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HP 8453E UV-VIS User Manual (G1819

1. 93 NOTE Service and Maintenance Handheld Controller and Spectrophotometer Logbooks Troubleshooting tools are implemented in the software Refer to the sections Troubleshooting on page 79 Checking the Keyboard on page 84 Spectrophotometer Tests on page 96 Spectrophotometer Recalibrating the Wavelength Scale on page 99 and Accessories Recalibrating the Multicell Transport on page 101 94 Service and Maintenance Spectrophotometer Lamp History and Limits Spectrophotometer Lamp History and Limits The software of the handheld controller has the capability to prompt you when the hours of usage of the lamps or the number of ignitions exceeds a certain limit Limits can be set individually for both lamps by the user Checking the Lamp History and Setting the Lamp Limits The number of ignitions and the hours the lamps have been used is displayed on the Spectrophotometer EMF Limits screen To check or set the lamp hours and ignitions do the following Choose a task e g Single WL 2 Press the F5 key System and then press the F4 key Records 3 Inthe Records screen press the F1 key EMF select Setup Limits and press Enter In the Spectrophotometer EMF Limits screen use horizontal keys to select the appropriate edit box and use the numerical keys to type in your limits Press the F6 key Done to leave the screen Resetting the Lamp Counters Choose a task
2. NOTE Table 8 Service and Maintenance Spectrophotometer Tests Choose a task e g Single WL Press the F5 key System Press the F3 key Tests select Diagnostics amp Maintenance and press Enter In the Tests screen press the F2 key Intensity and the test will start For the intensity test the light path of the spectrophotometer must be free from any obstructions e g cells filters 5 By pressing the F8 key Take you can redo the test 6 Press the F6 key Print to print out your results NOTE 1 2 3 Press Escape to exit the intensity test The intensity test recommendations are listed in Table 8 Recommended Values for the Intensity Test Wavelength Range Number of Counts 190 220 nm gt 2000 190 350 nm gt 5000 350 500 nm gt 2000 500 950 nm gt 4000 950 1100 nm gt 200 Stability Test at 340 nm To check the stability of your baseline do the stability test During this test the HP 8453 spectrophotometer must not be exposed to any airflow ambient temperature changes and spikes coming from the line power Choose a task e g Single WL Press the F5 key System Press the F3 key Tests select Diagnostics amp Maintenance and press Enter 97 Service and Maintenance Spectrophotometer Tests 4 Inthe Tests screen press the F3 key Stability and the test will start 5 Press the F6 key Print to print out your results 6 Press Esca
3. e Standard sequence 76 Operating your HP 8453E UV visible Spectroscopy System Triggering the Spectrophotometer from an External Device When triggering a sample standard measurement the software of the handheld controller will start performing the associated sample standard sequence you have defined for your multicell transport 77 Operating your HP 8453E UV visible Spectroscopy System Triggering the Spectrophotometer from an External Device 78 Troubleshooting An overview over how you do a logical troubleshooting when your system fails Troubleshooting When your HP 8453E UV visible Spectroscopy System does not come up or does not work properly you have to apply troubleshooting procedures This chapter provides with troubleshooting procedures for the e HP 8453 spectrophotometer e handheld controller e HP 8453E UV visible Spectroscopy System 80 NOTE Troubleshooting Troubleshooting Your Spectrophotometer Troubleshooting Your Spectrophotometer This chapter gives you hints and tips how you can troubleshoot your HP 8453 spectrophotometer by checking the starting sequence of the instrument Starting Sequence of the Spectrophotometer When the spectrophotometer is turned on it runs through a selftest sequence The different stages of the selftest sequence are indicated by the e colour of front panel LED e speed of fan e movement of shutter To troubleshoot your instrument
4. A brief description accessories compatible with the HP 8453E UV visible Spectroscopy System and how to install them is given in Chapter 6 Installing Accessories Contents Installation and Start Up Full details of how to install and startup your system 9 Site Requirements for Your HP 8453 Spectrophotometer 11 Unpacking Your HP 8453E UV visible Spectroscopy System 14 Installing Your HP 8453 Spectrophotometer 15 Connecting the Handheld Controller 17 Installing the Printer 18 Starting the HP 8453E UV visible Spectroscopy System 19 Installation Checkout 22 Good Measurement Practices General operating conditions of the spectrophotometer 23 General Considerations 25 Inserting a Cell 36 Operating your HP 8453E UV visible Spectroscopy System General operating conditions of the handheld controller and spectrophotometer 37 Handheld Controller Overview 39 Spectrophotometer Overview 40 Software Overview 42 General Navigation Through the Tasks 53 Single Wavelength Task 55 Multi wavelength Task 56 Equation Task 57 Contents Spectrum Task 58 Quantification Task 59 Kinetics Task 61 Displaying of Data on the Screen 63 Saving Loading and Deleting Your Samples Standards and Timetraces 64 Saving Loading and Deleting Your Methods 67 Printing your Results 70 Defining a Sequence for the Multicell Transport 71 Setting the Parameters for the Sipper System 73 Switching the Lamps On and Off 74 Changing the PC c
5. Installing Accessories Sipper System 134 Appendix A Software and Firmware Upgrade How to upgrade the software of the handheld controller and firmware of the spectrophotometer Software and Firmware Upgrade How you upgrade the e software of the handheld controller or the e firmware of the spectrophotometer is described in this section The upgrade procedures can only be applied when a PC card with the appropriate system files loaded is available 136 NOTE 1 2 3 4 5 6 7 8 9 NOTE Software and Firmware Upgrade Upgrading the Software of the Handheld Controller Upgrading the Software of the Handheld Controller As outlined in the last section of this chapter Compatibility on page 104 the software of the handheld controller and the firmware of the spectrophotometer have to match This section describes the procedure how the software of the handheld controller is upgraded Prerequisite for this task is a PC card with the new software loaded Disconnect the handheld controller from the HP 8453 spectrophotometer Insert the PC card into the PC card slot of the handheld controller Reconnect your handheld controller to the HP 8453 spectrophotometer Choose a task e g Single WL Press the F5 key System Press the F4 key Records Select Controller G1S19A in the Records list box using the vertical arrow keys and press Enter Press the F5 key FW Update which brin
