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Scanning spectra

3-61

A progress bar reports the degree of fluorescence, in emission or energy

units (EU).

Sample scan progress bar

Tip:

When you perform a zero-scan before a sample scan, the detector

indicates that the zero-scan is being subtracted from the sample scan in

progress.

Subtracting the zero-scan progress bar

After the scan is complete, the detector displays the sample scan

graphically.

Graph of sample anthracene scan

5. Press Next to display the parameters for up to three of the highest peaks

scanned within the specified range.

Содержание 2475

Страница 2: ...t may appear in this document This document is believed to be complete and accurate at the time of publication In no event shall Waters Corporation be liable for incidental or consequential damages in...

Страница 3: ...disposal of any Waters product You can reach us via the Internet telephone or conventional mail Safety considerations Some reagents and samples used with Waters instruments and devices can pose chemi...

Страница 4: ...ted in this section Applicable symbols Audience and purpose This guide is intended for personnel who install operate and maintain the 2475 Multi Fluorescence detector Symbol Definition Manufacturer Au...

Страница 5: ...ne Help system for calibration instructions Quality control Routinely run three QC samples that represent subnormal normal and above normal levels of a compound Ensure that QC sample results fall with...

Страница 6: ...vi EC authorized representative Waters Corporation Micromass UK Ltd Floats Road Wythenshawe Manchester M23 9LZ United Kingdom Telephone 44 161 946 2400 Fax 44 161 946 2480 Contact Quality manager...

Страница 7: ...trument v Calibrating v Quality control v ISM classification v ISM Classification ISM Group 1 Class B v EC authorized representative vi 1 Theory of Operation 1 1 Fluorescence theory 1 2 Fluorescence d...

Страница 8: ...12 Electronics 1 13 Wavelength verification and test 1 14 Operational modes 1 14 Single channel mode 1 14 Multichannel mode 1 15 Spectrum scanning 1 16 Lamp energy and performance 1 16 Auto optimize g...

Страница 9: ...20 Connecting other devices 2 23 Required materials 2 23 Connecting cables 2 23 Connecting a data system using a Bus SAT IN module 2 24 Connecting a 746 data module 2 27 Connecting a chart recorder 2...

Страница 10: ...ion mode via RS 232 3 29 Remote control operation via Ethernet connection using 2475 instrument control software 3 34 Verifying the detector 3 34 Manual wavelength calibration 3 35 Normalizing emissio...

Страница 11: ...68 Manually lighting the lamp 3 69 Using a timed event method to program the lamp 3 70 Shutting down the detector 3 70 4 Maintenance Procedures 4 1 Contacting Waters technical service 4 2 Maintenance...

Страница 12: ...iagnostic tests and settings 5 12 Change lamp function 5 15 Testing the keypad 5 16 Testing the display 5 17 Other diagnostic tests and settings 5 17 Generating test peaks 5 17 Overriding the optical...

Страница 13: ...ation checklist C 2 Water C 2 Buffers C 3 Tetrahydrofuran THF C 3 Solvent miscibility C 3 How to use miscibility numbers C 5 Buffered solvents C 6 Head height C 6 Solvent viscosity C 6 Mobile phase so...

Страница 14: ...xiv Table of Contents...

Страница 15: ...strument s features Contents Topic Page Fluorescence theory 1 2 Fluorescence detection 1 3 Measuring fluorescence 1 4 Detector description 1 7 Principles of operation 1 9 Operational modes 1 14 Spectr...

Страница 16: ...erfere with a compound s ability to fluoresce diminishing analytical performance pH changes The loss or gain of protons and their accompanying increase or decrease of charge affects an analyte s elect...

Страница 17: ...ight sources Xenon lamps are the preferred source for general purpose fluorescence detectors Excitation wavelength selection The excitation wavelength of choice requires some source light filtering In...

Страница 18: ...nt of stray light that can affect the measurement and it maximizes the fluorescence signal The sample compartment is arranged so that the fluorescence energy is collected at an angle perpendicular to...

Страница 19: ...he 2475 detector reports intensity using normalized units to compensate for variability between individual detectors and offset any age related decrease in lamp intensity When using normalized units c...

Страница 20: ...iables such as lamp intensity optics efficiency and gain directly influence the fluorescence emission signal strength As a result energy units are less reliable Nonetheless when you must calculate ene...

Страница 21: ...Interscience New York 1972 Detector description The 2475 Multi Fluorescence Detector is a multichannel tunable fluorescence detector designed for high performance liquid chromatography HPLC applicati...

Страница 22: ...ols to optimize functionality and performance Data communications and control By an Empower system or Millennium 32 chromatography workstation version 3 2 or 4 0 Backward compatibility Operates as a 4...

Страница 23: ...verification and test Flow cell Electronics Detector optics The optics are based on a pair of tunable monochromators and include the following parts Xenon arc lamp Two ellipsoidal mirrors and one par...

Страница 24: ...ly light path The detector demonstrates superior performance by employing several unique design elements Its novel flow cell design minimizes stray background light Xenon lamp Grating Parabolic mirror...

Страница 25: ...nochromator to select the appropriate excitation wavelengths defined by its geometry The grating can rotate quickly responding to multiple excitation wavelengths and or scanning Emission monochromator...

Страница 26: ...sensitivity After calibrating the PMT you must choose a gain setting for the photomultiplier tube prior to a chromatographic injection Saturation which occurs when the sample concentration is high or...

Страница 27: ...erformed simultaneously This component ensures the best rejection of common mode noise in the two beams leading to a quiet baseline Personality board Receives inputs from the preamplifier board and ex...

