761 Compact IC METROHM Ltd. CH-9101 Herisau Switzerland Phone ++41 71 353 85 85 Fax ++41 71 353 89 01 8.761.
CH-9101 Herisau/Switzerland Phone ++41 71 353 85 85 Fax ++41 71 353 89 01 Internet www.metrohm.ch E-Mail info@metrohm.ch 761 Compact IC Program «761 PC Software 1.1» 8.761.1063 Instructions for Use 07.07.
Table of contents Table of contents 1 Introduction ............................................................................................................ 1 1.1 Instrument description .......................................................................................... 1 1.2 Parts and controls .................................................................................................. 3 1.3 Information on the Instructions for Use ........................................................
Table of contents 2.8 Suppressor module ............................................................................................. 38 2.8.1 General information on suppressor module ........................................ 38 2.8.2 Preparation of the peristaltic pump...................................................... 38 2.8.3 Connection of supply bottles ............................................................... 41 2.8.4 Connection of the suppressor module ........................................
Table of contents 4.4 4.5 761 Compact IC Menu options for PC icon............................................................. 83 Select processing method and data source................................ 83 4.3.6 Watch window....................................................................................... 84 Menu options for screen icon....................................................... 84 4.3.7 Instrument icon ....................................................................................
Table of contents 4.5.4 4.5.5 4.5.6 IV Appearance ................................................................................ 145 Other graphical functions........................................................... 149 Peak editor.......................................................................................... 150 Switching on/off the peak editor ................................................ 150 Peak editor functions..................................................................
Table of contents 5 Notes – Maintenance – Faults .................................................... 169 5.1 Practical notes on ion chromatography .........................................................169 5.1.1 Separating columns............................................................................ 169 5.1.2 High-pressure pump .......................................................................... 170 5.1.3 Eluents ..............................................................................
Table of contents List of figures VI Fig. 1: Front of the 761 Compact IC .......................................................................... 3 Fig. 2: Rear of the 761 Compact IC........................................................................... 4 Fig. 3: Interior of the 2.761.0010 Compact IC ........................................................... 6 Fig. 4: Interior of the 2.761.0020 Compact IC ........................................................... 8 Fig.
Table of contents List of numbered parts and controls 1 Door to interior .................................3,7,9 40 Aspirating capillary..............................7,9 2 Connection for syringe...........................3 41 Fastening screws ................................7,9 3 Feedthrough for aspirating tubing.........3 42 Pump head...................................7,9,177 4 Aspirating tubing..............................3,7,9 43 Connection capillary............................
Table of contents VIII 79 4 Steel meshes .................................... 32 102 Bottle attachment.................................42 80 Manufit pressure screw ....................... 32 103 Supply bottle ........................................42 81 Separating column .................... 32,37,40 104 Screw..................................................177 82 End fitting ............................................. 34 105 Zircon piston ......................................
1.1 Instrument description 1 Introduction 1.1 Instrument description The 761 Compact IC is a PC-controlled system for ion chromatographic analyses. The two following versions are available: • 2.761.0010 Compact IC without suppressor module • 2.761.
1 Introduction The operation of the 761 Compact IC takes place via a PC connected to the RS232 interface with the help of the control and evaluation program «761 Compact IC». This PC program can be used to create systems for recording and evaluating chromatograms. Time programs can also be created in which a large number of instrument functions can be triggered for each program step.
1.2 Parts and controls 1.2 Parts and controls 10 761 Compact IC 1 2 3 4 POWER 9 8 7 6 5 Fig. 1: Front of the 761 Compact IC 1 Door to interior 6 Connection for drain tube for discharge of spilled liquid from the interior 2 Connection for 6.2816.
1 Introduction 11 12 13 14 13 12 10 11 15 15 Waste B Waste A 16 17 15 15 25 Transport security screws 18 Type 1.761. WARNING - Fire Hazard - 24 23a For continued protection replace only with the same type and rating of fuse f = 50-60 Hz S = 100 VA Analog Output Remote 23 100-120V: 220-240V: Detector Block Fuse 1,0A(T) 0,5A(T) RS 232 Made by Metrohm Herisau Switzerland 19 20 21 22 Fig.
1.2 Parts and controls 10 Bottle rack for holding supply bottles with eluent, regeneration solution, and rinsing solution 18 Transport security screws to secure the pump head when the instrument is transported 11 Opening for detector cable 19 Mains switch to switch instrument on and off: I = ON 0 = OFF 12 Opening for inlet capillaries for supply of eluent, regeneration solution, and rinsing solution into the inner compartment 20 Mains connection plug mains connection, see section 2.
1 Introduction 46 45 1 44 26 43 27 28 29 42 41 30 31 40 4 39 27 32 38 37 36 Fig. 3: 6 35 34 33 Interior of the 2.761.0010 Compact IC (with permanently attached accessories and 1.733.
1.2 Parts and controls 1 Door to interior 36 Filter unit PEEK (6.2821.120) 4 Aspirating tubing for aspirating the sample; 6.1803.020 PTFE tubing, length L = 52 cm 37 Connection capillary 6.1831.010 PEEK capillary, length L = 13 cm 26 Inlet capillary for injector 6.1831.010 PEEK capillary, length L = 24 cm 38 Connection capillary 6.1831.010 PEEK capillary, length L = 15 cm 27 Mounting rail for 6.2027.0X0 column holder 39 Purge valve 28 Column connection capillary 6.1831.
1 Introduction 46 45 1 44 26 43 27 28 29 42 47 41 30 31 40 4 39 27 32 48 38 49 37 36 35 34 33 Fig. 4: 8 53 52 51 50 Interior of the 2.761.0020 Compact IC (with permanently attached accessories and 1.733.
1.2 Parts and controls 1 Door to interior 39 Purge valve 4 Aspirating tubing for aspirating the sample; 6.1803.020 PTFE tubing, length L = 52 cm 40 Aspirating capillary Connection for 6.1834.010 aspirating tubing 26 Inlet capillary for injector 6.1831.010 PEEK capillary, length L = 24 cm 41 Fastening screws for pump head 42 27 Mounting rail for 6.2027.0X0 column holder 42 Pump head (6.2824.100) 28 Column connection capillary 6.1831.
1 Introduction 1.3 Information on the Instructions for Use Please read through these Instructions for Use carefully before you put the 761 Compact IC into operation. The Instructions for Use contain information and warnings to which the user must pay attention in order to assure safe operation of the instrument. 1.3.1 Organization These 8.761.
1.3 Information on the Instructions for Use 1.3.2 Notation and pictograms The following notations and pictograms (symbols) are used in these Instructions for Use: Range SYSTEM STATE Menu item, parameter or entry value Program window Button [ Ctrl ] Key 35 Part or control of 761 12 Part or control of 750 26 Part or control of 766 Hazard This symbol draws attention to a possible danger to life or of injury if the associated directions are not followed correctly.
1 Introduction 1.4 Safety notes 1.4.1 Electrical safety While electrical safety in the handling of the 761 Compact IC is assured in the context of the specifications IEC 1010-1 (protection class 1, degree of protection IP20), the following points should be noted: • Mains connection Setting of the mains voltage, checking the mains fuse and the mains connection must be effected in accordance with the instructions in section 2.4.
2.1 Overview 2 Installation 2.1 Overview 2.1.1 Flow chart The following flow chart provides an overview of all installation work. You will find more detailed information in the relevant sections. Setting up sect. 2.2 Installing accessories sect. 2.3 Mains connection sect. 2.4 Connecting PC sect. 2.5 Connecting high pr. pump sect 2.
2 Installation 28 44 26 43 81 45 46 29 32 42 Detector Column 40 36 35 Injection valve 37 39 4 63 38 60 30 66 67 68 Waste Sample Eluent Fig. 5: Connecting diagram for 2.761.0010 Compact IC without suppressor 28 44 26 43 81 96 97 33 45 46 29 32 42 Detector Column 40 36 35 4 38 36 92 90 60 30 66 89 93 91 95 91 102 103 67 102 103 68 Eluent 100 99 37 39 63 47 98 101 Sample H2SO4 H2O Waste Fig. 6: Connecting diagram for 2.761.
2.2 Setting up the instrument 2.2 Setting up the instrument 2.2.1 Packaging The 761 Compact IC is supplied together with the separately packed accessories in special packagings containing shock-absorbing foam linings designed to provide excellent protection. The instrument itself is packed in an evacuated polyethylene bag to prevent the ingress of dust. Please store all these special packagings as only they assure transport of the instrument free from damage. 2.2.
2 Installation • Insert the cable permanently attached to the detector block 46 in one of the openings 11 and the outlet capillary in one of the openings 13 of the rear panel 17. • Replace rear panel 17 and screw to the 761 Compact IC using the four knurled screws 15. 2.3.
2.3 Attaching the accessories 2.3.4 Connection of the drain tube for bottle rack The 761 Compact IC has a connection at the rear to which a drain tube for discharged liquids in the bottle rack can be attached. Proceed as follows: 2.3.5 1 Connect drain tube • Mount 6.1816.020 Silicone tubing on connection nipple 14 (see Fig. 2). 2 Lead drain tube to collecting vessel • Lead the other end of the drain tube to a suitable collecting vessel and fix in place.
2 Installation 2.3.6 Filter unit PEEK One 6.2821.120 Filter unit PEEK (see Fig. 8) is already installed between the high-pressure pump and the injection valve at the 761 Compact IC. This filter unit serves to avoid contamination by abrasive particles of the piston seals. The two other filter units PEEK supplied with the 2.761.0020 Compact IC (with suppressor) are installed between the pump tubings of the peristaltic pump and the inlet capillaries for regeneration and rinsing solution (see section 2.8.2).
2.4 Mains connection 2.4 Mains connection Follow the instructions below for connecting to the power supply. If the instrument is operated with a mains voltage set wrongly and/or wrong mains fuse, there is a danger of fire! 2.4.1 Setting the mains voltage Before switching on the 761 Compact IC for the first time, check that the mains voltage set on the instrument (see Fig. 9) matches the local mains voltage.
2 Installation 220 – 240 V 100 – 120 V 19 19 Mains switch 20 100 - 120 V 220 - 240 V 220 - 240 V 21 20 Mains connection plug 21 Fuse holder 100 - 120 V Fig. 9: Setting the mains voltage 2.4.2 Fuses One of the two fuses 1 A/slow-blow for 100…120 V or 0.5 A/slow-blow for 220…240 V is installed in fuse holder 21 of the 761 Compact IC as standard.
2.5 Connection to the PC 2.5 Connection to the PC 2.5.1 Connecting cable Always switch off 761 Compact IC and PC before you connect the two instruments with the 6.2134.100 Cable. Connect the RS232 interface 22 at the 761 Compact IC to one of the serial COM ports at the PC using the 6.2134.100 Cable (9 pin/9 pin). If only a 25-pin COM interface is available on the PC then the 6.2125.110 Adapter cable or a commercially available adapter must be used. 2.5.