6. Key Characters Behind Key Key Characters Behind Key 0 1 2 5 M N O 1 A B C 6 P OQ R 2 DEF 7 S T U 3 G H 8 V W X 4 J K L 9 Y Z Escape and Enter Keys Escape Key The Escape key is always the appropriate key when you want to exit a screen without saving your settings Enter Key In dialogs you e confirm the settings you typed in e select an item in a list box 49 Operating your HP 8453E UV visible Spectroscopy System Software Overview by pressing the E nter Key In all task screens except for Single WL task you can select individual samples standards or timetraces in a list box Select one of the samples standards or timetraces and press Enter This will bring you in a dialog where you can edit the name of this sample standard or timetrace Online Help i key Context Sensitive Help When pressing the i key the software brings you into the help system The help topic which appears is always context sensitive that is it is related to the screen you are in or the item you highlighted You can select different items in the help menu by using the arrow keys and pressing enter to get more details on these topics Previous F6 key When you browse through the help menu a history file is logged internally This log file holds the different items screens you have been chosen since you entered the help menu With the Previous key you can scroll backwards in this history log file success
7. PC card 3 Select a method using the vertical arrow keys in the left list box and press the F6 key Delete Select whether you want to delete a Selected Method or All Methods and press Enter 69 NOTE Operating your HP 8453E UV visible Spectroscopy System Printing your Results Printing your Results In each of the tasks you can print your results Before applying the following procedure you should ensure the printer parameters are setup correctly Refer to Printer Printer Configuration on page 100 to get hints how you have setup the parameters for your printer Press the F3 key File Print select Print Results with the vertical arrow keys and press Enter In the Dialog Box that comes up enter e the number of copies you want to print e if you want to print to a PCL file or a printer Press the F6 key or select Print and press Enter to start printing You can stop and resume as well as delete print jobs from the spooler by pressing the F7 key 70 Operating your HP 8453E UV visible Spectroscopy System Defining a Sequence for the Multicell Transport Defining a Sequence for the Multicell Transport Your multicell transport can be used with the HP 8453E UV visible Spectroscopy System as an autosampler with 8 cell positions G1120A or 7 cell positions 89075D The software allows you to setup a measurement sequence which defines the cell position used for your e reference measure
8. Quartz Cells with transparent apertures Fluorescence Cells Plastic Cells Flow Cells We recommend a sipper system with a flow cell for obtaining the high precision measurements Using a flow cell eliminates the necessity of moving the cell between blank measurement and sample measurement Also the cell can be rinsed thoroughly with the solution to be measured The design of the flow cell should minimize entrapment of bubbles and flow channeling to provide the most reliable results 28 Figure 10 Good Measurement Practices General Considerations Handling and Maintaining Cells or Cuvettes Passivating New Cells When filling a non passivated new cell with your sample you will observe that air bubbles stick on the windows of your cell To prevent the formation of sticky bubbles rinse the cell with cleaning and passivating fluid part number 5062 8529 The cleaning procedure you should apply is described on the label of the cleaning fluid container Cleaning Cells The fats in fingerprints are significant absorbers in the UV region and if left on optical surfaces can cause erroneous results Wipe off all fingerprints and contaminants before using a sample cell Use only high quality lens tissues part number 9300 0761 and never dry the inside of a cell with lens tissues Dry the inside of the cell with pressurized oil free air that prevents the cell from getting contaminated with tissue particles or rinse the cell wi
9. and to power the cell stirring module If you need a faster stirring speed than can be obtained by connecting the manifold and cell stirring module in series you can connect separate supplies to the manifold and stirring module Figure 23 Tubing Connections for a Cell Stirring Module N B A Ve J D C N Table 13 Tubing Connections for a Cell Stirring Module Connection Comment A in B out Without stirring C in D out Without cell thermostatting A in B to D C out In series with cell thermostatting A and C in Band D out In parallel with cell thermostatting 111 Figure 24 Installing Accessories Long Path Cell Holder Long Path Cell Holder The HP 89076A long path cell holder is a sample cell holder which can be adjusted to hold most cylindrical and rectangular sample cells with path lengths of up to ten centimeters It uses the same mounting system as the other sample cell holders Long Path Cell Holder Cell stops The long path cell holder includes built in cell stops for accurate positioning of 1 2 5 and 10 cm sample cells The optical filter wheel 08451 60302 can be mounted on the long path cell holder in the same way it is mounted on other cell holders see Optical Filter Wheel on page 115 for details However instead of a screwdriver a 2 5 mm hex wrench is required to install the optical filter wheel on the long path cell holder Installing the Long Pa
10. set it up in the software Select a task e g Single WL Press the F5 key System Press the F2 key Configure select Printer with the vertical arrow keys and press Enter In the Dialogue Box that comes up select the printer model Deskjet or Laserjet using the vertical arrow keys and press Enter In the Connected to list box select HP 8453 using the vertical arrow keys and press Enter 6 To print a test page by highlight the Print Test Page button and press Enter Press the F6 key Done to exit the dialogue and save your settings 100 e wo Do Service and Maintenance Accessories Recalibrating the Multicell Transport Accessories Recalibrating the Multicell Transport Changes of the optimum positions of the individual cells of the multicell transport G1120A as well as 89075D can be checked by using the MCT Test Calibration tool To check and in case recalibrate the wavelength scale of your spectrophotometer apply the following procedure Choose a task e g Single WL Press the F5 key System Press the F3 key Tests select Diagnostics amp Maintenance and press Enter In the Tests screen press the F4 key Maintenance select MCT Test Calibration and press Enter Select the cell positions you want to test by marking the appropriate check boxes 6 Press the F8 key Execute to execute the test Select Adjust and press Enter to recalibrate the wavelength scale or select Cancel to leave