Страница 28: ...nt mobile phase You can initiate a manual wavelength calibration anytime to replace the previous calibration data with new data Tip The combined wavelength accuracy specification of the detector is 3...

Страница 29: ...fy a higher sampling rate in the instrument method If the value is greater than 50 you should specify a lower sampling rate in the instrument method Set the sampling rate to the lowest value required...

Страница 30: ...by performing the following types of scan on the flow cell Zero scan Characterizes the baseline spectrum of a solvent Excitation sample scan Subtracts the zero scan so the displayed or charted result...

Страница 31: ...ed the detector to operate as independently of lamp output as possible After the unit has verified the calibration of the monochromator the instrument evaluates the energy levels in a number of charac...

Страница 32: ...alog outputs during data collection it displays a minimum EUFS value that applies to the entire chromatogram Like the ideal gain value the EUFS value assumes a 2 margin to account for any variations i...

Страница 33: ...small peak that is best detected at a gain of 1000 The next change at 2 0 minutes is the required wavelength pair change Initial gain setting or conditions are not critical The only requirement for th...

Страница 34: ...ple energy units changing the gain does affect the magnitude of the output signal Ensuring gain optimization for each peak of interest Refer to the figure Gain optimized chromatogram on page 1 19 If y...

Страница 35: ...any test fails The startup diagnostic tests are as follows Central processing unit CPU test Serial communication interface SCI test Electrically erasable programmable read only memory EEPROM test RAM...

Страница 36: ...solvent absorbs some of the available excitation light intensity which in turn reduces the fluorescence emission response for the sample For a complete list of UV cutoff ranges for common solvents and...

Страница 37: ...Up the Detector Contents Topic Page Before you begin 2 2 Installing the detector 2 3 Plumbing the detector 2 3 Making signal connections 2 5 Connecting other devices 2 23 Connecting to the electricit...

Страница 38: ...and your local Waters representative Customers in the USA and Canada should report damage and discrepancies to Waters Technical Service 800 252 4752 Others should phone their local Waters subsidiary...

Страница 39: ...irmly and then tighten the compression screw Warning To avoid injury Waters recommends that two people lift the 2475 detector Warning Risk of fire To avoid overheating and to provide clearance for cab...

Страница 40: ...nections Assembling fittings Slide the compression screw over the tubing end Follow it with the ferrule mounted so that its taper faces the end of the tubing Compression screw Tube Ferrule Tubing end...

Страница 41: ...ht Tip To ensure accurate verification during installation be sure to pump fresh degassed and filtered 100 water through the flow cell before powering it Making signal connections See also Ethernet In...

Страница 42: ...summarizes the signal connections needed to connect the 2475 detector to other HPLC system components Component connector types Connector type Component Ethernet connection Used to connect to a Water...

Страница 43: ...accompany the instrument control software for details Single Waters instrument connection In a single Waters instrument system configuration the connection hardware requires only one CAT 5 shielded Et...

Страница 44: ...u must install the Waters instrument control software in the acquisition computer so that the computer can control the Waters instrument Consult the software installation instructions that accompany t...

Страница 45: ...mmarizes the inject start connections for different system configurations 2475 detector inject start connections Inject start output source Inject start input connection on the 2475 detector connector...

Страница 46: ...led according to the EUFS emission energy units full scale setting for each channel The detector allows the EUFS to be set individually for the output on each channel Volts per EU are calculated for t...

Страница 47: ...cribes each signal available on the I O connectors See Appendix B for the signal s electrical specifications I O signals for the detector Signal Description Inject Start 1 TTL contact closure Configur...

Страница 48: ...og output channels Detector Out 1 and Detector Out 2 Auto Zero 1 Configurable input to Auto Zero both channels Detector Out 1 and Detector Out 2 Detector Out 1 2 1 V full scale analog output signal of...

Страница 49: ...ads of the signal cable to the connector 2 Slide the clamp with the bend facing down into the protective shield 3 Insert the clamp and shield with the bend facing down into the connection cover and lo...

Страница 50: ...second connection cover over the first cover and snap it into place Connecting an Alliance separations module You can connect an Alliance separations module to the detector to perform the following fu...

Страница 51: ...r auto zero on injection Connections for generating an auto zero on inject Alliance separations module B inputs and outputs 2475 detector A inputs Pin 1 Inject Start Pin 9 Auto Zero Pin 2 Inject Start...

Страница 52: ...n injection Connections for generating a chart mark on inject Alliance separations module B inputs and outputs 2475 detector A inputs Pin 1 Inject Start Pin 6 Chart Mark Pin 2 Inject Start Pin 7 Chart...

Страница 53: ...ging the default lamp configuration parameter from Ignore to High or Low see page 3 25 Connections for starting a method Alliance separations module B inputs and outputs 2475 detector A inputs Pin 1 I...

Страница 54: ...tions port in an Empower system or Millennium 32 chromatography Connections for turning the detector lamp on or off Alliance separations module A Outputs 2475 detector A Inputs Pin 1 Switch 1 Pin 4 La...

Страница 55: ...onnecting the detector to a Waters data system all detector parameters not configurable by the data system in use defer to local control Caution To avoid possible damage to components shut down all in...

Страница 56: ...ctions for starting a method on injection on page 2 17 Connecting Ethernet devices The detector can be controlled using Ethernet communications when Empower software build 2154 or build 1154 with Inst...

Страница 57: ...ge 2 22 You must install the Waters instrument control software in the acquisition computer before the computer can control the Waters instrument See the software installation instructions that accomp...

