http://documents.metrohm.com.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents Table of contents 1 Introduction 1.1 1 Description ............................................................................ 1 1.2 About the documentation ................................................... 1 1.2.1 Content and scope .................................................................. 1 1.2.2 Symbols and conventions ........................................................ 2 2 Overview 3 3 Installation 4 3.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Table of figures Figure 1 Figure 2 Figure 3 IV ￭￭￭￭￭￭￭￭ Thin-Layer cell – Parts and connectors ............................................... 3 Ag/AgCl reference electrode (6.1257.720) ......................................... 6 Disassembling the measuring cell ....................................................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction 1 Introduction 1.1 Description The Thin-Layer cell is used for amperometric detection with the Amperometric Detector. The Thin-Layer cell especially qualifies for applications with double detector mode, e. g. if an amperometric detection is followed by another detection technique. In the Thin-Layer cell, the sample flows in a thin layer between the auxiliary electrode and the working electrode and is analyzed with amperometric methods. 1.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1.2 About the documentation 1.2.2 Symbols and conventions The following symbols and formatting may appear in this documentation: Cross-reference to figure legend The first number refers to the figure number, the second to the instrument part in the figure. Instruction step Carry out these steps in the sequence shown.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview 2 Overview 1 7 9 8 10 6 2 3 5 4 Figure 1 Thin-Layer cell – Parts and connectors 1 Fastening screw For fixing the reference electrode in place. Labeled with RE. 2 Measuring part With built-in auxiliary electrode. 3 Spacer 4 Pressure screw For fixing the working electrode (WE) in place. 5 Base part 6 Stopper For sealing the deaeration opening. 7 Chip With intelligence. For inserting the measuring cell into the detector. 8 Eluent input Labeled with In.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.1 Inserting the working electrode 3 Installation Caution Never switch on the measuring cell.. ￭ ￭ 3.1 ... if it is not simultaneously being rinsed by a conductive eluent; or ... if the electrode cables are not completely connected. Inserting the working electrode The measuring cell is supplied without electrodes. The working electrode must be ordered separately.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.2 3 Installation Inserting the reference electrode The measuring cell is supplied without electrodes. Reference electrodes must be ordered separately. Insert the reference electrode as follows: Inserting the reference electrode The reference electrode itself and one sealing ring are contained in the packaging for the reference electrode. 1 Slide the sealing ring over the reference electrode. 2 Unscrew the fastening screw on the RE connector and remove it.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.2 Inserting the reference electrode 3 5 2 1 Figure 2 4 Ag/AgCl reference electrode (6.1257.720) 1 Plug 2 Reference electrode cable Permanently mounted on the reference electrode. 3 Sealing screw For sealing the storage vessel. 4 Reference electrode 5 Storage vessel For storing the Ag/AgCl reference electrode. Insert the reference electrode as follows: Inserting the Ag/AgCl reference electrode 1 Take the Ag/AgCl reference electrode out of the storage vessel.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 2 Unscrew the fastening screw from the reference electrode holder. Push the fastening screw over the cable of the Ag/AgCl reference electrode. 3 Check whether the sealing ring is seated on the reference electrode and insert the reference electrode into the reference electrode holder. 4 Tighten the reference electrode to the reference electrode holder with the fastening screw.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.3 Connecting the detector capillaries 3.3 Connecting the detector capillaries The amperometric detector has a preheating capillary in its interior that ensures that the eluent flows through the measuring cell at a constant temperature. Connecting the preheating capillary is optional. If the ambient conditions are optimal or if the eluent in the column is heated, then the measuring results can be sufficiently accurate, even without the use of the preheating capillary.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Connect the cell output Use a pressure screw (6.2744.014) to fasten a 1–1.5 m long piece of the PEEK capillary (6.1831.010) to the Out connector on the measuring cell. Note This capillary must be tested with the IC instrument the first time the detector is put into operation, see Chapter "Start-up" in the manual for the detector.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.4 Connecting the electrode connection cables 3.4 Connecting the electrode connection cables Caution The electrode cables may not be plugged or unplugged unless the measuring cell is switched off in the software. Note The sockets and the plugs of the cables must be clean and dry. Connecting the electrode connection cables to the detector Prerequisites: ￭ The measuring cell is switched off.