11. switch the instrument off Then push the power button of the spectrophotometer to switch it on again and check the starting sequence of the instrument as shown in Figure 19 The handheld controller should be connected to the spectrophotometer while you are troubleshooting the system When a check of the hardware of the spectrophotometer is necessary e g check cable connection of the fan refer to the Reference Manual of the HP 8453 spectrophotometer or call your service representative 81 Figure 19 Troubleshooting Troubleshooting Your Spectrophotometer Starting Sequence for Troubleshooting the HP 8453 Spectrophotometer Starting Sequence Error Indications Possible Cause s Action s Powerbutton is lit Voltage not in range check voltage range 90 V 264 V Power cable not connected or damaged exchange power cable No YES Power supply defective call service Front panel LED shows different electronic board lz dal Service colors then stays defective a Orange No YES Rar slats running fan gefectiveror not gt check connector cable high speed connected No call serv
12. that is the lever is horizontal 5 Put the tubing cassette on the pressure wheel by placing the cassette on the mounting pivot Figure 41 Replacing the Tubing Cassette Union Conical Adapter Mounting pivot 6 Press the cassette down to lock the right side snap lever on the locking bar 7 Connect the pump tubing to the other accessories see relevant handbook 130 Installing Accessories Sipper System Connecting the Sipper Tubing 1 Connect the tubing with the short cell fitting to the outlet of the flow cell The outlet of the flow cell is the connector that is not marked with an arrow Figure 42 Connecting Tubing to Flow Cell Short fitting at outlet D C Inlet Y U 2 Insert the flow cell into the cell holder of the spectrophotometer 3 Connect the fitting and ferrule to a union Figure 43 Connecting Tubing to Pump Fitting Ferrule Pump Tubing AO fe i 4 Connect the conical adapter to the union and insert the conical adapter in the pump tubing at the inlet side left side of the pump 5 Choose the 0 35 m long tubing with the long cell fitting on one end and the other end open Connect the long cell fitting to the inlet The inlet of the flow cell is at connector that is marked with an arrow 131 Installing Accessories Sipper System Figure 44 Connecting Tubing to Flow Cell 6 Insert the other end of the tub
13. How you can export data of the HP 8453E UV visible spectros copy system to other software applications 141 Exporting Data 143 Warranty Statement 155 Safety Information 158 Solvent Information 160 Lithium Batteries Information 161 Hewlett Packard on Internet 162 Installation and Start Up Full details of how to install and startup your system Installation and Start Up The following topics are covered in this section Site Requirements for Your HP 8453 Spectrophotometer on page 11 contains information about electrical requirements i e power lines power cords etc It also gives recommendation for minimum available bench space and environmental conditions in the laboratory Unpacking Your HP 8453E UV visible Spectroscopy System on page 14 contains information about what you do when the packing material is damaged or the shipment is incomplete It also gives a list of items which come with the instrument and handheld controller Installing Your HP 8453 Spectrophotometer on page 15 gives an overview of the instrument and explains pushbuttons indicators and line power switch It gives instructions where and how to do line power connection communication connections and where to install the waste drain tubing Starting the HP 8453E UV visible Spectroscopy System on page 19 describes the turn on procedure of the spectrophotometer and the warm up time required to fulfil all specifications In
14. Path Cell Holder Figure 26 Installed 10 cm Cylindrical Cell in the Long Path Cell Holder 114 Figure 27 Installing Accessories Optical Filter Wheel Optical Filter Wheel To achieve optimum measurement conditions optical filters may be necessary for spectral measurements of photosensitive samples Hewlett Packard offers an optical filter wheel assembly 08451 60302 see Figure 27 which can be mounted on the standard cell holder the adjustable cell holder or the thermostattable cell holder An optical filter wheel with the same filters but with a different mounting can be used with the multicell transport see User s Guide of the multicell transport Optical Filter Wheel Assembly Notches indicate filter The filter wheel rotates to four different positions Position zero is empty and permits 100 transmittance at all light wavelengths Positions one two and three have filters which absorb varying amounts of the UV spectrum Figure 27 shows the transmission characteristics of each filter 115 Figure 28 Table 14 Installing Accessories Optical Filter Wheel Transmission Characteristics of Filter Wheel Filters l 400 500 600 700 800 820 Filter Wheel Positions Position Filter 0 None 1 UV roll off 2 265 nm UV cut off at 50 T 3 295 nm UV cut off at 50 T The choice of when to use a filter and which filter to use should be made only after considering al
15. Service and Maintenance Compatibility Compatibility Spectrophotometer Hardware You connect the handheld controller through the CAN connector to the spectrophotometer The handheld controller is powered by and communicates through the CAN interface with the spectrophotometer Only spectrophotometers with serial number DE60400900 US53400500 or higher are compatible with the handheld controller Spectrophotometer Firmware Only spectrophotometers having firmware revisions Rev A 03 20 or later are compatible with the handheld controller For detailed information how to upgrade the firmware of the HP 8453 spectrophotometer refer to Upgrading the Firmware of the Spectrophotometer on page 138 HP ChemStation for UV Visible Spectroscopy The HP 8453 spectrophotometer can instead of connecting a handheld controller be controlled by a PC with HP ChemStation software loaded 104 Installing Accessories How to install accessories that are available to enhance the capabilities of your HP 8453 spectrophotometer Installing Accessories Many simple mechanical optical accessories are available to expand the capabilities of your HP 8453 spectrophotometer The first part of this section briefly describes these accessories and outlines how to install them These accessories include e Thermostattable cell holder e Cell stirring module e Long path cell holder e Optical filters The following more complex acce