Страница 58: ...or different system configurations Tip For pin out connections to the 2475 detector see the figure I O signal inputs and outputs on page 2 11 2475 detector inject start connections Inject start output...

Страница 59: ...you need the following tools Small flat blade screwdriver startup kit Electrical insulation stripping tool Connecting cables To connect the cables from other HPLC system devices to the A and B termina...

Страница 60: ...nel To connect an Empower system or Millennium32 chromatography workstation to the detector 1 Connect the Bus SAT IN module to the busLAC E or LAC E32 card in an Empower system or Millennium 32 comput...

Страница 61: ...ting the Bus SAT IN module channel 2 to the detector on page 2 26 and the figure I O signal inputs and outputs on page 2 11 Connect the white wire to pin 4 on B Detector Out 2 1 V Connect the black wi...

Страница 62: ...SAT IN module 2475 detector B inputs and outputs 1 2 3 4 5 6 7 8 9 10 Detector out 1 Detector out 1 Ground Detector out 2 Detector out 2 Switch 1 Switch 1 Ground Switch 2 Switch 2 Bus SAT IN module 24...

Страница 63: ...module use the cable provided in the detector s startup kit to make the connections shown in the following table and figure Tip To minimize the chance of creating a ground loop that can adversely affe...

Страница 64: ...and figure Tip To minimize the chance of creating a ground loop that can adversely affect measurement connect the shield of the cable to the chassis ground at one end only Detector inputs and chart r...

Страница 65: ...generate a chart mark A chart mark signal is generated at the chart mark inputs on the analog connector Connecting a 600 series pump To connect a 600 series pump 1 Place the detector on a level surfa...

Страница 66: ...ontroller to the detector shown in the following table and figure Lamp on off connections for the 600 series pump Detector inputs and 600 series pump terminal connections 600 series pump terminal 2475...

Страница 67: ...t mark connections To make chart mark connections 1 Make the connections shown in the following table and figure using a signal cable Auto zero connections for the 600 series pump 600 series pump term...

Страница 68: ...nitiate data acquisition To make inject start connections 1 Make the connections shown in the following table and figure with a signal cable Chart mark connections for the 600 series pump 600 series p...

Страница 69: ...zero at the start of an injection Inject start connections for the 600 series pump 600 series pump terminal 2475 detector A inputs S1 S2 S3 S4 1 or inject 1 You may also connect the pump s Inject ter...

Страница 70: ...autosampler Auto zero connections for the 717plus autosampler Auto zero connections for the 717plus autosampler 717plus autosampler terminal 2475 detector A inputs Inject Start any one of many paired...

Страница 71: ...art terminals on the autosampler Inject start connections for the 717plus Autosampler Inject start connections for the 717plus Autosampler 717plus Autosampler terminal 2475 detector A inputs Inject St...

Страница 72: ...bility 1 Place the Off On switch in the Off position 2 Connect the female end of the power cord to the receptacle on the rear panel of the detector 3 Connect the male end of the power cord to a suitab...

Страница 73: ...in the Empower Online Help to set parameters for controlling the detector As part of a Millennium 32 chromatography workstation You can configure the detector for use with a Millennium 32 chromatograp...

Страница 74: ...ges 1 Initializing grating 2 Initializing system 3 Lighting lamp 4 Warmup time left counts down from five minutes Warning Always observe Good Laboratory Practices when you use this equipment and when...

Страница 75: ...p failure If one or more of the internal startup checks fails the detector beeps and displays an error message For serious errors the detector displays the word Error in brackets Error in place of the...

Страница 76: ...V light from reaching the detector s optics bench 2475 detector idle mode screen Using the operator interface Using the display The detector s operator interface includes a 128 64 bitmap graphic displ...

Страница 77: ...play the icons or fields shown on page 3 4 and described in the following table For a list of ranges and defaults for the function icons and fields in the following table see the table titled Primary...

Страница 78: ...Channel trace When you press TRACE displays the fluorescence intensity also known as emission for the channel indicated A or B Numerical field 0 00 Fluorescence in emission units or sample energy unit...

Страница 79: ...erating in triple channel mode Icon only appears if instrument is under control of an external data system remote mode only Quad wavelength Indicates the detector is operating in quadruple channel mod...

Страница 80: ...current method number or an asterisk which indicates current conditions are not stored as a method RS 232 control Indicates that the 2475 detector is controlled by a data system and displays a remote...

Страница 81: ...ggles between channels A and B Direct access to specific screens HOME METHOD CONFIGURE DIAG Diagnostics TRACE and SCAN Primary functions Chart Mark Auto Zero and Run Stop Primary function keys take ef...

Страница 82: ...entry on a list or menu as follows For numerical entries 1 through 9 on lists or menus enter the number corresponding to a desired item and then press Enter For the number 10 select 0 and then press...

Страница 83: ...d description Key Description Unshifted After pressing shift HOME Displays the home screen which displays icons excitation and emission wavelengths EUFS and Gain fields Displays context sensitive Help...

Страница 84: ...ps freezes the run clock and initiates scans The elapsed time appears near the lower right hand side of the home screen The shutter opens when you press Run while the idle mode function is enabled Res...

Страница 85: ...s for creating and clearing timed and threshold events and storing retrieving and resetting methods DIAG Displays the list of diagnostic routines CONFIGURE Displays the first Configuration screen TRAC...

Страница 86: ...of the lamp is indicated by an icon on the home screen 2 See 0 9 above Lock When you are viewing the home screen enables or disables the keypad lock feature Use the lock to prevent inadvertent changes...

