CH-9101 Herisau/Switzerland Phone ++41 71 353 85 85 Fax ++41 71 353 89 01 CompuServe 100031,3703 Internet http://www.metrohm.com E-Mail sales@metrohm.ch 732 IC Detector 733 IC Separation Center 5.732.0012 Program Metrohm 732 IC Detector +0.023 µS/cm 15.2 min Full Scale 5.00 µS/cm OVERLOAD THERMOSTAT CONFIG PUMP R/S METHOD 7 8 9 ZERO OFF EVENT PROGRAM 4 5 6 PLOT REPORT PRINT 1 2 3 SELECT CLEAR .
Table of contents Table of contents 1 Introduction ............................................................................................ 1 1.1 Instrument description............................................................................. 1 1.2 Parts and controls..................................................................................... 3 1.2.1 732 IC Detector ............................................................................. 3 1.2.2 733 IC Separation Center .............
Table of contents 2.8 Separating columns and suppressor module.................................... 32 2.8.1 General information on separating columns .............................. 32 2.8.2 Selection of the sample loop ...................................................... 32 2.8.3 General information on suppressor module ............................... 33 2.8.4 One-channel system without suppressor module...................... 35 2.8.5 Two-channel system without suppressor module ......................
Table of contents 4.6 Triggering of functions ........................................................................103 4.6.1 keys ............................................................................. 103 4.6.2 keys........................................................................ 104 4.6.3 key ............................................................................ 105 4.6.4 key ................................................................... 106 4.
Table of contents 6 Interfaces .......................................................................................... 161 6.1 RS232 interfaces ................................................................................... 161 6.1.1 General rules for remote control ............................................... 161 6.1.2 Call-up of objects ...................................................................... 162 6.1.3 Triggers .....................................................................
Table of contents List of figures Fig. 1: Block diagram of the ion chromatography system ........................................... 2 Fig. 2: Front of the 732 IC Detector .............................................................................. 3 Fig. 3: Rear of the 732 IC Detector ............................................................................... 4 Fig. 4: Front of the 733 IC Separation Center............................................................... 5 Fig.
Table of contents List of numbered parts and controls 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 VI Display ................................................ 3 Main function keys .............................. 3 Numeric keys ...................................... 3 Auxiliary function keys......................... 3 Program status display ....................... 3 Auto-zero display ...................
1.1 Instrument description 1 Introduction 1.1 Instrument description The 732 IC Detector is a conductivity detector especially designed for ion chromatography with an extensive operating range and high sensitivity for the recording of chromatograms with and without chemical suppression. The associated thermostattable detector block is normally installed in the 733 IC Separation Center, but can also be used as a separate detector. The two following versions are available: • 2.732.
1 Introduction The 732 IC Detector and 733 IC Separation Center are the main components of a modular ion chromatography system that can be expanded to meet the wishes of the individual user (see Fig. 1). The minimum configuration of the one-channel system also includes a 709 IC Pump, a separating column and a recorder. The two-channel system requires at least a second 732 IC Detector and a second 709 IC Pump. Printers, integrators, data recording devices, PC and autosamplers can be attached to both systems.
1.2 Parts and controls 1.2 Parts and controls 1.2.1 732 IC Detector 8 1 2 3 4 732 IC Detector CONFIG +0.023 µS/cm 15.2 min Full Scale 5.00 µS/cm OVERLOAD THERMOSTAT PUMP R/S METHOD 7 8 9 ZERO OFF EVENT PROGRAM 4 5 6 PLOT REPORT PRINT 1 2 3 SELECT CLEAR . -/+ QUIT ENTER MARK ZERO 7 PARAM FULL SCALE PROG R/S 6 0 5 Fig.
1 Introduction 10 9 11 12 13 Output Type 1.732.0010 Nr. 0...1V 0...10mV Detector Block f=50-60 Hz S=70 VA Fuse 100-120V: 0,63A(T) 220-240V: 0,315A(T) Remote 733 IC Separation Center RS 232 709 IC Pump WARNING - Fire Hazard - For continued protection replace only with the same type and rating of fuse 19 S 18 Made by Metrohm Herisau Switzerland 17 16 15 14 Fig.
1.2 Parts and controls 1.2.2 733 IC Separation Center 733 IC Separation Center STEP FILL INJECT FILL A 20 21 22 23 INJECT B 24 25 26 27 28 Fig. 4: Front of the 733 IC Separation Center 20 Door to interior 25 "FILL" key for valve B or "STEP" for suppressor module 21 Connection for 6.2816.020 Syringe 26 "INJECT" key for valve B 22 Feedthrough for aspirating tubing 27 733.0010: Feedthrough for capillary 733.0X20: Connection for 6.2816.020 Syringe 733.
1 Introduction 29 30 31 32 33 34 34 Waste B Waste A l d l t r . l s i a o A R C U .gerntI S R C U 732 IC Detector t i R C U G r F Inject P o F t R C U .gerntI S B 732 IC Detector O O M 37 46 45 36 N M N O O N M 37 34 Made by Metrohm Herisau Switzerland N 47 Type: 1.733.00X0 Nr.: XX XXX M 48 External Power 24VDC/2A 5VDC/0,5A G r F Inject P o F i i a o s r u l . l u l t 34 n n l l d 35 38 Inlet B Inlet A 39 37 37 44 43 42 41 40 Fig.
1.
1 Introduction 1.3 Information on the Instructions for Use Please read through these Instructions for Use carefully before you put the 732 IC Detector and 733 IC Separation Center into operation. The Instructions for Use contain information and warnings which must be heeded the user to assure safe operation of the instruments. 1.3.1 Organization These 8.732.
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: Key "Range" Parameter or entry value 35 Part or control of 732/733 22 Part or control of 709 >PARAM/detector range: 1.00 mS/cm Display Text in display 1 of the 732 IC Detector 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 732 IC Detector and 733 Separation Center is assured in the context of the specifications IEC 1010-1 (protection class 1, degree of protection IP40), 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 Flow chart 2 Installation 2.1 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 Yes 733.0X20 No Connecting 733 sect. 2.3.1 Installing accessories Connecting 733 sect. 2.3.2 Passivation sect. 2.6.7 Precolumn with twin cartridge holder Precolumn with cartridge head IC anion precolumn SUPERSEP sect. 2.7.2 sect. 2.7.3 sect. 2.7.4 Connecting separating column sect. 2.8.
2 Installation 2.2 Setting up the instruments 2.2.1 Packaging The 732 IC Detector and 733 IC Separation Center are supplied together with the separately packed accessories in special packagings containing shock-absorbing foam linings designed to provide excellent protection. The actual instruments are 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 instruments free from damage. 2.2.
2.3 Connection of 733 IC Separation Center 2.3 Connection of 733 IC Separation Center 2.3.1 2.733.0010/2.733.0X30 IC Separation Center The instrument versions 2.733.0010 and 2.733.0030 of the IC Separation Center are operated with a 732 IC Detector whose standard equipment also includes the 1.732.0100 Detector block. For the metal-free 2.733.0130 instrument version the metal-free 1.732.0110 Detector block must be used.
2 Installation 2.3.2 3 Connect waste container • Lead the outlet capillary of the detector block to a sufficiently large waste container and fix in place. 4 Connect 732 to 733 • Plug one end of the 6.2125.090 Connecting cable into connection 14 "733 IC Separation Center” of the 732 IC Detector and fasten to the instrument by tightening the screws in the cable connector (see Fig. 6). • Plug the other end of the 6.2125.
2.3 Connection of 733 IC Separation Center 3 Connect waste container • Lead the outlet capillaries of the two detector blocks to a sufficiently large waste container and fix in place. 4 Connect 732 to 733 • Plug one end of the 6.2125.090 Connecting cable into connection 14 "733 IC Separation Center“ of the first 732 IC Detector and fasten to the instrument by tightening the screws in the cable connector (see Fig. 7). • Plug other end of the 6.2125.
2 Installation 2.3.3 Connection of syringe and aspirating tubing For manual filling of the sample loops mounted on the injection valves, the 6.2816.020 Syringe and the PTFE aspirating tubing already screwed to the valve are needed. These accessories are mounted or adjusted as follows: 2.3.4 1 Connect syringe • Push 6.2816.020 Syringe (without needle) as far as it will go into connection socket 21 (for valve A) or 27 (for valve B) (see Fig. 4).
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 732 IC Detector for the first time, check that the mains voltage set on the instrument (see Fig. 8) matches the local mains voltage.
2 Installation 220 – 240 V 100 – 120 V 9 9 Mains switch 18 18 Mains connection plug 19 19 Fuse holder 220 - 240 V 100 - 120 V 220 - 240 V 100 - 120 V Fig. 8: Setting the mains voltage 2.4.2 Fuses One of the two fuses 0.63 A/slow-blow for 100…120 V or 0.315 A/slowblow for 220…240 V is installed in fuse holder 19 of the 732 IC Detector as standard.
2.5 Capillary connections 2.5 Capillary connections 2.5.1 Capillaries Some of the connections under high pressure between the feed pump and the detector block must be set up by the user. For metal-free systems, the 6.1831.010 PEEK capillary (i.d. = 0.25 mm, e.d. = 1/16", length = 3 m) must be used. For non metal-free systems, the 6.1831.
2 Installation 49 50 51 52 Fig. 9: Connectors for capillaries 2.5.3 49 Ferrule (6.2620.010) 50 Pressure screw (6.2620.000) 51 Capillary 6.2620.020 Steel capillary or 6.1831.010 PEEK capillary 52 Compression fitting (6.2744.010) PEEK connectors For the connection of 6.1822.010 PEEK capillaries (i.D. = 0.3 mm) or 6.1822.010 PTFE microcapillaries, the 6.2744.010 PEEK compression fittings are used. Proceed as follows: 20 1 Mount compression fitting Slide a compression fitting 52 (6.2744.
2.6 Connection of 709 IC Pump 2.6 Connection of 709 IC Pump 2.6.1 Electrical connection For operation of the 732 IC Detector and 733 IC Separation Center you can use any commercial HPLC pump. However, as the attainable sensitivity depends to a large extent on the quality of the pump, Metrohm advises use of the 709 IC Pump, which has been specially developed for the demands of ion chromatography and has minimal pump pulsation and an outstanding flow constancy.
2 Installation 2.6.3 Filter unit PEEK The 6.2821.100 Filter unit PEEK (see Fig. 11) supplied with the 709 IC Pump is installed between the 709 IC Pump and the injection valve at the 733 IC Separation Center. This filter unit serves to avoid contamination of the piston seals of the 709 IC Pump by abrasive particles and can be used in the pressure range 0…25 MPa (0…250 bar). The two filter units PEEK supplied with the 2.733.
2.6 Connection of 709 IC Pump 2.6.4 Filter unit Manufit The optional 6.2821.000 Filter unit Manufit (see section 7.3.1) is installed between the 709 IC Pump and the injection valve at the 733 IC Separation Center. The filter unit serves to avoid contamination of the piston seals by abrasive particles and can be used in the pressure range 0…50 MPa (0…500 bar) for non metal-free systems together with steel capillaries. It is installed as follows (see Fig.
