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January 2004

Thermo Electron

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de référence peuvent fournir des indices précieux pour l’identification
et la résolution de problèmes futurs.

Toxicité chimique

Bien que l’utilisation et l’entreposage dans les laboratoires de grandes
quantités de solvants inflammables et toxiques puissent représenter un
danger, ne pas négliger les dangers potentiels posés par les
échantillons. Veiller particulièrement à lire et à suivre toutes les
précautions indiquées pour assurer la ventilation, le stockage, la
manutention et l’élimination des solvants et des échantillons. Se
familiariser avec les données sur la toxicité et les dangers potentiels
associés à tous les produits chimiques en consultant les fiches
techniques sur la sécurité des substances (FTSS) du fabricant.

Préparation des échantillons

Toujours considérer la solubilité de l’échantillon dans la phase
mobile. La précipitation des échantillons peut boucher la colonne, les
tubes et/ou la cellule de dilution, et en limiter le débit. Cette
obstruction peut endommager le système de façon irréparable.
L’accumulation de particules peut être évitée par la filtration des
échantillons à travers des filtres de 0,45 ou 0,2 µm (ou moins).

Caractéristiques des solvants

Un grand nombre de fabricants de produits chimiques fournissent des
réactifs de pureté élevée ou de qualité spectrographique dépourvue de
toute impureté chimique. La filtration systématique de tous les
solvants ou éluants à travers un filtre fluorocarboné de 0,45 ou 0,2 µm
(ou moins) avant de les placer dans le réservoir de solvants prolonge
de façon significative la durée de vie et l’efficacité des filtres
d’entrée, des clapets et des joints d’étanchéité, de l’injecteur et de la
colonne. De façon générale, les solvants pour chromatographie
liquide sous haute pression ne nécessitent pas de filtration.

Choisir une phase mobile qui est compatible avec l’échantillon et la
colonne sélectionnés pour la séparation. Noter que certains solvants
sont corrosifs pour l’acier inoxydable. Des versions inertes et
biocompatibles des instruments sont disponibles auprès de
Thermo Electron.

Dégazage des éluants

Effectuer le dégazage des éluants selon la méthode de dégazage par le
vide ou à l’hélium. Une description complète de ces méthodes est
disponible dans la documentation fournie séparément avec les
accessoires de dégazage.

Élimination des solvants

S’assurer qu’il existe un conteneur pour solvants à éliminer ou tout
autre système de vidange au niveau de la table de travail ou
au-dessous de celle-ci. La plupart des solvants doivent être éliminés
dans des conditions particulières et ne doivent pas être évacués

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Содержание Finnigan SpectraSYSTEM UV6000LP

Страница 1: ...Finnigan SpectraSYSTEM UV6000LP Detector Reference Manual A0099 595 Revision F ...

Страница 2: ...o Milano 39 02 95059 226 Japan C 2F 3 9 Moriya cho Kanagawa ku Yokohama Kanagawa 221 0022 81 45 453 9100 Japan Esaka Grand Building 2 3 1 Esaka cho Suita City Osaka 564 0063 81 06 6387 6681 Netherlands Takkebijsters 1 NL 4817 BL Breda 31 076 5878 722 P R China Room 901 Ping an Mansion No 23 Jin Rong Street Xi Cheng District Beijing 100032 86 010 6621 0839 Spain Sepulveda 7 A ES 28108 Alcobendas Ma...

Страница 3: ...nistration Lab Management Operator Other ___________________________ Reader Survey Help us to improve the quality of our documentation by answering a few questions Finnigan SpectraSYSTEM UV6000LP Detector Reference Manual Revision F A0099 595 Strongly Agree Agree Disagree Strongly Disagree The manual is well organized 1 2 3 4 The manual is clearly written 1 2 3 4 The manual contains all of the inf...

Страница 4: ...AL PUBLICATIONS THERMO ELECTRON SAN JOSE 355 RIVER OAKS PARKWAY SAN JOSE CA 95134 1991 UNITED STATES OF AMERICA From _______________________________ ____________________________________ ____________________________________ fold fold ...

Страница 5: ...nalog Output Connections 2 6 Analog Output Settings 2 6 Remote Communications Connections 2 8 Connecting and Installing the Flowcell 2 9 Powering On for the First Time 2 11 Connecting the Remote Communications Outputs 2 11 Setting the Output Polarities From ChromQuest 2 12 Setting the Output Polarities From Atlas 2 12 Calibrating the UV6000LP 2 13 Operation Verification 2 13 Specifications 2 14 UV...

Страница 6: ...ight Intensity From Chromquest 4 19 Reloading the Firmware 4 20 Chromquest and HyperTerminal 4 20 Atlas and the EXE960 exe Utility 4 22 Operation Re verification 4 23 Diagnostics 5 1 Introduction 5 1 The Diagnostics Program in ChromQuest 5 1 Accessing the Diagnostics Program 5 1 The Lamps Page 5 2 The Control Page 5 4 The display Page 5 8 Using Control and Display Pages 5 12 The Error Log Page 5 1...

Страница 7: ... 4 Log Entries 6 4 Warning Messages 6 4 Critical Error Messages 6 6 Crash Error Messages 6 7 Technical Assistance with Error Log Messages 6 8 Accessories and Replacement Parts 7 1 Field Service Repair Procedures 8 1 Introduction 8 1 Tools Required 8 1 Removing and Replacing UV6000LP Detector Assemblies 8 4 Index ...

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Страница 9: ... Phone 1 770 516 5589 Fax 1 770 516 6916 Central Region Phone 1 847 310 0140 Fax 1 847 310 0145 Western Region Phone 1 408 965 6000 Fax 1 408 965 6123 Canada Phone 1 905 712 2258 Fax 1 905 712 4203 In the Americas use the following telephone number or fax number to order parts for all instruments Thermo Electron Customer Service Operations 1400 Northpoint Parkway Suite 10 West Palm Beach FL 33407 ...

Страница 10: ...92 48 00 Fax 33 01 60 92 49 00 Dreieich Germany Phone 49 06103 408 0 Fax 49 06103 408 1222 Milano Italy Phone 39 02 95 059 226 Fax 39 02 95 320 370 Breda Netherlands Phone 31 076 587 8722 Fax 31 076 571 4171 Madrid Spain Phone 34 091 657 4930 Fax 34 091 657 4937 Barcelona Spain Phone 34 093 223 0918 Fax 34 093 223 0982 Stockholm Sweden Phone 46 08 556 468 00 Fax 46 08 556 468 08 Hemel Hempstead Un...