Страница 87: ...value Sets the value to a unique word for some fields For example in the voltage offset diagnostic you can enter either a numeric offset value or press CE to change it to OFF Clear Field Blanks the c...

Страница 88: ...e number corresponding to a choice you can press that number without pressing Enter first The and keys do not incrementally increase or decrease numerical field entries To change field entries use the...

Страница 89: ...figure Secondary functions of the home screen on page 3 17 Secondary functions of the home screen Fluorescence home screen Press Next filter type analog out and time constant available for both and P...

Страница 90: ...he shutter by pressing Reset or waiting until the run ends To avoid the automatic opening and closing of the shutter you can disable the idle mode by checking the Selection box in the Configuration sc...

Страница 91: ...setting must have a linear relationship with the actual fluorescence signal Filter type Defines your choice of noise filter Hamming filter is the default Data units Defines data units Emission The st...

Страница 92: ...nnel regardless of which channel is larger Volts out Larger fluorescence A or B 1 V EUFS of selected channel Difference Plot A B and B A Charts the difference in fluorescences at two different wavelen...

Страница 93: ...eline maintains the previous baseline level when the gain or wavelength change is made To baseline is the default setting Enable keypad event in chart mark Selected by default this parameter results i...

Страница 94: ...nce energy A Output off Emission A Time constant 2 of 4 Numeric sec Hamming 0 1 to 5 0 Hamming 1 to 50 RC 0 1 to 99 RC 1 to 99 0 to disable filtering 1 5 Data units 3 of 4 Choice None Emission Energy...

Страница 95: ...tion of the trace Displaying the scale parameters To display the scale parameters 1 Press Scale 2 Press Next to display T2 starting time The default is 0 3 Press Next again to display EU1 starting or...

Страница 96: ...tion wavelength set to 240 nm and emission to 355 nm Scaled trace of continuous injections with T1 changed to 60 The following figure shows a 4 minute scaled trace or zoom of the 60 minutes of continu...

Страница 97: ...s Disabling shutter idle mode You can disable the shutter idle mode in the first Configuration screen When selected the shutter does not close to protect the detector s optics after the completion of...

Страница 98: ...You can configure the auto zero input to auto zero fluorescence readings on channel A and or channel B To determine the response of the channel enable the auto zero function see the table titled Prima...

Страница 99: ...is programmed to initiate a rectangular wave as a timed or threshold event then this field specifies the period of the signal the width of one pulse period in a rectangular wave or pulse train range...

Страница 100: ...ive Help When you select Shift HOME from a point in the program associated with a Help screen the screen appears If Online Help is not available selecting effects no response Press Enter to return to...

Страница 101: ...3 29 Standalone operation When using the detector as a standalone instrument you can store up to 10 methods each containing up to 48 timed and 2 threshold events see page 3 43 An asterisk in the metho...

Страница 102: ...ilable Tip The same parameters apply to a 474 detector Method parameters The initial conditions for the method are specified on the General tab of the fluorescence method editor in Empower or Millenni...

Страница 103: ...t a value close to the actual value in the method for sample detail archival purposes in Empower or Millennium32 software Filter Type Either a digital Hamming or RC filter The digital filter tends to...

Страница 104: ...to wait for the lamp to warm again Tip It is best to shut the lamp off only when all runs are completed You should program the lamp to turn off or turn off the lamp manually only when you do not expe...

Страница 105: ...wavelength or gain is changed Polarity Defines the polarity of the analog output only Operation details Inject Start The detector is configured with a switch closure signal input to the chart mark ter...

Страница 106: ...are Remote control operation via Ethernet connection using 2475 instrument control software This mode of operation uses the Ethernet connection and appears in the Empower software Configuration window...

Страница 107: ...gth 1 Select Calibrate Shift 3 from the keypad Wavelength calibration message 2 Ensure the flow cell is prepared and then press Enter The detector cycles through the calibration procedure and momentar...

Страница 108: ...with filtered degassed and sparged HPLC grade water Then pump the mobile phase provided you encounter no miscibility problems at 1 mL min for 15 minutes minimum Tip Normalize emission units weekly To...

Страница 109: ...operation the default operating mode To specify single channel mode when the detector is in multichannel mode 1 From the home screen select l Shift Auto Zero Result The detector displays an appropria...

Страница 110: ...the detector with expanded chart out selections in multichannel mode which offers the following functions Emission A and B Sample energy A and B Reference energy A and B MaxPlot Difference A B or B A...

Страница 111: ...not set the gain setting for each channel individually Obtaining a MaxPlot or difference plot You can obtain a MaxPlot or difference plot by monitoring fluorescence at two selected wavelengths while p...

Страница 112: ...s the pre amplifier and a value of 9999 9 appears in the Emission Energy units field Gain set too high fluorescence pinned to 9999 9 EU Gain set too high alarm message The value of 9999 9 EU in the Em...

Страница 113: ...am This can be done by entering a method via the keypad or by retrieving a previously created method from a stored memory location If you are using Empower or Millennium 32 software you must enter the...

Страница 114: ...at proper times relative to the peaks Select Make Injection if you are running under Empower or Millennium32 control or start the injection through other devices such as an Alliance 2695 Separations M...

Страница 115: ...on scale Gain and EUFS optimally set Programming methods and events Storing methods You can store and retrieve up to ten methods The detector designates stored methods as the numerals 1 through 10 If...

Страница 116: ...down are restored However any timed events or thresholds associated with the method are deactivated when power is restored Thus on startup an asterisk always appears inside the method icon on the home...