2 Installation The installed files (incl. system and method files) are generally not write-protected. To prevent these files from being deleted by mistake, switch on the write-protection or make a backup copy in another directory. 2.5.3 Basic settings When the program is started for the first time several basic settings must be made for the 761 Compact IC. Proceed as follows: 1 Start program • Double-click the software icon to start the program.
2.5 Connection to the PC • Click on Options / 761 Compact IC:COM1 to open the Links window: • Click on COM1 using the right mouse button and select the Change menu item to open the following window listing all available COM ports at the PC: • Select the desired COM port to which the 761 Compact IC has been connected and click on . The window is closed. • Close the Links window by clicking on . 3 761 Compact IC Open a system • Click on File / Open / System in the main window.
2 Installation • Select the Connect to workplace menu item of the Control menu in this window. • If the connection between PC and Compact IC is working the message Hardware settings file for 761 unit with serial number '#####' not found! Create? will appear. Click in order to create the configuration file #####.761 for this instrument. • If the connection between PC and Compact IC does not work then the message Detection of hardware failed[761 Compact IC [ COM# ]] appears in the SYSTEM STATE window.
2.6 High-pressure pump 2.6 High-pressure pump In order to avoid damage to the pump it must never be operated dry. Each time that the pump is switched on always first check that the eluent supply has been connected up correctly and that sufficient eluent is present in the eluent bottle. 2.6.1 Removing the transport security screws In order to prevent the pump drive from being damaged during transport the pump head is fitted with three transport security screws 18 (see Fig. 2).
2 Installation 26 37 39 36 35 62 61 60 32 Fig. 10: Connection of the pulsation dampener 26 26 Inlet capillary for injector 6.1831.010 PEEK capillary, length L = 24 cm 39 Purge valve 32 Injection valve 60 Pulsation dampener (6.2620.150) 35 Connection capillary 6.1831.010 PEEK capillary, length L = 13 cm 61 Connection to injection valve 36 Filter unit PEEK (6.2821.120) 62 Connection to purge valve 37 Connection capillary 6.1831.
2.6 High-pressure pump 2.6.3 Connecting the eluent bottle The eluent supply line from the storage bottle to the high-pressure pump is connected as follows (see Fig. 11): Only degassed (with N2, He or vacuum) and microfiltered (0.45 µm filter) eluents should be used! The 6.1608.070 Eluent bottle (2 L) supplied is not suitable for vacuum degassing. Use a pressure-resistant container for this.
2 Installation 3 Mount CO2 absorber tube • First place a piece of cotton wool 70 followed by CO2 absorber 69 (e.g. Merck soda-lime pellets with indicator, no. 6839.1000) in the large opening of absorber tube 72 and then close it with the plastic lid. • Fasten absorber tube 72 to bottle attachment 66 with the aid of SGJ clip 71. 4 Connect aspirating tubing to pump • Insert the free end of aspirating tubing 63 into one of the openings 12 in the interior of the 761 Compact IC (see Fig. 2).
2.6 High-pressure pump 2.6.4 Deaerating the pump and rinsing the pulsation dampener The first time that it is started up the high-pressure pump must be deaerated. Proceed as follows: 1 Prepare for deaeration • Open the rotary knob on purge valve 39 by approx. ½ turn in the counterclockwise direction (see Fig. 3 and Fig. 4). • Remove the plastic stopper from connection 8 on the front panel of 761 Compact IC (see Fig. 1). • Push 6.2816.
2 Installation 30 4 Deaerate pump • Make sure that the aspirating tubing 63 for the high-pressure pump has been immersed into the eluent. • Click the button for IC pump to switch on the highpressure pump. • Use the syringe inserted into connection 8 to aspirate air until eluent flows into the syringe. • Click the button for IC pump to switch off the highpressure pump. • Close the rotary knob on purge valve 39 by turning it in a clockwise direction (see Fig. 3 and Fig. 4).
2.7 Precolumns and separating columns 2.7 Precolumns and separating columns 2.7.1 General information on precolumns The use of easily exchangeable precolumns protects the separating columns and prolongs their lifetime. The precolumns available from Metrohm (see section 6.3.2) are either real precolumns or precolumn cartridges, which are used together with the 6.2821.040 Cartridge head or the 6.2828.010 Precolumn cartridge holder.
2 Installation 28 54 73 74 75 76 77 76 75 78 75 79 80 81 Fig. 12: Installation of precolumn cartridges with cartridge head 28 Column connection capillary from injector 77 Precolumn cartridge 54 Compression fitting (6.2744.010) 78 Steel spacer (6.2821.080) 73 Manufit housing 79 4 Steel meshes (6.2821.020) 74 Steel connector (of IC separating column) 80 Manufit pressure screw 75 PTFE gasket (6.2821.010) 81 IC separating column 76 2 Steel meshes (6.2821.
2.7 Precolumns and separating columns 2.7.3 Precolumn glass cartridges with cartridge holder The precolumn glass cartridge METROSEP Anion Dual 1 (6.1006.030) is inserted in the 6.2828.010 Precolumn cartridge holder as follows (see Fig. 13): 1 Insert cartridge • Remove end fittings 82 from screw caps 83. • Insert precolumn cartridge 85 in sleeve 84 (mark flow direction of the column cartridge on sleeve, the column cartridge should always be operated in the same flow direction).
2 Installation 28 54 82 83 84 85 83 82 86 54 87 56 Fig. 13: Installation of precolumn glass cartridges with cartridge holder 28 Column connection capillary from injector 84 Sleeve for precolumn cartridge 54 Compression fitting (6.2744.010) 85 Precolumn cartridge (6.1006.030) 56 PEEK capillary (6.1831.010) 86 Connection piece for connection precolumn – column 82 End fitting 87 Screw cap for column 83 Screw cap for precolumn 2.7.4 IC anion precolumn SUPERSEP The 6.1009.
2.7 Precolumns and separating columns 2.7.5 General information on separating columns New IC separating columns are normally filled with solution and sealed at both ends. Before the column is installed in the system, it must be ensured that this solution is freely miscible with the eluent used (check manufacturer's specifications). The IC separating columns and precolumns currently available from Metrohm are listed in section 6.3.2.
2 Installation 2.7.7 Installation of the separating column without suppressor With the 2.761.0010 Compact IC without suppressor module, the IC separating column is installed as follows (see Fig. 14): 36 1 Connect column to injector • Remove end caps from column 81. • without precolumn: Screw inlet end of separating column 81 (note flow direction) to column connection capillary 28 mounted on the injector.
2.7 Precolumns and separating columns 46 45 27 Mounting rail for column holder 88 28 Column connection capillary Connection injection valve 32 – separating column 81 32 Injection valve 45 Inlet capillary for detector block PEEK capillary, fixed mounting 46 Detector block (1.733.0110) 81 Separating column 88 Column holder (6.2027.0X0) 88 27 32 81 27 88 28 Fig. 14: Installation of column without suppressor 2.7.8 Installation of the separating column with suppressor With the 2.761.
2 Installation 2.8 Suppressor module 2.8.1 General information on suppressor module The Metrohm Suppressor Module MSM for chemical suppression installed in the 2.761.0020 Compact IC comprises a total of 3 suppressor units which are in turn used for suppression, regenerated with sulfuric acid and rinsed with water. To record every new chromatogram under comparable conditions, work is normally carried out with freshly regenerated suppressor.
2.8 Suppressor module • Press contact pressure lever 49 on both tubing cartridges down as far as it will go. • Insert the pump tubings 92 and 93 (6.1826.060) into each of the tubing cartridges as shown in Fig. 15. The white-yellow stopper 94 must click into the corresponding holder on the left-hand side of the tubing cartridge. • Place the tubing cartridges on mounting pin 53 and press down on the right-hand side until snap-action lever 51 clicks into position on holding clamp 50.
2 Installation 45 46 96 33 27 88 97 81 47 27 88 101 100 90 89 32 48 98 28 99 49 91 91 50 51 53 36 36 95 95 91 91 52 92 93 Fig. 16: Connection of the separating column with suppressor 40 27 Mounting rail for column holder 88 81 Separating column 28 Column connection capillary PEEK capillary (6.1831.010; 30 cm) 88 Column holder (6.2027.0X0) 32 Injection valve 89 Aspirating tubing for H2O 6.1803.020 PTFE tubing 33 PEEK coupling (6.2744.040) 90 Aspirating tubing for H2SO4 6.1803.
2.8 Suppressor module 47 Suppressor module 95 PTFE tubing (6.1803.020) 48 Tubing cartridge (6.2755.
2 Installation pump tubing 92. • Mount a 6.2744.010 Compression fitting at the end of the aspirating tubing 90 and screw this compression fitting on to the coupling 91 (see Fig. 16). 3 Prepare supply bottle for H2O • Prepare rinsing solution suited for the desired application and separating column (normally dist. H2O). • Fill rinsing solution into supply bottle 103 (amber glass, 1 L) and label the bottle. • Screw bottle attachment 102 on to supply bottle 103.
2.8 Suppressor module 2.8.4 Connection of the suppressor module The three inlets and outlets numbered 1...3 on the suppressor module 47 each have 2 permanently mounted PTFE capillaries, which must be connected as described as follows (see Fig. 16 and Fig. 18). H2SO4 1 Inlet capillary for eluent • Screw inlet capillary 96 marked with "Eluent" of suppressor module 47 to outlet end of separating column 81 using a 6.2744.010 Compression fitting.
2 Installation 44 5 Inlet capillary for H2O • Attach inlet capillary 98 marked with "H2O" of suppressor module 47 using a 6.2744.010 Compression fitting to the filter unit PEEK 36 connected to the front pump tubing 93. 6 Outlet capillary for H2O • Pull outlet capillary 100 marked with "Waste" of the suppressor module 47 from below through one of the openings 13 out of the inner compartment of the 761 Compact IC. • Lead outlet capillary 100 to a sufficiently large waste container and fix it in place.
2.9 Putting into operation 2.9 Putting into operation 2.9.1 Putting into operation without suppressor Before sample solutions can be injected at the 2.761.0010 Compact IC (without suppressor), the entire system must be tested for leaks and then conditioned with eluent until the baseline is stable. Proceed as follows: 761 Compact IC 1 Open and connect system • Start the «761 Compact IC» PC program, if it has not already been started (see section 2.5.3).
2 Installation 2.9.2 3 Start system • Make sure, that the aspirating tubing 63 for the high-pressure pump is immersed in the eluent. • Select Startup hardware (Measure baseline) from the Control menu in the system window. The high-pressure pump is started, at the same time, a chromatogram window is opened where the baseline is recorded continuously. 4 Check for leaks • Check all capillaries and their connections between the highpressure pump and the detector block for escaping liquid.
