Metrohm 2.792.0020 Basic IC Скачать руководство пользователя страница 89

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4 Operation

792 Basic IC

4.4 Methods

A method contains all information necessary for

data

acquisition

in-

tegration

peak

evaluation

and

quantification

. It can be considered

as the chromatogram template, i.e. chromatogram without raw data.
Methods are stored as

method files

(

*.mtw

) in the

Methods

directory. 35

prepared, write-protected methods are copied to this directory at pro-

gram installation.
Each system is linked to a method. This method is called

processing

method

and is opened automatically at the start of a new determina-

tion.

4.4.1

Method file handling

The following menu items are used for opening and saving of methods:

SYSTEM / PC icon / Open

By clicking this menu item or by double-clicking the PC icon in the sys-

tem window, the method file (

*.mtw

) belonging to the system is loaded

from the

Methods

directory. At the same time, an empty chromatogram

window is opened.
The name of the method is displayed in the title bar of the system win-

dow. A star (

) at the end of the name indicates that the method has

been changed since the last saving.

792 BASIC IC / File / Save / Method

Save the method of the current chromatogram in a method file (

*.mtw

) in

the

Methods

directory.

4.4.2 Passport

792 BASIC IC / Method / Passport

This menu item opens the

Passport

window that includes a detailed tex-

tual description of the chromatographic run and consists of the follow-

ing tabs:

General

General information on determination.

Sample

Sample information.

Column

Column information.

Eluent

Eluent information.

Comment

User comments on chromatogram.

Method Log

GLP log with date/time stamp for method.

Data Log

GLP log with date/time stamp for chromatogram.

Содержание 2.792.0020 Basic IC

Страница 1: ...and Phone 41 71 353 85 85 Fax 41 71 353 89 01 Internet www metrohm com E Mail info metrohm com 792 Basic IC Program 792 PC Software 1 0 POWER Basic IC 792 Basic Basic Basic Basic 8 792 1003 Instructio...

Страница 2: ...Mains connection 17 2 4 1 Setting the mains voltage 17 2 4 2 Fuses 18 2 4 3 Mains cable and mains connection 18 2 4 4 On off switching of the instrument 18 2 5 Connection to the PC 19 2 5 1 Connectin...

Страница 3: ...ndows 59 4 1 4 Main window elements 60 4 1 5 Icons of the main window 60 4 1 6 Overview of file types 61 4 1 7 Context sensitive menus 62 4 1 8 Keyboard and mouse functions 62 4 1 9 Help 63 4 2 Instru...

Страница 4: ...port calibration data 105 Put out calibration curves 105 4 4 6 Report output 106 Report options 106 4 5 Chromatograms 118 4 5 1 Chromatogram window 118 4 5 2 Chromatogram file handling 119 Open chroma...

Страница 5: ...Maintenance Faults 139 5 1 Practical notes on ion chromatography 139 5 1 1 Separating columns 139 5 1 2 High pressure pump 140 5 1 3 Eluents 141 5 1 4 Peristaltic pump 141 5 1 5 Suppressor module 142...

Страница 6: ...s connection 162 6 1 9 Safety specifications 162 6 1 10 Electromagnetic compatibility EMC 162 6 1 11 Ambient temperature 163 6 1 12 Housing 163 6 2 Standard equipment 164 6 3 Optional accessories 167...

Страница 7: ...ains voltage 18 Fig 9 Connection of the pulsation dampener option 24 Fig 10 Installing precolumn cartridges 29 Fig 11 Installation of precolumn glass cartridges with cartridge holder 31 Fig 12 Install...

Страница 8: ...37 Inlet capillary for detector block 6 33 37 38 38 38 38 Detector block 6 33 37 39 39 39 39 Suppressor module 6 37 40 40 40 40 Tubing cartridge 6 36 37 41 41 41 41 Contact pressure lever 6 36 37 42 4...

Страница 9: ...Sapphire supporting ring 147 88 88 88 88 Piston guide sleeve 147 89 89 89 89 Piston seal 147 90 90 90 90 Inlet valve 147 149 91 91 91 91 Outlet valve 147 149 92 92 92 92 Screw holder 147 93 93 93 93 S...

Страница 10: ...for cations or organic acids the 792 Basic IC can accommodate them all x Suppressor integrated Metrohm Suppressor Module MSM pressure resistant with fully automatic regeneration highest per formance a...

Страница 11: ...n internal or external standard selectable algorithms for non linear calibration various integration modes with integration pa rameters and integration events different methods for peak recognition pe...

Страница 12: ...2 2 2 2 1 1 1 1 3 3 3 3 4 4 4 4 Fig 1 Front of the 792 Basic IC 1 1 1 1 Door to interior 3 3 3 3 Feedthrough for syringe tubing for connection of the 6 2816 020 syringe used f r aspirating the sample...

Страница 13: ...ly Fuse 100 120V 220 240V 1 0A T 0 5A T Made by Metrohm Herisau Switzerland RS 232 Detector Block Waste B Waste A Transport security screws 9 9 9 9 10 10 10 10 11 11 11 11 12 12 12 12 13 13 13 13 6 6...

Страница 14: ...ith plastic stopper for additional supply and discharge lines to and from the inner compartment 14 14 14 14 RS232 interface connection of the PC 8 8 8 8 Knurled screw for fastening the rear panel 9 9...