Страница 117: ...vity EUFS 1 to 100 000 Yes 6 Chart mark 10 of full scale Does not apply Does not apply Yes 7 Polarity 1 2 Yes 8 Auto Zero Does not apply Does not apply Yes 9 Lamp 1 Off 2 On Off No 10 Switch 1 1 High...

Страница 118: ...ifying the time of the event appears 3 Specify the time for the event Tip When you begin additional fields appear Timed events screen 4 Press Enter To advance to the Set field Events list press 12 Thr...

Страница 119: ...hen the time field is active to change it to OFF 9 Press HOME to return to the home screen then press Run Stop to start the method 10 Select Reset Shift Run Stop to reset the run clock to 0 Tip If the...

Страница 120: ...vents An active field EU for entering the threshold appears When you begin to enter a number in the EU field additional fields appear Tip The threshold event allows you to specify a threshold value EU...

Страница 121: ...to the threshold parameter you are programming 6 Press A B to set the threshold on the other channel and repeat the procedure Storing a method A method consists of all programmable parameters shown on...

Страница 122: ...ot box 3 Specify the number of the method you wish to retrieve and press Enter A brief message Retrieving method n appears and then the method number you specified appears within the method number ico...

Страница 123: ...her operating parameters x e UFS etc are set to defaults If you select Cancel Shift 0 the Method list appears Tip To prevent loss of the current conditions before you clear the method store them in a...

Страница 124: ...solvent to provide the actual spectrum of the sample The detector can measure the spectrum of a sample using the flow cell see page 3 64 for scanning procedures Before you begin Before you run a spect...

Страница 125: ...000 nm min Tick marks Generates tick marks at a specified wavelength interval which helps to interpret charted data The figure Scan of water without tick marks on page 3 54 shows a scan of water stand...

Страница 126: ...e detector s scan function to run a new zero or sample scan store review subtract obtain scan information and replay When you select a sample or zero scan the detector displays three additional screen...

Страница 127: ...tor displays one additional screen labeled 2 of 2 Note that you cannot change the starting parameter value ending wavelength parameter value or the pace parameter value Zero scan screen 1 of 4 Sample...

Страница 128: ...the subsequent sample scans you perform The sample scan uses the starting and ending wavelength values and the pace value of the most recent zero scan Only when these parameter values are identical fo...

Страница 129: ...eens 4 On the first New scan screen specify the type of scan For a sample scan press 1 or press Enter to display the list For a zero scan press 2 or press Enter to display the list The detector displa...

Страница 130: ...ts Range or default Type 1 n a Sample scan 1 Zero scan 2 Default 1 range 2 nm Range 200 to 900 nm Default 200 or 210 nm Pace 3 nm min Range 30 to 1000 nm min Default 100 nm min EUFS 3 EU Range 1 to 10...

Страница 131: ...alue and then press Enter 7 Specify a value in the Pace field for the rate at which the detector scans the specified wavelength range Tip The default is 100 nm min and the allowable range is from 30 t...

Страница 132: ...and solvent conditions run the sample scan for the corresponding zero scan within 15 minutes of running the zero scan 1 Set up and run the zero or reference scan see page 3 59 2 Return to the first N...

Страница 133: ...a sample scan the detector indicates that the zero scan is being subtracted from the sample scan in progress Subtracting the zero scan progress bar After the scan is complete the detector displays the...

Страница 134: ...wavelength displayed EU1 Minimum fluorescence displayed The default is auto EU2 Maximum fluorescence displayed The default is auto 8 Press Next to advance through the four scaling parameters The follo...

Страница 135: ...age 3 64 shows a series of scans of anthracene dissolved in acetonitrile The zero scan is not displayed For the scaling parameters EU1 and EU2 the default is auto You can change the EU parameter based...

Страница 136: ...ell with the analyte 4 Run a sample scan keeping the pressure below 145 psi to avoid overpressuring the flow cell 5 Use the functions storage review subtract and review and replay to compare scanned d...

Страница 137: ...pectrum being subtracted You can replay the current spectrum or a stored one in real time using the real time replay function on the scan list The detector plays the selected spectrum in real time bot...

Страница 138: ...for the selected spectrum other The wavelength setting of the stationary monochromator Pace Displays the pace for the selected spectrum Gain The gain setting for the PMT it can sometimes be necessary...

Страница 139: ...current spectrum and after a brief wait displays the difference spectrum You can store the results in one of the five storage slots Replaying a spectrum To replay a spectrum 1 Select SCAN Shift Chart...

Страница 140: ...mp manually When the lamp is unlit the home screen displays the words Lamp off and an X is superimposed on the lamp icon Select the Lamp key Shift 1 to extinguish or light the lamp manually and to dis...

Страница 141: ...ght the lamp 1 Select Lamp Shift 1 The lamp control screen appears with 0 hours and 00 minutes in the Lamp has been on field 2 Select Lamp Shift 1 again to light the lamp Tip When the lamp is lit the...

Страница 142: ...ore information on programming the lamp through the external contact closure Shutting down the detector Before you shut down the detector you must remove any buffered mobile phase present in the fluid...

Страница 143: ...ic Page Contacting Waters technical service 4 2 Maintenance considerations 4 2 Routine maintenance 4 3 Inspecting cleaning and replacing the flow cell 4 5 Replacing the lamp 4 8 Replacing the fuses 4...

Страница 144: ...he symptom Instrument serial number Solvent s Method parameters sensitivity and wavelength Type and serial number of column s Sample type Empower software version and serial number For complete inform...

Страница 145: ...is shut down Tip Flushing prevents the following problems Plugging of the solvent lines and flow cell Damage to various components Microbial growth Warning Avoid electric shock Do not open the detect...