2.9 Putting into operation parameters. 761 Compact IC 3 Start system • Make sure, that the aspirating tubing 63 for the high-pressure pump is immersed in the eluent. • Select Startup determination from the Control menu in the system window. The high-pressure pump and the peristaltic pump are started, at the same time, a chromatogram window is opened where the baseline is recorded continuously. The suppressor module is automatically switched to the next position every 20 min and conditioned in this way.
2 Installation 6 Condition system • Rinse the system with eluent until the desired stability of the baseline is reached (normally 30…60 min; if the eluent is changed, the establishment of the ion exchanger equilibrium on the separating column can take longer). After this time the suppressor module is sufficiently conditioned too. • The instrument is now ready for sample determinations using the selected system. Pump tubings are consumable material with a lifetime which depends on the contact pressure.
2.10 Connection of external devices 2.10 Connection of external devices 2.10.1 Connection of the 750 Autosampler The 750 Autosampler available from Metrohm as an option is an automatic sampler for ion chromatography. It accommodates max. 128 samples each of 730 µL, which are automatically transferred to the sample loop attached to the injection valve of the 761 Compact IC.
2 Installation 2.10.2 4 Settings at the 750 Autosampler • Set parameter "Run time" to 0.0 to activate the external start of the 750 Autosampler (see section 3.5 of the 750 Instructions for Use). Filling the sample loop of the injection valve only takes place when the impulse produced by the 761 Compact IC at remote output 3 (see point 5) makes contact at the "EXTERNAL INJECT INPUT" of the 750 Autosampler. The run time will then be determined externally.
2.10 Connection of external devices • Connect the end of the 6.2141.110 Cable marked with "732/1" to the remote interface 24 of the 761 Compact IC (see Fig. 2). 2 Tubing connection 766 – injection valve • At the 761 Compact IC, loosen the rotary nipple 31 screwed onto the interior side of connection 3 (see Fig. 3 and Fig. 4). • Take aspirating tubing 4 completely out of connection 3 and unscrew from connection "1" of injection valve 32.
2 Installation 2.10.3 5 Settings in the «761 Compact IC» program • A time program must be drawn up for the selected system which first produces an impulse at remote lead 3 to start sample changing on the 766 IC Sample Processor and then switches the injection valve to the "Fill" position. A further impulse is then produced to start filling the sample loop within 120 s. At the end the injection valve is switched to the "Inject" position, which also starts data acquisition.
3.1 Requirements 3 Operating tutorial This section introduces you to the operation of the 761 Compact IC by means of a brief operating tutorial which describes the basic operating steps needed for the recording of an ion chromatogram using one of the system files supplied. The determination of the anionic content of a drinking water sample with the METROSEP Anion Dual 2 column with chemical suppression is used an illustrative example.
3 Operating tutorial 3.2 Preparations Before you start this brief tutorial, the entire IC system must be correctly installed as described in section 2. In what follows, the most important points for the installation are described once again (for details, see the sections mentioned). 1 2 3 4 54 Install 761 Compact IC ⇒ Setting up instrument section 2.2 ⇒ Installing and connecting detector block section 2.3.1 ⇒ Mounting syringe and aspirating tubing section 2.3.
3.3 Calibration 3.3 Calibration After the complete IC system has been installed as described in section 3.2, the first calibration can be started. A standard solution is required for this; it should contain the substances to be determined in approximately the same concentrations in which they can be expected in the sample. In our example of drinking water determination using the METROSEP Anion Dual 2 IC-anion column a 20 µL sample loop is used; this is filled with the following standard solution: 0.
3 Operating tutorial module is switched to the next position every 20 min and conditioned in this way. 5 Condition system "PrepMSM2.smt" ⇒ Rinse IC system with eluent until the desired stability of the baseline is achieved and the suppressor module is sufficiently conditioned (at least 1 h). 6 Stop system "PrepMSM2.smt" ⇒ Select Stop determination of the Control menu in the system window. Data recording and time program are stopped, highpressure pump and peristaltic pump keep running on.
3.3 Calibration 9 Enter information for determination ⇒ Click on or select Passport of the Method menu. The passport opens with the General page, which contains the general information about the determination. ⇒ Enter a title for the calibration as Ident (e.g. Standard). ⇒ Change the analysis time under Duration if required. ⇒ Change other parameters on the passport tabs to characterize sample and acquirement conditions if required.
3 Operating tutorial 11 Fill sample loop ⇒ Immerse the aspirating tubing 4 attached to connection 3 in the standard solution. ⇒ Using the syringe fixed to connection 2 siphon in ca. 1 mL standard solution. 12 Switch injection valve to "INJECT" position ⇒ Click on the button of the 761 icon in the system window to switch the injection valve to the "INJECT" position. At the same time, the data recording is started automatically.
3.3 Calibration ⇒ Click on . The Integration parameters window is opened and the chromatogram is reintegrated. ⇒ Repeat this procedure for all other integration parameters until the result satisfies your expectations. Click on for each parameter change. ⇒ Close the Integration parameters window with . 15 Modify peak allocation ⇒ Click on or select Calibration / Components from the Method menu.
3 Operating tutorial This is done by clicking on the chromatogram and moving the cursor with the aid of the cursor keys <> and < > to the middle of the peak and reading off the corresponding retention time in the status line. Enter this value (rounded off if necessary) into the Time column. The optimized table could, for example, then appear as follows: 16 Start calibration ⇒ Click the button in the component window. ⇒ Click on . The Add level window appears.
3.3 Calibration ⇒ Confirm Calibration level 1 in this window with . A new column Level 1 is added in the Concentrations window. ⇒ Enter the concentrations of all components of the standard solution used in this column: ⇒ Click on . The following window appears: ⇒ Confirm Level 1 with . ⇒ Click on in the Concentrations window.
3 Operating tutorial 17 Display calibration curves ⇒ Click on in the Components window. ⇒ Select the desired component in the Component field for which the calibration curve should be displayed (e.g. for chloride). ⇒ Close the Component - chloride window with . ⇒ Close the Components window below the chromatogram by clicking on . 18 Save chromatogram and method ⇒ Close the chromatogram window. A window appears with the message Changes in *.chw. Modified: Calibration. Save changes?.
3.4 Sample determination 3.4 Sample determination Following the calibration of the IC system as described in section 3.3 the first sample solution can be injected. 1 Enable "Verify sample" ⇒ Switch on the Verify sample option of the Control menu in the system window. This causes the Edit sample description window to open at the start of each determination; the most important data for the sample can then be entered in this window. 2 Start system "s-03.
3 Operating tutorial 5 Fill sample loop ⇒ Immerse the aspirating tubing 4 attached to connection 3 in the vessel containing the drinking water sample. ⇒ Using the syringe fixed to connection 2 siphon in ca. 1 mL drinking water. 6 Switch injection valve to "INJECT" position ⇒ Click on the button of the 761 icon in the system window to switch the injection valve to the "INJECT" position. At the same time, the data recording is started automatically.
3.4 Sample determination 7 Open chromatogram ⇒ Click on or File / Open / Chromatogram in the main window. Select the chromatogram file *.chw just recorded and click on . The chromatogram window is opened where the found peaks are numbered and the baselines are drawn in. 8 Report output ⇒ Click on or select Make report of the Process menu in the main window. The Report Options window appears. ⇒ Under Report destination, switch on the desired target option for report output.
3 Operating tutorial 9 Print report ⇒ Click on or select Print of the File menu in the main window. The standard printing window is opened where printer, printing range and number of copies can be selected. After confirmation with the results including the chromatogram are printed out.
4.1 Fundamentals of the operation 4 Operation This section describes the most important points concerning the operation of the 761 Compact IC. For further details please refer to the on-line help in the PC program which can provide you with the required information rapidly and conveniently from any place in the program. 4.1 Fundamentals of the operation 4.1.1 Starting/closing the program Start the «761 Compact IC» program Start the program Double-click this icon or the Metro761.
4 Operation 4.1.2 Glossary System The term “system“ is used to describe the combination of instrument settings, time program and process method which have been optimized for the specific separating column and the determination to be carried out with it. A system is used to start single determinations or determinations with the help of a sample queue. Systems are stored as system files (*.smt) in the Systems directory.
4.1 Fundamentals of the operation Integration Integration is to be understood as being the method for determining the peak area and peak height with the aid of approximate baselines. The integration algorithm included in the program is influenced by the integration parameters and the optionally programmable integration events which are defined in the method. In addition, the integration can be manually corrected later with the aid of the peak editor.
4 Operation 4.1.4 Main window elements The elements of the main window 761 COMPACT IC are the menu bar, the tool bar and the status bar, indicating prompts and logged-in user. Menu bar Tool bar Status bar Prompts, information 4.1.
4.1 Fundamentals of the operation Enable/disable peak editor mode View whole chromatogram Help Lock system Connected system 4.1.6 Overview of file types The following file types are produced by the «761 Compact IC» software: 761 Compact IC *.bar Batch reprocessing file This binary file contains data of the batch reprocessing queue. The *.bar file is stored automatically in the Data folder. *.
4 Operation 4.1.7 Context sensitive menus Some of the menu functions of the program windows are also accessible by clicking on the desired window or item and pressing the right mouse button. The pop up windows have different contents and functions depending on the selected active window or item type. 4.1.8 Keyboard and mouse functions The mouse can be used to carry out the normal program operating functions such as the selection of menu items and fields.
4.1 Fundamentals of the operation [ Ctrl ] + [ right ] Moves one window right (without change of scale on X and Y axes). [ Ctrl ] + [ left ] Moves one window left (without change of scale on X and Y axes). [ Home ] Shows the beginning of a chromatogram (without change of scale on X and Y). [ End ] Shows the end of a chromatogram (without change of scale on X and Y). [ 0 (Zero) ] Adjusts a zero on the lowest level in the window. Cursor is active: 4.1.
4 Operation 4.2 Instrument and software settings 4.2.1 Fonts 761 COMPACT IC / Options / Fonts This option allows the selection of fonts used by the system. 4.2.2 Font for dialog... Selection of font used for dialog boxes. Default setting: MS Sans Serif / Standard / 8 pt. Font for reports... Selection of font used for report output to the screen or printer. Default setting: Courier New / Standard / 10 pt. Font for tables... Selection of font used for data presentation in tables on the screen.
4.2 Instrument and software settings Enter user name, password and access level for all users. Don't forget to make one of the user an Administrator, otherwise this window will not open again. At the end, click on . After configuration of the security system the program prompts for the password every time the system starts. This user name stamps all methods, chromatograms and reports. It is possible at any time to change the user with the menu item 761 COMPACT IC / Options / Lock system. 4.2.
4 Operation Data file overwrite If method changed save If disk method is newer write Data file overwrite = = Never Don't ask to = Ask to over- Overwriting of chromatogram files: Never Chromatogram files cannot be overwritten. A modified chromatogram is saved as a new file with the file name number raised by 1. Ask The user is asked if the chromatogram should be overwritten. Always Chromatogram files are always overwritten without confirmation.