Страница 15: ...36 36 36 1 1 1 1 18 18 18 18 19 19 19 19 19 19 19 19 20 20 20 20 21 21 21 21 22 22 22 22 35 35 35 35 34 34 34 34 33 33 33 33 32 32 32 32 31 31 31 31 30 30 30 30 28 28 28 28 27 27 27 27 26 26 26 26 37...

Страница 16: ...ength L 65 cm 38 38 38 38 Detector block 1 732 0110 24 24 24 24 Coupling 6 2744 120 for connection of the 6 2816 020 syringe 39 39 39 39 Suppressor module inlet and outlet capillaries are not shown 25...

Страница 17: ...ion 4 Operation Detailed description of the operation Section 5 Notes Maintenance Faults Notes on ion chromatography maintenance fault rectifi cation diagnostic tests validation Section 6 Appendix Tec...

Страница 18: ...35 Part or control of 792 Hazard This symbol draws attention to a possible danger to life or of injury if the associated directions are not followed correctly Warning This symbol draws attention to p...

Страница 19: ...of coming into contact with components which are live Hence always disconnect the instrument from all voltage sources before you open it and ensure that the mains cable is discon nected from mains co...

Страница 20: ...Conditioning sect 2 9 sect 2 9 sect 2 9 sect 2 9 Precolumn Precolumn Precolumn Precolumn Precolumn with twin cartridge holder Precolumn with twin cartridge holder Precolumn with twin cartridge holder...

Страница 21: ...35 20 20 20 20 66 66 66 66 75 75 75 75 39 39 39 39 76 76 76 76 26 26 26 26 37 37 37 37 38 38 38 38 28 28 28 28 29 29 29 29 31 31 31 31 30 30 30 30 18 18 18 18 21 21 21 21 22 22 22 22 78 78 78 78 79 7...

Страница 22: ...ation free from vibrations and protected against a corrosive atmos phere and contamination by chemicals To avoid disturbing temperature influences on the insulated column compartment the instrument mu...

Страница 23: ...yringe the syringe tubing 25 25 25 25 with coupling 24 24 24 24 and the PTFE aspirating tubing 23 23 23 23 are needed These accessories are mounted as follows 1 Connect syringe to syringe tubing x Pul...

Страница 24: ...apillaries it is best to use the 6 2621 080 Capillary tubing cutter 1 Mount compression fitting Slide a compression fitting 46 46 46 46 6 2744 010 or a compression fitting 47 47 47 47 6 2744 070 over...

Страница 25: ...er and 51 51 51 51 without filter screwed into the housing 50 50 50 50 For the connection of capillaries 48 48 48 48 PEEK compression fittings 46 46 46 46 6 2744 010 or 47 47 47 47 6 2744 070 must be...

Страница 26: ...a screwdriver loosen fuse holder 13 13 13 13 below the mains connection plug 12 12 12 12 and take out completely 3 Check and change fuse if necessary Carefully take the fuse installed for the desired...

Страница 27: ...es x 6 2122 020 with plug SEV 12 Switzerland x 6 2122 040 with plug CEE 7 VII Germany x 6 2133 070 with plug NEMA 5 15 USA which are three cored and fitted with a plug with an earthing pin If a dif fe...

Страница 28: ...ndows 98 Win dows NT and Windows 2000 operating systems and is installed as fol lows 1 Install program x Insert 6 6045 003 Installation CD into CD drive x Select Start and Run Browse for the setup exe...

Страница 29: ...the opening picture is opened and the Log In window appears on the screen x Do not enter any password here just click on Log In The following window appears x Enter company division and name and clic...

Страница 30: ...and click on Open The corresponding system window is opened x If the connection between PC and 792 Basic IC is working the message Hardware settings file for 792 unit with serial number not found Cre...

Страница 31: ...ings can normally be used for all other parameters x Click the 792 icon using the right mouse button and select the Hardware item The Hardware settings window is opened x In the Cell constant field en...

Страница 32: ...pulsation dampener option To protect the column material of sensitive separating columns e g methacrylate based columns against pressure drops caused by the in jector the use of the optional 6 2620 15...

Страница 33: ...18 Inlet capillary for injector PEEK capillary length L 24 cm 31 31 31 31 Purge valve 22 22 22 22 Injection valve 52 52 52 52 Pulsation dampener 6 2620 150 27 27 27 27 Connection capillary PEEK capil...

Страница 34: ...illed with either isopropanol or methanol water If this is not the case then the pump must first be rinsed with a solvent which is miscible with both the previous eluent and the following eluent e g a...

Страница 35: ...te to 2 mL min x Double click the 792 icon in the system window to open the window for manual control of the 792 Basic IC see below x Set the flow rate to 2 mL min in the Flow field x Click to Send to...

Страница 36: ...the rotary knob on purge valve 31 31 31 31 by turning it in a clockwise direction see Fig 3 x Remove the syringe from coupling 24 24 24 24 5 Rinse pulsation dampener if present x Place a beaker beneat...

Страница 37: ...x Insert inlet capillary 55 55 55 55 with end piece for precolumn cartridge in Manufit housing 56 56 56 56 x Insert outlet capillary 61 61 61 61 with end piece for precolumn car tridge in Manufit pres...