Страница 146: ...raw the top of the cover gently and store the cover nearby 2475 detector with the front left hand panel cover removed Caution Because no user serviceable parts are housed inside the detector never rem...

Страница 147: ...Discontinue the flow of mobile phase 2 Remove the column 3 Attach tubing from the detector to the injector outlet from which the column has been removed 4 Flush the mobile phase from the detector wit...

Страница 148: ...Flush and dry the flow cell see page 4 5 and then disconnect and cap the inlet and outlet LC tubing 3 Remove the front left hand panel cover 4 Use a 1 4 inch flat blade screwdriver to loosen the three...

Страница 149: ...low cell installed Replace the flow cell when it becomes damaged Before you begin 1 Unpack and inspect the new flow cell 2 Shut down the detector 3 Remove the front left hand panel cover 4 Disconnect...

Страница 150: ...stic tests for 2000 hours or 1 year from the date of purchase whichever comes first Tip Always perform the procedure on page 3 34 each time you change the lamp When to replace the lamp Replace the lam...

Страница 151: ...extremely hot during lamp operation To prevent burn injuries allow the lamp to cool for 60 minutes before removing it keep the lamp in the housing when handling the lamp Warning To avoid eye injury f...

Страница 152: ...4 10 Maintenance Procedures b Pinch the locking mechanism on the bottom connector before pulling it out Unplugging the lamp assembly...

Страница 153: ...mbly Warning To avoid injury always keep the lamp facing away from you when removing it Lamp gas is under positive pressure To prevent shattering the glass use care when disposing of the lamp Waters s...

Страница 154: ...place 5 Close and secure the lamp access door 6 Connect the power cord and start the detector Allow at least 60 minutes for the lamp to warm before resuming operations 7 Record the new lamp s serial...

Страница 155: ...isplay keypad 3 Press 1 Change lamp Tip Be sure to enter the lamp s serial number and not its part number when performing this procedure 4 Specify the serial number of the new lamp in the active field...

Страница 156: ...fective when the detector fails to power on the display is blank the fans do not operate To replace the fuses Replace both fuses even when only one is open or otherwise defective 1 Power off the detec...

Страница 157: ...he new fuses suit your requirements 5 Insert the new fuses into the fuse holder 6 Insert the fuse holder into the receptacle and gently push until it locks into position on the rear panel 7 Start the...

Страница 158: ...4 16 Maintenance Procedures...

Страница 159: ...el can access the service diagnostics Error messages Startup calibration and other error messages and recommended actions for correcting the errors Diagnostic tests User diagnostic tests for troublesh...

Страница 160: ...rifying the detector on page 3 34 and Manual wavelength calibration on page 3 35 have verification and calibration information and procedures Startup error messages Error message Description Correctiv...

Страница 161: ...n the home screen If a catastrophic error appears Lamp external input conflict A timed event or front panel action attempts to change the lamp state in conflict with enabled lamp input contact closure...

Страница 162: ...ce A D A D communication test failed 1 Power off and power on again 2 If the problem persists call Waters Technical Service Communication failure Sample A D A D communication test failed 1 Power off a...

Страница 163: ...persists power off and power on again 3 If the problem persists call Waters Technical Service Filter initialization failure Order filter position Unit sensors cannot find the order filter position 1 E...

Страница 164: ...on again 3 If the problem persists call Waters Technical Service Filter initialization failure Shutter position Unit sensors cannot find the shutter position 1 Ensure solvent is flowing 2 If the prob...

Страница 165: ...tch is open 1 Close the lamp door 2 Remove any cooling vent obstructions 3 If the problem persists call Waters Technical Service Method not found Stored method data is not valid Power off and power on...

Страница 166: ...form the tests and change settings 1 Press DIAG on the keypad The Diagnostics list appears System cannot respond Error occurs while unit is positioning next wavelength or changing modes during initial...

Страница 167: ...sticky diagnostic test is active the home screen displays a wrench icon If no tests are active the wrench icon does not appear on the home screen Home screen showing active sticky diagnostic settings...

Страница 168: ...100 EU using a standard clean water reference 2 Raman S N Test Runs the 15 minute signal to noise test for water 3 Auto Optimize Gain Displays a table of recommended gain settings for a method based...

Страница 169: ...urrent sample and reference energy readings appear in energy units from 1 to 10 000 Sample and reference energy tests To perform sample and reference energy tests 1 Press DIAG then press 5 Sample ref...

Страница 170: ...you start the signal to noise test the detector sets the excitation wavelength to 350 nm it sets the emission wavelength and gain to the values stored during the normalize units test Clean degassed wa...

Страница 171: ...nput output list press 1 Auto zero offsets Auto zero offsets screen 2 Select Cancel Shift 0 if you want to clear the offset on both channels to zero Setting the fixed EU value This function sets the v...

Страница 172: ...Input output list press 3 Fix voltage to select a voltage for the analog output You can select a voltage for both output channels range 0 10 to 1 10 V Fix voltage screen Monitoring contact closures a...

Страница 173: ...to OFF or vice versa c Press Enter to select the second switch Change lamp function Whenever you change the lamp use this function to enter a new serial number and installation date See page 4 12 and...

Страница 174: ...and then press Enter Testing the keypad To test the keypad 1 Press DIAG and then press 7 Lamp display keypad 2 Press 2 Test keypad Keypad test 3 Press any key to begin the test and then press each ke...

Страница 175: ...ttings screen provides three additional diagnostic functions Generate test peaks Generates test peaks to calibrate a chart recorder or data system Manually override the optical filter Selects a filter...