16. Spectrophotometer Wavelength range System options promt for task settings Display contrast Printer settings Tests Performance Tests Maintenance and diagnostics Records Logbooks system error maintenance Firmware Software update Context Menu m key Date and Time About Restart Using Applications Spectrophoto meter Control Module Applications Measure Data Files Save Load Spectra Save Load Methods Save Load Sample Identification Quantification Timebased Measurements Background Correction Spectrophotometer Installing and Using Good Measurement Practice Diagnostic and Tests Troubleshooting Error Messages Hardware and Measurement Problems Control Module Configuring and Servicing Software structure and conventions Method Protection 52 Operating your HP 8453E UV visible Spectroscopy System General Navigation Through the Tasks General Navigation Through the Tasks A roadmap which helps you to access different tasks settings actions and informations in the software of the handheld controller is given in Figure 17 First try to locate the item you are interested in in the roadmap For example Wavelength Recalibration Then follow the lines connecting this item with boxes back until you finally hit the upper left corner task list box Now follow your path from the upper left corner d
17. Spectrum from the task list box Select your Data Type using the horizontal arrow keys Press the F6 key Done to save your settings and exit the screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Sample to make a measurement on your sample If you want to apply a mathematical operation on the spectra press the F4 key Math and select an operation Follow the instructions on the screen When the mathematical operation has been applied the screen is automatically updated How you save your results and your measurement parameters is described in Saving Loading and Deleting Your Samples Standards and Timetraces on page 64 and Saving Loading and Deleting Your Methods on page 67 58 e wo Dd 91 nn 11 12 13 14 a A A V NS Operating your HP 8453E UV visible Spectroscopy System Quantification Task Quantification Task Calibration Curve Select Quantification from the task list box Type in the appropriate analytical Wavelength using the numerical keys Select your Data Type using the horizontal arrow keys Select a Background Correction if necessary and type in the Reference Wavelength s Press the F6 key Done to save your settings and exit the screen Press the F2 key Settings and select Calibration Type in the name of your Analyte using the horizontal arrow keys Select a Unit and Calibration Curve Type Press the F6 key Done to save your
18. Values listed by ascending wavelengths File Structure of csv Files All files stored under the extension csv contain e a header to identify the method parameters e data points time versus absorbance The structure of csv file is shown in Figure 48 145 Figure 48 Table 20 Data Export Exporting Data Structure and Contents of csv Files Line 1 Line 2 Line 3 Line 4 Line 5 Line 6 Line Name of Timetrace Time Date Integration Time Wavelength Run Time Cycle Time Time Scale No of Pairs of Data Time Absorbance A detailed description of the meanings of the different items in Figure 48 is given in Table 20 Description of csv File Items of Figure 48 Item Description Name of Timetrace Time Date Integration Time Wavelength Run Time Cycle Time Time Scale No of Pairs of Data Time Absorbance Name assigned to timetrace in software Time at which the data were measured Date at which the data were measured Integration time default 0 5 sec Wavelength at which data has been measured nm Total measurement time Time interval for data acquisition 0 seconds 1 minutes Number of data pairs of timetrace Elapsed time absorbance value 146 NOTE NOTE Data Export Exporting Data Loading wav Files into the HP ChemStation UV visible Software The data export functionality of the HP 8453E UV visible spectr
19. YES YES YES spectrophotometer Handheld controller YES NO NO NO NO Spectrophotometer Logbooks Messages coming from the firmware of the spectrophotometer are logged in the following logbooks I System Logbook System Log which logs all actions carried out or seen by the spectrophotometer such as e UV lamp ignition e UV lamp off e Multicell transport disconnected e Blank e Shutter open closed e Stray light filter open closed e Analysis making a Sample or Standard measurement e Method saved deleted 91 Service and Maintenance Handheld Controller and Spectrophotometer Logbooks e System parameters changed For a complete list refer to the help system i key All entries of the system logbook will be lost after the spectrophotometer has been powered down 11 Error Logbook Error Log which logs all errors coming from the spectrophotometer or the software of the handheld controller such as e Vis lamp overcurrent e Lamp door open e raw data buffer overflow e no current through Tungsten lamp For a complete list refer to the help system i key or the service handbook of the HP 8453 spectrophotometer The entries in the error logbook are stored on the mainboard of the spectrophotometer They are reloaded when the system is booted up again 11 Maintenance Logbook Maint Log which logs maintenance tasks like e Firmware upgrade e UV or Vis lamp replaced e Filter assembly replaced e O
20. a Blank on Water with Bubbles Causing a Poor Baseline Figure 13 T T T T T T T T 0 8 Cc 2 fo 7p Ko lt 0 05 1 1 1 1 1 f 1 f 200 400 600 800 1000 Wavelength nm NOTE If your blank or spectra shows artifacts similar to the one in Figure 13 see Solvents on page 30 to optimize the measurement procedure 35 Good Measurement Practices Inserting a Cell Inserting a Cell Your spectrophotometer is shipped with the standard single cell cell holder you first have to install in the sample compartment This cell holder accommodates standard cells or flow cells To insert a sample cell cuvette in the cell holder 1 Move the locking lever to its up position 2 Insert the sample cell making sure you orient it correctly The frosted non clear sides of the sample cell should not be in the path of the light beam 3 Lock the sample cell in place by pushing the locking lever back down Small volume flow cells and particularly any cells with less than a 2 mm aperture may require use of the optional adjustable cell holder The adjustable cell holder helps you ensure the cells are properly centered in the light path 36 Operating your HP 8453E UV visible Spectroscopy System General operating conditions of the handheld controller and spectrophotometer Operating your HP 8453E UV visible Spectroscopy System This chapter gives you an overvi
21. and the short circuiting of fuseholders must be avoided Some adjustments described in the manual are made with power supplied to the instrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided as much as possible When inevitable this should be carried out by a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of 158 Table 22 WARNING CAUTION Safety Information rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting Safety Symbols Safety Symbols used on Instruments and in Manuals Symbol Description The apparatus is marked with this symbol when the user should refer to the J