Страница 38: ...g 6 2744 120 46 46 46 46 Compression fitting 6 2620 000 55 55 55 55 Inlet capillary 56 56 56 56 Manufit housing 57 57 57 57 PTFE gasket 6 2821 010 58 58 58 58 2 Steel meshes 6 2821 020 59 59 59 59 Pre...

Страница 39: ...hand then firmly using a screwdriver turn 2 Connect precolumn x Provide the column connection capillary 20 20 20 20 mounted on the injection valve with a PEEK compression fitting 46 46 46 46 see sec t...

Страница 40: ...1 Connect precolumn x Remove end caps from the precolumn x Fit PEEK compression fitting 46 46 46 46 to column connection capil lary 20 20 20 20 see section 2 3 4 x Screw precolumn to column connectio...

Страница 41: ...umn used Normally the following sample loops are used Cation columns 10 PL Anion columns with suppressor 20 PL Anion columns without suppressor 100 PL In the 792 Basic IC the 6 1825 210 sample loop 20...

Страница 42: ...let end of separating column 66 66 66 66 to the inlet capillary 37 37 37 37 permanently mounted on the detector block 38 38 38 38 4 Fix column x Insert one or two column holders 67 67 67 67 6 2027 030...

Страница 43: ...20 20 20 20 or to the already installed precolumn procedure see section 2 7 7 2 Rinse column x Place a beaker beneath the column outlet x Open software window for manual system control x If necessary...

Страница 44: ...suppressor units flow rate of 0 5 mL min The three inlets and outlets numbered 1 3 on the suppressor module each have 2 permanently mounted PTFE capillaries which must be connected as described in se...

Страница 45: ...ubings 71 71 71 71 and 72 72 72 72 x Attach a filter unit PEEK 28 28 28 28 see section 2 3 5 to the other end of this coupling note flow direction 68 69 68 69 68 69 68 69 70 70 70 70 71 72 71 72 71 72...

Страница 46: ...mn with suppressor 19 19 19 19 Mounting rail for column holder 67 67 67 67 66 66 66 66 Separating column 20 20 20 20 Column connection capillary PEEK capillary 6 1831 010 30 cm 67 67 67 67 Column hold...

Страница 47: ...ws 1 Prepare supply bottle for H2SO4 x Prepare regeneration solution suited for the desired applica tion and separating column normally 20 mmol L H2SO4 x Fill regeneration solution into supply bottle...

Страница 48: ...ted PTFE capillaries which must be connected as follows see Fig 14 and Fig 15 1 Inlet capillary for eluent x Screw inlet capillary 75 75 75 75 marked with Eluent of suppressor module 39 39 39 39 to ou...

Страница 49: ...et capillary 79 79 79 79 to a sufficiently large waste container and fix it in place 7 Fasten capillaries to the side walls x If necessary the two aspirating tubings 68 68 68 68 and 69 69 69 69 can be...

Страница 50: ...System in the main window Select the sys tem file suited for the inserted column e g anionsupp smt and click on Open 2 Open control window x Double click the 792 icon in the system window The control...

Страница 51: ...cted system 2 9 2 Putting into operation with suppressor Before sample solutions can be injected at the 792 Basic IC with use of the suppressor the entire system must be tested for leaks and then cond...

Страница 52: ...once more to obtain optimal contact pressure 5 Check for leaks x Check all capillaries and their connections in the 792 Basic IC for escaping liquid If eluent escapes anywhere the appropri ate compre...

Страница 53: ...2 Installation 792 Basic IC 44...

Страница 54: ...t be modified appropriately For further explanations of the operation please refer to section 4 3 1 Requirements For the determination of anions in drinking water described in this tuto rial the follo...

Страница 55: ...detector block section 2 3 1 Mounting syringe and aspirating tubing section 2 3 2 Mains connection section 2 4 Connection to PC section 2 5 2 Prepare eluent Preparing eluent 2 4 mmol L NaHCO3 2 5 mmol...

Страница 56: ...program display and the parameter values may occur In the description of the calibration procedure it is assumed that the PC and 792 Basic IC are not in operation and that the system must first be con...

Страница 57: ...oncerning the sample in the automatically opened Edit sample description window Set Cali bration level to 0 and confirm with OK 8 Condition system Let the system run for several minutes If the system...

Страница 58: ...utton of the 792 icon in the system window to switch the injection valve to the INJECT position At the same time the data recording is started automatically The status bar of the chromatogram window s...

Страница 59: ...tion from the Method menu in the main window to open the integration parameters window If required e g if the fluoride peak is not detected change the time delay Delay before starting peak integration...

Страница 60: ...this retention time is indicated by the cursor vertical line If the Peak column contains a 0 the peak must be manually allocated to a component In this case insert the peak num ber from the chromatog...

Страница 61: ...e Enter this value rounded off if necessary into the Time column The optimized table could for example then appear as follows 15 Start calibration Click the Concentrations button in the component wind...

Страница 62: ...splayed e g for chloride Close the Component chloride window with OK Close the Components window below the chromatogram by clicking on OK 17 Save chromatogram and method Close the chromatogram window...

Страница 63: ...iption window is opened automatically 2 Enter information for determination Enter the desired information concerning the sample in the Edit sample description window and confirm with OK Set Ca librati...

Страница 64: ...ve been found are num bered and the baseline drawn In the SYSTEM STATE window the message Finished 792COM appears It is now possible to record further samples with the same system At the end of the de...