4.2 Instrument and software settings Chromatogram units Flow Pressure 4.2.4 Units for chromatograms: Unit for flow rate: µL/min, mL/min Unit for pressure: MPa, psi, bar, atm Print via print spooler Switch on/off printing via print spooler. Switch off this option if you use a GDI printer. Measuring priority Setting the priority of program execution. realtime means that the «761 Compact IC» program has the highest priority, normal means that all active programs have the same priority.
4 Operation 4.3 Systems The term “System“ describes the combination of instrument settings, time program and process method which has been optimized for a specific separating column and the determination to be carried out with it. A system is used to start single determinations or determinations with the help of a sample queue. Systems are stored as system files (*.smt) in the Systems directory. 4.3.
4.3 Systems SYSTEM / System / Save Save the current system settings in a system file (*.smt) in the Systems directory. SYSTEM / System / Close Disconnect the selected system (if it is connected) and close the system window. 4.3.3 System functions Connect and disconnect system To make possible manual control of the instrument and start of determinations the selected system must be connected to the PC. Only one system can be connected at the same time.
4 Operation SYSTEM / Control / Shutdown hardware High-pressure pump and (if present) peristaltic pump at the 761 Compact IC are immediately stopped. A running determination and an active sample queue are also stopped and the remote output lines are set to the values defined under Hardware / Remote lines after power on. SYSTEM / Control / Stop data acquisition Stop recording of the baseline.
4.3 Systems Ident User defined identifier (title) for the chromatogram to be displayed in the title bar of the chromatogram window and in the Chromatogram open window. Calibration level Calibration level (0 = sample; 1…n = calibration solutions). Info 1 / Info 2 Sample description. Volume Injected volume in µL. Dilution Dilution of the sample. Vial number Autosampler vial position to take sample from. Amount Sample amount.
4 Operation 4.3.4 System settings Modify system window SYSTEM / Setup / Drag icons If this option is enabled, the system icons can be resized and moved in the SYSTEM window and the SYSTEM window itself can be resized. To resize an icon or the window, move the cursor to the desired object until appears. Press the left mouse button and resize the object to the desired size. To move an icon, move the cursor to the desired object until appears.
4.3 Systems Print system parameters SYSTEM / Setup / Parameters / Print A report of the system parameters including the time program is created and opened using the «Wordpad» program. The *.txt file opened can be printed, saved and exported into other programs. The system report includes the name of the method linked to the system, the configuration settings for the 761 Compact IC, the system startup values and the time program (incl.
4 Operation Connected data source Data source for main measurement channel. By clicking on , the Data source window is opened for selection of the data source: This window contains the following two fields: Connected Connected data source. Default setting: Cond[ 761 Compact IC] Available Available data sources of the 761 Compact IC: # Cond Conductivity # Press Pressure The data sources can be moved from one field to the other using the or 4.3.
4.3 Systems 4.3.7 Instrument icon Menu options for instrument icon System disconnected System connected Injection valve in "INJECT" position System connected Injection valve in "FILL" position The instrument icon for the 761 Compact IC is one of the three components of the SYSTEM window. If the system is connected, the 761 icon contains two buttons for manual control of the injection valve: Switch injection valve to "INJECT" position. Switch injection valve to "FILL" position.
4 Operation Flow, mL/min Pressure max, MPa Pressure min, MPa Full scale, µS/cm Remote lines Startup value for flow rate of the high-pressure pump. Entry range: 0.20 ... 2.50 mL/min Startup value for maximum pressure limit for high-pressure pump. Entry range: 0.0 ... 25.0 MPa Startup value for minimum pressure limit for high-pressure pump. Entry range: 0.0 ... 25.0 MPa Startup value for full scale range. Selection: 50, 250, 1000 µS/cm Startup value for remote line settings 1…8.
4.3 Systems mouse button and selecting the menu item Choose color / ... . Actual values Flow, mL/min Pressure max, MPa Pressure min, MPa Full scale, µS/cm Remote lines Valve Suppressor IC pump Peristaltic pump System startup values Flow, mL/min Pressure max, MPa Pressure min, MPa Full scale, µS/cm Remote lines 761 Compact IC Display of actual values Display of flow rate of the high-pressure pump. Display of maximum pressure limit for highpressure pump.
4 Operation Time program On the Program tab of the system settings window a user-defined time program for instrument control can be entered. This program is started automatically as defined in the Start mode window (see section 4.3.3) either at the moment the determination is started (Start with determination) or at the moment the sample is injected (Start with inject). The Program tab contains the two following subpages: Program Main time program with all program steps.
4.3 Systems List of program instructions The following program instructions can be added to the time program on the Program subpage: Instruction Parameter entry Meaning Valve Inject, Fill Switch injection valve to "INJECT" or "FILL" position. FullScale 50, 250, 1000 µS/cm Set full scale range to the selected value. ICPump on, off Switch on or off the high-pressure pump. Flow 0.2 ... 2.5 mL/min Set flow rate of the high-pressure pump to the desired value. Pmax 0.0 ... 25.
4 Operation Name (1st column) User-definable name of the remote command (e.g. Start_766). Remote command (2nd column) Setting the remote output lines 1…8. Selection: 0 (line off, inactive, open) 1 (line on, active, 0 V) p (pulse) * (leave line in current status) For entry of the first value, enter 1, 0, p or *. For entry of the other values, move the cursor in front of the value to be changed and enter 1, 0, p or *. Add new remote command. Delete selected remote command.
4.3 Systems Suppressor Autostep with Suppressor module: Automatic switching to the next position each time the injection valve is switched either to the Fill or to the Inject position. Use peristaltic pump If this option is disabled, the peristaltic pump is not switched on automatically at the start of a determination or with Startup hardware.
4 Operation Flow correction Factor for correction of the difference between displayed and actual flow rate of the highpressure pump. Range: 0.9 ... 1.09 The flow correction is determined by measurement of the actual flow rate with the aid of a measuring cylinder as follows: Displayed flow rate Flow correction = Measured flow rate Cell constant Cell constant of the conductivity cell for correct display of the absolute conductivity. Enter the cell constant printed on the detector block into this field.
4.3 Systems Event Inject Fill Suppressor step Events for automatic remote signal output: Switching of the injection valve to the "INJECT" position. Switching of the injection valve to the "FILL" position. Switching of the suppressor module to the next position. Pump stop (P max/min) Hardware error Alarm leak detector Pump stopped because pressure limits are exceeded. Hardware error detected at the 761 Compact IC (high-pressure pump, injection valve, or suppressor not working correctly).
4 Operation Leak Power on 4.3.8 Leak detector has detected solvent in the instruments interior. This information is also stored in the instrument itself, so that it is stopped automatically even without connection to the PC. Temporary power failure at the 761 Compact IC hardware. Timer the timer can be used to program system tasks which are started automatically daily or once at the desired time.
4.3 Systems Open Close Startup Start Stop Shutdown 4.3.9 Open the selected system. Close the selected system and disconnect it from the workplace. Startup hardware of the selected system. Start determination using the selected system. Stop determination using the selected system. Shutdown hardware of the selected system. System state window The SYSTEM STATE window is automatically opened if a system is connected. It shows status and error messages for this system.
4 Operation Error messages 96 Detection of hardware failed Bad connection between PC and 761 Compact IC or instrument switched off (check connecting cable or switch on instrument). LEAK DETECTED The leak detector has detected a leak (check IC system and connections). E1 Program checksum wrong (call Metrohm service). E2 RAM faulty (call Metrohm service). E200 Invalid instrument adjustment (call Metrohm service).
4.4 Methods 4.4 Methods A method contains all information necessary for data acquisition, integration, peak evaluation and quantification. It can be considered as the chromatogram template, i.e. chromatogram without raw data. Methods are stored as method files (*.mtw) in the Methods directory. Each system is linked to a method. This method is called processing method and is opened automatically at the start of a new determination. 4.4.
4 Operation General Tab General of the passport with general description of the method and determination. Ident Duration METHOD DATA Date/time Last update Calibration level User Detector Run 98 User defined identifier (title) for the chromatogram to be displayed in the title bar of the chromatogram window and in the Chromatogram open window. Duration of the chromatogram in minutes. You can modify this value when the chromatogram is running.
4.4 Methods To reset the Run number press [Ctrl] [F8]. The Analysis number window is opened where the run number for the next run can be modified to the desired value. Batch X/Y: total number of started sample queues / current analysis number in the sample queue (read-only). Sample Tab Sample of the passport with sample information. Info 1 Info 2 Volume Dilution Vial number 761 Compact IC First sample description (max. 256 characters). Second sample description (max. 256 characters).
4 Operation Column Tab Column of passport with column information. Number ID Length Serial number of column (max. 256 characters). Internal diameter of the column in mm. Length of the column in mm. This parameter is used to calculate Linear flow. Packing material Column Particle size Void volume Column description (max. 256 characters). Particle size of the column in µm. This value is used for the calculation of reduced theoretical plate height Reduced TP height. Void volume for the column in %.
4.4 Methods Eluent Tab Eluent of passport with eluent information. Eluent A Eluent B Eluent C Flow Pressure Temp. Description of eluent composition (max. 256 characters). Description of eluent composition (max. 256 characters). Description of eluent composition (max. 256 characters). Flow rate of the high-pressure pump in mL/min. The flow rate is used to recalculate the time axis into volumetric units.
4 Operation Method Log Tab Method Log of passport with GLP Log for the method. The Method Log displays all automatically produced GLP messages concerning modifications made on a method. In addition to this messages free-text user comments can be entered. All this entries are stamped automatically with date and time of the entry. 102 Add a new GLP comment to the Method Log. Text can be entered in the New comment window, date/time and logged-in user are automatically added.
4.4 Methods Data Log Tab Data Log of passport with GLP Log for the recorded chromatogram. Here a GLP message is automatically produced for every modification made on a recorded chromatogram. In addition to this messages freetext user comments can be entered. All this entries are stamped automatically with date and time of the entry and cannot be cleared. 761 Compact IC Add a new GLP comment to the Data Log.
4 Operation 4.4.3 Method setup 761 COMPACT IC / Method / Method setup This menu item opens the Method setup window which includes the most common parameters for data acquisition and evaluation of the method and consists of the following tabs: General General information on determination. Measure Important data acquisition parameters. Filters Parameters for noise filtration. Processing Set actions that are performed when the chromatogram finishes.
4.4 Methods Filters Tab Filters of Method setup window with parameters for noise filtration of raw data. Three different filtration algorithms are available to reduce noise and increase apparent signal-to-noise ratio. 761 Compact IC Spikes Spikes filter. The Spikes filter smoothes the first and last points of the chromatogram and the points identified as spikes. The spike is exchanged with half of the sum of two neighboring signal values. Slit Median Median filter.