2 Installation 2.6.5 Connection to injection valve with PEEK capillaries For metal-free systems and for non metal-free systems in the pressure range 0…25 MPa (0…250 bar) we recommend to use 6.1831.010 PEEK capillaries, a 6.2620.150 Pulsation dampener (see section 2.6.2) and a 6.2821.100 Filter unit PEEK (see section 2.6.3) to connect the 709 IC Pump and the injection valve of the 733 IC Separation Center. Proceed as follows: For the connection of capillaries to the injection valve, use only the 6.2744.
2.6 Connection of 709 IC Pump 22 64 65 66 67 68 65 733 709 Fig. 13: Connection to injection valve with PEEK capillaries 22 Connection capillary 6.1831.010 PEEK capillary 66 Pulsation dampener (6.2620.150) 64 Filter unit PEEK (6.2824.100) 67 Column connection capillary 6.1831.010 PEEK capillary 65 PEEK capillary (6.1831.010) 68 Injection valve 2.6.6 Connection to injection valve with steel capillaries For the pressure range 25…50 mPa (250…500 bar) we recommend to use 6.2620.
2 Installation 2 Installation of the capillary in the IC Separation Center • Unscrew the four knurled screws 37 of the bottom rear panel 39 of the 733 IC Separation Center and remove rear panel (see Fig. 5). • Insert steel capillary 71 from the back into the inner compartment of the IC Separation Center. • Install rear panel 39 so that the capillary is positioned in opening 40 „Inlet A“ or 44 „Inlet B“ and screw on with the four knurled screws 37.
2.6 Connection of 709 IC Pump 2.6.7 Passivation of the IC system With non metal-free IC systems, the entire IC system (without precolumn, separating column and suppressor module) must be passivated with nitric acid before being put into operation for the first time. Proceed as follows: 1 Connect detector block to injection valve • Connect column connection capillary 67 using a 6.2620.060 Coupling directly to inlet capillary 82 of the detector block (see Fig. 16).
2 Installation 2.7 Precolumns 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 7.3.2) are either real precolumns or precolumn cartridges, which are used together with the 6.2821.050 Twin cartridge holder or a 6.2821.040 Cartridge head. New IC precolumns are normally filled with solution and sealed at both ends.
2.7 Precolumns with 6.2821.050 Twin cartridge holder with 6.2821.040 Cartridge head Säule 76 72 77 57 60 59 59 78 59 73 74 73 74 73 73 59 59 79 62 80 49 75 50 67 Injektor Injektor Fig. 15: Installing precolumn cartridges 49 Ferrule (6.2620.010) 73 2 Steel meshes (6.2821.020) 50 Pressure screw (6.2620.000) 74 Precolumn cartridge 57 Manufit pressure screw 75 Inlet capillary 59 PTFE gasket (6.2821.010) 76 IC separating column 60 4 Steel meshes (6.2821.
2 Installation 2.7.3 Precolumns with cartridge head The precolumn cartridges are installed in the 6.2821.040 Cartridge head as follows (see Fig. 15): 30 1 Prepare separating column • Remove end caps from separating column 76. 76 • Unscrew fastening screw from column inlet. • Take steel connector 79 for ferrule out of fastening screw. 2 Install cartridge • Remove end caps for precolumn cartridge 74 (the steel mesh 73 and gaskets 59 are already installed in the cartridge).
2.7 Precolumns 2.7.4 IC anion precolumn SUPERSEP The 6.1009.010 IC Anion Precolumn SUPERSEP has two connections for steel or PEEK capillaries and is installed as follows: 1 Connect precolumn • Remove end caps from the precolumn. • Fit connectors to column connection capillary 67 mounted on the injection valve (see section 2.5). • Screw precolumn to column connection capillary 67. 67 • Cut a piece from the 6.2620.020 Steel capillary or the 6.1831.
2 Installation 2.8 Separating columns and suppressor module 2.8.1 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 7.3.2.
2.8 Separating columns and suppressor module 2.8.3 General information on suppressor module The Metrohm Suppressor Module MSM for chemical suppression installed in the 2.733.0X30 IC Separation Center 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 Installation 81 82 83 84 76 68 83 84 67 85 66 STEP FILL INJECT FILL A 86 INJECT B 65 87 88 Fig. 16: Interior of the 2.733.0010 IC Separation Center 34 65 Capillary to 709 IC Pump 83 Mounting rail 66 Pulsation dampener (6.2620.150) 84 Column holder (6.2027.0X0) 67 Column connection capillary 85 Capillary for syringe PEEK capillary, fixed mounting 68 Injection valve 86 Sample loop (6.2620.
2.8 Separating columns and suppressor module 2.8.4 One-channel system without suppressor module With the one-channel system without suppressor module, the IC separating column is installed in the 2.733.0010 IC Separation Center as follows (see Fig. 16): 2.8.5 1 Connect column to injector • Remove end caps from column 76. 76 • without precolumn: Screw inlet end of separating column 76 (note flow direction) to column connection capillary 67 mounted on the injector.
2 Installation 89 81 83 82 83 84 84 76 68 96 83 95 1 2 3 84 94 93 92 67 85 66 STEP FILL INJECT FILL A 86 INJECT B 65 87 88 90 91 Fig. 17: Interior of the 2.733.0X30 IC Separation Center 36 43 Rear panel opening 83 Mounting rail 65 Capillary to 709 IC Pump 84 Column holder (6.2027.0X0) 66 Pulsation dampener (6.2620.150) 85 Capillary for syringe PEEK capillary, fixed mounting 67 Column connection capillary PEEK capillary 86 Sample loop (6.1825.
2.8 Separating columns and suppressor module 91 Suppressor outlet capillary for H2SO4 94 Suppressor outlet capillary for eluent 92 Suppressor outlet capillary for H2O 95 Suppressor module 93 Suppressor inlet capillary for H2O 96 Coupling (6.2620.060; steel) or Coupling (6.2744.040; PEEK) 2.8.6 One-channel system with suppressor module In the case of the one-channel system with suppressor module, first the IC separating column is installed in the 2.733.0X30 IC Separation Center (see Fig.
2 Installation Eluent H2SO4 89 90 94 Detector 1 89 Suppressor inlet capillary for eluent 90 Suppressor inlet capillary for H2SO4 91 Suppressor outlet capillary for H2SO4 92 Suppressor outlet capillary for H2O 93 Suppressor inlet capillary for H2O 94 Suppressor outlet capillary for eluent 2 3 Waste 91 93 92 H2O Waste Fig. 18: Connections at suppressor module • Screw outlet capillary 94 to coupling 96 using a 6.2744.010 Compression fitting.
2.8 Separating columns and suppressor module • Attach inlet capillary 90 using a 6.2744.010 Compression fitting to the connector 55 of the filter unit PEEK (see section 2.6.3). • Attach a piece of the 6.1803.020 PTFE tubing (from 752 accessories) cut to the required length using a 6.2744.010 Compression fitting to the connector 53 with filter at the other end of the Filter unit PEEK. • Attach the other end of the PTFE tubing using a 6.2744.010 Compression fitting to the 6.2744.
2 Installation 2.8.7 Leak testing and conditioning Before sample solutions can be injected in the IC system, the entire system must be tested for leaks and then conditioned with eluent until the baseline is stable. Proceed as follows: 40 1 Switch on 709 IC Pump • Immerse aspirating capillary of the 709 IC Pump in eluent. • Set flow rate recommended on the 709 IC Pump for the separating column used (normally 0.5…2 mL/min). • Set maximum shutoff pressure on the 709 IC Pump (normally ca.
2.9 Connection of external devices 2.9 Connection of external devices 2.9.1 Connection of a recorder For the connection of a recorder the 732 IC Detector has the two analog outputs 11 (0…1 V) and 12 (0…10 mV) available (see Fig. 3). A diagram of the circuit of the two analogue outputs can be found in section 6.3. The polarity of the output signals at the analog output sockets can be switched at any time under the key (see section 4.5.1).
2 Installation 2.9.6 Connection of a printer External printers are normally connected to the 732 IC Detectorr via the RS232 interfaces 16 (see Fig. 3). If no 709 IC Pump is connected, a printer can also be attached to connection 15 "709 IC Pump". You will find more detailed information on the RS232 interfaces in section 6.1.
2.9 Connection of external devices Printer Seiko DPU-411 Seiko DPU-414 Cable 6.2125.020 6.2125.
2 Installation If you connect other printers, ensure that these emulate a printer mode supported by the 732 IC Detector. Most printers with a serial interface are connected using the 6.2125.050 Cable. Printers with a parallel interface need a serial/parallel converter (e.g. 2.145.0300) and the 6.2125.020 Cable. 2.9.7 Connection of a PC IBM-compatible PCs are connected to the 732 IC Detector via RS232 interface 16 (see Fig. 3). You will find more detailed information on the RS232 interface in section 6.
3.1 Requirements 3 Operating tutorial This section introduces you to the operation of the 732 IC Detector and 733 IC Separation Center by means of a brief operating tutorial which describes the basic operating steps needed for the recording of an ion chromatogram and the development of a method. The determination of the anionic content of a drinking water sample with the PRP-X100 IC Anion Column using the single column technique is used an illustrative example.
3 Operating tutorial • 6.2821.100 Filter unit PEEK Filter between 709 IC Pump and injection valve to avoid contamination. • 6.1005.000 PRP-X100 IC Anion Column • Eluent 2 mmol/L phthalic acid / 8% acetone / pH 5.0 in dist. H2O flow: 2 mL/min • Standard Standard solution with 5 ppm Cl– and 10 ppm each of NO3– and SO42– (in dist. H2O) • 2.714.
3.2 Preparations 3 Install 709 IC Pump ⇒ ⇒ ⇒ ⇒ ⇒ ⇒ 4 5 6 *(see 709 Instructions for Use) Setting up pump Mounting pump head Tubing connections Power supply connection Switching on pump Degassing pump Connect 709 IC Pump ⇒ Electrical connection at 732 IC Detector (requires 6.2125.
3 Operating tutorial 3.3 Putting into operation After the complete IC system has been installed as described in section 3.2, it can be put into operation. In what follows, all operating steps up to the first calibration with the standard solution are described in sequence. Please note that all displays refer to the condition in which the instrument was put into operation for the first time (initial condition).
3.3 Putting into operation 4 Switch on 732 IC Detector ⇒ Switch on 732 IC Detector with mains switch 9 at the rear of the instrument. 151.2 µS/cm method After the instrument has been switched on, display 1 lights up and shows the status messages for the basic instrument condition. The 732 IC Detector is now in the standby mode of conductivity measurement. The displayed values have the following meaning: 0.0 min DEFAULT Measured absolute conductivity 151.2 µS/cm 0.2 min full scale 1.