Страница 65: ...utput Under Items to report and More items to report click all desired elements for the report output Click on Report to start the report output to the selected target 8 Print report Click on or selec...

Страница 66: ...e operation 4 1 1 Starting closing the program Start the 792 Basic IC program Start the program Double click this icon or the Metro792 exe file to start the 792 Basic IC 1 0 program The Login window a...

Страница 67: ...tograms are stored as chromatogram files chw in the Data directory As well as the measuring data the chromatogram files also contain the method parameters and system settings which have been used for...

Страница 68: ...queue During reprocessing with a selected method the set tings for calibration integration passport appearance and report can be altered at will 4 1 3 Overview of program windows The 792 Basic IC prog...

Страница 69: ...in the 792 BASIC IC main window Open chromatogram Save chromatogram Open last batch reprocessing file Report settings Print preview Print report Passport General method settings Integration parameter...

Страница 70: ...t calibra tion The cal file is stored automatically in the Methods folder chw Chromatogram file This binary file contains chromatogram system and method data of a determination The chw file is stored...

Страница 71: ...leasing of the left mouse button the selected region will be zoomed full screen If the cursor is active in the peak editor mode then it can be moved by pressing down the right hand mouse key The keybo...

Страница 72: ...sor left to right Shift right Quickly moves cursor left to right left Moves cursor right to left Shift left Quickly moves cursor right to left Home Moves cursor to beginning of a window End Moves curs...

Страница 73: ...e chosen font configuration 4 2 2 Security system The 792 Basic IC program has a security system based on the list of users Every user has his unique password and one of the following ac cess levels N...

Страница 74: ...iguration of the security system the program prompts for the password every time the system starts This user name stamps all methods chromatograms and reports It is possible at any time to change the...

Страница 75: ...ser is asked if the method should be overwritten Overwrite without asking Method files are overwritten without confirma tion Opening chromatograms Opening of chromatograms Ignore last data directory I...

Страница 76: ...ion 4 5 3 4 2 4 COM port 792 BASIC IC Options 792 Basic IC COM1 This menu item opens the Links window for COM port serial RS232 in terface selection and settings If COM1 is clicked with the right mous...

Страница 77: ...ns to start and stop a determination 4 3 2 System file handling The following menu items are used for opening changing saving and closing of systems 792 BASIC IC File Open System Load an existing syst...

Страница 78: ...In this case the user is asked if the recorded baseline should be saved or not SYSTEM Control Shutdown hardware High pressure pump and peristaltic pump at the 792 Basic IC are im mediately stopped A...

Страница 79: ...qual to the date and time when the chromatogram starts SYSTEM Control Stop determination Stop running determination Data acquisition and time program are terminated immediately The recorded chromatogr...

Страница 80: ...selection of processing method Processing method Directory and name of the method file mtw linked to the system The method file can be selected with choose and opened with show Connected data source D...

Страница 81: ...stem is connected the icon contains two buttons for manual control of the injection valve Inject Switch injection valve to INJECT position Fill Switch injection valve to FILL position If the system is...

Страница 82: ...ystem the Control tab is displayed It allows manual control of the 792 Basic IC functions and setting of startup values to be sent to the instrument This tab shows the current measurement values for c...

Страница 83: ...s connected a determination is started or the values are sent manually with Send to unit Flow mL min Startup value for flow rate of the high pressure pump Entry range 0 20 2 50 mL min Pressure max MPa...

Страница 84: ...ns can be added to the time program on the Program subpage Instruction Parameter entry Meaning Valve Inject Fill Switch injection valve to INJECT or FILL position ICPump on off Switch on or off the hi...

Страница 85: ...he Fill or to the Inject position Use peristaltic pump If this option is disabled the peristaltic pump is not switched on automatically at the start of a determination or with Startup hardware Polarit...

Страница 86: ...1 99 9 cm For a precise determination of the cell constant pump a calibration solution of known conduc tivity through the IC system observe the dis played conductivity and change the cell con stant u...

Страница 87: ...of subfolder containing the system file Status messages Checking on line Checking connection between PC and 792 Basic IC On line Connection between PC and 792 Basic IC ok UploadStartupValues System s...

Страница 88: ...peat last action if error reappears call Metrohm service E295 Storage of memory values failed repeat last action if error reappears call Metrohm service E296 Instrument stopped restart instrument if e...

Страница 89: ...the sys tem window the method file mtw belonging to the system is loaded from the Methods directory At the same time an empty chromatogram window is opened The name of the method is displayed in the...

Страница 90: ...and file name of the current chroma togram read only Date time Date and time of the chromatogram start read only Last update Date and time of the last chromatogram modifi cation and saving read only C...

Страница 91: ...Second sample description max 256 charac ters Volume Injected volume in PL Dilution Dilution of the sample Vial number Autosampler vial position to take sample from Amount Sample amount If this value...

Страница 92: ...max 256 characters Particle size Particle size of the column in Pm This value is used for the calculation of reduced theoretical plate height Reduced TP height Void volume Void volume for the column...

Страница 93: ...ts The system startup value for the flow rate is entered automatically into this field at the start of a determination Pressure Pressure in MPa The measured value for the pressure is entered automatic...

Страница 94: ...these messages free text user comments can be entered All this entries are stamped auto matically with date and time of the entry Add new Add a new GLP comment Text can be entered in the New comment...