Страница 11: ...of the Thermo Electron offices as follows Rydalmere N S W Australia Phone 61 02 9898 9000 Fax 61 02 9898 9800 Yokohama Japan Phone 81 45 453 9100 Fax 81 06 453 9110 Osaka Japan Phone 81 06 6387 6681 Fax 81 06 6387 6641 Beijing P R China Phone 86 010 6621 0839 Fax 86 010 6621 0851 For all other countries contact your local Thermo Electron San Jose products dealer ...

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Страница 13: ...roperly followed All statements of this nature are called to your attention through the use of bold type and the following icons CAUTION HOT SURFACE HIGH VOLTAGE Every instrument has specific hazards so be sure to read and comply with the following precautions They will help ensure the safe long term use of your system 1 Before plugging in any of the instrument modules or turning on the power alwa...

Страница 14: ...type of maintenance 9 Capacitors inside the instrument may still be charged even if the instrument is turned off 10 Never try to repair or replace any component of the system that is not described in this manual without the assistance of your service representative GOOD LABORATORY PRACTICES Keep Good Records To help identify and isolate problems with either your equipment or your methodology we re...

Страница 15: ...obile phase that s compatible with the sample and column you ve selected for your separation Remember that some solvents are corrosive to stainless steel Inert biocompatible versions of instruments are also available from Thermo Electron Degas the Eluents Degas your eluent solvents using either the vacuum degassing or the helium sparging technique A complete description of these techniques is foun...

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Страница 17: ...IDENTIFICATION DES INFORMATIONS SUR LA SÉCURITÉ Ce manuel de référence contient des précautions d usage afin de prévenir tout dommage corporel ou matériel ainsi que toute perte de données lorsque l opérateur se conforme aux instructions indiquées Ces instructions sont accompagnées des icônes suivantes et sont affichées en caractères gras pour attirer l attention de l opérateur MISE EN GARDE SURFAC...

Страница 18: ...e système montre des signes visibles d endommagement ou si les conditions de transport ont été extrêmement difficiles 7 L instrument peut également être endommagé s il est entreposé pendant une période de temps prolongée dans de mauvaises conditions par exemple s il est exposé à la chaleur à l humidité etc 8 Toujours débrancher le cordon d alimentation avant d effectuer n importe quel type d entre...

Страница 19: ... Un grand nombre de fabricants de produits chimiques fournissent des réactifs de pureté élevée ou de qualité spectrographique dépourvue de toute impureté chimique La filtration systématique de tous les solvants ou éluants à travers un filtre fluorocarboné de 0 45 ou 0 2 µm ou moins avant de les placer dans le réservoir de solvants prolonge de façon significative la durée de vie et l efficacité des...

Страница 20: ...tés d énergie car ils ne sont pas hautement compressibles Par conséquent le risque d un danger immédiat causé par les pressions élevées dans un système CL est faible En revanche si une fuite survient il est nécessaire de la réparer le plus rapidement possible Enfin il est recommandé à l opérateur de se protéger en permanence les yeux et la peau lorsqu il travaille sur un système CL De plus il doit...

Страница 21: ...N Dieses Handbuch enthält Warnhinweise deren genaue Befolgung Personenschäden Schäden am Gerät oder Datenverluste verhindern kann Auf alle derartigen Warnhinweise wird durch Fettschrift und durch Verwendung der nachfolgenden Symbole gesondert aufmerksam gemacht VORSICHT OBERFLÄCHE HEISS HOCHSPAN NUNG Jedes Gerät kann unter bestimmten Umständen gefährlich sein Lesen Sie daher in jedem Fall die nach...

Страница 22: ...zu dieser Untersuchung keinesfalls das Gerät in Betrieb zu nehmen Eine Beschädigung der Elektrik kann z B eingetreten sein wenn das Gerät äußere Schäden aufweist oder unter problematischen Umständen transportiert wurde 7 Schäden können auch eintreten wenn das Gerät längere Zeit unter ungünstigen Umständen gelagert wurde z B unter der Einwirkung von Hitze oder Wasser 8 Ziehen Sie vor allen Wartungs...

Страница 23: ...ß hemmen Durch eine solche Verstopfung können irreparable Schäden am System entstehen Die Ablagerung von Partikeln läßt sich durch Filtrieren der Proben durch ein Filter mit einer Porengröße von 0 45 oder 0 2 µm oder weniger vermeiden Anforderungen an das Lösungsmittel Viele chemische Hersteller bieten eine Produktserie hochreiner Reagenzien in spektroskopisch reiner Qualität an die frei von chemi...

Страница 24: ... die einschlägigen Vorschriften streng zu beachten Hochdrucksysteme und Undichtigkeiten Flüssigchromatographen arbeiten unter hohem Druck Da Flüssigkeiten kaum komprimierbar sind können sie nicht viel Energie speichern Dementsprechend stellt der hohe Druck in einem Flüssigchromatographen auch kaum eine unmittelbare Gefahr dar Jedoch sollten auftretende Undichtigkeiten umgehend beseitigt werden Sch...

Страница 25: ... chapter Refer to the ChromQuest Software User s Guide or the Atlas SpectraSYSTEM Control manual for software operating procedures Manual Organization This manual is organized as follows Technical Assistance and Product Support Lists all of the phone numbers you will need for technical assistance service product support and ordering parts and accessories Safety Information Contains a statement of ...

Страница 26: ...on part numbers Chapter 8 Field Service Procedures provides detailed instructions for factory trained service personnel to perform field repairs UV6000LP Functional Description This brief functional description of the UV6000LP is included to assist you with troubleshooting potential problems and performing routine maintenance on your detector For more detailed information contact your Thermo Elect...

Страница 27: ...V6000LP optical system The light focused on the inlet window of the flowcell travels down the cell is partially absorbed by the sample flowing through the cell and exits into the beam shaper The beam shaper is a fiber bundle Its entrance aperture is circular to collect light from the flowcell The other end of the bundle is arranged to produce a narrow slit of light for the grating The beam shaper ...