3 Operating tutorial 151.2 µS/cm pump ready 1.2 min The bottom line of the display shows the status message for the 709 IC Pump. If the remote operation is switched on correctly (see point 4), the status message "pump ready" now appears. If the IC Pump is operated independently, the message "pump not responding" appears instead. ⇒ Press the
3.3 Putting into operation >CONFIG/detector 'zero' unit: The next inquiry of the submenu "detector" appears, namely the unit for display of the auto-zero value. This parameter also contains the character ":". The
3 Operating tutorial The title of the submenu "auxiliaries" appears in the bottom line of the display. This submenu contains, among other things, the inquiries for entry of the date, time and dialog language. CONFIG >CONFIG/auxiliaries ⇒ Press the key to move to the inquiries. ENTER >CONFIG/auxiliaries run number 0 The display shows the selection of the run number as the first inquiry. As we have no further interest in this here, we can proceed directly to the next inquiry.
3.3 Putting into operation If you wish to change the displayed time, enter the new numeric values in the order hours – minutes – seconds using the numeric keys, e.g. "08:32:00". The new time does not become active until you confirm it by pressing the key. ⇒ Confirm the new time by pressing the key. ENTER The display now shows the selection of the dialog language, which is set to "english", as the next inquiry. The character ":" again appears with this display.
3 Operating tutorial Fundamentals of the instrument dialog Main menu Each key of the 732 IC Detector opens a main menu whose thematically arranged submenus can be selected by repeated pressing of this key. The name of the key always appears in the top line of the display. 7 Submenu Each submenu has a title which is marked by ">" and appears in the bottom line of the display.
3.3 Putting into operation ⇒ Confirm the selected measuring range by pressing the key. ENTER The next inquiry which appears concerns the full-scale range. The full-scale range (operating range) is used to set the desired sensitivity for the display and analog output of the measuring signal during the recording of the chromatogram. This value is set using the key, but not until later (see section 3.4, point 2).
3 Operating tutorial >PARAM/analog output damping: off ENTER PARAM >PARAM/plot 9 The electronic damping of the analog output signal must normally not be switched on. ⇒ Confirm the switched-off status of the damping with the key. The title of the submenu "plot" appears. This submenu contains various inquiries regarding the graphics printout on an external printer. As we shall not deal with the settings for such a printer in this brief tutorial, we can switch directly to the next inquiry.
3.3 Putting into operation The maximum admissible pressure for the PRP-X100 IC Anion Column is 34 MPa, the normal operating pressure is 2 mL/min at ca. 7 MPa. A value of 10 MPa is thus entered as the maximum shutoff pressure. >PARAM/709 IC Pump Pmax 10.0 MPa ⇒ Confirm the set maximum shutoff pressure with the key. ENTER The parameter "Pmin" denotes the minimum shutoff pressure for the 709 IC Pump. If the pressure drops below this value for a considerable length of time (e.g.
3 Operating tutorial 10 Start 709 IC Pump If you do not operate the 709 IC Pump by remote control via the 732 IC Detector, the pump must be switched on directly using the key (see 709 Instructions for Use). ⇒ Press the key. The pump drive of the 709 IC Pump is started. PUMP R/S 8 151.2 µS/cm pump running 8.9 min 6.9 MPa After the start of the 709 IC Pump, an automatic switch is made to the status message for the pump.
3.4 Calibration 3.4 Calibration After putting into operation and conditioning the IC system as described in section 3.3, the first calibration can now be performed. This requires a standard solution which contains the analyte substances in about the same concentration as expected in the sample.
3 Operating tuturial OVERLOAD 3 Trigger auto-zero ZERO +0.000 µS/cm 56.4 min full scale: 4.00 µS/cm 4 ⇒ Press the key. This starts the automatic electronic background compensation. During zeroing, the green LED in the key starts to flash. As soon as zeroing is at an end, the green LED in the key is permanently on. The top line of the display shows the auto-zero value in place of the absolute conductivity.
3.4 Calibration As soon as injection valve A is in the "INJECT" position, the current time is reset to "0.0 min". This marks the start time of the chromatogram. The ion chromatogram of the standard is plotted in the next 20 min or so. Fig. 19 shows an example of a calibration with 5 ppm Cl–, 10 ppm NO3– and 10 ppm SO42–. +0.000 µS/cm 0.0 min full scale: 4.00 µS/cm 7.00e+005 Standard 6.00e+005 5.00e+005 Cl– 4.00e+005 3.00e+005 NO3– SO42– 2.00e+005 1.00e+005 0.
3 Operating tutorial 3.5 Sample determination Following the calibration of the IC system as described in section 3.4 the first sample solution can be injected. 1 Filter drinking water sample ⇒ Filter the drinking water sample with a 0.45 µm microfilter. 2 Trigger auto-zero ZERO ⇒ Press the key. This starts the automatic electronic background compensation. During zeroing, the green LED in the key starts to flash.
3.5 Sample determination 7.00e+005 6.00e+005 Drinking water 5.00e+005 Cl– 4.00e+005 3.00e+005 NO3– 2.00e+005 SO42– 1.00e+005 0.00e+005 0 2 4 6 8 10 12 14 16 18 FULL REPORT Ret Time (Min) -------1.749 3.160 10.323 Component Name --------------Chloride Nitrate Sulphate Concentr. ppm ----------5.487972 9.647280 7.142281 Area (uV*Sec) ---------3064128.00 2320973.25 3322615.75 Height (uV) ---------381971.937 189443.562 112246.203 Fig.
3 Operating tutorial 3.6 Storing as a method The parameter settings used for the drinking water determination can be stored in the 732 IC Detector as a method and hence later recalled at any time. Proceed as follows to store the inputted settings under the name "Water": ⇒ Press the key to open the main menu for method management. METHOD 9 The title of the submenu "METHOD/recall" appears. This is used to load a method already stored in the working memory. Proceed further to the next submenu.
3.6 Storing as a method >METHOD/store name: The second letter of the name is now the desired "a". Wabcdefg ⇒ Press the key to confirm the second letter. ENTER >METHOD/store name: Waabcdef ⇒ Press the <è> key repeatedly until the letter "t" appears at the flashing position. -/+ >METHOD/store name: The third letter of the name starts to flash and can be selected with the <ç> and <è> keys. The third letter of the name is now the desired "t".
3 Operating tutorial >METHOD/store name: Water ENTER +0.000 µS/cm 28.4 min full scale: 4.00 µS/cm The display shows the complete method name "Water" for confirmation. ⇒ Press the key to confirm the method name. The parameters are now stored in the instrument under the name "Water". The 732 IC Detector is now again in the standby mode and the display shows the status messages. A method report of the method "Water" just stored can be outputted with the key (see section 4.8.
4.1 Operating sequences 4 Operation This section provides a detailed description of the operation of the 732 IC Detector and 733 IC Separation Center using the keypad and dialog display. After an overview of the various operating sequences (section 4.1), the fundamentals of the operation are explained (section 4.2). This is followed by a detailed description of the display (section 4.3) and key functions (section 4.4 – 4.8). A few selected illustrative methods complete this section 4 (section 4.9). 4.
4 Operation 4.1.2 Flow chart for basic settings The following flow diagram shows the basic SETUP and CONFIG settings which must be selected for the 732 IC Detector as a function of the attached devices. You will find detailed information in section 4.4. Start Remote connection? yes SETUP/output SETUP/input assign yes SETUP/graphics no SETUP/peripherals operation with 733 = off no SETUP/peripherals operation with 709 = off yes CONFIG/RS settings CONFIG/printer yes CONFIG/print meas.
4.1 Operating sequences 4.1.3 Flow chart for putting into operation The following flow diagram shows how the IC system can be put back into operation after a separating column has been removed and all devices have been switched off (shutdown, see section 5.2.4). A requirement is that the installation (section 2.1) is complete and the basic settings (section 4.1.2) have been made. You will find further information in the sections mentioned. Start Preparing eluent sect. 5.1.
4 Operation 4.1.4 Flow chart for injection The following flow diagram shows how an injection is started on the IC system with and without a program. If the points , and "Siphoning in sample" are not programmed or must be performed by the Autosampler, they must also be manually triggered. You will find further information in the sections mentioned. Start no Program? yes sect. 4.6.3 sect. 4.6.1 Siphoning in sample New program? yes Editing program sect. 4.7.
4.2 Fundamentals of the operation 4.2 Fundamentals of the operation 4.2.1 Display LCD 1 on the 732 IC Detector comprises two lines each of 24 characters. What appears on the display depends on whether the instrument is in the standby mode or the edit mode. Standby mode After the 732 IC Detector has been switched on, the instrument is always automatically in the standby mode of conductivity measurement.
4 Operation 4.2.2 Overview of key functions Key field of 732 IC Detector +0.023 µS/cm 15.2 min Full Scale 5.00 µS/cm OVERLOAD THERMOSTAT CONFIG PUMP R/S 7 8 METHOD 9 ZERO OFF EVENT PROGRAM 4 5 6 PLOT REPORT PRINT 1 2 3 SELECT CLEAR . -/+ QUIT ENTER MARK ZERO PARAM FULL SCALE PROG R/S Main function keys 0 Numeric keys Auxiliary function keys The key field of the 732 IC Detector contains 4 colored main function keys, 12 gray numeric keys and 4 gray auxiliary function keys.
4.2 Fundamentals of the operation Main function keys of 732 IC Detector Key ZERO PARAM Standby mode Trigger auto-zero • Automatic zeroing of the current conductivity (the green LED in the key lights up). Trigger auto-zero • Automatic zeroing of the current conductivity (the green LED in the key lights up). Open parameter menu • Opens the main menu for setting the parameters for the conductivity detector, analog output, graphics plot and 709 IC Pump.
4 Operation Numeric keys of 732 IC Detector Key CONFIG 7 PUMP R/S 8 METHOD 9 ZERO OFF 4 EVENT 5 PROGRAM 6 74 Standby mode Edit mode Open configuration menu • Opens the main menu for configuration of the 732 IC Detector. • The settings in the configuration menu are retained until they are changed or the working memory (RAM) is initialised. Numeric entry ('7') or select submenu or parameter • Selection of the next submenu in the main menu. • Selection of the next parameter in the submenu.
4.2 Fundamentals of the operation Key PLOT 1 REPORT 2 PRINT 3 MARK 0 Standby mode Edit mode Start graphics plot • Output of measured value curve on an external printer (abort with ). Numeric entry ('1') Start report output • Selection of report and output on an external printer (abort with ).
4 Operation Auxiliary function keys of 732 IC Detector Key SELECT Standby mode Edit mode Select status message • Selection of the status messages for full-scale range, absolute conductivity, 709 IC Pump, program, method, date and time. Select preset parameter values • Selection from preset parameter values for parameters which are marked by a colon ":". No function Delete parameter values • Deletion of the displayed parameter values and resetting to default values or "0".
4.2 Fundamentals of the operation 4.2.3 Instrument dialog The instrument dialog of the 732 IC Detector is organized in the form of so-called rolling inquiries which are arranged in menu levels in a hierarchical manner and are subject to the following rules: Main menu The main function keys as well as most numeric keys of the 732 IC Detector open a main menu whose thematically arranged submenus are selected by repeated pressing of this key.