Страница 176: ...The gain is automatically set to 1000 Generate test peaks message Tip You must manually disable the Generate test peaks function to stop it 3 Press 1 Disable test peaks to stop generating test peaks O...

Страница 177: ...ng the available linear gain range of 1 to 1000 This feature is intended for use when samples or mobile phase solvents exhibit high fluorescence emissions that saturate the PMT signal but reducing con...

Страница 178: ...uments as well as with the detector Most detector problems are relatively easy to correct If you are unable to correct a problem or failed condition after running the user diagnostics applicable to th...

Страница 179: ...led General hardware troubleshooting on page 5 21 describe error messages that can appear onscreen as you start up or operate the detector and it suggests corrective actions Power surges Power surges...

Страница 180: ...nd if necessary replace fuse s Bad LCD or control board Call Waters Technical Service Front panel displays odd characters Faulty EPROMs or bad LCD control board Call Waters Technical Service Keypad no...

Страница 181: ...nd if necessary replace the RS 232 cable Xenon lamp does not light Faulty lamp Replace the lamp Lamp not plugged in Plug in the lamp connector Bad lamp power supply Contact Waters Technical Service La...

Страница 182: ...5 24 Error Messages Diagnostic Tests and Troubleshooting...

Страница 183: ...des also include the hazard symbols with accompanying text statements describing the hazards and telling you how to avoid them This appendix presents all the safety symbols and statements that apply t...

Страница 184: ...electric shocks ultraviolet radiation exposures and others When the following symbols appear in a manual s narratives or procedures their accompanying text identifies the specific risk and explains ho...

Страница 185: ...ing Risk of explosion Warning Risk of eye injury Warning Pressurized nonmetallic or polymer tubing can burst Observe these precautions when working around such tubing Wear eye protection Extinguish al...

Страница 186: ...Ensure that the nitrogen supply pressure never falls below 690 kPa 6 9 bar 100 psi during an analysis in which flammable solvents are used Also ensure a gas fail connection is connected to the LC syst...

Страница 187: ...nisms and other biological materials To avoid infection with these agents assume that all biological fluids are infectious observe Good Laboratory Practices and consult your organization s biohazard s...

Страница 188: ...ler le droit de l utilisateur exploiter l quipement Achtung Jedwede nderungen oder Modifikationen an dem Ger t ohne die ausdr ckliche Genehmigung der f r die ordnungsgem e Funktionst chtigkeit verantw...

Страница 189: ...e trouvant proximit de l instrument Evitez d utiliser des tubes s v rement d form s ou endommag s Evitez d utiliser des tubes non m talliques avec du t trahydrofurane THF ou de l acide sulfurique ou n...

Страница 190: ...iamenti nei tubi non metallici riducendo notevolmente la pressione di rottura dei tubi stessi Advertencia se recomienda precauci n cuando se trabaje con tubos de pol mero sometidos a presi n El usuari...

Страница 191: ...Warnings that apply to all Waters instruments A 9 Nonmetallic Tetrahydrofuran THF Methylene chloride Dimethyl sulfoxide THF...

Страница 192: ...tueuses Vorsicht Der Benutzer wird darauf aufmerksam gemacht dass bei unsachgem er Verwenddung des Ger tes die eingebauten Sicherheitseinrichtungen unter Umst nden nicht ordnungsgem funktionieren Atte...

Страница 193: ...l instrument Vorsicht Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen ersetzen deren Typ und Nennwert auf den Tafeln neben den Sicherungsabdeckungen des Ger ts gedruckt sind Attenzione per...

Страница 194: ...e can appear in instrument user manuals and on the instrument s front or rear panels Electrical power on Electrical power off Standby Direct current Alternating current Protective conductor terminal F...

Страница 195: ...ng symbols A 13 Handling symbols These handling symbols and their associated text can appear on labels affixed to the outer packaging of Waters instrument and component shipments Keep upright Keep dry...

Страница 196: ...A 14 Safety Advisories...

Страница 197: ...ecification Operating temperature 4 to 40 C 39 2 to 104 F Operating humidity 20 to 80 noncondensing Shipping and storage temperature 40 to 70 C 40 to 158 F Shipping and storage humidity 20 to 80 nonco...

Страница 198: ...this grounding system is connected to the third pin ground pin on the electrical power cord plug b Overvoltage Category II Pertains to instruments that receive their electrical power from a local lev...

Страница 199: ...to 5 0 seconds Hamming default 0 1 to 99 seconds RC Multichannel 1 to 50 seconds Hamming default 1 to 99 seconds RC Optical Component Specifications Lamp source Xenon arc lamp 150 W Flow cell Axial Il...

Страница 200: ...B 4 Specifications...

Страница 201: ...Solvent Considerations Contents Topic Page Introduction C 2 Solvent miscibility C 3 Buffered solvents C 6 Head height C 6 Solvent viscosity C 6 Mobile phase solvent degassing C 7 Wavelength selection...

Страница 202: ...ntain their purity from lot to lot use them to ensure the best possible results Preparation checklist The following solvent preparation guidelines help to ensure stable baselines and good resolution F...

Страница 203: ...re not totally miscible for example from chloroform to water require an intermediate solvent such as isopropanol Temperature affects solvent miscibility If you are running a high temperature applicati...

Страница 204: ...15 4 2 Tetrahydrofuran 0 55 66 0 17 220 4 3 Ethyl acetate 0 47 77 1 19 260 4 3 1 propanol 2 30 97 2 15 210 4 3 2 propanol 2 35 117 7 15 4 4 Methyl acetate 0 45 56 3 15 17 260 4 5 Methyl ethyl ketone...