Страница 28: ...PCBA As the data points are stored through one RAM port the CPU reads the data it needs based on user parameters entered through the software through the other RAM port processes the data and sends it to the personal computer The CPU PCBA also processes remote inputs and outputs through the Transition PCBA which functions as a rear panel A dual 20 bit digital to analog converter on the CPU PCBA pr...

Страница 29: ... Perform the installation in the sequence presented on the Installation Checklist and detailed in this chapter Unpacking Carefully remove the detector from the shipping container and inspect both the detector and packing for any signs of damage If you find any damage save the shipping materials and immediately contact the shipping company The shipping container should contain the detector an acces...

Страница 30: ...ake initial rear panel connections pg 2 5 Connect and install the flowcell pg 2 9 Connect the power cord and turn on the instrument pg 2 11 Install appropriate software on the connecting PC software manual Download the firmware if required pg 4 20 Adjust the sense of the remote communications outputs using the UV6000LP Diagnostics program in ChromQuest or Atlas if required pg 2 11 Calibrate the de...

Страница 31: ...ay from an opened window air conditioner vents or other circulating air source A stable room temperature is necessary for applications requiring maximum detection sensitivity Allow at least five inches 13 cm of clear space between the detector s rear panel and any wall or obstruction This provides access to the rear panel connectors and a free flow of cooling air You will need the following tools ...

Страница 32: ...odule located at the lower right on the detector s rear panel Figure 2 1 Use the following procedure to check the fuses and change the voltage setting if necessary NOTE Locations with 230V electrical power service may select a detector voltage setting of 220V or 240V for proper operation Voltage Selector Fuse Holder Fuses Fuse Holder Release Tab PD Z002E ST Figure 2 1 Selecting the proper voltage ...

Страница 33: ... yet Wait until the Power On section of this chapter Making Initial Rear Panel Connections Use the cables supplied with your detector to make the connections described in this section see Figure 2 2 For each connection insert the cable s bare wire into the appropriate detector terminal Hold the wire in place while you tighten the small terminal set screw firmly onto the wire P D Z003E 1 2 3 4 5 6 ...

Страница 34: ... to any earth ground on your data system This would lead to an increased noise level and a subsequent decrease in sensitivity The data system should have a floating ground input Typically the positive and negative data system inputs are connected to the and terminals of the detector respectively The ch1 and ch2 output terminals of the detector are isolated from chassis ground and the ground termin...

Страница 35: ...o 6 for ch 2 For each channel only the switch corresponding to the desired range should be up ON The other two switches for that channel should be down OFF Normally the full scale voltage should match the data system input span Figure 2 3 shows both channels set to 1000 mV 1 and 4 on 2 3 5 and 6 off NOTE If more than one switch for a given channel is set to the up ON position the instrument will n...

Страница 36: ...f the COM terminals on the rear of the detector are tied to a single digital ground or return line You can use any COM terminal for any digital input or output signal return connection Zero The ZERO connection on the rear panel is used to zero the detector from a remote source generally at the start or end of each sample run It can be triggered from a remote device by either a TTL low signal or a ...

Страница 37: ...re 2 4 Detector with front panel removed The flowcell is packed in a small separate box within the detector shipping carton This small box contains the flowcell with protective caps on each end and a plastic bag containing the inlet and outlet tubing and finger tight fittings Unpack the flowcell and install it as follows 1 Remove the front cover of the detector by pulling out at the bottom edge an...

Страница 38: ...end NOTE The inlet tube is 005 I D and colored red with an external Teflon sheath The outlet tube for the flowcell is 010 I D and colored blue 4 Place the detector s outlet line in the waste reservoir When using an optional backpressure regulator P N 802259 connect the oulet line to the low pressure union and waste tubing HINT If you have several detectors fluorescence refractive index electrochem...

Страница 39: ...ngage it in position Note that the power indicator briefly lights red and then turns solid green If it does not light at all refer to the troubleshooting chart on page 6 3 If it stays red or flashes red or green turn power off for several seconds and then back on again If the indicator comes on as a flashing rather than a solid green light the firmware must be downloaded Refer to Reloading the Fir...

Страница 40: ...ght click in the UV6000 Instrument Status page Then select Diagnostics from the pop up menu 6 Click the Control tab to display the Control page SETTING THE OUTPUT POLARITIES FROM ATLAS To set the output polarities from Atlas do the following 1 From the Windows taskbar open the Instrument Manager by selecting Start Programs or All Programs Atlas Instrument Manager 2 Right click on the icon that rep...

Страница 41: ...and jars which might occur in shipping and during the installation process can affect this alignment Easy calibration procedures are included in the UV6000LP Diagnostics section Refer to Chapter 5 for information on performing the wavelength and dark current calibration procedures Operation Verification Once the detector has been successfully installed refer to Operation Verification in Chapter 4 ...

Страница 42: ...Warm up 1 5 hour Linearity 2 0 AU 257 nm Scan Rate 20 Hz Data Rate Settings 0 5 to 20 Hz Cell Pathlength 50 mm Cell Volume 10 µL Cell Pressure 1200 psi Diodes 512 Diode Spacing 1 2 nm Rise Time 0 0 to 10 0 seconds Light Source Deuterium and tungsten halogen lamps pre aligned According to ASTM E1657 94 Standard Practice for Testing Variable Wavelength Photometric Detectors Used in Liquid Chromatogr...

Страница 43: ...ettes with different concentrations of potassium dichromate in perchloric acid NIST traceable Analog Outputs 2 20 bit unattenuated at 10 mV 100 mV or 1 0 V per AU Remote Controls Start Zero RJ45 serial interface to ChromQuest or Atlas Dimensions 20 cm 35 cm 43 cm H W D Weight 15 kg Power Requirements 100 120 220 240 Vac 50 to 60 Hz 200 VA max Operating Temperature 10 to 40 ºC Storage Temperature 4...

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Страница 45: ...re is properly installed and that you have created a system configuration as described in the appropriate software reference manual LC System Setup In order to perform this quick start procedure you will need one ampule of the Thermo Electron LC Test Mix 75 methanol and 25 water as the mobile phase and a Hypersil C8 column If required you can substitute other samples solvents and columns that are ...

Страница 46: ...the chromatographic method for running the Thermo Electron LC Test Mix with the Microsoft Windows NT 2000 XP based ChromQuest software Click on the Windows taskbar Start button and move the cursor up the menu to Programs Click on the ChromQuest icon located in the Chromatography program group Select the appropriate system icon from the ChromQuest main menu window The default ChromQuest windows wil...