4 Operation Standby mode KEY Key title >Submenu 1 QUIT ENTER >Submenu 1 Inquiry 1 ENTER KEY QUIT >Submenu 1 Inquiry 2 Key title >Submenu 2 ENTER >Submenu 1 Inquiry n ENTER >Submenu 2 Inquiry 1 ENTER KEY QUIT >Submenu 2 Inquiry 2 ENTER >Submenu 2 Inquiry n Key title >Submenu n KEY Fig.
4.2 Fundamentals of the operation 4.2.4 Data entry Numeric entry PLOT 1 With inquiries in which the parameter title has no colon ":", the parameter values can be entered directly with the numeric keys.
4 Operation 4.2.5 Text entry With certain inquiries which require the entry of a text, any ASCII characters can be entered to write the texts. Opening the text editor The "ç" " or "è" keys open the text editor. . -/+ "ç" is used to delete an existing character string and to position the text cursor at the left edge of the entry field. With "è" an existing character string is retained, the text cursor is positioned on the last character of the existing text.
4.3 Displays in the standby mode 4.3 Displays in the standby mode 4.3.1 Measured value and current time In the standby mode of the conductivity measurement, the top line of the display always shows the current measured value (left) and the current time (right). 151.2 µS/cm method 13.5 min DEFAULT Measured value The following possibilities exist for the display of the measured value: Measured value without sign 151.2 µS/cm Absolute conductivity in µS/cm or mS/cm.
4 Bedienung 4.3.2 Status messages SELECT Pressing the
4.3 Displays in the standby mode stopped: YY-MM-DD HH:MM The 709 IC Pump was stopped at the time indicated owing to violation of the shutoff limit "Pmin" or "Pmax". To restart a pump stopped in this manner, the pump keys and must be pressed in succession and then pressed again (see also section 4.5.1).
4 Operation 4.4 Basic settings 4.4.1 Setup Under "Setup", various basic settings of the 732 IC Detector are combined which normally seldom need to be changed. They are accessible only when the key is pressed at the same time as the instrument is switched on.
4.4 Basic settings Assignment of the remote input lines The 732 IC Detector has 4 programmable remote input lines which can be used to trigger a total of 15 different instrument functions (for details, see section 6.2.1). The default assignment of the individual functions to the status of the 4 input lines 2…5 (defined by the corresponding decimal code 1…15) can be changed if need be. Several functions can thus also be assigned the same status.
4 Operation >SETUP/input assign ZERO OFF 9 Switch off auto-zero Equivalent to pressing the key. 1…15 >SETUP/input assign PLOT 10 Plot output Equivalent to pressing the key. 1…15 >SETUP/input assign polarity 11 1…15 >SETUP/input assign SELECT 13 Switch the polarity The polarity of the signal at the analog output is switched. Select Equivalent to pressing the
4.4 Basic settings Setting the peripherals >SETUP >SETUP/peripherals >SETUP/peripherals operation with 733: on on, off >SETUP/peripherals operation with 709: on on, off 732 IC Detector / 733 IC Separation Center Operation with 733 IC Separation Center on The 732 IC Detector is operated with the 733 IC Separation Center (normal case). Off The 732 IC Detector is operated without the 733 IC Separation Center. All parameters which affect the 733 IC Separation Center are suppressed in the dialog.
4 Operation 4.4.2 Configuration, key CONFIG 7 The key is used for the entry of basic settings of general applicability which are also retained when the instrument is switched off. The key opens the following main menu: CONFIG >CONFIG/detector Settings for the conductivity detector CONFIG >CONFIG/printer Settings for external printer CONFIG >CONFIG/print meas.
4.4 Basic settings When the heating is switched on, the green display lamp 7 "THERMOSTAT" is on. Thermostatting of the conductivity detector is switched off by pressing the key. The display shows the value "off °C", at the same time the green display lamp 7 goes out. Thermostatting functions only if the ambient temperature is at least 5 °C lower than the operating temperature.
4 Operation >CONFIG/printer id.2 18 ASCII characters >CONFIG/printer print header: once once, always, off >CONFIG/printer date&time: on on, off >CONFIG/printer send to: IBM IBM, Epson, Seiko, Citizen, HP Identification 2 for 2nd line of print header Freely selectable ASCII character string for the second line of the print header (text entry, see section 4.2.5).
4.4 Basic settings >CONFIG/print meas.value time interval 1.0 s Time interval for measured value printout 0.4…99999 s Time interval in seconds between printout of the individual measured values. >CONFIG/print meas.value stop time off min 1…999 min, off This inquiry appears only with "print crit. = time". Stop time for measured value printout This inquiry appears only with "print crit. = time". Time to stop of the measured value printout. off >CONFIG/print meas.
4 Operation Settings for events >CONFIG/auxiliaries >CONFIG/aux/event Submenu >CONFIG/aux/event enabled in program: off on, off >CONFIG/auxiliaries date YY-MM-DD YYYY: 1995…2094; MM: 01…12; DD: 01…31 >CONFIG/auxiliaries time HH:MM:SS HH: 00…23 MM: 00…59 SS: 00…59 >CONFIG/auxiliaries dialog: english english, deutsch, français, español >CONFIG/auxiliaries device label 8 ASCII characters >CONFIG/auxiliaries program 732.
4.4 Basic settings >CONFIG/aux/beep repeat time 60 s 5…999 s, off Repeat time for beep This inquiry appears only with "status = on". The three beeps with error messages are repeated each time the inputted time has elapsed until the error message is confirmed with . off No repeat (press ). Settings for RS232 interface For further details on the RS232 interface, see section 6.1.
4 Operation >CONFIG >CONFIG/RS settings 709 Settings for RS interface "709 IC Pump" This RS232 interface is normally used for connection of the 709 IC Pump. However, it can also be used to attach an external printer if the instrument is appropriately configured in the Setup program ("operation with 709 = off", see section 4.4.1). For detailed information on the RS232 interface, see section 6.1.
4.4 Basic settings >CONFIG >CONFIG/733 IC Sep.Cent. Settings for 733 IC Separation Center This submenu appears only with "operation with 733 = on". >CONFIG/733 IC Sep.Cent. valve A display only Configuration 733 IC Separation Center Depending on the instrument configuration, the following messages appear: valve A valve A + valve B valve A + suppressor 733 not accessible >CONFIG/733 IC Sep.Cent. control: no restriction no restriction, 732 only >CONFIG/733 IC Sep.Cent. >CONFIG/733/valve A 733.
4 Operation >CONFIG/733 IC Sep.Cent. >CONFIG/733/valve B submenu Settings for injection valve B This submenu appears only with the 733.0020 IC Separation Center with 2 injection valves. >CONFIG/733/valve B status fill display only >CONFIG/733/valve B trigger: fill inject, fill >CONFIG/733 IC Sep.Cent. >CONFIG/733/suppressor submenu Switching of the valve After confirmation with , the valve is moved to the selected position: fill Filling of sample loop. inject Injection of loop contents.
4.5 Measurement parameters 4.5 Measurement parameters 4.5.1 key PARAM The key combines the most important parameter settings for the 732 IC Detector. The parameter values entered here are available for the measurement immediately following their confirmation. They can be stored and recalled together with the current existing program as a method.
4 Operation >PARAM/detector full scale: 1.00 mS/cm 0.05 µS/cm…10 mS/cm Full-scale range (operating range) The full-scale range (operating range) sets the desired sensitivity for the display and analog output of the measuring signal during the recording of a chromatogram. The following points should be noted: • The possible values of the full-scale range which can be selected with the
4.5 Measurement parameters >PARAM/detector temp.coeff.: 2.5 %/°C 1.5, 2.5 %/°C Temperature coefficient The temperature coefficient is used to take into account the temperature dependence of the conductivity measurement. Two values can be selected: 1.5 %/°C Temperature coefficient for cations 2.5 %/°C Temperature coefficient for anions When the thermostatting of the measuring cell is switched on (thermostat display 7 lit up), the conductivity κT measured at the set operating temperature (25...
4 Operation Settings for graphics plot These settings are effective with the graphics plot on an external printer triggered using the key (see section 4.8.2). >PARAM >PARAM/plot >PARAM/plot auto start: off on, off >PARAM/plot time interval 1.0 s 0.4…99999 s >PARAM/plot time scale 10.0 mm/min 0.1, 0.2, 0.5, 1, 2, 5, 10, 20, 60, 120 mm/min >PARAM/plot time scale label: rel rel, abs >PARAM/plot stop time off min 1…999 min, off >PARAM/plot left: 0.
4.5 Measurement parameters Settings for 709 IC Pump >PARAM >PARAM/709 IC Pump This submenu appears only with "SETUP/peripherals/operation with 709 = on". These settings are effective only if the 709 IC Pump is connected to the 732 IC Detector and the remote control is activated with the key (see section 2.6.1). >PARAM/709 IC Pump flow 0.50 mL/min Flow rate Flow rate of the 709 IC Pump. 0.01…5.00 mL/min >PARAM/709 IC Pump Pmax 10.0 MPa 0.1…50 MPa >PARAM/709 IC Pump Pmin 0.0 MPa 0.
4 Operation of the 732 IC Detector shows the message "stopped: YY-MM-DD HH:MM" with details of the time when the pump was stopped. The LED "Pmin" on the 709 IC Pump flashes, the shutoff pressure can be requested under "Pactual". A 709 IC Pump stopped in this manner is put back into operation as follows: • Press key to switch off remote operation. • Press key to remove the block. The LED "Pmin" no longer flashes. • Press key to switch the remote operation back on.
4.6 Triggering of functions 4.6 Triggering of functions 4.6.1 keys The two keys at the 733 IC Separation Center each have the following function, which depends on the instrument version: FILL 733.0010 (1 valve) 733.0X20 (2 valves) 733.0X30 (valve+ suppr.
4 Operation 4.6.2 keys The two keys at the 733 IC Separation Center have the following function, depending on the instrument version: INJECT 733.0010 (1 valve) 733.0X20 (2 valves) 733.0X30 (valve+ suppr.
4.6 Triggering of functions 4.6.3 key ZERO The key is used to trigger the auto-zero function. "Auto-zero" is the name used for the automatic electronic background compensation, i.e. the current measured conductivity value is set to zero and hence lies in the middle of the selected full-scale range. The diagram below shows the operating principle of the auto-zero function.
4 Operation 4.6.4 key ZERO OFF 4 The key is used to switch off the auto-zero function. The auto-zero function can be triggered using the key in the standby mode or when a program is running, but not in the edit mode. When the green LED 6 in the key goes out, this shows that the electronic background compensation is no longer active. 4.6.5 key MARK 0 The key is used to trigger a marking signal. In addition to the measuring signal, a signal of ca.
4.7 Programming 4.7 Programming 4.7.1 key PROGRAM 6 The key can be used to develop and edit time programs which can comprise maximum 20 program steps each with up to 14 individual program points. This allows the chronological sequence of actions at the 732 IC Detector and 733 IC Separation Center to be automated virtually at will. The program loaded in the working memory can be stored together with the parameter values currently under the key as a method and recalled.