4 Operation Processing Tab Processing of Method setup window for definition of actions that are performed during the run or when the chromatogram finishes. Automatic post-run data processing is especially useful for chromatographic systems that include an autosampler. Save chromatogram after the run If checked, autosaving of the chromatogram will be performed on data acquisition ending. while running every ...
4.4 Methods Math Tab Math of Method setup window with parameters that are used for various types of calculations. Parameter Formula set Theoretical plates Resolution Asymmetry Formula Custom formulae Selection of calculation parameter: Formula setting by customer (Custom formulae) or according either to European Pharmacopoeia or US Pharmacopoeia. Selection of calculation formula for number of theoretical plates if Formula set = Custom formulae is set.
4 Operation 1st peak tion time replaces the previous value of the void time. If the first component is not identified, the expected retention time is used. The first detected peak is used as a void time marker for the run and its retention time is stored in the Void time field. From void volume % For the calculation of the void time, the % value entered in the Void volume field is multiplied by the ratio of empty column volume and eluent flow rate. Void volume Void volume in mL and % of column volume.
4.4 Methods 4.4.4 Integration 761 COMPACT IC / Method / Integration This menu item opens the Integration parameters window which contains parameters and events for peak integration and consists of the following two tabs: Setup Integration parameters. Events Integration events. The «Compact IC 761» software includes a built-in automatic integration algorithm to detect peaks on the chromatographic curve and to evaluate them using calculated baselines.
4 Operation Setup Tab Setup of Integration parameters window with integration parameters. The two most important of these parameters for peak recognition are Width and Slope. If the signal-to-noise ratio of the chromatogram is high enough (e.g. 100:1 or higher), the integration algorithm is not too sensitive to changes in integration parameters. On the contrary, if the baseline noise is high, careful tuning of these parameters may be needed. Number of peaks Number of peaks detected (read-only).
4.4 Methods Broadening Broadening for peaks in the end of the chromatogram compared to peaks in the beginning. This parameter is used for automatic adjustment of Width. Entry range: 0.1…100 Slope Threshold for peak recognition. The value of the first derivation (slope) of the curve is divided by the baseline noise (which is estimated using a special algorithm) and the result is compared with the Slope threshold value. Reasonable range of Slope parameter is 0.5...5. Entry range: 0.
4 Operation This function sets up reasonable integration parameters in the following way (assumes that several peaks are marked manually in the peak editor mode (see section 4.5.4) and wrong peaks deleted): − Slope is set to 3. − Asymmetry is set to 1.5. − Width and Broadening are calculated by fitting a straight line through the measured peak halfwidth values vs. retention time.
4.4 Methods If an integration event is added or modified, the Edit integration event window is opened where the following parameters can be set: Time Start time for integration event in min. Event List box with integration events to be selected (see below). Value Parameter value for selected integration event. This field appears for events that demand input of an additional parameter. Integration events for peak detection Disable detection Set this mode to stop detection of new peaks.
4 Operation Stop single peak mode Disable peak end detection. All peaks of any group after this event will be treated as one peak. The group end will be treated as peak end. Start single peak mode Set normal detection mode, when valley causes perpendicular drop or skim line separation. Split peak Terminates the current peak and starts a new one. Integration events for baseline Enable valley-to-valley Enable valley-to-valley Disable perpendicular drop peak separation.
4.4 Methods Set baseline point at 4.5, 6, 7.2, 8.9 and 9.8 min Set baseline point Set defined baseline point for better evaluation of peaks on descending or ascending baselines. The baseline between two successive baseline points is set to zero for optimum integration. Force horizontal baseline Force horizontal baseline without Set baseline point Cancel horizontal baseline Set horizontal baseline for a single peak. The baseline is drawn forwards from the peak start point.
4 Operation Force horizontal base back Set horizontal baseline for a single peak. The baseline is drawn backwards from the peak end point. The intersection of the baseline with the signal is defined as peak start point. Cancel horizontal base back Clear Force horizontal base backmode. Enable baseline penetration Disable baseline penetration Enable baseline penetration Allow crossing of the signal by the baseline. Disable baseline penetration Clear Enable baseline penetration mode.
4.4 Methods 4.4.5 Calibration and quantification General information The aim of any chromatographic analysis is to answer the question "What components are present in the sample and what are their concentrations?". Two procedures are used to achieve this goal: the first step is called calibration, the second step includes quantification.
4 Operation Notations R Stands for response value, either area or height, depending on setting selected in the Calibration graphs window. V Sample Volume injected. D Dilution V' = V / D Adjusted volume of injected sample. A correction is made for the dilution coefficient. C Concentration of the component in the initial solution (before dilution). Q = C • V' Quantity of component, used for calibration curve construction. t Retention time.
4.4 Methods External standard calibration External standard calibration (absolute calibration) is a key way of calibration. Basically this procedure calculates the dependence of injected component's quantity versus area (or height) of the corresponding peak. This dependence is showed as a calibration plot with injected quantity along the Y axis and peak area (or height) along the X axis.
4 Operation 120 Number Row number (read-only). Peak Number of the peak in the chromatogram that corresponds to the given component. If this field contains a 0, the peak number must be entered manually. Time Expected retention time of the component in the calibration run. After a new entry of the peak number the corresponding retention time is entered automatically as soon as this field is clicked on with the mouse. Wind.% Identification window of the component.
4.4 Methods Additionally, the Components table contains the following buttons: Add a new component (an empty column) to the component table. Delete the current component from the component table. Open the Peak identification window (see Identification). Open the Concentration table (see Concentration table). Open the component window with display of calibration curve and calibration parameters.
4 Operation Identification Reference peaks Other peaks Identification parameters. Identification parameter for reference components. Default is Height. Identification parameter for ordinary components. Default is Time. Retention units Choice of retention units. Default is min. Retention time Retention time. Updates expected retention times of components according to the current chromatogram. Worst case...
4.4 Methods Concentration table 761 COMPACT IC / Method / Calibration / Concentrations Selecting this menu item or clicking on in the component table opens the Concentrations window with the concentration table containing concentrations of all components for all Calibration levels. Each calibration level corresponds to a sample used for calibration and to a point on the calibration curve.
4 Operation Add a new Calibration level to the concentration table. The following window appears: Create calibration level Number of calibration level to add. Fill level with concentration Concentration to be filled in for all components. Copy concentrations from level Number of calibration level from which concentrations are copied. Calibrate immediately Recalibration with new calibration levels.
4.4 Methods Calibration curve 761 COMPACT IC / Method / Calibration / Graphs Selecting this menu item or clicking on in the component table opens the Component window. In this window the results of the calibration are shown for each component together with the calibration curve. The parameters for calculating the calibration curve can also be entered here.
4 Operation Calibration points table This table contains the basic information used to construct the calibration curve: Level Number of Calibration level. Conc. Concentration of the current component in the calibration sample. It is taken from the concentration table. Area (or Height) Peak height or area of the current component, depending on calibration base. File File name of calibration chromatogram that stores data on the given calibration level.
4.4 Methods Base Base for calculations (Area or Height) in quantification and calibration procedures. Indicates, which parameter is to be used as a peak response. Reference channel Channel which is used to measure area or height (read-only). Formula Formula for calibration function. There are six possible calibration dependencies for linear and nonlinear calibration curves.
4 Operation sponse factor of this component so, that the total amount of the injected components becomes equal to the declared value. This declared summary amount is entered into the Concentration field of the universal component for This run level. Load and save calibration data 761 COMPACT IC / Method / Calibration / Load from method Load the calibration from the method. This option is used to update the calibration for the current run by the one taken from the method used for acquisition.
4.4 Methods 4.4.6 Report output Report options 761 COMPACT IC / Method / Report options 761 COMPACT IC / Process / Make report The Report options window is divided into several regions that combine parameters for report output on their functionality and includes several different areas. The report output is started by clicking on .
4 Operation Sample information from the Sample tab of the passport. Sample SAMPLE: : Vial number: Volume: Dilution: Tap water from Application Laboratory Herisau, Switzerland 2 20.0 µl 1.00 Column information from the Column tab of the passport. Column COLUMN: Size: Number: Part.size: METROSEP Anion Dual 2 (6.1006.100) 4.6 x 75 mm A106 6.0 µm Eluent information from the Eluent tab of the passport. Eluent ELUENT: 2.0 mM NaHCO3 / 1.3 mM Na2CO3 Flow: 0.80 mL/min Temperature: 20.0°C Pressure: 3.
4.4 Methods Comment User defined comment from the Comment tab of the passport. Method example for water determination. GLP Log Method and Data GLP messages from the Method Log and Data Log tabs of the passport. METHOD GLP LOG 15/02/1999 17:35:47 Method created ! 15/02/1999 17:35:56 Modified: Passport; Method saved to disk file C:\IC761\Methods\s-03.mtw DATA GLP LOG Time constant: 0.
4 Operation Calibration parameters defined in the component window and on the Math tab of the Method setup window. Calibration defaults CALIBRATION Channel: Cond Method: External standard Response: Area Standard: No Index: Linear Internal Effectivity: 2*Pi*(T*H/A)^2 IDENTIFICATION Reference peaks: Time Other peaks: Time Retention units: min Component table. Component table No Retention Window% 1 2 3 4 5 6 7 2.85 4.94 6.78 8.48 10.56 13.65 16.86 RF 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Conc. 1.095e+00 1.
4.4 Methods Parameters of the data acquisition channel used. Channel table CHANNELS TABLE Cond No 1 Name Units Input Cond uS/cm # Name/Units 1 Cond uS/cm Minimum Zero 1 -8388607 0 Noise 5.6 5.63e-05 RMS 63047.3 0.63 Maximum Range Coefficient 8388607 8.389e+01 PeakToPeak 796371.8 7.96 Noise Shift 1.000e-05 5.63 0 Drift/hour 15119.570 0.151 Name Channel’s name. This text appears as Channel label in the chromatogram. Units Units of detector response (µS/cm).
4 Operation Peak table The following parameters can be selected for peak table output with determination results: Quantification method Selection of the method to calculate concentrations of components: Response normalization The method normalizes the sum of responses for all peaks of the chromatogram to the NORM factor entered in the Total % for normalization field: Ri% = NORM • Ri / Σ Ri. All peaks are calculated and reported no matter whether they have been recognized or not.
4.4 Methods and the concentration of this internal standard must be entered in the Concentration of std field. As long as no universal component is defined, only peaks with non-zero concentrations are listed. The peak table includes the following columns: Peak number, Retention time, Height, Area, Response factor, Relative concentration, Relative concentration%, Name Index This column reports retention indexes of identified components.
4 Operation By components Missing components are always included into the report, even those with concentration equal to zero. In the case of presence of universal component the summary for all unidentified peaks is presented as a single line. Calls up a box with a list of columns that can be included into the report (see Report elements). It is available only if Quantification method = Custom has been selected.