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23. cable to the HP 8453 spectrophotometer 18 Connecting the Sipper Tubing 131 connecting tubing 107 connector GPIO 129 consumption line power 11 Contents item 51 contents of shipping container 14 Context Menu 46 Context Sensitive Help 50 Control 44 Control Module Keys 39 controlling the eight position multicell transport 122 cooling air 12 cut off filter 32 cut off wavelength 32 Cycle Time 61 cyclohexane 31 cyclopentane 31 D Dark Current Test 96 Data Type 55 56 57 58 59 Data type 67 Date amp Time 46 Defining a Measurement Sequence 71 definitions of the keys 39 degassed 32 delete methods 44 delete results 44 Deleting a Method on the Instrument 68 Deleting a Method on the PC card 69 Deleting a Timetrace 66 Deleting Your Samples Standards and Time Traces 66 Derivative 45 Deskjet 100 Diagnostics amp Maintenance 53 Dilution Factor 59 dimethyl formamide 31 dimethyl sulfoxide 31 dirty filters 117 display a selected spectrum or time trace 47 display contrast 45 Displaying a Spectrum or Timetrace 63 Displaying Multiple Spectra on the Screen 63 Displaying of Data on the Screen 63 Dissolution 147 Documentation 103 Done F6 key 48 dust 32 E electronic self tests 20 EMF Logbook 93 english language software 20 149 Index Enter Key 49 entrapment of bubbles 28 Equation 42 57 Equation Task 57 E
24. connector on the rear of the pump see Figure 37 When this cable is connected the control switch on the front panel does not function This prevents you using the pump manually during automatic operation 128 Installing Accessories Sipper System 5 Connect the other end of the cable to the GPIO connector on the rear of the spectrophotometer Figure 38 Rear View of Spectrophotometer Zp cE OOo p GPIO connector Installing the Pump Tubing 1 Remove the tubing cassette from the pressure wheel on the front of the pump by pressing the snap lock lever to the left and upwards Figure 39 Removing the Tubing Cassette 2 Move the pressure control lever of the tubing cassette see Figure 39 clockwise to the right most position that is the lever is horizontal 3 Put the pump tubing in the tubing cassette locating the fixing collars on each side of the cassette in the locating holes Make sure the fixing collars are 129 Installing Accessories Sipper System pointing upwards and the tubing cannot slide out of the cassette Figure 40 Tubing Cassette with Pump Tubing Pressure control lever Fixing collar must disappear in the locating hole Il 4 Make sure the pressure control lever of the tubing cassette is in the right most position
25. corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCI O gt gt 2COCl 2HCI This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Analysis grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solutions of organic acids acetic acid formic acid and so on in organic solvents For example a 1 solution of acetic acid in methanol will attack steel Solutions containing strong complexing agents for example EDTA ethylene diamine tetra acetic acid Mixtures of carbon tetrachloride with 2 propanol or THF 160 Lithium Batteries Information Lithium Batteries Information WARNING Danger of explosion if battery is incorrectly replaced Replace only with the same or equivalent type recommended by the equipment manufacturer Do not dispose of lithium batteries in domestic waste Transportation of discharged lithium batteries through carriers regulated by IATA ICAO ADR RID IMDG is not allowed Discharged lithium batteries must be disposed of locally according to national waste disposal regulations for batteries 161 Hewlett Packard on Internet Hewlett Packard on Internet For the latest informati
26. could damage the electronics of the multicell transport 120 Installing Accessories Eight position Multicell Transport Figure 32 Connector at Rear of Spectrophotometer 200000000 ieee Multicell transport connector 4 Turn on the spectrophotometer at the lower left part of the instrument The transport initializes that is the turnabouts moves to the HOME position 5 Wait until the boot process of the software has finished 6 To verify proper installation use the numerical keys of the handheld controller to move the multicell to different positions See Table 15 for key numbers and related multicell transport positions 121 Table 15 Installing Accessories Eight position Multicell Transport Key Numbers and related Multicell Transport Positions Key Number Multicell Transport Position 0 HOME position Cell 1 Cell 2 Cell 3 Cell 4 Cell 5 Cell 6 Cell 7 Cell 8 mo N oOo wo A WO N For controlling the eight position multicell transport from the software of the handheld controller refer to Defining a Sequence for the Multicell Transport on page 71 Accessories for the Eight position Multicell Transport Three accessories are available for the multicell transport to enhance the capabilities of your multicell transport e Stirring Module e Filter Kit e Cell Holder A brief description of the features of the different accessories will be g
27. damaged save them until the contents have been checked for completeness and the spectrophotometer handheld controller or printer have been mechanically and electrically checked If the shipping container or cushioning material is damaged notify the carrier as well as Hewlett Packard Save the shipping material for the carrier s inspection Check the contents of the shipping container against the list below If any items are missing or obviously damaged call Hewlett Packard 1 Unpack the spectrophotometer You should have the following components e Power cord to connect the spectrophotometer to line power e Waste tubing to connect the sample pan of your spectrophotometer to a waste container e Standard cell holder e Standard Quartz Cell e Checkout sample caffeine solution C1 Unpack the handheld controller You should have the following components e handheld controller with flexible connector cable fixed e Serial parallel printer cable for connecting parallel port of printer with serial port RS 232 of the spectrophotometer e 4 MByte PC card C1 Unpack the printer You should have the following components e Power module e Printer accessories for example ink cartridge in case of a DeskJet printer 14 _ Figure 1 Installation and Start Up Installing Your HP 8453 Spectrophotometer Your spectrophotometer is very easy to install This section provides an overview of the instrument and a checklist of