4 Operation â Program steps 1…k â return â Program steps m…n â end >PROGRAM/parameters number of cycles 1 1…999 No. of cycles remote Single program with start via remote A remote program is started externally via a remote input line (see section 6.2.1) and executed once only. inject Single program with start via "INJECT" An inject program is started each time injection valve A is switched to the "INJECT" position and executed once only.
4.7 Programming test Program test The test status is used to test a program. After the program status has been set to "test" and return to the standby mode, a switch is automatically made to the test mode, which runs as follows: • The bottom line of display shows the message "test step" with details of the time "X.XXX min" when the first program step should be executed. • Pressing the key executes the actions associated with the program step.
4 Operation program step can be edited. Change time for existing program steps For a program step selected with
4.7 Programming >PROGRAM/edit. XXX.X min range: 100 µS/cm 100, 200, 500 µS/cm 1, 2, 5, 10 mS/cm Reset measuring range This inquiry appears only with "FS change = on". The measuring range is set to the inputted value (for further details of the parameter "range", see section 4.5.1). If the measuring range just entered differs from the measuring range valid at the start of the program, an auto-zero function that is switched on will be switched off.
4 Operation >PROGRAM/edit. XXX.X min valve B: -----, fill, inject >PROGRAM/edit. XXX.X min suppressor: -----, step Switch injection valve B This inquiry appears only with "SETUP/peripherals/operation with 733 = on" and with the 733.0020 IC Separation Center with two injection valves. fill Switching of injection valve B to "FILL" position (equivalent to the key, see section 4.6.1). inject Switching of injection valve B to "INJECT" position (equivalent to the key, see section 4.6.2).
4.7 Programming >PROGRAM/edit. XXX.X min Pmax: --- MPa ---, 0.1…50 MPa Reset maximum shutoff pressure This inquiry appears only with "SETUP/peripherals/operation with 709 = on". The maximum shutoff pressure for automatic shutoff of the 709 IC Pump is set to the inputted value (for further details of the parameter "Pmax", see section 4.5.1). >PROGRAM/edit. XXX.X min Pmin: --- MPa ---, 0.0…50 MPa Reset minimum shutoff pressure This inquiry appears only with "SETUP/peripherals/operation with 709 = on".
4 Operation 4.7.2 key PROG R/S The key is used to start or stop the program loaded in the working memory. The status of the LED in the key indicates what it can trigger: LED off Program disabled No action is triggered with the key. A loop program can not be started until the parameter "PROGRAM/parameters/status = enabled" has been set. LED lit up Program enabled The key is used to start a loop program. The current time is automatically set to "0.0 min".
4.7 Programming Enter new event >EVENT >EVENT/new >EVENT/new format: date date, daily Event format date The event is triggered once at a particular time. daily >EVENT/new event:YY-MM-DD HH:MM:SS YY: 00…99 HH: 00…23 MM: 01…12 MM: 00…59 DD: 01…31 SS: 00…59 >EVENT/new event: HH:MM:SS HH: 00…23 MM: 00…59 The event is triggered daily at a particular time. Date and time for a new event This inquiry appears only with "format = date".
4 Operation Edit existing event >EVENT >EVENT/edit >EVENT/edit event:YY-MM-DD HH:MM:SS Select existing event Selection of the event with the
4.7 Programming 4.7.4 key METHOD 9 The key is used for the management of maximum 9 userdefined methods, which can be stored and recalled under freely selectable names. A method comprises the measurement parameters defined under the key and the program defined under the key.
4 Operation Store method >METHOD >METHOD/store >METHOD/store name: XXXXXXXX 8 ASCII characters Enter or select method name Entry of a new name (text entry, see section 4.2.5) under which the method should be stored or selection of an existing method name with the
4.8 Data output 4.8 Data output 4.8.1 key PRINT 3 The key is used for the output of single measured values or to start the automatic measured value output on an external printer or PC connected to the RS232 interface. The output is triggered directly at a keystroke, no inquiries appear. Preparations • For the output on an external printer, printer type and RS232 settings must be correctly selected under (see section 4.4.2).
4 Operation • Identification "ZEROREF" Reference value for the auto-zero function (measured value which is compensated). • Identification "OVERLOAD" The measured value is 50…80% outside the selected full-scale range. • Identification "BACKGROUND" The measured value is more than 80% outside the selected full-scale range. The absolute conductivity (background) is outputted in place of the auto-zero value.
4.8 Data output Automatic measured value output • For the automatic measured value output of measured values at selectable time intervals, ">CONFIG/print meas.value/print crit. = time" must be selected (see section 4.4.2). When the key is pressed, the measured value output defined by the parameters "time interval" and "stop time" is started via the RS232 interval. The measured value output can always be aborted with .
4 Operation 4.8.2 key PLOT 1 The key is used to start the graphics plot on an external printer connected to the RS232 interface. The output is started directly at a keystroke, no inquiries appear. Preparations • Under "SETUP" the general graphics parameters (frame, grid, print width) must be set to the desired values (see section 4.4.1). • Under printer type and RS232 settings for the output on an external printer must be correctly selected (see section 4.4.2).
4.8 Data output Example • Graphics plot of a chromatogram with the PRP-X100 IC Anion column on a Citizen printer IDP562 RS >SETUP/graphics grid: frame: width off off 1.0 >CONFIG/printer id.1 column PRP-X100 id.2 standard print header: always date&time: on send to: Citizen >PARAM/printer auto start: on time interval 1.0 s time scale 10.0 mm/min time scale label: rel stop time 10 min left: -0.200 µS/cm right: 1.800 µS/cm 732 IC Detector 01104 id.1 column PRP-X100 id.
4 Operation 4.8.3 key REPORT 2 XXXXXX µS/cm report: The key is used for the output of reports on an external printer or PC connected to the RS232 interface.
4.8 Data output Example of "event" report Example of "param" report Two daily events (adjust pump flow) and a date event (switch off pump supply) Measurement parameters for drinking water determination with PRP-X100 IC Anion Column EVENT daily: 07:00:00 2.00 mL/min 19:00:00 pump flow 0.
4 Operation 4.9 Examples of methods 4.9.1 Cation determination with Metrosep Cation 1-2 This example shows a method for the determination of monovalent and divalent cations with the 6.1010.000 IC Cation Column Metrosep Cation 1-2, which can be used with or without an autosampler. General conditions • Separating column: • Sample loop: • Eluent: • Flow: • Eluent conductivity: • Full scale: 6.1010.000 Metrosep Cation 1-2 10 µL 4 mmol/L tartaric acid, 1 mmol/L dipicolinic acid 1 mL/min ca.
4.9 Examples of methods Method METHOD method name date: 1995-10-16 Cat.1-2 10:57:42 PARAM >PARAM/detector range: 1.00 mS/cm full scale: 5.00 µS/cm temp.coeff.: 1.5 >PARAM/analog output polarity: offset: 0 damping: off >PARAM/plot auto start: off time interval 1.0 time scale 10.0 time scale label: rel stop time off left: 1.000 right: -4.000 >PARAM/709 IC Pump flow 1.00 Pmax 10.0 Pmin 1.0 flow corr. 1.00 PROGRAM progr.type: 11.9 zero: 12.
4 Operation Chromatogram for cation standard Na+ Li+ NH4+ Mg2+ Ca2+ K+ FULL REPORT Ret Time (Min) -------2.682 3.252 3.624 4.566 6.937 9.982 Component Name --------------Li Na NH4 K Ca Mg Concentr. ppm ----------1.000000 5.000000 5.000000 10.000000 10.000000 10.000000 Area (uV*Sec) ---------3100993.50 4215109.00 4517200.50 4022451.00 6971803.50 15063622.0 Height (uV) ---------537565.125 627987.062 508054.437 313609.843 396256.875 501869.562 Fig.
4.9 Examples of methods 4.9.2 Anion determination with Metrosep Anion Dual 2 This example shows a method for the determination of monovalent and divalent anions with the 6.1006.100 IC Anion Column Metrosep Anion Dual 2 and the Metrohm suppressor module, which can be used with or without an autosampler. General conditions • Separating column: • Sample loop: • Eluent: • • • • Flow: Eluent conductivity: Full scale: Suppressor module: Configuration 6.1006.100 Metrosep Anion Dual 2 20 µL 1.
4 Operation Method METHOD method name date: 1995-10-16 An.Dual 14:30:39 PARAM >PARAM/detector range: 100 µS/cm full scale: 50.00 µS/cm temp.coeff.: 2.5 %/°C >PARAM/analog output polarity: + offset: 0 %fs damping: off >PARAM/Plot auto start: off time interval 1.0 s time scale 10.0 mm/min time scale label: rel stop time off min left: -5.000 µS/cm right: 45.00 µS/cm >PARAM/709 IC Pump flow 0.80 mL/min Pmax 7.0 MPa Pmin 1.0 MPa flow corr. 1.00 PROGRAM progr.type: cycle number of cycles 1 9.
4.9 Examples of methods Settings for 709 IC Pump • Installation: • key: as shown in Fig. 10 (see section 2.6) Switched on (remote operation activated) Settings for 752 Pump Unit • Installation: as described in section 2.8.6 Chromatogram for anion standard Cl– Full Scale 5 µS/cm NO3– SO42– HPO42– FULL REPORT Ret Time (Min) -------4.918 11.505 13.399 16.617 Component Name --------------Chloride Nitrate Phosphate Sulphate Concentr. ppm ----------19.661419 2.010445 1.973833 19.
4 Operation 132 732 IC Detector / 733 IC Separation Center
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 732/733 IC system 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 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. Regeneration If the separation properties of the column have deteriorated, it can be regenerated in accordance with the column manufacturer’s specifications. With the separating columns available from Metrohm (see section 7.3.
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 high sensitive measurements, the eluent should be continuously stirred with a magnetic stirrer, particularly when the recycling procedure is employed or when alkaline eluents are used.
5 Notes – Maintenance – Faults 5.1.4 Suppressor module To avoid contamination of the suppressor module by foreign particles or bacterial growth, it is advantageous to install an in-line filter between the 752 Pump Unit and the suppressor module. The two 6.2821.100 Filter units PEEK (see section 2.6.3 and section 2.8.3) supplied with the 2.733.0X30 IC Separation Center are eminently suitable for this purpose. 5.1.
5.2 Maintenance and servicing corrosive chemicals, it may be necessary to shorten the interval between servicing. The Metrohm service department is always willing to offer expert advice on the maintenance and servicing of all Metrohm instruments. 5.2.2 Passivation Passivation of the entire IC system (without column) by rinsing with 20...50 mL 0.2 mol/L HNO3 is appropriate in the following cases: • in the installation (only with non metal-free IC systems, see section 2.6.