Страница 47: ...Run Time 5 min Rise Time 2 sec Collect Scans checked Min Wavelength 220 nm Scan Rate 1 Hz Max Wavelength 500 nm Bandwidth 1 nm Step 1 nm Discrete Channels Three Wavelength A 254 nm Bandwidth A 7 nm Wavelength B 430 nm Bandwidth B 7 nm Wavelength C 220 nm Bandwidth C 7 nm Scan Rate 10 Hz ...

Страница 48: ...o collect the complete spectrum of tartrazine which is the compound that gives the LC Test Mix its yellow color Tartrazine has a wavelength maximum at approximately 430 nm The bandwidth setting for the scan data is 1 nm for optimal spectral resolution The discrete channels are set to monitor at 254 430 and 220 nm with a bandwidth setting of 7 nm and a sample rate of 10 Hz To increase spectral reso...

Страница 49: ...starts If scan data is collected individual chromatograms at other wavelengths can be viewed after the run CUSTOM REPORT The ChromQuest Custom Reporting feature allows the analytical chemist to consolidate test results into a single report with a maximum amount of flexibility To simplify the process Thermo Electron has included four of the most common report formats as report templates Additional ...

Страница 50: ...selected by clicking on File Print from the Menu bar If the correct printer is selected click on the Cancel button PREVIEW Verify that the system is fully equilibrated by monitoring the baseline before the sample is injected To monitor the baseline click on the Preview button on the Command Toolbar at the top of the Applications Window The baseline is displayed in real time for all signals configu...

Страница 51: ... box Data file LCTestMix Vial A01 Injection volume 10 µl Select the Print Method Report check box Other fields can be left blank or at their default settings Figure 3 5 Starting a Single Analysis When the sample is injected the chromatogram s will be displayed in real time If the chromatograms for the UV6000LP are not displayed verify that there is a run start connection between the autosampler an...

Страница 52: ...Results for LC Test Mix Injection Amount ng Compound Ret Time min UV1000 Peak Area UV6000 Peak Area 60 Tartrazine 0 61 150908 723005 20 Acetophenone 1 48 23336 119167 1000 Toluene 2 07 103254 526428 5 Anthracene 3 60 139472 688661 VIEW REPORT In addition to viewing the analysis on screen in the discrete wavelength windows and the spectral analysis window the complete LC Test Mix analysis is printe...

Страница 53: ...nge for a preventive maintenance program please contact your local Thermo Electron representative Recommendations Table 4 1 lists recommendations for routine maintenance of the UV6000LP Detector Use the table as a basis for developing your maintenance program in accordance with your company s practices Table 4 1 Recommended Routine Maintenance Procedure Interval Flowcell Cleaning After each applic...

Страница 54: ...cleaning of your detector s flowcell For other flowcell problems such as a cracked window or leaks that occur in locations other than at the inlet outlet fittings contact your Thermo Electron representative NOTE Flowcells are factory assembled units that should not be disassembled under any circumstance REMOVING THE FLOWCELL The flowcell must be removed to clean it To access the flowcell do the fo...

Страница 55: ...e flowcell windows If dirty the window surface should be cleaned only with spectroscopic grade methanol or isopropanol and lint free lens paper 6 Carefully pull the assembly toward you to remove it from the detector CLEANING THE FLOWCELL The exterior and or interior surfaces of the flowcell can become contaminated Flowcell contamination is usually caused by precipitation or solubility problems suc...

Страница 56: ...ater methanol or isopropanol You should pump the solvent through the flowcell with the chromatographic pump 3 When using an LC pump to flush the flowcell first remove the column from your chromatographic system to avoid column degradation Replace the column with an appropriate length of tubing ensuring that all connections are snug and leak free If you use a syringe always draw the solution throug...

Страница 57: ...olvents pump another 25 to 40 mL of water through the flowcell to remove all traces of nitric acid The pH of the outlet stream of the flowcell can be monitored to ensure that all of the acid has been completely flushed out 7 Reinstall the flowcell assembly INSTALLING THE FLOWCELL To install the flowcell do the following 1 Connect the inlet and outlet tubing to the flowcell 2 With the inlet tube on...

Страница 58: ...e following operation verification procedure uses the UV6000LP diagnostics suite described in Chapter 5 to verify the operation of the detector You should become familiar with the diagnostics portion of the relevant software before attempting this verification Because the UV6000LP can be used with either ChromQuest or Atlas we have included operation verification procedures for both software platf...

Страница 59: ...ftware will not initiate an analysis if the filter wheel is not in position 1 10 After both lamps have warmed up for 1 hour perform a dark current calibration and a wavelength calibration as specified in Chapter 5 Use the wavelength calibration file appropriate for your normal operation Don t forget to apply the results by clicking on the Apply button 11 Turn the tungsten halogen W lamp off 12 Aft...

Страница 60: ...o the Control page and changes the individual channels to monitor pixels 94 177 and 260 16 Go to the Display page and once again click on the Status On and Data Start buttons See Figure 4 3 Use the Print Screen key to print out a copy of the scan This scan should also be kept for future comparisons to see if there is any intensity degradation Date the printout and add it to your maintenance record...

Страница 61: ...th W Lamp 17 Turn the deuterium D2 lamp off 18 Repeat the above steps to display the emission intensity spectrum of the tungsten halogen W lamp See Figure 4 4 Set the individual channels to monitor pixels 219 302 and 427 Figure 4 4 Intensity scan with both lamps ...

Страница 62: ... your instrument by double clicking on its icon c From the bank of tabs located at the bottom of the Instrument Status window click on the Detector tab d Click on the Maintenance tab at the top of the window to display the Maintenance page 2 Check each lamps status and usage 3 If they are not already on turn on both lamps by selecting their respective Lamp On checkboxes NOTE Atlas software will no...

Страница 63: ... Operation in Atlas version 2003 R2 7 Select the Diode Number Intensity option button 6 Set the individual channels to monitor diodes 35 52 and 77 Then click on the Start button 7 Return to the Maintenance page and turn the tungsten halogen W lamp on 8 Return to the Display page and set the individual channels to monitor diodes 94 177 and 260 Then click on the Start button ...