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Plug in the angled plug of the auxiliary electrode connection cable (labeled with AE) into the socket (labeled with AE).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up The measuring cell must be put into operation together with the amperometric detector. Additional information in this regard can be found in the manual for the detector.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance 5 Operation and maintenance 5.1 Operation The measuring cell is operated together with the detector and the entire IC system with the MagIC Net™ software. Additional information for operation with MagIC Net™ can be found in the "Tutorial for MagIC Net™" or in the MagIC Net™ online help. 5.2 Maintenance The measuring cell must be taken out of the detector for the following maintenance tasks.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.2 Maintenance 1 Unscrew the pressure screw (1-4) on the base part of the cell and remove it. 2 Take out the working electrode. 3 Insert the new working electrode. The working electrode is formed in such a way that it can be inserted into the measuring cell in only one position. 4 Slide the pressure screw over the working electrode and screw it tightly. 5.2.2 Replacing the reference electrode Note These instructions apply analogously to the Ag/AgCl reference electrode.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance 2 Unscrew the fastening screw for the reference electrode and remove it. 3 Take out the reference electrode. 4 Insert the new reference electrode. 5 Retighten the fastening screw. Note Important: After an Ag/AgCl reference electrode has been taken out! The Ag/AgCl reference electrode may not be allowed to dry out. Follow the directions for storage contained in the leaflet for the Ag/AgCl reference electrode. 5.2.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.2 Maintenance To disassemble the measuring cell, you need a 2.5 mm hexagon key. 1 2 3 4 5 Figure 3 Disassembling the measuring cell 1 Fastening screw (4x) 2 Pressure screw For fastening the working electrode. 3 Base part 4 Spacer 6.1257.820 or 6.1257.840 5 Measuring part With auxiliary electrode. 1 Remove the reference electrode. 2 Remove the working electrode. 3 Unscrew the four screws on the base part of the measuring cell with the hexagon key and remove them.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance Replace the spacer as follows: Replacing the spacer Prerequisites: ￭ ￭ The measuring cell is disassembled. The new spacer is dry, clean and lint-free. You will need a 2.5 hexagon key and a pair of tweezers to replace the spacer. Wear latex gloves when replacing the spacer. 1 Positioning the spacer ￭ ￭ Hold the measuring part in your hand as shown in Figure 3, page 16. Use tweezers to place the new spacer on the measuring part.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.2 Maintenance The working electrode has been removed from the measuring cell. ￭ 1 Note When cleaning the auxiliary electrode, the edges of the spacer may get damaged. The spacer must then be replaced. ￭ ￭ Moisten a cotton swab with 2 mol/L of nitric acid. Use this to carefully wipe the auxiliary electrode. The edges of the spacer may be damaged when wiping the auxiliary electrode.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance Inserting the reference electrode 1 Reinsert the reference electrode (see Chapter 3.2, page 5).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Technical specifications Structure Flow cell with working, reference and auxiliary electrode. Material Cell body made of PEEK. Cell volume Is dependent on the thickness of the spacer: 50 µm Spacer < 0.35 µL 25 µm Spacer < 0.18 µL Maximum operating pressure 0.8 MPa (200 psi) Cell recognition Intelligent cell with automatic identification and monitoring.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Accessories 7 Accessories 7.1 Qty. 1 IC equipment Thin-Layer cell: without electrodes Order no. Description 6.1257.100 Thin-Layer cell 6.1257.820 Spacer 50 µm to Thin-Layer cell Spacer 50 µm for the amperometric Thin-Layer cell, 3 pieces. 1 6.1257.840 Spacer 25 µm to Thin-Layer cell Spacer 25 µm for the amperometric Thin-Layer cell, 3 pieces. 1 6.1831.010 PEEK capillary 0.25 mm i.d. / 3 m For all IC components.
7.1 IC equipment Thin-Layer cell: without electrodes Qty. Order no. Description 1 6.2621.140 Hexagon key 2.5 mm 1 6.2744.014 Pressure screw 2x ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ With UNF 10/32 connector. For the connection of PEEK capillaries. Material: PEEK Length (mm): 26 1 6.2802.000 Polishing set for solid-state electrodes Polishing set wit 1 polishing cloth and about 2 g aluminum oxide powder (grain size 0.3 µm).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index Index A Accessories ............................... 21 Auxiliary electrode Cleaning ............................. 17 E Electrode cable Connecting ........................ 10 I Installation Insert Ag/AgCl reference electrode .................................... 6 Insert reference electrode ..... 5 Insert working electrode ....... 4 Measuring cell ...................... 4 M Measuring cell Cleaning .............................