5 Notes – Maintenance – Faults 5.2.5 Changing separating columns Identical separation system If you wish to replace an IC separating column by a column of the same type, proceed as follows (see Fig. 16 and Fig. 17): 1 Remove old column • Switch off pump drive of the 709 IC Pump. • Unscrew column from inlet capillary 82 of the detector block or from suppressor inlet capillary 89. 89 • Unscrew column from column connection capillary 67 or the precolumn.
5.2 Maintenance and servicing 4 Rinse with dist. H2O • Rinse IC system with dist. Or demin. Water (flow rate 1 mL/min) for ca. 10 min. 5 Rinse with eluent • Rinse IC system with the eluent needed for the separating column you intend to install until the absolute conductivity displayed on the 732 IC Detector is stable. 6 Remove coupling • Remove 6.2620.060 Coupling between column outlet capillary 67 and inlet capillary 82 (see Fig. 16).
5 Notes – Maintenance – Faults 5.2.6 Regeneration of the suppressor 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 2 Regenerate suppressor • Connect the inlet capillary 90 marked "H2SO4" to the 709 IC Pump using the 6.2620.060 or 6.2744.040 coupling. • Set the flow at the 709 IC 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 709 IC Pump to 2 mL/min. Do not exceed a maximum pressure of 2 MPa (20 bar). • Switch suppressor to the next position using the key.
5 Notes – Maintenance – Faults 3 Clean input and output leads • Connect each of the 6 capillary tubings attached to connection piece 98 to the pump one after another, and pump through ultrapure water. • Check whether solution emerges from connection piece 98. 98 If one of the input or output leads remains blocked, replace the connection piece (order number 6.2832.010). 4 Clean suppressor rotor • Clean the sealing surface of suppressor rotor 99 using a lintfree cloth and ethanol.
5.2 Maintenance and servicing 5.2.8 7 Insert connection piece • Insert connection piece 98 in suppressor holder 100 in such a way that connection "1" is at the top, and that the three lugs on the connection piece fit in the corresponding openings of the holder. • Screw nut 97 onto the thread of suppressor holder 100 manually (do not use tools). 8 Connect and condition the suppressor • Reconnect the suppressor to the IC system.
5 Notes – Maintenance – Faults • If the rotor has been inserted correctly, its sealing surface will be about 4 mm inside the holder. If this is not the case, bring the rotor into the correct position from below with the aid of a sharp object (e.g. a screwdriver). 144 5 Clean connection piece • Clean the sealing surface of new connection piece 98 (6.2832.010) with the aid of a lint-free cloth and ethanol.
5.3 Faults and malfunctions 5.3 Faults and malfunctions 5.3.1 Error messages If any type of malfunction occurs during operation of the 732 IC Detector, this is shown by an error message which appear in the top line of display 1 and (if switched on under ) by three beeps. To return to the instrument standby mode, the error messages must be confirmed with the key.
5 Notes – Maintenance – Faults 146 Error message Meaning/Causes Rectification Err5 RS232 interface at 732 IC Detector faulty. Inform Metrohm service. Err6 Clock faulty. Inform Metrohm service. Err7 LCD write/read error. Inform Metrohm service. Err8 AD converter faulty. Inform Metrohm service. ErrC RS232 interface at 709 IC Pump faulty. Inform Metrohm service. faulty method # Method # (0…9) can no longer be recalled. Re-enter method and store.
5.3 Faults and malfunctions Error message Meaning/Causes Rectification range error # Error in internal hardware test. Inform Metrohm service. RS error 36 RS receive error; wrong parity. , set same parity for both devices. RS error 37 RS receive error; wrong stop bit. , set same stop bit for both devices. RS error 38 RS-receive error; overflow (at least 1 character could not be read). , set same baud rate for both devices, restart sender.
5 Notes – Maintenance – Faults 5.3.2 Malfunctions and their rectification If difficulties appear with the IC system during analyses, their causes are best investigated in the order separating column → pump → eluent → 732/733 IC System. Several of the malfunctions which may appear are listed in the following table with details of possible causes and countermeasures. Malfunction Cause Rectification Baseline with high noise level, pulsation • Contaminated pump values • Clean the valves (see section 5.1.
5.4 Diagnostic tests 5.4 Diagnostic tests 5.4.1 General The 732 IC Detector and 733 IC Separation Center are very precise and dependable instruments. Thanks to their rugged construction, it is highly unlikely that external mechanical or electrical influences will have any adverse effect on their functions.
5 Notes – Maintenance – Faults 5.4.2 Prepare instruments • Power off. • Disconnect all external connections at the 732 IC Detector (except mains cable). • Power on and immediately press and hold <9> key until initialisation EEPROM? ENTER>yes '9'>diagnosis • Press <9> key to open the following diagnostic menu: diagnosis >diag/EEPROM initial.
5.4 Diagnostic tests 5.4.3 Checking working memory (RAM) This diagnostic step executes a non-destructive test over the entire area of the RAM content (working memory). • Prepare instrument for diagnostic test (see section 5.4.2). • If need be, press <9> key repeatedly until diagnosis >diag/RAM test • If no faults are found, the display shows: >diag/RAM test RAM test ok • diagnosis >diag/keyboard test 5.4.
5 Notes – Maintenance – Faults Key table Code Key Code 0 <9 / METHOD> 12 1 <8 / PUMP R/S> 13
5.4 Diagnostic tests 5.4.6 Check RS232 interfaces With this diagnostic step all outputs and inputs of the two RS232 interfaces 16 "RS 232" and 15 "709 IC Pump" can be checked for functionality. • Prepare instrument for diagnostic test (see section 5.4.2). • If need be, press <9> key repeatedly until diagnosis >diag/RS test • >diag/RS test >diag/RS test/RS232 • >diag/RS test/RS232 RS connector? • Without switching off the instrument, plug the 3.496.8480 Test plug into socket "RS232".
5 Notes – Maintenance – Faults 5.4.7 Check remote interfaces This diagnostic step can be used to check all outputs and inputs of the two remote interfaces 17 "Remote" and 14 "733 IC Separation Center" for functionality. • Prepare instrument for diagnostic test (see section 5.4.2). • If need be, press <9> key repeatedly until diagnosis >diag/IO test • >diag/IO test >diag/IO test/remote • >diag/IO test/remote IO connector? • Without switching off the instrument, plug the 3.496.
5.4 Diagnostic tests 5.4.8 Internal hardware test This diagnostic step can be used to check the hardware for measured value acquisition in the 732 IC Detector for functionality. The test is divided into separate tests performed in succession. All these tests are carried out with the possibilities included in the IC Detector and are thus not dependent on working aids such as test plugs or test adapters.
5 Notes – Maintenance – Faults range test ok • >diag/internal test >diag/int/sensitivity Check sense With this diagnostic step the sense amplifier is checked for functionality. • The test runs automatically and lasts ca. 2 min. During this time various measurement results appear in the display, but these should be ignored. If the test discovers results which lie outside the specified tolerance zones, the number of deviations found appears following completion of the test.
5.4 Diagnostic tests • The test runs automatically and lasts ca. 3 min. During this time various measurement results appear in the display, but these should be ignored. If the test discovers results which lie outside the specified tolerance zones, the number of deviations found appears following completion of the test. If all results of the test are within the specified tolerance zones, the following appears: err: 0 DAC fine test ok • >diagnosis >diag/external test 5.4.
5 Notes – Maintenance – Faults • Press key to open the following diagnostic menu: >diag/EEPROM initial. block: USER ü ü ü ü ü ü >diag/EEPROM initial. block: CONFIG ü >diag/EEPROM initial. block: INFO ü >diag/EEPROM initial. block: SETUP ü >diag/EEPROM initial. block: ASSEMBLY ü >diag/EEPROM initial. block: EVENT ü >diag/EEPROM initial. block: METHOD >diag/EEPROM initial. block: ALL Set config parameters with default values.
5.5 Validation / GLP 5.5 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. The 732 IC Detector and 733 IC Separation Center as part of the complete ion chromatography system, whose most important components also include separating column, pump and evaluation system, must be incorporated in its comprehensive validation.
5 Notes – Maintenance – Faults 160 732 IC Detector / 733 IC Separation Center
6.1 RS232 interfaces 6 Interfaces 6.1 RS232 interfaces The 732 IC Detector has two RS232 interfaces 15 and 16 (see Fig. 3) which have the same features (see section 6.1.7 – 6.1.9), but can be used differently. RS232 interface 16 is reserved for the connection of a PC or a printer (see section 2.9.4 – 2.9.5) and allows remote operation of the 732 IC Detector 732 and 733 Separation Center 733 by an attached PC (see section 6.1.1 – 6.1.6).
6 Interfaces &Config.Aux.Dialog Once you are at the desired location in the tree, you can request the value of the object: Q for query &Config.Aux.Dialog $Q The inquiry ‘$Q’ initiates the output of the value on the instrument, in other words the value output is triggered. Entries which begin with the character ‘$’ always trigger something and are hence referred to as triggers in what follows. However, values of objects can not only be requested, they can also be modified.
6.1 RS232 interfaces 6.1.3 Rules Example Until a new object is called up, the old object remains in force. Entry of a different dialog language: "deutsch" New objects can be addressed relative to the old object: From the root to the node 'Aux': &C.A A leading point leads one node forwards in the tree. Forwards from the node 'Aux' to 'Prog': .P More than one leading point leads one node backwards in the tree. n nodes backwards require n+1 leading points.
6 Interfaces 6.1.4 Status messages To ensure appropriate control of an external control unit is possible, it must also be possible to request status conditions which provide information on the status of the 732 IC Detector. The output of a status message is triggered by the trigger '$D'. Status messages comprise the global status '$R' and the detailed status messages listed below, which can also appear in combination, e.g. '$R.Cond.ProgWait'.
6.1 RS232 interfaces 6.1.5 Error messages Error messages ‘EXXX’ are appended to the status message and separated from this by a ‘;’. Error Meaning Exit/Corrective action E28 Wrong object call-up. Correct path. E29 Wrong value. Enter correct value or new path. E30 Wrong trigger. Enter correct trigger or new path. E36 RS232 receive error; parity. , set same parity for both devices. E37 RS232 receive error; stop bit. , set same stop bit for both devices.
6 Interfaces 6.1.
6.1 RS232 interfaces Object Meaning Ã.Aux ³ Ã.RunNo ³ ³ ³ Ã.Cycles ³ Ã.CEvent ³ ³ À.CEenable ³ Ã.Set ³ ³ Ã.Date ³ ³ À.Time ³ Ã.Dialog ³ ³ ³ Ã.DevLabel ³ Ã.Prog ³ À.Beeper ³ Ã.Status ³ À.Repeat ³ Ã.RSset ³ Ã.Baud ³ ³ ³ Ã.DataBit ³ Ã.StopBit ³ Ã.Parity ³ À.Handsh ³ ³ Ã.RSSet709 ³ Ã.Status ³ Ã.709 ³ ³ À.Baud ³ ³ ³ À.Printer ³ Ã.Baud ³ ³ ³ Ã.DataBit ³ Ã.StopBit ³ Ã.Parity ³ À.Handsh ³ ³ À.SepCenter Ã.Config Ã.Control Ã.AValve ³ Ã.StatusA ³ À.TriggerA Ã.BValve ³ Ã.StatusB ³ À.TriggerB À.Suppressor Ã.