Страница 64: ...f the Tungsten W lamp alone 10 Return to the Display page and set the individual channels to monitor diodes 219 302 and 427 11 Return to the Maintenance page and turn the deuterium D2 lamp on again Exit the Instrument Manager application and allow sufficient warm up time before acquiring data Figure 4 6 UV6000 Instrument Status Display page Atlas 2003 R1 ...

Страница 65: ...detector chassis open as shown in Figure 4 5 To access the deuterium and tungsten halogen lamps 1 Turn the power switch at the front of the detector to off released position and disconnect the power cord from the rear panel 2 Remove the front cover by gently pulling out on the bottom of the cover and lifting up 3 Remove the LightPipe assembly and secure its location CAUTION Intense UV light can da...

Страница 66: ... 4 8 Detector with Front Panel Removed Figure 4 9 Accessing Lamp Assembly Enclosure retaining screws recessed Detector case Lamp compartment cover Chassis Lamp cover Front chassis attenuators some models Internal chassis attenuators some models ...

Страница 67: ...s and connectors behind the lamps attached to the lamp power supply board The larger connector is for the deuterium lamp 3 leads and the smaller connector is for the tungsten halogen lamp 2 leads NOTE Some models of the UV6000LP have a captive Philips head screw instead of the knurled black knob Figure 4 10 Removing the Lamp Cover NOTE Do not try to remove the lamps from their mounting assemblies ...

Страница 68: ... users on page 5 29 Adjusting Attenuators During the lifetime of the UV6000LP it may be necessary to manually adjust the attenuators in order to increase the amount of light falling upon the array or to decrease the light levels to prevent saturation of the array For optimal performance the light intensity values should fall within the following ranges in the region where analyses will be performe...

Страница 69: ... from the right side of the instrument 5 Free the lamp compartment cover from the detector chassis by pressing on the metal tab inside the chassis wall 6 Remove the foam insulation located on top of the optical bench assembly 7 Loosen the attenuator locking screw which is a small Phillips head screw located in the center of the internal metal wall separating the optical bench from the lamp compart...

Страница 70: ...Number Intensity option button Then verify the following settings Spectrum Start Diode 2 Spectrum Stop Diode 511 Channel A Diode 40 Channel B Diode 55 Channel C Diode 450 7 Click on the Start button 8 Adjust the attenuator with the longer black tab left tab for front chassis attenuators UV attenuation to achieve the following Channel A values Units with S N 106000 to 107999 640 000 to 660 000 Unit...

Страница 71: ...sage box will appear Click on OK 7 Go to the Status page and click on both green buttons Status On and Data On 8 Adjust the attenuator with the longer black tab left tab for front chassis attentuators UV attentuation to achieve the following Channel A values Units with S N 106000 to 107999 640 000 to 660 000 Units with S N 109000 and higher 780 000 to 800 000 9 Adjust the attenuator with the short...

Страница 72: ...HYPERTERMINAL The Windows NT 2000 XP HyperTerminal utility is a program that allows you to transfer files from one computer to another In this case you will be transferring a firmware file that is supplied with your chromatography data system to the CPU board in the UV6000 detector The firmware file for the CPU of your UV6000 detector is the PDA cof file You can find the PDA cof file on the ChromQ...

Страница 73: ...the computer monitor You will see a symbol every time you press Enter 4 Initiate the download process a At the last prompt type the following download command do for download b Then press Enter The system will echo back information a series of squares from the UV6000LP Immediately proceed with the next step otherwise an error message will appear Download failed communication error c Immediately st...

Страница 74: ...munication conflicts by way of the COM port 4 Turn on the UV6000LP detector 5 Insert the Atlas installation CD ROM into the CD drive on the data system computer 6 Open the Command Line window For Windows NT or Windows 2000 click on the Windows taskbar Start button and go to Programs Accessories Command Prompt For Windows XP click on the Windows taskbar Start button and go to All Programs Accessori...

Страница 75: ...two minutes 9 After the file is downloaded turn the UV6000LP detector off Reconnect it for normal use Then turn it back on Operation Re verification Once you have completed diagnostics or maintenance procedures repeat the Operation Verification procedures on page 4 6 ...

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Страница 77: ... UV6000LP diagnostics program during an analysis The Diagnostics Program in ChromQuest To use the UV6000LP diagnostics software the detector must be powered on and its RS232 port connected to a serial port on the data system computer From the Diagnostics dialog box in ChromQuest you can do the following Check lamp status and usage View lamp intensity or absorbance spectra Test the digital inputs a...

Страница 78: ...e displayed Figure 5 1 Figure 5 1 The Diagnostics dialog box Note that there are five diagnostic areas organized into pages with tabs across the top for ease of selection The pages are Lamps Control Display Error Log and Calibration The tabs at the top of each page can be used to quickly move from page to page Each time you open the diagnostics program it automatically defaults to the Lamp page TH...

Страница 79: ...on the application When you press either Reset button the stored total run time for the associated lamp is reset to zero and the Last Reset field is updated to the current date and time After you replace a lamp press the Reset button The lamp buttons also provide on off control When you turn on the deuterium lamp its Status field reads Starting during the 30 second ignition period and then changes...

Страница 80: ...default settings for operation in the Absorbance mode Figure 5 4 shows the default settings for the Intensity mode Figure 5 3 The Control Page Absorbance Mode Mode Group The Mode group contains two radio buttons for selecting either intensity mode or absorbance mode In the absorbance mode see Figure 5 5 the following apply A bandwidth filter is used in the wavelength axis A rise time filter is use...

Страница 81: ...ge Intensity Mode There are 512 photodiodes in the detector s array The first two diodes 0 and 1 are not used Diode 2 is at 190 nm and diode 511 is at 800 nm when the detector is properly calibrated This gives a diode spacing of 611 nm 509 diodes 1 2 nm diode In the absorbance mode the detector interpolates between diodes to store absorbance at integer wavelengths Filter Group The Rise Time field ...

Страница 82: ...d 5V or the LED should light when the output is ON and its Sense is Low or the output is OFF and its Sense is High Remember that you are changing the sense of the return line not the 5V To toggle the remote outputs first select Instrument Status from the Control drop down menu Right click anywhere in the Instrument Status window and select Output from the pop up menu The remote outputs will then a...