Страница 205: ...or their critical solution temperature is above 75 C Some solvents prove immiscible with solvents at either end of the lipophilicity scale These solvents receive a dual M number The first number alwa...

Страница 206: ...duled to be more than one day Use a minimum of 15 mL for sparge equipped units and a minimum of 45 mL for inline vacuum degasser equipped units Some modern systems such as Waters Alliance may require...

Страница 207: ...lubility Only a finite amount of gas can be dissolved in a given volume of liquid This amount depends on The chemical affinity of the gas for the liquid The temperature of the liquid The pressure appl...

Страница 208: ...from solution by displacing dissolved gases in the solvent with a less soluble gas usually helium Well sparged solvent improves pump performance Helium sparging brings the solvent to a state of equil...

Страница 209: ...w rates most of the dissolved gas is removed as the solvent passes through the vacuum chamber At higher flow rates lesser amounts of gas per unit volume of solvent are removed Surface area of the dega...

Страница 210: ...tropropane 380 Ethylene glycol 210 2 Butoxyethanol 220 Iso octane 215 Acetone 330 Isopropanol 205 Acetonitrile 190 Isopropyl chloride 225 Amyl alcohol 210 Isopropyl ether 220 Amyl chloride 225 Methano...

Страница 211: ...nm Acetic acid 1 230 Sodium chloride 1 M 207 Ammonium acetate 10 mM 205 Sodium citrate 10 mM 225 Ammonium bicarbonate 10 mM 190 Sodium dodecyl sulfate 190 BRIJ 35 0 1 190 Sodium formate 10 mM 200 CHA...

Страница 212: ...en sample scanning over a range of wavelengths can be necessary to determine the best wavelength for a particular analysis 1 Willard H H and others Instrumental Methods of Analysis 6th ed Litton Educa...

Страница 213: ...lder 12 Allene C C 2 acyclic 210 230 21 000 Allene C C 3 260 35 000 Allene C C 4 300 52 000 Allene C C 5 330 118 000 Allene C C 2 alicyclic 230 260 3000 8000 Ethylenic Acetylenic C C C C 219 6 500 Eth...

Страница 214: ...C 14 Solvent Considerations...

Страница 215: ...al 3 22 other parameters 3 20 signal adjusting 3 20 single wavelength signal 3 22 single channel 3 20 analog signals 2 6 anthracene 3 53 3 64 audience and purpose iv Auto Zero key 3 12 automatic secon...

Страница 216: ...r connecting 2 28 2 29 charting difference plot 3 20 MaxPlot function 3 20 chemical hazard warning A 5 chemiluminescence 1 2 chromatography fluorescence 1 2 cleaning the flow cell 4 5 cleaning detecto...

Страница 217: ...ns C 9 deleting a timed event 3 47 design electronic 1 9 optical 1 9 detector exterior cleaning 4 15 overview 1 7 setup 2 2 DIAG key 3 13 diagnostic settings auto zero offset 5 10 5 13 contact closure...

Страница 218: ...excitation 1 3 energy units 1 6 3 19 Enter key 3 15 entering negative numbers 3 15 entrance slits 1 9 environmental specifications 2 2 B 1 equipment guidelines iv A 6 erbium filter 1 8 scan 3 53 erro...

Страница 219: ...hold timed event parameter 3 46 trace 3 13 Fluorescence screen display 3 11 icons 3 5 flushing flow cell 4 5 front left hand panel cover 4 4 functions analog outputs single channel 3 20 auto zero on w...

Страница 220: ...ests 5 10 5 12 inputs disabling 3 16 enabling 3 16 signals 2 11 inspecting flow cells 4 5 installation columns 2 3 network guidelines 2 8 2 21 installing a new lamp 4 12 intended use v inverting the c...

Страница 221: ...stics 3 14 warranty 4 13 Lamp key 3 14 lamp off icon 3 7 lamp on icon 3 6 lamp on off connections to 600 Series Pump 2 30 light filters 1 3 light sources excitation 1 3 line spikes 5 21 local remote c...

Страница 222: ...xt arrow 3 13 Next icon 3 8 Next key 3 13 noise adjusting filter 3 20 filters 3 19 specifications B 3 noise filtering 1 12 normalized units of fluorescence 1 5 numerical keys 3 14 O obtaining MaxPlot...

Страница 223: ...s B 2 performing verification procedures 3 34 personality board 1 13 photomultiplier tube 1 4 1 9 calibrating 1 12 gain setting 1 17 sensitivity 1 12 physical specifications B 1 plus minus key 3 15 PM...

Страница 224: ...maintenance 4 2 sample and reference energy diagnostic tests 5 10 5 11 sample energy 3 56 sample scan procedure 3 55 3 56 screens 3 55 when to run 3 56 sample exciting 1 4 Scale key 3 13 3 23 scale z...

Страница 225: ...entrance 1 9 slits exit 1 9 solvent buffered solvents C 6 guidelines C 2 miscibility C 3 C 6 reservoirs C 6 UV cutoff C 9 C 11 viscosity considerations C 6 spare parts 4 3 sparging overview C 8 specif...

Страница 226: ...operation 1 1 threshold events clearing 3 51 programming 3 47 tick marks generating 3 53 time constant changing 3 16 function 3 20 parameter 3 22 timed event parameter 3 45 timed events and methods 3...

Страница 227: ...ions 2 31 chart mark connections 2 31 configuring the detector lamp signal 2 30 connecting 2 29 2 33 inject start connections 2 32 lamp on off connections 2 30 Waters 717plus Autosampler auto zero con...

Страница 228: ...Index 14...

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