4.4 Methods Mode The two options Overwrite (overwrite the file) or Append (append to existing file) are available. Character set The two options Windows (ANSI) or DOS (ASCII) are available. This settings are essential for printing of non-English symbols (e.g. ö, ä, ü). Custom program Path and name of the program to be started after report output. This option enables to transfer the report to a database, an electronic table or another application for further processing.
4 Operation R = (ti+1 - ti) / (w0.607i + w0.607(i+1)) where i and i+1 indexes refer to the neighboring peaks, and w0.607 stands for the peak width at 60.7 % of the peak height. effectivity, TP Effectivity for the peak in number of theoretical plates. The number of theoretical plates Ni per column for a chosen peak is calculated for a chromatographic peak by one of two formulas: Ni = 2 PI (ti • Hi / Ai)2, where PI = 3.1415926..., ti = retention time, Hi = height, Ai = area of the peak.
4.4 Methods raw concentration Absolute concentrations (raw quantity) of the components, calculated as Ci = Wi(Ri) / V' Total value for the column is the sum of concentrations for all components. Normalization of concentrations for all peaks using the NORM value entered in the Total % for normalization field (default setting 100%): concentration% Ci% = NORM • Wi(Ri) / Σ Wi(Ri) Total value for the column equals NORM for the main table, and the sum of concentrations in the group for the group table. rel.
4 Operation ? Some points of corresponding peak are out of ADC or detector range – suspicious result. ! Component concentration is outside of minimum (min C) and maximum limits (max C), set in the component table. p Special component (it has one of the special flags checked on in the COMPONENT window). N The component response is outside of calibrated region.
4.5 Chromatograms 4.5 Chromatograms 4.5.1 Chromatogram window The CHROMATOGRAM window is used to show a running or recorded chromatogram. Title bar Status bar Chromatogram The title bar of the chromatogram window contains buttons for minimizing, maximizing and closing the window. The window name consists of the elements "Ident (method name) chromatogram name". A star ( * ) at the end of the name indicates that the chromatogram has been changed since the last saving.
4 Operation 4.5.2 Chromatogram file handling Open chromatogram 761 COMPACT IC / File / Open / Chromatogram Load an existing chromatogram file (*.chw) from the Data directory and open the chromatogram window. The following window appears: Filename Selected Directory File window 142 Filename (common wildcards as * and ? are possible). Number of selected chromatograms and their total size. Path name of the working directory.
4.5 Chromatograms Directories Box with the list of directories. Allows to change the working directory defined in the method, if necessary. Chromatogram description A set of fields with the description of the current chromatogram. Selected fields from the passport are listed here. Load all selected chromatogram files (*.chw) and open each in its own window. Close this window without any action.
4 Operation Represent raw data as Default units (float) Output of raw data: Y values are exported in default units for the channel (µS/cm). ADC response (integer) Y values are exported in bits. Include retention time In seconds (float) As point number X values are exported in seconds. X values are exported as point number. Import chromatogram 761 COMPACT IC / File / Import / Chromatogram Import chromatogram of the following formats: *.chm Chromatogram files of the «Chrom&Spec» program (DOS version).
4.5 Chromatograms 4.5.3 Graphical representation Appearance 761 COMPACT IC / View / Appearance This menu item opens the Appearance window. It determines the appearance of the chromatogram and consists of four tabs: Chromatogram axes Labels Select channel Colors Scaling of chromatogram axes. Settings for peak labels and baseline drawing. Select channels to be displayed (only available for multi-channel chromatograms). Color settings for chromatogram elements.
4 Operation Response axis Y from Y to Tic marks Beginning of the window on Y axis. End of the window on Y axis. Plot axes labels and tic marks on Y axis with no, relative or absolute scaling. View all Set scales on X and Y axes so that the whole chromatogram is visible. Drift compensation Turns the chromatogram screen image so that the last and first points of the chromatogram are on the same level. This option is useful for gradient chromatograms.
4.5 Chromatograms Component name + Quantity Name and quantity of the component. Channel labels At start In corner Label for data acquisition channel. Channel label is shown at the start of the chromatogram. Channel label is shown in the upper right corner of the chromatogram. Show baseline and peaks Baselines are shown. Baseline marker Start and end of baselines are marked. Label always visible Label is shown always with zooming.
4 Operation Colors Tab Colors of the Appearance window with color settings parameters for chromatograms. this color is default Hair Background Axes Baseline AlterGround Channel 1...8 148 Reset the selected element to the default color. Choose a new color for the selected element. An example of the chosen color is shown beside the button. Cursor's color. Background color. Axes and axes labels color. Baseline color. Alternative background color for Measure baseline option.
4.5 Chromatograms Other graphical functions 761 COMPACT IC / View / X full scale By selecting this menu item or pressing [ Ctrl ] + [ Home ] the X axis is scaled so that the chromatogram perfectly fits the window horizontally. 761 COMPACT IC / View / Y full scale By selecting this menu item or pressing [ Ctrl ] + [ End ] the Y axis is scaled so that the chromatogram perfectly fits the window vertically.
4 Operation 4.5.4 Peak editor Switching on/off the peak editor 761 COMPACT IC / Process / Peak editor The peak editor mode is used for subsequent manual correction of the automatic integration for chromatogram peaks (see section 4.4.4). It can be used to select the most important points for the peak evaluation (start, end and top of peak, valley between peaks) and move them to the required position. If the peak editor mode is enabled, the vertical bar cursor appears in the chromatogram window.
4.5 Chromatograms 761 COMPACT IC / Peak / Select end point Move the cursor to the end of the nearest peak and select the peak. 761 COMPACT IC / Peak / Select valley point Move the cursor to the valley of the two nearest peaks. 761 COMPACT IC / Peak / Unselect peak Delete the selection. [–] Move a selected point (start, top, end, valley) to the cursor position. 761 COMPACT IC / Peak / Move selected point [+] Merge two neighboring peaks into a single peak.
4 Operation 4.5.5 Printing Page layout for printing 761 COMPACT IC / File / Page layout The selection of this menu item or clicking on in the Report opwindow opens the Page layout window for page layout parameters. tions Length units inches centimeters Page margins Left Right Top Bottom Chromatogram plot size Width Height Calibration graph size Width Height 152 Selection of length units. Inches. Centimeters. Selection of page margins. Left margin. Right margin. Top margin. Bottom margin.
4.5 Chromatograms Printer settings 761 COMPACT IC / File / Printer setup By selecting this menu item the PRINT SETUP window is opened where printer, paper size and format can be defined. Print preview 761 COMPACT IC / File / Preview By selecting this menu item the Preview window appears on the screen where the report is shown in the appearance formatted for the desired printer as defined in the Report options window.
4 Operation Subtraction of a chromatogram 761 COMPACT IC / Process / More / Subtract This menu item opens the Subtract chromatogram window allowing the subtraction of any opened chromatogram from the active, selected chromatogram. Select the chromatogram that should be subtracted, click on and then on 761 COMPACT IC / View / View all.
4.5 Chromatograms Autodatabase options The «Autodatabase 1.0» PC program is a part of the 761 Compact IC standard accessories and is used to save and handle chromatograms and results produced with «761 Compact IC» in a database. You find a detailed description of this database program in the 8.110.8193 Instructions for Use supplied. . 761 COMPACT IC / Method / Autodatabase This menu item opens the Autodatabase options window with parameters and settings for the Autodatabase program.
4 Operation 4.6 Sample queue A sample queue is a table containing sample-specific data which is used to facilitate work with autosamplers and multiple analyses. The number of rows of the sample queue table defines the number of determinations which are run automatically. Once the queue has been started, the sample-specific data are transferred line-by-line to the running determination overwriting the corresponding fields of the method. A sample queue is stored in a sample queue file *.
4.6 Sample queue 4.6.2 Sample queue control Sample queue overview table 761 COMPACT IC / File / Open / Sample queue SYSTEM / System / Sample queue These two menu items open the OPEN window for opening an existing sample queue file *.que or creation of a new sample queue file *.que by entering a new name. After confirmation with the sample queue overview table is opened showing the current status of the sample queue: No Row number. System System file to be used for the determination.
4 Operation Started Indication whether the sample has been started or not: 0 sample not started 1 sample started number of injections done 2…n Level Calibration level (see section 4.4.5) for the sample: Level 0 stays for normal analysis, levels 1 and greater for calibration runs. Correct filling of this column enables to calculate calibration coefficients automatically. Volume Injected volume of sample in µL. Amount Sample amount.
4.6 Sample queue Pause sample queue SAMPLE QUEUE OVERVIEW / Control / Pause Interrupt execution of the sample queue after the current determination has been finished. If processing the sample queue is interrupted with then it can be continued again with (with a running chromatogram only when data acquisition is finished). Cancel last run SAMPLE QUEUE OVERVIEW / Control / Cancel last run Cancel the last run (set Started = 0 for this row).
4 Operation No Row number. System System file to be used for the determination. The system is automatically opened and connected. Ident User defined identifier for chromatogram. Will be placed into appropriate passport field when starting the chromatogram. Vial Autosampler vial position to take sample from. This value will not be transferred automatically to the autosampler. Make sure that the vial positions entered in this column are identical to the vial positions used at the autosampler.
4.6 Sample queue Sample queue editor functions The functions in the editor window for sample queues can be triggered with the corresponding menu items of the Edit menu or with the corresponding symbols in the symbol bar. QUEUE EDITOR / Edit / Undo Undo the last modification of the sample queue table. QUEUE EDITOR / Edit / Cut row(s) Cut the selected rows of the sample queue table and copy them into the clipboard.
4 Operation 4.7 Batch reprocessing Reprocessing is understood to be the subsequent reprocessing of a series of chromatograms which have been loaded in a queue (Batch reprocessing queue). For reprocessing according to a selected method the settings for calibration, integration, passport, appearance and report can be altered at will. A batch reprocessing queue is stored in a batch reprocessing queue file *.bar in the Data directory. 4.7.
4.7 Batch reprocessing 4.7.2 Perform batch reprocessing Reprocess options window 761 COMPACT IC / File / Open / Batch reprocessing 761 COMPACT IC / File / Open / Last batch These two menu items are used to open the Reprocess window, in which the various options for reprocessing are set and can then be triggered. Use method from file for reprocessing Selection of the desired chromatogram file whose method should be used for reprocessing.
4 Operation Reprocess sample runs Open the batch reprocessing editor program for editing the batch reprocessing table (see section 4.7.3). Reprocess all sample chromatograms (calibra- tion level = 0). Reprocess calibration runs Reprocess all calibration chromatograms (cali- bration level > 0). Update method file in directory after reprocessing Save the method file *.mtw after reprocessing the method is changed.
4.7 Batch reprocessing Recalculate only Enable recalculation of chromatograms with values for Volume, Dilution, Amount and Internal standard amount entered in the batch reprocessing table. The recalculation is done automatically if the and/or Recalculate options are enabled. If the Recalculate only option is enabled, the Reintegrate and Recalculate options are disabled automatically.