Страница 83: ...Bandwidth values conflict an error message will automatically be displayed when they are downloaded to the detector Scan Rate Enter the scan rate in this field The acceptable values are 0 5 1 2 4 5 10 and 20 Hz with 2 Hz being the default for absorbance and 1 Hz for intensity NOTE The actual scanning of the diode array occurs at a fixed 20 Hz rate When you select slower scan rates and or increment...

Страница 84: ...to the limits than the Bandwidth value 1 2 HINT Enter a wider bandwidth to improve signal to noise ratio Default Get and Load Buttons The Default button sets all parameters to the default values applicable to the specified mode The Get From Detector button uploads and displays the parameters currently stored in the detector The Load To Detector button downloads the currently displayed parameters t...

Страница 85: ...ot ROM the firmware stored in battery backed up RAM and the I O Input Output driver After the Status On and Data Start buttons are clicked the diagnostics software reads and displays the current version numbers from the detector Lamps Group The D2 and W Lamp fields indicate the status of the lamps Starting On Off Dim or Failed The amount of time that each lamp has been used is also displayed Discr...

Страница 86: ... Status On button initiates a continuous update of the status fields The Status Off button stops the continuous update and freezes the status information in the fields Data Buttons Group The Data button group affects both scan and chromatogram plots The Data Start button turns the data on and begins a real time update of the spectral scan and the chromatogram plots for the channels selected on the...

Страница 87: ...range is displayed The Scan display is updated every few seconds By clicking the right mouse button and selecting Properties from the pop up menu you can adjust the display s wavelength axis and also set the minimum and maximum Counts or mAU for the respective intensity or absorbance axis The Scan display color scheme can also be adjusted from the Properties box Discrete Channel Display The Discre...

Страница 88: ...is as follows 1 Specify the parameters listed in the Control page and download them to the detector 2 Go to the Display page and click the Status On button 3 Verify that the detector Status field reads READY 4 When the detector is ready click the Data On button to begin data collection and view the results 5 Adjust the display parameters as desired 6 To change parameters turn the data off on the D...

Страница 89: ...sition 1 click the Zero button The absorbance spectrum upper display should now be a relatively flat line and the chromatogram display lower display will be monitoring the detector baseline at the three wavelengths that were specified on the Control page The mAU readings for the three discrete wavelengths are displayed in the top center section of the Display page Figure 5 7 Notice when the filter...

Страница 90: ...ecessary to turn data collection off before you rotate the wheel Once the wheel is in position 2 the holmium oxide absorbance spectra will be displayed as shown in Figure 5 8 Notice that the status indicator for the filter wheel now reads Off because the filter wheel is no longer in position 1 After inspecting the holmium oxide spectrum be sure to return the filter wheel to the open position posit...

Страница 91: ...January 2004 Thermo Electron 5 15 Figure 5 8 Holmium oxide absorbance spectrum ...

Страница 92: ...ng the on a weekly basis When you first open the Error Log page the event area will be blank Click on the Get button to retrieve the information from the detector and display it Figure 5 9 shows a sample log Figure 5 9 The Error Log page Note that the viewing area has horizontal and vertical scroll bars so you can view all of the entries Press the Print button to print a copy of the displayed log ...

Страница 93: ...lues can be converted to absorbance units the dark current must be subtracted from the intensity measurements Following dark current calibration light intensity values will be automatically corrected for dark current Remember that both lamps must be turned on during calibration NOTE Neither calibration program will run when data collection is enabled on the Display page HINT Be sure to check light...

Страница 94: ...cessary pre conditions 5 If all of the pre conditions have been met press the OK button Figure 5 11 Dark Current Calibration Start As the calibration proceeds its status is shown in the status group at the bottom of the page During the dark current calibration intensity scans are collected under four sets of conditions with both lamps on D2 lamp only on W lamp only on and both lamps off After the ...

Страница 95: ...y is dependent upon the physical alignment of various components of the optical bench and can become off set if the detector is sharply jolted for example in shipping PERFORMING A WAVELENGTH CALIBRATION To perform a wavelength calibration proceed as follows 1 Turn on both lamps and wait 1 hour for the deuterium D2 lamp to warm up 2 Pump water at 1 mL minute through the flowcell 3 Place the filter ...

Страница 96: ...dified using a text editor program to create a calibration file for a specific compound of interest Figure 5 14 Select Wavelength Calibration File The expected holmium oxide absorbance maxima are selected from a spectrum published in the ASTM Method E275 83 Standard Practice for Describing and Measuring Performance of Ultraviolet Visible and Near Infrared Spectrophotometers 5 Double click on the d...

Страница 97: ...f the pre conditions steps 1 2 and 3 Figure 5 16 Wavelength Calibration Pre conditions 8 If all preconditions are met press the OK button in the info box A background spectrum is now collected It is used to remove the mobile phase absorbance contribution The status box at the bottom of the page will display various pieces of information describing the calibration process ...

Страница 98: ...lmium oxide scan and then displays a new info box as shown in Figure 5 18 Figure 5 18 Wavelength Calibration Complete 10 Click on the OK button Figure 5 18 to close the info box and view the results as shown in Figure 5 19 All of the Delta values should be less than or equal to 1 nm If the Delta values exceed 1 nm click on the Apply button and repeat the wavelength calibration for verification If ...

Страница 99: ...on page can be pressed at any time a calibration is in process to abort it The Reset button calls up default calibration values The Atlas Instrument Manager The Atlas Instrument Manager lets you check the operation of the UV6000LP calibrate the detector and view the error log From the UV6000 Instrument Status window of the Instrument Manager you can do the following Check lamp status and usage Vie...

Страница 100: ...ee pages that are accessed by clicking on their respective tabs The pages are Operation labeled as Display in Atlas 2003 R1 Maintenance and Error Log STATUS The status section of the UV6000 Instrument Status window contains five group boxes Status Lamps Channel A Channel B and Channel C Status Group Box Device State The Device State read back displays the status of the UV6000 detector The possible...

Страница 101: ...rium lamp D2 The possible states are On Starting Off Failed or Unknown The deuterium lamp takes approximately 30 seconds to ignite and approximately 60 minutes to warm up The Tungsten State read back displays the status of the tungsten lamp W The possible states are On Starting Off Failed or Unknown Channel A B C The status for the discrete wavelength channels can be displayed in either the absorb...