Страница 95: ...for every modification made on a recorded chromatogram In addition to these messages free text user comments can be entered All this entries are stamped automatically with date and time of the entry a...

Страница 96: ...tab is identical to the General tab called with Method Passport see section 4 4 2 Processing Tab Processing of Method setup window for definition of actions that are performed during the run or when...

Страница 97: ...calculation parameter Formula set Formula setting by customer Custom formulae or according either to European Pharmacopoeia or US Pharmacopoeia Theoretical plates Selection of calculation formula for...

Страница 98: ...the run and its retention time is stored in the Void time field From void volume For the calculation of the void time the value entered in the Void volume field is multiplied by the ratio of empty col...

Страница 99: ...st deriva tive slope In order to decide whether the slope at some point is sig nificant the first derivative value is divided by the baseline noise and the result is compared with a threshold value ca...

Страница 100: ...in min Entry range 0 1440 min Width Peak width at the baseline in s This parameter is used for setting baseline start and end points If this value is too low exces sive narrow peaks are detected from...

Страница 101: ...d for fine tuning of the integration process They should be used only in the case when problems cannot be solved by tuning a set of parameters from the integration parameters window Number of events N...

Страница 102: ...Force the beginning of a new peak If a peak is available at the moment of the event it is either rejected upslope or terminated down slope Set peak end Force peak end at the time of the event Up slop...

Страница 103: ...ibrated component a calibration curve is constructed as a result With the 792 Basic IC three different procedures can be used for the construction of the calibration curve By far the most important me...

Страница 104: ...through the separation system t t t0 Corrected retention time called also net retention time L Column length v L t0 Linear Flow rate W R k2R2 k1R k0 Calibration function component quantity W vs de tec...

Страница 105: ...mponent is calculated using the RSD method Wi R RSD Qij Rij RSD Ci V Rij When quantification procedure is performed a concentration Ci abso lute concentration of a component in the sample is determine...

Страница 106: ...ts details see on line help Name Component s name cannot include spaces Rows with empty names are excluded from the ta ble of components when you leave the component table editor Group Number of the g...

Страница 107: ...or the names and retention times If the output of all peaks is required in the result report then a so called universal component can be defined in the component table for this purpose this receives t...

Страница 108: ...Retention units Choice of retention units Default is min Retention time Retention time Update Updates expected retention times of compo nents according to the current chromatogram Worst case Informati...

Страница 109: ...d units of concentration that will ap pear in the report Nevertheless entry of new concentration units does not cause recalcula tion of concentrations Data type Choice of the data type that will be sh...

Страница 110: ...all components Copy concentrations from level Number of calibration level from which concen trations are copied Calibrate immediately Recalibration with new calibration levels Delete Delete the curre...

Страница 111: ...s and curve Analytical expression A line above the calibration curve looking like Q k3 x x x xA3 k2 x x x xA2 k1 x x x xA k0 This formula is used for approximation of the calibration curve RSD RSD Res...

Страница 112: ...rop out of the calibration curve watching for RSD values Component information Component Allows to select the current component from the list It is possible also to scroll the list of com ponents by m...

Страница 113: ...0 Statistical weight Weighting parameter used to weight calibration points deviations on calculating coefficients of the calibration formula Apart from the uniform weighting 1 the values 1 x 1 x2 1 y...

Страница 114: ...port and export calibration data 792 BASIC IC Method Calibration Import calibration This option imports a calibration from a calibration file cal to the cur rent method or chromatogram It is used to t...

Страница 115: ...port Items to report This part of the Report options window contains a list of important report items that can be included into the report on the user s choice General General description on the analy...

Страница 116: ...ENT A 1 7 mM NaHCO3 1 8 mM Na2CO3 B C Flow 1 00 mL min Temperature 20 0 C Pressure 8 0 MPa Chromatogram plot Plot of the chromatogram only for Printer or File destination Peak table Peak table with re...

Страница 117: ...ata saved to disk file c programme ic 792 data K4111745 CHW More items to report This part of the Report options window contains a list of rarely used re port items that can be included into the repor...

Страница 118: ...5 0 6 027e 00 0 00 0 000 0 bromide 5 7 74 5 0 4 763e 00 8 74 0 000 0 nitrate 6 11 67 5 0 9 164e 00 0 00 0 000 0 phosphate 7 13 20 5 0 3 449e 00 6 58 0 000 0 sulfate Calibration results Calibration re...

Страница 119: ...rameter is used to detect an underflow condi tion Zero A signal level on a baseline in ADC conversion units This parameter is a result of the ADC calibration Maximum Maximum value of the linear range...

Страница 120: ...alization field Ci NORM Wi Ri Wi Ri As long as no universal component is defined only peaks with non zero concentrations are listed The peak table includes the following columns number retention time...

Страница 121: ...ize the peak table on the user s choice using the Customize button The peak table for the methods supplied con tains the following columns as standard number retention time height area response factor...

Страница 122: ...e rtt Several templates for different languages and applica tions are available Separator Defines which character separates report col umns in tables A separator other than Space is useful when the re...

Страница 123: ...column is equal to the chromatogram dura tion halfwidth Width of the peak at half height in minutes height Height of the peak in PS cm The total value in this column is the sum of heights for all iden...