4 Operation Start reprocessing. Combine all chromatograms of the batch reprocessing queue into a single multi-channel chromatogram. Close the Reprocess window. Merge chromatograms REPROCESS / Combine all chromatograms of the batch reprocessing queue into a single multi-channel chromatogram. The chromatograms are displayed in the same order as in the batch reprocessing table slightly displaced one upon the other.
4.7 Batch reprocessing 4.7.3 Batch reprocessing queue editor Open batch reprocessing queue editor window REPROCESS / This menu item opens the batch reprocessing editor program for editing the batch reprocessing table. No Row number. File name Name of the chromatogram file (read-only). Method Name of the method file *.mtw used for recording the chromatogram (read-only). Ident User defined identifier for chromatogram.
4 Operation of this column enables to calculate calibration coefficients automatically. Sample Info 1 First sample description. Will be placed into appropriate passport field. Sample Info 2 Second sample description. Will be placed into appropriate passport field. Batch reprocessing queue editor functions The functions in the editor window for the batch reprocessing queues can be triggered with the corresponding menu items of the Edit menu or with the corresponding symbols in the symbol bar.
5.1 Practical notes on ion chromatography 5 Notes – Maintenance – Faults 5.1 Practical notes on ion chromatography 5.1.1 Separating columns Separation efficiency The attainable quality of analyses with the 761 Compact IC depends to a large extent on the separation efficiency of the column used. When purchasing an IC column you should ensure that the separation efficiency suffices for the analysis problems at hand.
5 Notes – Maintenance – Faults Storage Always store the separating columns closed when not in use and filled in accordance with the manufacturer’s specifications. Dead volume Dead volume at the end of a column can be the cause of extreme peak broadening or splitting (appearance of double peaks). Filling the column with glass beads (∅ ≤ 100 µm) frequently improves the separation efficiency.
5.1 Practical notes on ion chromatography 5.1.3 Eluents Treatment For the preparation of the eluents only chemicals of a purity degree of at least "p.a." should be used. For diluting please use only high purity water. Fresh eluents should always be microfiltered (0.45 µm filter) and degassed (with N2, He or vacuum). For alkaline eluents and eluents with low buffering capacity one should preferably use a CO2 absorber (see section 2.6.3).
5 Notes – Maintenance – Faults 5.1.5 Suppressor module Protection To avoid contamination of the suppressor module by foreign particles or bacterial growth, the two 6.2821.120 Filter units PEEK (see section 2.6.3) supplied must be installed between peristaltic pump and inlet capillaries of the suppressor module (see section 2.8.2). Operation The Metrohm Suppressor Module MSM comprises a total of 3 suppressor units which are in turn used for suppression, regenerated with sulfuric acid and rinsed with water.
5.2 Maintenance and servicing 5.2 Maintenance and servicing 5.2.1 General information Care The 761 Compact IC requires proper care and attention. Excessive contamination of the instrument could possibly lead to malfunctions and a shorter service life of the inherently rugged mechanical and electronic parts. For protection against escaping liquids the two drain tubes for the inner compartment (section 2.3.3) and for the bottle rack (section 2.3.4) must be mounted.
5 Notes – Maintenance – Faults 5.2.3 Recycling To keep the eluent consumption between injections to a minimum when the system is at rest (e.g. overnight), the so-called recycling procedure can be used. In recycling the eluent exiting the outlet capillary of the detector block is led back directly to the eluent supply vessel 67. The IC system is thus quickly ready for new injections without a long conditioning period. Instead of threaded stopper 65 the 4.420.
5.2 Maintenance and servicing 2 Connect new column to injector • Remove end caps from column 81. • Screw inlet end of separating column 81 (note flow direction) to column connection capillary 28 or to the precolumn (see section 2.7.7/section 2.7.8). 3 Rinse column • Place beaker beneath the column outlet. • Switch on high-pressure pump and rinse column with eluent for ca. 10 min, then switch off pump.
5 Notes – Maintenance – Faults 5.2.6 Maintenance work at the pump head In many cases, an unstable baseline (pulsation, flow fluctuations) can be traced to contaminated valves or faulty, leaky piston seals at the high-pressure pump. For cleaning contaminated valves and/or replacement of wear parts such as pistons, piston seals and valves, proceed as follows: 1 Detach pump head • Disconnect aspirating tubing 63 from aspirating capillary 40 at the pump head 42 (see Fig. 3 and Fig. 4).
5.2 Maintenance and servicing 115 42 104 105 106 114 107 108 109 110 111 112 113 115 Fig. 19: Components of the pump head A 42 116 117 112 117 B 112 C 116 Fig. 20: Replacement of the piston seal 112 42 Pump head (6.2824.100) 111 Piston guide sleeve (4.709.4370) 104 Screw (3.709.1100) for piston cartridge 108 112 Piston seal (6.2741.000/6.2741.010) 105 Zircon piston (6.2824.070) with piston shaft 113 Inlet valve (6.2824.090) 106 Spring retainer 114 Outlet valve (6.2824.
5 Notes – Maintenance – Faults • To install a new piston seal 112 the special tool 117 is used. • First the new seal is inserted firmly in the recess of tool 117 by hand (see Fig. 20B). The seal spring must be located on the outside. • The tool 117 together with the seal is then inserted in the pump head 42 and the seal pressed into the pump head recess with the aid of tool 116 (see Fig. 20C).
5.2 Maintenance and servicing 6 Mounting the pump head • Reassemble the components of the pump head 42 as shown in Fig. 19. Tighten the screw 104 by hand. First screw in piston cartridge 108 manually until the stop is reached and then use a wrench to turn it through a further 15°. Firmly tighten the two valve screw holders 115 with a wrench. • Reattach pump head 42 to the pump with the help of the 4 fixing screws 41. Firmly tighten them with the 6.2621.030 Allen key.
5 Notes – Maintenance – Faults 5.2.7 Regeneration of the suppressor module Regenerating a suppressor operating at reduced capacity If the suppressor units are exposed to certain heavy metals (e.g. iron) or organic contaminants for long periods of time, these can no longer be completely removed by the regeneration solution normally used (20 mmol/L H2SO4).
5.2 Maintenance and servicing • Set the flow at the high-pressure pump to 0.5 mL/min and rinse the suppressor unit with 1 mol/L H2SO4 for 5 to 10 min. • As the pressure falls, slowly increase the flow at the highpressure pump to 2 mL/min. Do not exceed a maximum pressure of 2 MPa (20 bar). • Switch off high-pressure pump. • Switch suppressor to the next position using the button. • Connect the inlet capillary 98 marked "H2O" to the inlet capillary 26 using coupling 33 (see Fig. 10 and Fig. 16).
5 Notes – Maintenance – Faults 182 2 Dismantle suppressor • Unscrew nut 125 from suppressor holder 128. • Pull out connection piece 126 and suppressor rotor 126 from suppressor holder 128 (the connection piece and the rotor normally stick together). • Loosen connection piece 126 from suppressor rotor 127. 3 Clean input and output leads • Connect each of the 6 capillary tubings attached to connection piece 126 to the high-pressure pump one after another, and pump through ultrapure water.
5.2 Maintenance and servicing 125 126 127 128 Fig. 22: Assembling the suppressor 5.2.9 127 125 Screw nut 126 Connection piece (6.2832.010) 128 with input and output leads Suppressor rotor (6.2832.
5 Notes – Maintenance – Faults 184 3 Clean suppressor rotor • Clean the sealing surface of new suppressor rotor 127 (6.2832.000) using a lint-free cloth and ethanol. 4 Insert suppressor rotor • Insert new suppressor rotor 127 in suppressor holder 128 in such a way that the tubing connections at the rear of the rotor fit in the corresponding openings inside the rotor and that one of the three holes in the rotor can be seen from below in one of the openings of the holder.
5.2 Maintenance and servicing 5.2.10 Exchanging the pump tubing The pump tubings used by the peristaltic pump are consumable material with a limited lifetime and should be exchanged at regular intervals (approx. every 4 weeks under continuous use). The working life of pump tubing depends to a considerable extent on the contact pressure. This is why the contact pressure must be correctly set as described in section 2.9.2.
5 Notes – Maintenance – Faults 5.3 Faults and malfunctions 5.3.1 Error messages If any type of malfunction occurs during operation of the 761 Compact IC, this is shown by error messages in the PC program, which appear either in an error window or in the SYSTEM STATE window. Follow the instructions given in the error window and close this window with .
5.3 Faults and malfunctions Malfunction Cause Rectification Chromatograms with poor resolution, change in the retention times • Deterioration in separation efficiency of the IC column • Regenerate column (see section 5.1.
5 Notes – Maintenance – Faults 5.4 Diagnostic tests / Validation / GLP The requirements of GLP (Good Laboratory Practice) include a periodic check of analytical measuring instruments with regard to their reproducibility and accuracy using Standard Operating Procedures, SOP. Under the title «Application Bulletin No. 277 – Validation of Metrohm ion chromatographs» an example of such a standard operating procedure is available from Metrohm; it can be adapted and used with the 761 Compact IC.
6.1 Technical data 6 Appendix 6.1 Technical data 6.1.1 Conductivity measurement Measurement range 1 0…1000 µS/cm (resolution: 0.56 nS/cm) Measurement range 2 0…250 µS/cm (resolution: 0.14 nS/cm) Measurement range 3 0…50 µS/cm (resolution: 0.028 nS/cm) Maximum error ± 1 % of full scale value and ± 1 % of measurement value (k = 16.7/cm) Linearity Deviations < ± 0.5 % of full scale value Noise Measurement range 1 Measurement range 2 Measurement range 3 typ. 10 nS/cm typ. 2.5 nS/cm typ. 0.
6 Appendix 6.1.3 Injection valve Actuator switching duration 100…150 ms Pressure resistance 25 MPa (250 bar) 6.1.4 High-pressure pump Type Serial dual piston pump with two valves Pump capacity Flow range Maximum error Flow constancy Reproducibility of eluent flow 0.20...2.5 mL/min < ± 2 % of set value < 0.5 % of set value typ. better than ± 0.
6.1 Technical data 6.1.5 Peristaltic pump Type Pump capacity Rotational speed Flow range Maximum error 2-channel peristaltic pump 20 U/min at 50 Hz 24 U/min at 60 Hz 0.5…0.6 mL/min with 6.1826.060 Pump tubing ±5% Maximum pressure 0.4 MPa (4 bar) Pumpable liquids Clear liquids with no solid contents Pump tubing material PP (polypropylene) 6.1.6 Suppressor module Switching duration 140 ms Pressure resistance 2.5 MPa (25 bar) 6.1.7 Leak detector Type Detector with 2 electrodes approx.