Страница 102: ... option button allows you to display the absorbance values for up to 3 discrete wavelengths and a scan range as wide as 190 nm to 800 nm Intensity Option Button The Intensity option button allows you to display the intensity counts for up to 3 diode numbers and a scan range as wide as diode number 2 to diode number 511 Spectrum Start Text Box The Spectrum Start text box allows you to specify the b...

Страница 103: ... nm to 800 nm or a diode number from 2 to 511 Start Button Clicking on the Start button starts the collection and display of data from the detector Stop Button Clicking on the Stop button ends the collection of data Zero Button Clicking on the Zero button clears the displays and empties the data buffers of the detector THE MAINTENANCE PAGE The Maintenance page allows you to turn the lamps on and o...

Страница 104: ...for information on downloading a PDA cof file Ready Output State Turn On Button Click on this button to turn on the Ready Output state The Polarity of the Ready Output is set when the UV6000 detector is configured using the Add Instrument Wizard Turn Off Button Click on this button to turn off the Ready Output state Event Output State Turn On Button Click on this button to turn on the Event Output...

Страница 105: ... after you install a new deuterium lamp The maximum lifetime of the deuterium lamp is typically 2000 hours In general as the hours of usage increases the baseline noise increases Reset Button After you replace the deuterium lamp click on this button to reset the time clock to zero Tungsten Lamp Lamp On Select this checkbox to turn on the Tungsten lamp and deselect this checkbox to turn off the Tun...

Страница 106: ...ayed in the Log window A maximum of 100 messages is retained by the error log Once this number is reached the older messages are overwritten by the new ones Messages accrued during the run are copied to the Workbook instrument log file when the run has finished Click on Get Error Log button to download the error log messages from the detector Click on the Clear Error Log button to clear the error ...

Страница 107: ...lowing steps Checking lamp states Retrieving current method Retrieving current calibration Downloading calibration method The Next button is not active until these steps are complete Click on the Next button to proceed to the fourth page of the wizard 6 In the fourth page of the wizard you are instructed to turn the filter wheel of the UV6000 detector to position 2 The Next button is not active un...

Страница 108: ...t that is compensated for by performing an array calibration is a function of temperature 2 In the Array Calibration group box click on the New Calibration button to launch the Array Calibration wizard 3 In the first page of the wizard click on the Next button to proceed 4 In the second page of the wizard the following steps are performed as indicated Checking lamp states Retrieving current calibr...

Страница 109: ... types of problems Troubleshooting Table Symptom Cause Remedy 1 Spikes on baseline a Continuous gas bubbles in the flowcell a Degas mobile phase Connect back pressure device to flowcell check back pressure rating b Immiscible solvent bubbles following mobile phase changeover b Flush flowcell with 2 propanol then with mobile phase c Electrical interference c Check electrical lines for good connecti...

Страница 110: ...ivity f Lamp aging or defective f Replace lamp g Ground loop problem between integrator and detector g Check for proper cable connections for detector output do not ground at both ends of cable h Flowcell or lamps dirty h Clean dirty component as described in Chapter 3 i Integrator input voltage does not match detector output voltage i Connect integrator to appropriate output connectors on detecto...

Страница 111: ...voltage does not match detector output voltage c Connect integrator to appropriate output connectors on detector Check attenuation setting on integrator d Insufficient sample reaching the detector d Check entire chromatographic system for leaks Verify sample injection volume 5 Broad tailing peaks a Rise time is too large too slow a Lower the rise time selection b Poor connection at flowcell inlet ...

Страница 112: ...quired Error Messages For information on error messages that occur as part of the UV6000LP diagnostics program refer to the Log Entries section below Log Entries The diagnostics Error Log page chronologically records messages relating to detector system problems There are three categories of messages Warning messages Critical Error messages and Crash Error messages WARNING MESSAGES Warning message...

Страница 113: ...xit and reconnect In some cases you may have to cycle power on the detector Attach Could not negotiate baud rate with UV6000LP You may have to exit and reconnect In some cases you may cycle power on the detector Attach No response to version query was received for UV6000LP ROM You may have to exit and reconnect In some cases you may have to cycle power on the detector Attach No response to version...

Страница 114: ...ossible Critical Error messages include PM Attach has failed There may be an existing connection PM Queue creation failed exceeded maximum values PM The UV6000LP is running out of internal buffers Most probable cause data rate too high Injection will be aborted to prevent message depletion PM Could not write to a queue You should probably exit the software and or cycle the power on the UV6000LP to...

Страница 115: ...ensure future data integrity Init Exceeded number of allowed Link Layers You may have tried to connect to two different com ports in one session Exit and retry Init Creation of Physical Layer failed Make sure the com port exists and is available Init Could not create Transmit queue Please exit the application and retry Init Could not register Transmit Queue Please exit the application and retry In...

Страница 116: ...to exit and reconnect In some cases you may have to cycle power on the detector Read Could not allocate PM message buffer The UV6000LP will be unable to start TECHNICAL ASSISTANCE WITH ERROR LOG MESSAGES For further information document the log entry and contact Thermo Electron Technical Support ...

Страница 117: ...let tubing w insulation PEEK 1 16 x 005 I D Red 703950 Outlet tubing PEEK 1 16 x 010 I D Blue 803237 01 Flowcell Assembly w inlet outlet tubing fittings 126078 Fuse T 3 15A 5 x 20 mm for 100 120V operation 126079 Fuse T 1 6A 5 x 20 mm for 220 240V operation 803113 External Run Auto Zero Analog Signal Cables A3598 030 RJ 45 cable A3538 010 9 pin to RJ 45 adapter 106012 TL 5242 W Tadrian Lithium mem...

Страница 118: ......

Страница 119: ...pting repairs with the instrument turned on or connected to an AC power supply could result in serious injury NOTE Some components in the detector can be damaged by static electricity Before beginning any of the following procedures prepare a non conductive work surface for the detector and put on a properly grounded anti static wrist strap Tools Required Except where noted detector field service ...

Страница 120: ...f the UV6000LP detector are identified in Figure 8 1 and include the CPU PCBA Printed Circuit Board Assembly the transition PCBA the lamp power supply PCBA the lamp power supply input transformer the low voltage power supply the power entry module assembly the LED assembly the cooling fan assembly various connector cables ...