Страница 124: ...half width errors for those peaks are much greater than height or area errors Total for this column includes average value for the peaks listed effectivity TP m Effectivity for the peak in number of t...

Страница 125: ...wn in advance The concentration of the component is calculated by the formula C i Wi Ri V Wi Ri Cs Ws Rs where V Ws Rs Cs is the effective redu ced volume of injected sample The standard component con...

Страница 126: ...brated region In the case of peaks additional letters precede the component type information indicating how peaks are separated from other peaks for example BD_ Peak that starts on the baseline B and...

Страница 127: ...measuring points Measure Chromatogram is being measured Measure Baseline Recording of baseline Finished Measurement finished but the chromatogram is not processed Processing Chromatogram is being proc...

Страница 128: ...king directory File window Box with the list of files residing in the working directory sorted by time the last recorded chromatogram is at the top of the list As addi tional short information on the...

Страница 129: ...lected chromatograms and move them to the Windows wastebasket Save chromatogram 792 BASIC IC File Save Chromatogram Save the selected chromatogram in a chromatogram file chw in the working directory I...

Страница 130: ...port Raw data to txt Export chromatographic raw data into an ASCII text file txt The fol lowing window appears Represent raw data as Output of raw data Default units float Y values are exported in def...

Страница 131: ...chroma tograms Colors Color settings for chromatogram ele ments The appearance settings for a chromatogram are not saved automati cally on closing the chromatogram In order to have the same appear an...

Страница 132: ...the same level This option is useful for gradient chromatograms Drift compensation has no effect while a chromatogram is running Grid Plot dotted grid lines in the selected chroma togram window Set a...

Страница 133: ...tart of the chro matogram In corner Channel label is shown in the upper right corner of the chromatogram Set all Set peak labeling of all opened chromatograms automatically to the settings in the sele...

Страница 134: ...olor Baseline Baseline color AlterGround Alternative background color for Measure base line option Channel 1 8 Color of the selected channel Each channel can be of a unique color Line width Line width...

Страница 135: ...ram perfectly fits the window horizon tally and vertically 792 BASIC IC View Recorder autoscale This option allows to look at the chromatogram so that the last point is always visible on the screen wh...

Страница 136: ...mouse button somewhere in the chromatogram window and to select the Peak editor item You cannot edit the peak pattern while the component table is active and vice versa when the peak editor mode is s...

Страница 137: ...ursor position 792 BASIC IC Peak Split peaks Split a single peak into two peaks at the cursor position 792 BASIC IC Peak Delete all left Delete all peaks to the left of the selected point 792 BASIC IC...

Страница 138: ...entimeters Centimeters Page margins Selection of page margins Left Left margin Right Right margin Top Top margin Bottom Bottom margin Chromatogram plot size Selection of plot area for chromatograms Wi...

Страница 139: ...rt options window will be active except the des tination of the printout In order for the chromatogram to be printed the option Chromatogram plot must be switched on in the Report options window under...

Страница 140: ...ction of this menu item opens the Raw data compression window for compression of the raw data of the active chromatogram by summing up several neighboring points Divisor Coefficient of compression the...

Страница 141: ...Data direc tory and open the Reprocess window Create new batch reprocessing queue 792 BASIC IC File Open Chromatogram For creation of a new batch reprocessing queue open the Chroma togram open window...

Страница 142: ...ing are set and can then be trig gered Use method from file for reprocessing Selection of the desired chromatogram file whose method should be used for reprocess ing If the reprocessing includes reint...

Страница 143: ...updating the concentration table Default scheme Default setting for recalibration reprocessing The two options Apply final calibration and For get calibration points are switched on A new calibration...

Страница 144: ...eters can be modified The passport parameters Ident Sample Info 1 and Sample Info 2 entered in the batch reprocessing table are overwritten if these values are modified in the Passport window Modify c...

Страница 145: ...romatograms are displayed in the same order as in the batch re processing table slightly displaced one upon the other The distance between the curves can be increased by pressing Shift n and decreased...

Страница 146: ...field Volume Injected volume of sample in PL Will be placed into appropriate passport field Dilution Sample dilution prior to injection Will be placed into appropriate passport field Amount Sample amo...

Страница 147: ...n fields with values automatically incremented by 1 The last character of the first selected field must be a number This function is available for the fields Ident Vial Calibration level Sample Info 1...

Страница 148: ...chromatog raphy as well as detailed information on the separating columns available from Metrohm see section 6 3 2 in the leaflets supplied and in the 8 732 2013 IC Application Notes folder Protection...

Страница 149: ...ion dampener MF is rec ommended to protect sensitive separating columns e g methacrylate based columns It is used to reduce interfering pulsation in highly sen sitive measurements and also protects th...

Страница 150: ...ty x pH pH alterations lead to shifts in the dissociation equilibrium and thus to changes in the reten tion times x Organic modifiers Addition of an organic solvent e g methanol acetone acetonitrile t...

Страница 151: ...ated with H2SO4 in the same flow direction used for the eluent You should thus always install the inlet and outlet capillaries as described in section 2 8 4 according to the scheme shown in Fig 15 The...

Страница 152: ...ice if your instrument s have been damaged in such a way The instrument must not be opened by untrained personnel Please comply with the safety notes in section 1 4 1 Maintenance by Metrohm service Ma...