6 Interfaces Object Meaning &Methods Methods ³ Ã.FreeMemory ³ Ã.Recall ³ À.Name ³ Ã.Store ³ À.Name ³ Ã.Delete ³ À.Name ³ À.AllDelete &Parameter ³ Ã.Detector ³ Ã.Range ³ ³ ³ Ã.FullScale ³ À.TempCoeff ³ Ã.AnalogOut ³ Ã.Polarity ³ Ã.Offset ³ À.Damping ³ Ã.PlotPara ³ Ã.Autostart ³ Ã.Interval ³ Ã.TimeScale ³ ³ ³ Ã.TLabel ³ Ã.StopTime ³ Ã.Left ³ ³ ³ ³ ³ À.Right ³ ³ ³ À.Pump709 Ã.Flow Ã.Pmax Ã.Pmin À.
6.1 RS232 interfaces Object Meaning Ã.Parameter ³ Ã.Type ³ Ã.Cycle ³ ³ À.No ³ À.Status ³ Ã.Edit ³ À.Select ³ Ã.1 ³ ³ Ã.Time ³ ³ À.Action ³ ³ Ã.Flag ³ ³ Ã.FSChange ³ ³ Ã.Range ³ ³ ³ ³ ³ Ã.FullScale ³ ³ ³ ³ ³ Ã.Zero ³ ³ Ã.Polarity ³ ³ Ã.Mark ³ ³ Ã.ValveA ³ ³ Ã.ValveB ³ ³ Ã.Suppressor ³ ³ Ã.Remote ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.PumpRS ³ ³ Ã.Flow ³ ³ Ã.Pmax ³ ³ À.Pmin ³ : ³ À.20 ³ Ã.Time ³ À.Action ³ : ³ À.
6 Interfaces Object Meaning Entry range/Selection ³ Ã.Mark ³ Ã.AValve ³ Ã.BValve ³ Ã.Suppressor ³ Ã.Remote ³ ³ ³ ³ ³ ³ ³ Ã.ProgRS ³ Ã.PumpRS ³ Ã.Flow ³ Ã.Pmax ³ À.Pmin : À.4 Ã.Date À.Action : Trigger marking signal Switch injection valve A Switch injection valve B Advance suppressor module ---, on ---, fill, inject ---, fill, inject ---, step V, 0, 1 &Zero À.RefValue Start/stop of the auto-zero function Auto-zero ref.
6.1 RS232 interfaces Object ³ Ã.Change ³ ³ ³ ³ ³ ³ ³ À.Clear ³ ³ ³ Ã.Outputs ³ Ã.State ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.Change ³ ³ ³ ³ ³ ³ ³ À.Clear ³ Ã.MeasValue ³ Ã.Conductivity ³ Ã.Background ³ À.RunTime ³ Ã.Pump709 ³ Ã.State ³ Ã.Pactual ³ À.Error ³ ³ Ã.Method ³ Ã.Name ³ Ã.Status ³ À.Index ³ À.Display Ã.Select ³ ³ Ã.L1 Ã.L2 À.
6 Interfaces Object Meaning &Setup Operating mode ³ Ã.IdReport ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.Keycode ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.Tree ³ Ã.Short ³ ³ ³ ³ ³ À.ChangedOnly ³ ³ Ã.Trace ³ ³ ³ ³ Ã.Lock ³ Ã.Keyboard ³ Ã.Config ³ Ã.Event ³ Ã.FullScale ³ Ã.Mark ³ Ã.Method ³ Ã.Param ³ Ã.Plot ³ Ã.Print ³ Ã.ProgRS ³ Ã.Program ³ Ã.PumpRS ³ Ã.Report ³ Ã.Select ³ Ã.Zero ³ Ã.
6.1 RS232 interfaces Object Meaning ³ Ã.Methods ³ ³ Ã.Recall ³ ³ Ã.Store ³ ³ À.Delete ³ Ã.Display ³ ³ ³ À.Remote ³ Ã.AutoInfo ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.Message ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ À.DateTime ³ Ã.Error ³ Ã.Ready ³ ³ ³ Ã.Stopped ³ Ã.Wait ³ Ã.PowerOn ³ Ã.Inputs ³ À.Outputs ³ Ã.Save ³ ³ ³ ³ ³ Ã.InstrNo ³ À.Value ³ À.Interface Ã.OutputAssign ³ À.RemOut ³ ³ Ã.InputAssign ³ ³ ³ ³ ³ Ã.ProgRS ³ Ã.PumpRS ³ Ã.FillA ³ Ã.InjectA ³ Ã.FillB ³ Ã.InjectB ³ Ã.Report ³ Ã.
6 Interfaces Object ³ Ã.Mark ³ Ã.Zerooff ³ Ã.Plot ³ Ã.Polarity ³ Ã.Select ³ Ã.Quit ³ À.Enter Ã.Graphics ³ Ã.Grid ³ Ã.Frame ³ À.Recorder ³ À.Width À.Peripherals Ã.With733 À.With709 &Assembly ³ Ã.Meas ³ À.State ³ À.Outputs Ã.SmplX ³ Ã.AutoEOD ³ Ã.SetLines ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.L1 ³ Ã.L2 ³ Ã.L3 ³ Ã.L4 ³ Ã.L5 ³ Ã.L6 ³ Ã.L7 ³ Ã.L8 ³ Ã.L9 ³ Ã.L10 ³ Ã.L11 ³ Ã.L12 ³ Ã.L13 ³ Ã.L14 ³ Ã.L15 ³ À.L16 À.
6.1 RS232 interfaces Object Meaning &Diagnosis Diagnostic tests ³ ³ Ã.EEPROMInit ³ À.BlockSelect ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.RunMode ³ Ã.Report ³ À.Stop ³ Ã.RAMTest ³ Ã.KeyTest ³ Ã.DisplayTest ³ Ã.RSTest ³ ³ ³ ³ ³ Ã.RS232 ³ À.ICPump ³ Ã.IOTest ³ ³ ³ ³ ³ Ã.Remote ³ À.SepCent ³ Ã.IntTest ³ Ã.UcellTest ³ Ã.RangeTest ³ Ã.SenseTest ³ Ã.DACCoarse ³ À.DACFine ³ Ã.ExtTest ³ Ã.LowpassTest ³ Ã.OffsetTest ³ Ã.PolarTest ³ Ã.TCoeffTest ³ Ã.FreqTest ³ À.
6 Interfaces 176 Object Meaning Ã.SimulateKey ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ ³ Ã.Adjust ³ ³ Ã.InstrNo ³ ³ ³ À.PowerOn Simulate keystroke 0 9 (METHOD) 1 8 (PUMP R/S) 2 7 (CONFIG) 3 ZERO 4 PARAM 6 6 (PROGRAM) 7 5 (EVENT) 8 4 (ZERO OFF) 9 PROG R/S 10 FULL SCALE Entry range/Selection 0…22 12 13 14 15 16 18 19 20 21 22 CLEAR SELECT 3 (PRINT) 2 (REPORT) 1 (PLOT) ENTER QUIT –/+ (→) . (←) 0 (MARK) Instrument adjustment (security code necessary) $G Serial number (accessible by remote control only under &Setup.
6.1 RS232 interfaces 6.1.7 Data transmission protocol The two RS232 interfaces of the 732 IC Detectors are configured as DTE (Data Terminal Equipment) with the following technical specifications: • Standard Data interface in accordance with EIA standard RS 232C (DIN 66020, page 1), transmission parameters can be set under ">CONFIG/RS settings", see section 4.4.2. • Control characters CR LF XON XOFF • Max.
6 Interfaces 6.1.8 Handshake No handshake (none) The 732 IC Detector neither checks handshake inputs (CTS, DSR, DCD) nor sets handshake outputs (DTR, RTS). Reduced hardware handshake (HWs) 732 IC Detector as receiver: 732 External device RTS RTS DTR DTR LF RxD RxD Time IC Detector 732 as sender: 732 External device DTR DTR RTS RTS CTS CTS LF TxD TxD Time The data flow can be interrupted by deactivating the CTS line.
6.1 RS232 interfaces 732 IC Detector as sender: 732 External device DTR DTR RTS RTS DSR DSR DCD DCD CTS CTS LF TxD TxD Time The data flow can be interrupted by deactivation of the CTS line. Software handshake with character stop (SWchar) Handshake inputs (CTS, DSR, DCD) are not checked at the 732 IC Detector, handshake outputs (DTR, RTS) are set. As soon as an LF is recognized, the 732 IC Detector sends XOFF. After this time, it can still receive 6 characters and store them temporarily.
6 Interfaces 732 IC Detector as sender: 732 External device XOFF XON Data output RxD LF TxD max. 4 char. Data output blocked Data input Data output free Time Software handshake with line stop (SWline) Handshake inputs (CTS, DSR, DCD) are not checked at the 732 IC Detector, handshake outputs (DTR, RTS) are set. The 732 IC Detector has an input buffer which can accept a string of up to 80 characters + CR LF. As soon as an LF is recognized, the 732 IC Detector sends XOFF.
6.1 RS232 interfaces 6.1.9 Pin assignment RS232C interface external Transmitted Data (TxD) If no data transmission takes place, the line is maintained in the ”ON” condition. Data are sent only when CTS and DSR are in the ”ON” condition and DCD is in the ”OFF” condition. Pin 2 Transmitted Data Received Data (RxD) Data are received only when DCD is ”ON”. Pin 3 Received Data Request to Send (RTS) ON condition: 732 IC Detector is ready to send data.
6 Interfaces 6.1.10 RS232 error rectification Problem Questions for corrective action No characters can be received on an attached printer. ⇒ Are the devices switched on and the connecting cables plugged in properly? ⇒ Is the printer set to ”on-line”? ⇒ Do the baud rate, data bits and parity for the two devices have the same setting? ⇒ Is the handshake set properly? If everything appears ok, try to print out a report by pressing the key.
6.2 Remote interfaces 6.2 Remote interfaces The 732 IC Detector has the two remote interfaces 14 "733 IC Separation Center" and 17 "Remote" (see Fig. 3) which each have 8 input and 8 output lines. 6.2.1 "Remote" interface The remote interface 17 "Remote" is used for the connection of any type of external device (see section 2.9.8) and has the following pin assignment: 732 IC Detector Pin Function Inputs +5V Triggering the print command Equivalent to pressing the key (see section 4.8.1).
6 Interfaces 732 IC Detector Pin Function Outputs 5 Ready L = ready (program inactive or not started) H = not ready (program running) VCEO = 40 V IC = 20 mA 18 Remote 1 Programmable remote output line 1 (command "remote" in program or event) VCEO = 40 V IC = 20 mA 4 Remote 2 Programmable remote output line 2 (command "remote" in program or event) VCEO = 40 V IC = 20 mA 17 Advance pulse (EOD) The EOD signal is outputted in the following cases: • without program: on every "INJECT A" • with progra
6.2 Remote interfaces 6.2.2 "733 IC Separation Center" interface The “733 IC Separation Center” is normally attached to remote interface 14 "733 IC Separation Center" (see section 2.3). If the 732 IC Detector is operated without the 733 IC Separation Center, this remote interface can also be used for the connection of external devices.