28. fa Start e Data Evaluation with user 4 Derivative defined Equation Spectrum Complete range Absorbance Blank e Display of Sample Spectra Multicell Transport Transmittance Sample e Measurement Sequence or 1 Derivative Start Multicell Transp Sipper bad e Mathematical Operations 4 Derivative on Spectra Quantification 1 Absorbance Blank e Display of Sample Standard Multicell Transport Transmittance Sample Spectra or 1 Derivative Standard e Background Correction Sipper ae e Measurement Sequence 4 Derivative Start Multicell Transp e Calibration e Display of Calibration Curve e Single Component Analysis Kinetic 1 Absorbance Blank e Time resolved Measurement Multicell Transport Run Display of Timetrace or Rate Calculation Sipper Operating your HP 8453E UV visible Spectroscopy System Software Overview Settings F2 key Under Settings you have access to depending on the task you are in the e setpoints of your task e g wavelength data type e parameters of your accessories e g pump time of sipper pump measurement sequence of multicell transport e display range of graphic e settings of your calibration analyte name unit curve type e recalculation of your results only Kinetics task File Print F3 key When you press the File Print key you can e load results samples standards timetraces from the PC card e save results samples standards timetraces to the PC card e delete results samples
29. gives you a complete list of error codes and messages which may be created by the firmware of the HP 8453 spectrophotometer whenever a internal error is detected The software will prompt you for the error by displaying an error message box with the appropriate description To troubleshoot your HP 8453E Spectroscopy System refer to columns Possible Cause s and Action s in Table 5 Table 5 System Error Messages and Troubleshooting Procedures Error Message Possible Cause s Action s Multicell Transport Home Position Not Multicell transport mechanism is Found No Current Through VIS Lamp No Voltage at VIS Lamp jammed Electronics failed Ignition failed Lamp is probably disconnected Lamp is defective Lamp power supply defective Main board defective see error No Current Through VIS Lamp Check if fixing screws of Multicell Transport are screwed down Check manually if the multicell transport can move freely along it s range Check for defective HOME switch defective MCT cable defective motor defective MCT interface Retry to start the lamp Reconnect tungsten lamp Replace tungsten lamp Replace SLS lamp power supply board Replace SPM main board See error No Current Through VIS Lamp 85 Troubleshooting Troubleshooting Your HP 8453E UV visible Spectroscopy System Error Messages Table 5 System Error Messages and Troubleshooting Procedures con
30. instruction manual in order to protect the apparatus against damage p Indicates dangerous voltages Indicates a protected ground terminal P Eye damage may result from directly viewing light produced by deuterium lamps used in detectors and spectrophotometers Always turn off the deuterium lamp before opening the lamp door on the instrument A warning alerts you to situations that could cause physical injury or damage to the equipment Do not proceed beyond a warning until you have fully understood and met the indicated conditions A caution alerts you to situations that could cause a possible loss of data Do not proceed beyond a caution until you have fully understood and met the indicated conditions 159 Solvent Information Solvent Information Observe the following recommendations on the use of solvents Flow Cells Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of flow cells Solvents Always filter solvents small particles can permanently block capillaries Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like nitric acid sulfuric acid especially at higher temperatures replace if your analysis method allows by phosphoric acid or phosphate buffer which are less
31. instructions refer to the Service Manual of the HP 8453 UV visible spectrophotometer which comes with your system 88 Service and Maintenance An overview over service and maintenance features of the HP 8453E UV visible spectroscopy system and accessories Service and Maintenance This chapter describes the service capabilities of your HP 8453E UV visible Spectroscopy System such as e logbook entries e lamp counters e system tests e printer configuration and basic maintenance tasks which are supported by the software of the handheld controller such as e recalibrating the wavelength scale of the spectrophotometer e recalibrating the multicell transport e replacement parts It also provides you with compatibility information on software firmware and hardware 90 Table 6 Service and Maintenance Handheld Controller and Spectrophotometer Logbooks Handheld Controller and Spectrophotometer Logbooks If the HP 8453E UV visible spectroscopy system does not work properly the logbooks for the spectrophotometer and the handheld controller will help you to find out what specific reasons cause the malfunction of the system Table 6 shows the logbooks available for the HP 8453 spectrophotometer and the handheld controller Logbooks Available for the Handheld Controller and Spectrophotometer System Error Maintenance Info EMF Module Logbook Logbook Logbook Logbook Logbook HP 8453 YES YES
32. least 15 minutes This time allows the system to thermally equilibrate If the instrument was not stored at room temperature before it was turned on allow more time for the instrument to stabilize In general the life of your rophotometer will n switching it off at frequent intervals eave the instrument powered up bud switch off the deuterium lamp if it is not expected a measurement will be made for the next 2 hours Lamp intensity of the deuterium lamp and lifetime of lamps decrease with use 21 3 Figure 6 Installation and Start Up Installation Checkout Installation checkout is used to determine if the HP 8453E UV visible spectroscopy system is functioning properly Be sure to verify the successful completion of the turn on selftest of the spectrophotometer that is the indicator ED on the front panel of the HP 8453 spectrophotometer is lit and Use the vertical arrow keys of your handheld controller to select the Single WL task then press Enter To exit the dialogue coming up press the F6 key Done Fil the Quartzcell which is shipped with the system with distilled watenand take ablan measurement by pressing the Blank Duttom at the front of the instrument see Figure 5 Empty the cell and fill it with the affein sample which is also shipped with your system Take a sample measurement by pressing the S mpl button at the front of the instrument see Figure 5 Press the F6 key Graphic to display
33. of the handheld controller see label on rear of controller to identify whether it s a 2 MB or 1 MB version you can choose between english and french language versions of the software In the Startup dialog box that appears use the up and down arrow keys to select the appropriate language and then press Enter To exit this dialog and to confirm your settings press the F6 key Done Changing the Language of the Software You select the language of the software of your handheld controller at the first startup of your system Having selected the language of the software in the start up dialog this dialog will not reappear when the system is restarted To change the language of the software you have to do the following Go into one of the task dialogs e g Single WL In the task dialog press the F5 key System 20 Installation and Start Up Starting the HP 8453E UV visible Spectroscopy System In the System dialog press the m key and select Language in the list box using the left and right arrow keys Select the appropriate language then press Enter and the F6 key Done to confirm your setings In the dialog that appears highlight the Yes button and press Enter to restart the system After restart of the system the new language setting will be active Instrument Warm up Technically once your spectrophotometer has passed the self tests it is ready to run samples For r may wan let th rophotometer warm up for at