6 Appendix 6.1.9 Remote interface Connector Dsub 25 pin (female) Circuit diagram for output lines 1…8 Remote Assignment of output lines 1…8 Potentials Remote 1 Remote 2 Remote 3 Remote 4 Remote 5 Remote 6 Remote 7 Remote 8 Pin Pin 18 Pin 4 Pin 3 Pin 1 Pin 2 Pin 16 Pin 17 Pin 5 +5V Pin 15 0V Pin 14 Pin 25 6.1.10 6.1.11 6.1.12 Analog output Connector Dsub 9 pin (male) Pin assignment 0V Measurement signal (0...
6.1 Technical data Safety directions 6.1.13 6.1.14 6.1.15 The Instructions for Use include information and warnings which must be heeded by the user to assure safe operation of the instrument.
6 Appendix 6.2 Standard equipment Subject to changes ! All dimensions are given in mm. The 761 Compact IC is available in two versions: • 2.761.0010 Compact IC without suppressor module • 2.761.0020 Compact IC with suppressor module These instruments include the following parts: Description 2.761.0020 Order No. 2.761.0010 Quant. 1 1 1.732.0110 Detector block (metal-free) with permanently attached connecting cable to 761 Compact IC - 2 6.1602.150 Bottle attachment GL45 for 6.1608.
6.2 Standard equipment 2.761.0010 2.761.0020 Quant. 1 1 Order No. Description 6.1609.000 CO2 Absorber tube incl. 6.2701.020 Stopper For 6.1602.160 Bottle attachment. - 2 - 1 1 2 2 1 6.1803.020 6.1816.020 6.1826.060 6.1834.010 PTFE capillary Length = 5 m Silicone tubing Drain tube for inner compartment and bottle rack, length = 1 m 0.97 6 9 150 Pump tubing made of PP (polypropylene) with 2 firmly attached white-yellow stoppers; in.d. = 0.51 mm, ex.d. = 2.
6 Appendix 2.761.0010 2.761.0020 Quant. 1 1 1 1 Order No. Description 6.2122.0X0 Mains cable to customer's specifications: 6.2134.100 Cable socket Cable connector Type IEC 320/C 13 Type IEC 320/C 13 Type CEE (22), V Type SEV 12 (CH…) ............................... 6.2122.020 Type CEE (7), VII (D…) ........................... 6.2122.040 Type NEMA 5-15 (USA…) ...................... 6.2122.070 Connecting cable Connecting cable 761 Compact IC (RS232) – PC 9 pol. neg. 9 pol. neg. 5m 1 1 6.
6.2 Standard equipment 2.761.0010 2.761.0020 Quant. 1 1 - 1 1 1 Order No. Description 6.2744.020 Coupling 1⁄16" – Luer Coupling for connection of a 6.1803.000 PTFE capillary to connection 2 of the 761 Compact IC when a 750 Autosampler or a 766 IC Sample Processor is used 6.2744.030 6.2816.020 19 PEEK coupling Connection between 6.2744.010 PEEK compression fitting and 6.1826.060 Pump tubing; Set of 4 25 Syringe made of PP, volume = 10 mL; for manual filling of the sample loop 76 1 1 6.
6 Appendix 6.3 Optional accessories 6.3.1 Accessories for capillary connections Order No. 6.1825.XXX Description Sample loop, made of PEEK For injection valve; incl. two 6.2744.010 PEEK compression fittings 6.1825.210: Volume = 6.1825.230: Volume = 6.1831.010 6.2620.040 20 µL 10 µL PEEK capillary Length = 3 m 0.25 1 ⁄16" Coupling 1⁄16" – 1⁄4" Connector for plastic separating columns with 1⁄4"-28 thread. 80 6.2621.080 Capillary tubing cutter for plastic capillaries For 6.1831.
6.3 Optional accessories 6.3.2 High-pressure pump Order No. Description 6.2824.100 Pump head (metal-free) Complete, with fixations screws 6.2741.000 Piston seal Spare part for 6.2824.100 Pump head 6.2741.010 6.5 3 6.5 3 PE piston seal Spare part for 6.2824.100 Pump head (only suitable for aqueous eluents) 6.2744.070 PEEK compression fitting short Spare part for 6.2824.100 Pump head Set of 5 21 6.2824.070 Zircon piston Spare part for 6.2824.100 Pump head ∅3 65.5 6.2824.
6 Appendix Order No. Description 6.2824.080 Outlet valve (metal-free) ∅8 Spare part for 6.2824.100 Pump head 16 6.2824.090 Inlet valve (metal-free) ∅8 Spare part for 6.2824.100 Pump head 16 6.3.3 Separating columns and precolumns Order No. Description 6.1005.000 IC anion column PRP-X100 (125 mm) For the determination of anions without chemical suppression. Column dimensions: 125 × 4.0 mm 140 Precolumn: 6.1005.020 6.1005.
6.3 Optional accessories Order No. Description 6.1005.050 IC precolumn cartridge PRP-1 To prolong the service life of the 6.1009.000 IC anion column SUPERSEP and the 6.1006.100 IC anion column METROSEP Anion Dual 2. ∅6.4 27 Column dimensions: 20 × 4.0 mm Installation using 6.2821.040 Cartridge head. 6.1005.100 IC anion column Star-Ion A300 For the determination of anions with chemical suppression. Column dimensions: 100 × 4.6 mm 6.1005.
6 Appendix Order No. Description 6.1007.000 IC cation column Nucleosil 5SA For the determination of divalent cations without chemical suppression. Column dimensions: 125 × 4.0 mm Precolumn: 6.1007.010 6.1007.010 6.1008.010 6.1009.000 6.1009.010 140 IC precolumn cartridge Nucleosil 5SA To prolong the service life of the 6.1007.000 IC cation column Nucleosil 5SA. Column dimensions: 20 × 4.0 mm Installation using 6.2821.040 Cartridge head. ∅6.
6.3 Optional accessories Order No. Description 6.1012.X20 Sample pretreatment cartridge IC-Ag Cation exchanger in Ag+ form. Removes halides. 15.5 With Luer connection. 34 6.1012.020: set of 50 6.1012.120: set of 10 6.1012.X30 Sample pretreatment cartridge IC-OH Cation exchanger in OH– form. For highly acidic samples. 15.5 With Luer connection. 34 6.1012.030: set of 50 6.1012.130: set of 10 6.1012.
6 Appendix Order No. Description 6.2828.000 Glass cartridge holder To hold the 6.1006.0020 Column cartridge METROSEP Anion Dual 1. 12 172 6.2828.010 Precolumn cartridge holder To hold the 6.1006.0030 Precolumn cartridge METROSEP Anion Dual 1. 12 54 6.2828.020 Glass cartridge holder To hold the 6.1006.0040 Column cartridge METROSEP Anion Dual 1. 12 92 204 6.2832.000 Suppressor rotor Replacement cartridge for Metrohm suppressor module 6.2832.
6.3 Optional accessories 6.3.4 Additional devices and cables Order No. Description 2.750.0010 750 Autosampler Sampler for the automation of sample injection. Capacity: 128 sample vessels each with an effective volume of ca. 700 µL; incl. accessories. Accessories: 2.766.
6 Appendix 6.4 Warranty and conformity 6.4.1 Warranty The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error which occur within 12 months from the day of delivery. In this case, the defects will be rectified in our workshops free of charge. Transport costs are to be paid by the customer. For day and night operation, the warranty is limited to 6 months. Glass breakage in the case of electrodes or other parts is not covered by the warranty.
6.4 Warranty and conformity 6.4.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the instrument: 761 Compact IC meets the requirements of EC Directives 89/336/EEC and 73/23/EEC.
6 Appendix 6.4.3 Certificate of conformity and system validation Certificate of Conformity and System Validation This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity: 761 Compact IC System software: Stored in ROMs Name of manufacturer: Metrohm Ltd.
6.5 Index 6.5 Index 1 1st component .................................... 107 1st peak............................................... 108 7 750 .......................... see Autosampler 750 761 Compact IC ........................... 69,70,82 761 unit version ..................................... 90 766 ............ see IC Sample Processor 766 A Abrasive particles ............................... 170 Absolute calibration..................... 119,126 Absolute concentration ................
6 Appendix Output ............................................. 128 Plot area .......................................... 152 Preview............................................ 128 Print ................................................. 128 Report ............................................. 132 Results ............................................ 125 Weighting ........................................ 127 Calibration data Export .............................................. 128 Import.....................
6.5 Index Connection capillary 35 Connection of pulsation dampener 60 .................... 25 Figure.......................................... 7,9,26 Connection capillary 37 Figure.......................................... 7,9,26 Connection capillary 38 Figure............................................... 7,9 Connection capillary 43 Detaching ....................................... 176 Figure............................................... 7,9 Connection capillary 44 Figure..................................
6 Appendix Eluents Notes............................................... 171 EMC .................................................... 193 Emitted interference............................ 193 Enable baseline penetration ................ 116 Enable detection .................................. 113 Enable negative peaks ......................... 113 Enable peak reject ............................... 113 Enable valley-to-valley ......................... 114 ENABLED ...............................................
6.5 Index IC precolumn cartridge Nucleosil 5SA ................................. 202 IC precolumn cartridge PRP-1 ........... 201 IC precolumn cartridge PRP-X100..... 200 IC precolumn cartridge PRP-X300..... 200 IC pump ................................................ 87 IC Sample Processor 766 Connection ....................................... 50 Ordering designation ..................... 205 Settings............................................. 51 IC separating columns .........................
6 Appendix Merge peaks ........................................ 151 Method ....................................98,142,167 Definition ...................................... 68,97 File handling...................................... 97 File type............................................. 72 GLP Log .......................................... 102 Open ................................................. 97 Overwrite ........................................... 76 Path .............................................
6.5 Index Power consumption ........................... 192 Power failure ......................................... 94 Power on ............................................... 94 PowerOn values .................................... 93 Practical notes .................................... 169 Precautionary rules............................... 12 Precipitates.................................. 170,171 Precolumn ........................................... 100 Precolumn cartridge 77 Figure.........................
6 Appendix Replacement of piston seals................................. 170 Replacing the suppressor .................. 183 Report Auto-printing ................................... 106 Calibration....................................... 132 Calibration curve............................. 132 Component table ............................ 132 Directory for report output .............. 136 File name ........................................ 136 File output ....................................... 133 Integration ..
6.5 Index Set min height ..................................... 116 Start with inject ......................................82 Set normal baseline ............................ 114 Started .................................................158 Set peak end ....................................... 113 Starting ..................................................95 Set peak start ...................................... 113 Startup ...................................................95 Set rider ratio .........
6 Appendix Tic marks ............................................. 146 Void volume .................................. 100,108 Time...............................81,98,99,113,120 Time axis ............................................. 145 Time delay........................................... 104 Time program Enable ............................................... 88 Entry .................................................. 88 Report ............................................... 83 Start mode ..............