6 Interfaces 732 IC Detector Pin Function Outputs H Valve A → "FILL" Valve A is switched to position "FILL". 5 L H Valve A → "INJECT" Valve A is switched to position "INJECT". 18 L 4 Lock 733 keypad L = and keys are locked H = and are not locked 17 Valve B → "FILL" or suppressor → "STEP" Valve B is switched to position "FILL" or suppressor module is switched to next position. H Valve B → "INJECT" Valve B is switched to position "INJECT".
6.3 Analog output 6.3 Analog output For the attachment of recorders or integration systems, the 732 IC Detector offers the two analog outputs 11 (0…1 V) and 12 (0…10 mV) (see section 3). The attachment of these instruments is described in detail in section 2.9. The polarity of the output signal at the analog output sockets can always be switched under the key (see section 4.5.1).
6 Interfaces 6.5 Valve interfaces The two valve interfaces 38 and 46 of the 733 IC Separation Center can be used for the attachment of external devices (e.g. 750 Autosampler, «IC Metrodata for Win95») which can be employed to control the injection valves or the suppressor module (see section 2.3). The two valve interfaces for the injection valves A and B (or the suppressor module) are identical and have the following connections 733 IC Sep.
7.1 Technical data 7 Appendix 7.1 Technical data 7.1.1 732 IC Detector Conductivity measurement Measurement ranges 100, 200, 500, 1000, 2000, 5000, 10 000 µS/cm Full scale 0.05…10 000 µS/cm Temperature correction Automatic correction of the measured conductivity to reference temperature 20°C with the adjustable temperature coefficients (1.5 %/°C or 2.
7 Appendix Conductivity detector Construction Thermostatted conductivity detector with 2 ringshaped steel electrodes Measurement principle Alternating current measurement with following cell supply: Meas. Range Amplitude Frequency µS/cm µS/cm µS/cm mS/cm mS/cm mS/cm mS/cm 1 V peak 1 V peak 1 V peak 1 V peak 0.5 V peak 0.2 V peak 0.1 V peak 714 Hz 5000 Hz 5000 Hz 5000 Hz 5000 Hz 5000 Hz 5000 Hz 100 200 500 1 2 5 10 Cell volume 1.5 µL Cell constant 16.7 /cm; adjustable 13.0…21.
7.1 Technical data Interfaces RS232 interfaces Specifications, see section 6.1 Remote interfaces Specifications, see section 6.2 Analog output Specifications, see section 6.3 Safety specifications Construction/testing According to IEC 1010 / EN 61010 / UL 3101-1, protection class 1, degree of protection IP40 Safety directions The Instructions for Use include information and warnings which must be heeded by the user to assure safe operation of the instrument.
7 Appendix 7.1.2 733 IC Separation Center Parts and controls Keypad Chemically resistant membrane keypad made of polyester with function keys Indicators LEDs for display of valve position Power supply Internal Internal supply of 732 IC Detector via connecting cable External External supply via DIN connector: 5 V / 0.5 A 24 V / 2 A (transient, 200…300 ms) Interfaces Valve interfaces Specifications, see section 6.
7.2 Standard equipment 7.2 Standard equipment Subject to changes ! All dimensions are given in mm. 7.2.1 732 IC Detector The 732 IC Detector is available in two versions: • 2.732.0010 IC Detector with standard detector block • 2.732.0110 IC Detector with metal-free detector block These instruments include the following parts: Description 2.732.0110 Order No. 2.732.0010 Quant. 1 - 1.732.0100 Detector block with permanently attached connecting cable to 732 IC Detector - 1 1.732.
7 Appendix 7.2.2 733 IC Separation Center The 733 IC Separation Center is available in the following versions: • • • • • 2.733.0010 2.733.0020 2.733.0120 2.733.0030 2.733.0130 Instrument with 1 injection valve Instrument with 2 injection valves Instrument with 2 injection valves, metal-free Instrument with 1 injection valve and 1 suppressor module Instrument with 1 inj. valve and 1 suppr. module, metal-free These instruments contain the following parts: 2.733.0010 2.733.0020 2.733.0120 2.733.
7.2 Standard equipment 2.733.0010 2.733.0020 2.733.0120 2.733.0030 2.733.0130 Quant. 1 1 - 1 - Order No. Description 6.2621.000 Adjustable spanner max. 20 150 1 1 - 1 - 6.2621.050 Open-end spanner 1⁄4" 73 1 1 - 1 - 6.2621.060 Open-end spanner 5⁄16" 93 1 2 2 2 2 6.2744.010 PEEK compression fitting For the connection of 6.1831.010 PEEK capillaries or 6.1822.010 PTFE microcapillaries, set of 5 26 1 - 2 - 2 4 1 - 1 2 6.2744.020 6.2744.
7 Appendix 7.3 Optional accessories 7.3.1 Accessories for 733 IC Separation Center Order No. 6.1825.XXX Description Sample loop, made of PEEK For injection valve; incl. 2 PEEK compression fittings 6.2744.010 6.1825.230: Volume = 6.1825.210: Volume = 6.1825.220: Volume = 6.2620.000 10 µL 20 µL 100 µL Pressure screw, made of steel For connection of 6.2620.020 Steel capillaries, set of 5. 10.8 6.2620.010 Ferrule, made of steel For connection of 6.2620.020 Steel capillaries, set of 5. 3.7 3.9 6.
7.3 Optional accessories Order No. Description 6.2621.080 Capillary tubing cutter for plastic capillaries For 6.1831.010 PEEK capillaries and 6.1822.010 PTFE microcapillaries 55 incl. 5 additional blades 6.2744.030 6.2821.000 PEEK Coupling Connection between 6.2744.010 PEEK compression fitting and 6.1826.0X0 Pump tubing; set of 4 25 Filter unit Manufit To avoid contamination through abrasive particles from piston seals. For the pressure range 25…50 MPa with steel capillaries. 6.2821.
7 Appendix Order No. Description 6.2821.110 Filter for Filter unit PEEK 2 µm Spare part for 6.2821.100 Filter unit PEEK. Set of 10. 11 13.5 6.5324.000 7.3.2 Bottle rack For holding 3 supply bottles with eluent, regeneration solution and rinsing solution, incl. accessories (bottles, siphon, etc.) 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. 140 Column dimensions: 125 × 4.
7.3 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 or 6.2821.050 Twin cartridge holder. 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.
7 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 or 6.2821.050 Twin cartridge holder. ∅6.
7.3 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.
7 Appendix 7.3.3 Additional devices and cables Order No. Description 2.145.0300 Serial/parallel converter For the connection of printers with a parallel interface to the RS232 interface of 732 IC Detector 2.709.0X10 709 IC Pump Serial, high-performance dual piston pump with minimal residual pulsation and outstanding flow constancy; incl. accessories. Versions: 2.714.
7.3 Optional accessories Order No. Description 6.2115.060 Cable Connecting cable 732 IC Detector (analog output) – integrator or data acquisition system (analog cable) 6.2115.070 6.2125.010 2m Cable Connecting cable between 733 IC Separation Center and integrator or data acquisition system (start cable) 137 Cable Connecting cable 732 IC Detector (RS232 interface) – PC Adapter cable 25-pin to 9-pin. 9 pol. neg. 25 pol. 3m 6.2125.
7 Appendix 7.4 Warranty and conformity 7.4.1 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.
7.4 Warranty and conformity 7.4.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the instrument: 732 IC Detector meets the requirements of EC Directives 89/336/EWG and 73/23/EWG.
7 Appendix EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the instrument: 733 IC Separation Center meets the requirements of EC Directives 89/336/EWG and 73/23/EWG.
7.4 Warranty and conformity 7.4.3 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: 732 IC Detector System software: Stored in ROMs Name of manufacturer: Metrohm Ltd.
7 Appendix 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: 733 IC Separation Center Name of manufacturer: Metrohm Ltd.
7.5 Index 7.5 Index 7 709 ...............................see IC Pump 709 732 .......................... see IC Detector 732 733 ........... see IC Separation Center 733 733 not accessible ......................... 95 750 ........................ see Autosampler 750 752 ............................see Pump Unit 752 754 ......................... see Dialysis Unit 754 766 ...........see IC Sample Processor 766 791 ..........................see VA Detector 791 A Abort entry .................................
7 Appendix config ............................................... 124 CONFIG/733 IC Sep.Cent. ................. 95 CONFIG/733/suppressor .................... 96 CONFIG/733/valve A.......................... 95 CONFIG/733/valve B.......................... 96 CONFIG/aux/beep ............................... 92 CONFIG/aux/event ............................. 92 CONFIG/auxiliaries.......................... 91 CONFIG/detector ............................... 88 CONFIG/print meas.value ................
7.5 Index Disposal .............................................. 10 Door 20 Figure ................................................ 5 Double peaks ............................. 134,148 Drain tube............................................ 16 Drift ...................................... 135,148,189 E Earthing ............................................... 10 Edit event........................................... 116 Edit mode ....................................... 71,73 Edit program .....................
7 Appendix IC precolumn cartridge PRP-1........... 199 IC precolumn cartridge PRP-X100 .... 198 IC precolumn cartridge PRP-X300 .... 198 IC Pump 709 Automatic shutoff........................... 101 Connection at 732 ........................... 21 Electrical connection ....................... 21 Maintenance .................................. 134 Ordering designation..................... 202 Practical notes ............................... 134 RS232 settings ................................ 94 Settings........
7.5 Index Figure ......................................... 23,29 Installation .................................. 23,28 Manufit housing 80 Figure .............................................. 29 Montieren......................................... 30 Manufit pressure screw 57 Figure ......................................... 23,29 Installation .................................. 23,28 Manufit pressure screw 77 Figure .............................................. 29 Installation ................................
7 Appendix print header ...................................... 90 Printer ..... 42,89,94,119,122,124,161,182 Printer drivers....................................... 42 Printer settings..................................... 42 Printer type ................................... 90,122 Printout of date and time ................ 90,91 Printout of the print header .................. 90 .............................. 73,114 PROG R/S ............................... 85,115,116 prog.type .....................
7.5 Index Sample pretreatment cartridge IC-OH ............................................ 201 Sample pretreatment cartridge IC-RP ............................................. 200 Screw nut 97 Figure ............................................ 142 Mounting ....................................... 144 Seiko printer DPU-411/414............. 42,90
7 Appendix Terminal block 46 Figure ................................................ 7 Pin assignment .............................. 188 test ............................................ 108,109 Test chromatogram ............................. 32 Test mode................................... 108,109 Test plug (3.496.8480) ............... 149,153 Test plug (3.496.8510) ............... 149,154 Test status .................................. 108,109 test step ..................................