34. settings and exit the screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Standard to make a measurement on your standard Press Enter key and type in the concentration of your standard using the numerical kys Press F6 key to exit the screen The calibration curve is automatically calculated and displayed Select a standard by using the horizontal arrow keys and press the F6 key to display a standard spectrum on the screen Analysis Press the F4 key Samples to get access to the Evaluation screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Sample to make a measurement on your sample Select a sample using the vertical arrow keys and press Enter Type in the Sample Name using the horizontal arrow keys Type in a Dilution Factor using the numerical keys 59 NOTE Operating your HP 8453E UV visible Spectroscopy System Quantification Task 7 Press the F6 key Done to save your settings and exit the screen 8 The result of your analysis is displayed on the screen 9 Select a sample by using the horizontal arrow keys and press the F6 key to display a sample spectrum on the screen How you save your results and your measurement parameters is described in Saving Loading and Deleting Your Samples Standards and Timetraces on page 64 and Saving Loading and Deleting Your Methods on page 67 60 NOTE NOTE Oper
35. the main installation procedure If you have accessories for the spectrophotometer which are not covered in this section see Chapter 6 Installing Accessories or refer to the documentation that was delivered with your accessories for detailed information Installing the Waste Tubing There is a waste outlet for the sample area It is used to drain any liquids which may come from the sample area in case of a leak or a spill to a waste container To connect your waste tubing to the spectrophotometer Lift the front part of the spectrophotometer up so that you can locate the waste outlet underneath the sample pan as shown in Figure 1 2 Connect the waste tubing which comes with your spectrophotometer to the waste outlet underneath the sample pan 3 Put the other end of the waste tubing into the waste container 15 Figure 2 Installation and Start Up Installing Your HP 8453 Spectrophotometer 4 Make sure that the waste tubing has a constant downslope from the spectrophotometer to the waste container 1 Put the cell holder into the sample compartment and tighten the two fixing screws See Figure 2 Mounting the Cell Holder Fixing screws Connecting the Spectrophotometer to the Line Power Your line voltage must be between 100 120 or 220 240 V AC 10 with a line frequency of 50 or 60 Hz 5 There is no voltage selector on your spectrophotometer because the power supply has automatic wide ranging ca
36. the screen without recalibrating the wavelength scale Press the F6 key Done to leave the screen 101 Table 10 Table 11 Service and Maintenance Replacement Parts Replacement Parts This section gives an overview over the replacement parts and part numbers available for the HP 8453E UV visible spectroscopy system For replacement parts of the multicell transport G1120A the sipper system 89068D and the HP 8453 spectrophotometer G1103A refer to the individual service and user handbooks of these devices Handheld Controller Table 10 helps you to identify the replacement parts and related part numbers for your handheld controller Replacement Parts for Handheld Controller Part HP Part Number Handheld Controller G1819A PC Card 4MB F1231A PC Card 6MB F1215C PC Card 10MB F1013C PC Card 20MB F1014C Printer Interface Table 11 helps you to identify the replacement parts and related part numbers for your printer interface Replacement Parts for Printer Interface Part HP Part Number Serial Parallel Printer Cable 5181 1529 102 Table 12 Service and Maintenance Replacement Parts Documentation Table 12 helps you to identify the related part numbers for the user documentation of your handheld controller Part Numbers for User Documentation Part HP Part Number User Manual G1819 90000 Quick Reference Posters G1819 90001 103 NOTE
37. the spectrum on the screen of your handheld controller The spectrum should resemble the one shown in Figure 6 Spectrum of Caffeine measured with a 10 mm Standard Quartz Cell 0 8 06 T a 0 0 Absorbance AU 200 220 240 260 280 300 320 340 Wavelength nm 22 Good Measurement Practices General operating conditions of the spectrophotometer Good Measurement Practices This chapter describes making measurements selecting material optical specification and type of cell handling and maintaining cells checklist for good results solvents selection sample preparation use of filters stirring and temperature control of sample how to insert cuvettes into the cell holder 24 Good Measurement Practices General Considerations General Considerations There are many factors that can affect the results of your measurements This section provides brief discussions of some of the more important ones Spectrophotometer Design The sample compartment of the HP 8453 spectrophotometer is open Unlike conventional instruments the Gigh The open sample area makes it easier to access it generally and to connect tubing to a flow cell or thermostattable cell holder Blank Reference and Sample Measurement Your spectrophotometer is a single beam instrument so you must measure a for m r le For the high accuracy measurements the blank and the sample measurement should closely follow each othe
38. to identify the type of data and method parameters e wavelength information e g Absorbance values The structure of wav file is shown in Figure 47 Structure and Contents of wav Files Line 1 Line 2 Line 3 Line 4 Line 5 Line 6 Line 7 Line 8 Line Filetype not used Time Date Resolution Integration Time not used Derivative Order not used Name of Spectrum not used Concentration not used not used Data Type No of Points not used Wavelength1 Wavelength2 Data Point 144 Table 19 Data Export Exporting Data A detailed description of the meanings of the different items in Figure 47 is given in Table 19 Description of wav File Items of Figure 47 Item Description Filetype Number which represents the type of file default 11 Time Time at which the data were measured Date Date at which the data were measured Resolution Resolution of instrument default 1 nm Integration Time Derivative Order Name of Spectrum Concentration Data Type No of Points Wavelength1 Wavelength2 Data Point Integration time default 0 5 sec Order of derivative of data e g 1 for first derivative Name assigned to spectrum in software Concentration of a standard only Quantification Number represents data type 1 Absorbance 2 Derivative 3 Transmittance Number of data points in file Lowest wavelength of spectrum Highest wavelength of spectrum