Страница 153: ...equent damage For rinsing the connections to the separating column and the suppres sor module are removed the two capillaries 20 20 20 20 and 37 37 37 37 see Fig 12 and Fig 14 are directly connected t...

Страница 154: ...or inlet capillary 75 75 75 75 x Unscrew column 66 66 66 66 from column connection capillary 20 20 20 20 or the precolumn 2 Rinse with eluent x Place beaker beneath the column connection capillary 20...

Страница 155: ...e with Fig 16 Main and auxiliary pistons are identical with the following excep tions The spring 84 84 84 84 of the auxiliary piston right piston is more powerful longer than that of the main piston l...

Страница 156: ...1 81 81 Screw 3 709 1100 for piston cartridge 85 85 85 85 89 89 89 89 Piston seal 6 2741 020 82 82 82 82 Zircon piston 6 2824 070 with piston shaft 90 90 90 90 Inlet valve 6 2824 090 83 83 83 83 Sprin...

Страница 157: ...eedle inserted through the upper opening in the valve housing 95 95 95 95 The individual components are rinsed with dist water and or acetone and the sapphire sphere cleaned with a paper towel The val...

Страница 158: ...naturally accom modate the longest bolt If this is not the case the pump will not function properly x Screw connection capillary 35 35 35 35 to pump head 34 34 34 34 see Fig 3 x Connect aspirating tub...

Страница 159: ...ntamination with heavy metals 1 mol L H2SO4 Contamination with organic cationic complexing agents 0 1 mol L H2SO4 0 1 mol L oxalic acid acetone 5 Severe contamination with organic substances 0 2 mol L...

Страница 160: ...re pump 3 Connect suppressor to IC system x Connect inlet capillaries 77 77 77 77 and 78 78 78 78 to the peristaltic pump see section 2 8 4 x If the pressure problems persist replace the suppressor ro...

Страница 161: ...in suppressor holder 105 105 105 105 in such a way that the tubing connections at the rear of the rotor fit in the corresponding openings inside the rotor and that one of the three holes in the rotor...

Страница 162: ...mediable blockage of the suppressor the suppres sor can no longer deliver solutions Both the 6 2832 000 Suppressor rotor and the 6 2832 010 Connection piece with the input and output leads can be repl...

Страница 163: ...the case bring the rotor into the correct position from below with the aid of a sharp object e g a screwdriver 5 Clean connection piece x Clean the sealing surface of new connection piece 103 103 103...

Страница 164: ...er 41 41 41 41 on the tubing cartridge 40 40 40 40 down as far as it will go x Release tubing cartridge 40 40 40 40 from holding clamp 42 42 42 42 by press ing down snap action lever 43 43 43 43 and r...

Страница 165: ...ted in the following table with details of possible causes and countermeasures Malfunction Cause Rectification Baseline with high noise level pulsation x Contaminated pump valves x Faulty piston seals...

Страница 166: ...ends x Fill column with glass beads d 100 Pm or replace column No feed of regeneration or rinsing solution for suppressor x Contact pressure too low x Leak in system x Defective pump tubing x Contami...

Страница 167: ...tion can also be found in the brochure Quality management with Metrohm which is available from your local Metrohm agency Testing of the electronic and mechanical function groups of Metrohm instruments...

Страница 168: ...y detector Construction Thermostatted conductivity detector with 2 ring shaped steel electrodes Measurement principle Alternating current measurement with 1 kHz frequency and ca 1 7 V amplitude peak t...

Страница 169: ...oresistive measurement Response time 3 ms Measurement volume ca 50 PL Maximum error r 3 of set value Resolution 0 1 MPa conductivity measurements Sampling rate 1 measurement piston stroke pump running...

Страница 170: ...imum error r 5 Maximum pressure 0 4 MPa 4 bar Pumpable liquids Clear liquids with no solid contents Pump tubing material PP polypropylene 6 1 6 Suppressor module Switching duration 140 ms Pressure res...

Страница 171: ...ety directions The Instructions for Use include information and warnings that must be heeded by the user to assure safe operation of the instrument 6 1 10 Electromagnetic compatibility EMC Emitted int...

Страница 172: ...5 45 C at 20 80 atmospheric humidity Storage 20 70 C Transport 40 70 C 6 1 12 Housing Material of cover Polyurethane rigid foam PUR with fire protection for fire class UL94VO CFC free Material of base...

Страница 173: ...d 0 51 mm ex d 2 31 mm 400 150 1 6 1834 010 Aspirating tubing made of PTFE with connector for 6 2821 090 aspirating filter Length 2 5 m For the connection high pressure pump eluent bottle 1 6 2027 030...

Страница 174: ...onnection between 6 2744 010 PEEK compression fitting and 6 1826 060 Pump tubing set of 4 1 6 2744 040 PEEK coupling For connection of 1 e16 capillaries 2 6 2744 110 PEEK coupling Connection between 6...

Страница 175: ...6 6045 003 Software CD 792 Basic IC 1 0 1 Y 107 0150 Cable strap 1 8 732 2003 Metrohm Monograph Ion chromatography English 1 8 732 2013 IC Application Notes English 1 8 792 1003 Instructions for Use...

Страница 176: ...to reduce pulsation and prolong the life of separating columns 6 2621 080 Capillary tubing cutter for plastic capillaries For 6 1831 010 PEEK capillaries and 6 1822 010 PTFE microcapillaries incl 5 a...