Страница 121: ...004 Thermo Electron 8 3 Power Entry Module CPU PCBA Lamp Supply Transformer Fan Transition PCBA LowVoltage Power Supply Assy Lamp Power Supply PCBA Lamp Assembly Figure 8 1 Replaceable Assemblies and Components ...

Страница 122: ... cover and lifting up 3 Loosen the two captive 3 16 Phillips head screws that secure the chassis to the detector housing These screws are in a recessed location in the base of the detector Figure 8 2 The screws are spring loaded and will be retained when loosened 4 Slide the chassis out of the detector and place it on a non conductive work surface Enclosure Retaining Screws Recessed Power On LED P...

Страница 123: ...ining clips prior to removing 2 Using the flat of a small screwdriver blade gently push the two black snap latches free from their sockets at the top corners of the PCBA 3 Lift the PCBA out of the chassis PD Z110E JP16 to Array Acq PCBA JP7 to Front Panel LED JP10 to Filter Wheel Sensor JP1 to Main Power Supply PCBA JP5 to Lamp Power Supply PCBA P7 to Chassis Ground JP7 to Transition PCBA Figure 8...

Страница 124: ...nsition PCBA To remove the Transition PCBA do the following Figure 8 1 1 Disconnect all external rear panel connections to the detector 2 Disconnect the green and yellow ground lead 3 Disconnect the ribbon cable by spreading the retaining clips open and disengaging the connector 4 Gently pull the six black snap latches holding the Transition PCBA to the detector rear panel free and remove the boar...

Страница 125: ...CPU PCBA To Tungsten Lamp To Deuterium Lamp To Lamp Supply Transformer Ground Wire Figure 8 4 Lamp Power Supply PCBA connector layout Lamp Power Supply Transformer The Lamp Power Supply Transformer is located in the center of the detector chassis Refer to Figure 8 1 To remove this transformer do the following 1 Disconnect the connector in the cable bundle between the power entry module and the inl...

Страница 126: ...eft rear of the PCBA 2 Disconnect the two lead connector at rear of the PCBA 3 Disconnect the five lead connector at the front of the PCBA 4 Grasp the PCBA by its edges and lift the PCBA straight up and free from the mounting retaining pins on the chassis floor Install a new PCBA using the preceding procedure in reverse order Be sure to route the cable from the five lead connector under the PCBA s...

Страница 127: ...RNING FOR CONTINUED PROTECTIO N AGAINST FIRE HAZARD REPLACE FUSE ONLY WITH SA ME TYPE AND RATING SE RVICE BY QUALIFIED PERSO NNEL ONLY NO USE R SE RVICEABLE PA RTS WITHIN Made In U S A OUTPUT START ZERO COM COM 100 115 120 T3 15A 250V 220 230 240 T1 6A 250V 125 VA MAX LINE FUSE Figure 8 5 Cooling Fan Removal Install a new fan using the preceding procedure in reverse order Clean the fan guard befor...

Страница 128: ...age selector 3 Carefully turn the detector on to its side and remove the two 5 64 Allen head screws holding the Front Power Button and bracket to the chassis Figure 8 6 Pull the L shaped button protector aside to allow installation of the replacement assembly 4 Cut the plastic tie wrap holding the mechanical cable to the plastic mounting fixture on the underside of the chassis 5 Pull the mechanica...

Страница 129: ...January 2004 Thermo Electron 8 11 PD Z115E Figure 8 6 Power button and bracket removal ...

Страница 130: ...232 SPARE EVENT READY RUN 5V ch 1 ch 2 ch 2 ZERO COM COM COM COM COM SPARE 1 1000 mv 4 2 100 mv 5 3 10 mv 6 100 115 120 T3 15A 250V 220 230 240 T1 6A 250V 125 VA MAX LINE FUSE Power Entry Module Switch Cable to Front Button PD Z113E Power Entry Module Screws Figure 8 7 Removal of Power Entry Module Install a new Power Entry Module and Front Power Button assembly using the preceding procedure in re...

Страница 131: ...tic collar from the cable and set it aside for installation on the replacement LED 8 Cut the plastic tie wrap holding the cable to the mounting fixture on the underside of the chassis 9 Pull the old cable through the hole in the chassis bottom while guiding the new LED and cable through the grommeted hole in the inner chassis wall until the replacement LED comes through the hole in the chassis bot...

Страница 132: ... to CPU PCBA LED Retainer Front of Detector Partial Bottom View LED Figure 8 8 LED and cable removal Cable Assemblies Figure 8 10 identifies the replaceable cable assemblies inside the detector Refer to Figures 8 3 and 8 4 to identify the proper PCBA connector locations ...

Страница 133: ...er Wheel Magnetic Sensor and Cable Assy Lamp P S to Lamp Cables Grommet CPU to Array Acq PCBA Cable Front Panel LED and Cable Assy CPU to Lamp P S PCBA CAble CPU to Transition PCBA Ribbon Cable Figure 5 9 Replaceable cable assemblies in UV6000LP detector ...

Страница 134: ......

Страница 135: ...e outputs 2 8 2 11 customer support Australasia and Asia vii Europe vi North America v D dark current calibration performing from Atlas 5 32 performing from ChromQuest 5 18 detector version numbers 5 9 deuterium lamp lifetime 5 3 Diagnostics Program channel scan rate 5 7 channel selection 5 7 channel wavelength 5 8 collecting scans 5 6 data filtering Bessel 5 5 Savitsky Golay 5 5 Lamps page 5 2 la...

Страница 136: ...l scans 2 13 location of 4 13 run time 5 2 status 5 2 tungsten halogen 1 2 wavelength range 1 2 M maintenance reloading firmware EXE960 4 22 Hyperterminal 4 20 Maintenance page 5 27 maintenance tools 4 2 manual organization 1 1 N nitric acid safety precautions 4 5 North America customer support v O Operation page 5 25 optical system 1 3 organic solvents used to clean flowcells 4 3 output polaritie...

Страница 137: ... flowcell contamination 4 3 table of common problems 6 1 tungsten halogen lamp lifetime 5 3 U unpacking your detector 2 1 UPS uninterruptable power supply 6 1 UV6000LP installation 2 1 troubleshooting 6 1 V voltage AC line problems 6 1 changing the setting 2 5 W wavelength calibration performing from Atlas 5 30 performing from ChromQuest 5 19 Z ZERO input 2 8 ...

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