Страница 177: ...Spare part for 6 2824 100 Pump head 6 2824 090 Inlet valve metal free Spare part for 6 2824 100 Pump head 6 2824 100 Pump head metal free Complete with fixations screws 6 5324 000 Bottle rack Complet...

Страница 178: ...ridge holder 6 1005 030 IC exclusion column PRP X300 For the determination of organic acids without chemical suppression Column dimensions 250 u 4 0 mm Precolumn 6 1005 040 6 1005 040 IC precolumn car...

Страница 179: ...using 6 2828 100 Glass cartridge holder Precolumn 6 1006 030 6 2828 110 Note The 6 2620 150 Pulsation dampener must be used for operation of this column 6 1006 030 IC precolumn cartridge METROSEP Anio...

Страница 180: ...d To prolong the service life of the METROSEP A SUPP 4 5 anion columns 6 1006 510 IC anion column METROSEP A SUPP 5 100 For the determination of anions with chemical suppression Column dimensions 100...

Страница 181: ...without chemical suppression Column dimensions 100 u 4 6 mm Precolumns 6 1009 010 IC anion column SUPERSEP or 6 1005 010 IC precolumn cartridge 6 1009 010 IC anion precolumn SUPERSEP To prolong the s...

Страница 182: ...column METROSEP C 2 250 For the determination of monovalent and divalent cations without chemical suppression Column dimensions 250 u 4 0 mm Precolumn 6 1010 200 6 1010 300 Preconcentration column MET...

Страница 183: ...ations With Luer connection 6 1012 200 set of 50 6 2027 050 Column holder Diameter d 15 0 mm 42 d 6 2821 010 PTFE gasket Spare part for 6 1005 000 6 1005 010 6 1005 030 6 1007 000 and 6 1010 000 separ...

Страница 184: ...for suppressor rotor with input and output leads 6 3 3 Additional devices and cables Order No Description 6 2125 010 Cable Connecting cable 792 Basic IC RS232 interface PC Adapter cable 25 pin to 9 pi...

Страница 185: ...nteed features the orderer has no rights or claims ex cept those mentioned above If damage of the packaging is evident on receipt of a consignment or if the goods show signs of transport damage after...

Страница 186: ...cifications EN 50081 1 Electromagnetic compatibility basic specification Emitted Interference EN 50082 1 Electromagnetic compatibility basic specification Interference Immunity EN 61010 Safety require...

Страница 187: ...5 class 2 3 IEC801 6 IEC1000 4 6 class 2 EN50082 1 EN61000 3 2 3 IEC1000 3 2 3 EN61000 4 11 IEC1000 4 11 IEC61326 class B EN55011 class B EN55022 class B EN50081 1 Electromagnetic compatibility IEC101...

Страница 188: ...Color settings 125 Display 124 Evaluation 90 Marks 124 Baseline marker 124 Baseline noise 90 110 Baseline with high noise level 156 Basic settings 20 Batch 82 Batch reprocessing 132 133 Definition 59...

Страница 189: ...ation 103 Concentration of internal standard 112 137 Concentration of standard 104 Concentration of std 112 Concentration table 100 Concentration units 100 concentration 116 Concentrations 100 Concent...

Страница 190: ...07 Eluent A 84 Eluent B 84 Eluent bottle Connection 25 Eluent C 84 Eluent change 141 Eluent vessel Recycling 144 Eluents Notes 141 EMC 162 Emitted interference 162 Enable detection 93 Enable valley to...

Страница 191: ...n column PRP X300 169 IC precolumn A SUPP 4 5 Guard 171 IC precolumn C 2 Guard 173 IC precolumn cartridge METROSEP Anion Dual 1 170 IC precolumn cartridge METROSEP Cation 1 2 172 IC precolumn cartridg...

Страница 192: ...e 66 80 METHOD 81 Method 76 Method Log 85 108 Method setup 87 Metrohm Monograph Ion chromatography 8 139 Metrohm service 143 Metrohm suppressor module see Suppressor module Microfiltration 139 140 141...

Страница 193: ...olumn cartridge 64 64 64 64 Figure 31 Installation 30 Precolumn cartridge holder 6 2828 110 Figure 31 Installation 30 Ordering designation 174 Precolumns General information 28 Installation 28 Interna...

Страница 194: ...l pulsation 160 resolution 115 Resolution 88 139 157 160 Response 95 Response axis 123 response factor 115 Response factor 97 Response normalization 111 Result report 107 Retention index 89 97 105 112...

Страница 195: ...p determination 70 Stopper 73 73 73 73 Figure 36 Install pump tubing 155 Install pump tubings 35 Strap Y 107 0150 40 Subtract 131 Subtraction of a chromatogram 131 Sunlight 13 Supply bottle 38 Suppres...

Страница 196: ...upValues 78 US Pharmacopoeia 89 Use method from file for reprocessing 133 Use peristaltic pump 76 Used 103 User 81 V Validation 158 Valve 74 75 Valve housing 95 95 95 95 Figure 149 Verify 75 Vial 137...

Страница 197: ...6 Appendix 792 Basic IC 188...

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Содержание 2.792.0020 Basic IC

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Metrohm 2.792.0020 Basic IC, Инструкция по эксплуатации, Страница: 89 / 197

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Содержание 2.792.0020 Basic IC

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