39. when the HP 8453E UV vis Spectroscopy System was turned on To resolve the problem apply the following procedure Disconnect the handheld controller from the spectrophotometer by unplugging the Can connector Insert the PC card Reconnect the handheld controller to the spectrophotometer by plugging in the Can connector in the right Can interface If the problem still remains then insert another PC card and redo step 1 through 3 to check if your PC card was defective If the problem still remains call your service representative 83 a AeA WO N m Troubleshooting Troubleshooting Your Handheld Controller Checking the Keyboard When the handheld controller is used very frequently the keys might show aging effects and do not work properly any more To check the performance of the keys of your keyboard individually apply the following procedure Choose a task e g Single WL Press the F5 key System Press the F3 key Tests select Diagnostics amp Maintenance and press Enter In the Tests screen press the F5 key Keyboard Press all keys of the keyboard successively When a key is working properly the symbol on the screen representing the key will turn dark To exit the keyboard test press Escape twice in a row 84 Troubleshooting Troubleshooting Your HP 8453E UV visible Spectroscopy System Error Messages Troubleshooting Your HP 8453E UV visible Spectroscopy System Error Messages Table 5
40. which is below 0 1 degrees of an arc Shift of the Instrument Light Beam due to non Parallel Cell Walls Light Beam in Parallel Cell Walls Light Beam out Light Beam in Non parallel Cell Walls Soe Light Beam out In applications where sample volume is limited apertwred or microcells are used The width of these cells is reduced to reduce the volume and the blank part of the cell must be blackened to avoid unwanted transmission and reflection through the side walls If the side walls are not blackened the result will be poor photometric accuracy and if different concentrations are measured poor linearity 26 Figure 8 lt A Good Measurement Practices General Considerations The disadvantage of apertured and microcells is that part of the light beam is blocked Not all the light passes through the sample and there can be some loss in sensitivity See Figure 8 for recommended and Figure 9 for cells you should not use with the instrument l gt Quartz Cells Quartz Cells with black apertures Recommended Cells gt CAUTION Quartz Cells with apertures having a width of less than 2mm when used with a multicell transport can lead to measurements of poor reproducibility 27 Good Measurement Practices General Considerations Figure 9 Cells You Should Not Use With the Instrument LS
41. 131 adapter conical 133 Add 45 Add Scalar 46 adjusting length of sipper tubing 132 Advanced 147 air circulation 12 air for cooling 12 ambient temperatures 12 Analysis 59 Analyte 59 Analyte name 67 analytes 25 Apertured Cells or Cuvettes 26 apertures 33 arrow keys 48 arrow keys to type in characters 49 arrow mark on flow cell 131 ASCII data format 142 ASCII files 143 B Background Correction 56 59 benzene 31 Blank 25 34 76 blank 25 Blank F8 key 47 blank pushbutton 40 blank spectrum 47 bubble formation 32 C cable sipper sampler GPIO 128 sipper GPIO 128 Calculation Time 61 Calibration 59 calibration 44 Calibration Curve 59 Calibration curve 67 calibration curve 46 Calibration Curve Type 59 CAN interface 104 carbon disulfide 31 carbon tetrachloride 31 cell fittings 131 Cell Holder 122 cell holder 125 Cell stirring module 106 changing language settings 20 Changing the PC card 75 Checking the Keyboard 84 Checkout sample 14 chloroform 31 Cleaning Cells 29 Clear sample measurement s 46 Clear standard measurement s 46 Clear timetrace measurement s 46 colloidal dispersions 32 Comment 68 common solvents 31 Configure 45 configuring your HP 8453E UV visible spectroscopy system 50 conical adapter 131 133 connecting waste tubing 133 Connecting the CAN cable of the hand held controller 17 Connecting the printer
42. 45 spectroscopic idioms 50 Spectrum 42 58 Spectrum of Caffeine 22 Spectrum Task 58 speed of fan 81 spooler 70 Stability Test 97 Standard 47 76 standard cells 36 Standard measurement 47 standard pushbutton 40 Standard Quartz Cell 14 Standard sequence 76 standard single cell cell holder 36 Standards 46 standards 50 Start 47 starting the pump 44 stirring 32 Stirring Module 122 stirring module 33 stoppered sample cell 31 Subtract 46 sulfuric acid 31 supply line power 11 System 44 System Error Messages 85 system logbook 45 system options 45 system tests 90 T Task Menu 47 task related information 51 Tasks 42 temperature control 32 temperature fluctuations 12 temperatures 12 Tests 45 tests 51 tests for the spectrophotometer 45 Thermal Denaturation 147 thermal equilibrium 108 Thermostattable cell holder 106 thermostattable cell holder 33 thermostatted water 108 thermostatted water bath 107 time trace 61 Timescale 61 timetraces 50 toluene 31 transmission characteristics of filters 124 Transmittance 45 trigger a measurement 76 Trigger Inputs 76 troubleshooting 51 Troubleshooting Procedures 85 Troubleshooting your handheld Con troller 83 Troubleshooting your HP 8453E UV visible Spectroscopy System 85 Troubleshooting your Spectrophotom eter 81 tubing 127 adjusting length 132 installing waste 133 pump 133 waste 133 tubing cass
43. User Manual HP 8453E UV visible Spectroscopy System Copyright Hewlett Packard Company 1998 All rights reserved Reproduction adaption or translation without prior written permission is prohibited except as allowed under the copyright laws HP Part No G1819 90003 Second edition 11 98 Printed in Germany Warranty The information contained in this document is subject to change without notice Hewlett Packard makes no warranty of any kind with regard to this material including but not limited to the implied warranties or merchantability and fitness for a particular purpose Hewlett Packard shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing performance or use of this material WARNING For details of safety see Safety Information on page 158 Warning Symbols Used In This Book The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect the apparatus against damage gt a AD Eye damage may result from directly viewing the light produced by the Deuterium lamp used in this product Always turn off the Deuterium lamp before opening the metal lamp door on the side of the instrument Hewlett Packard GmbH Chemical Analysis Group Europe Hewlett Packard Strasse 8 D 76337 Waldbronn Germany HP 8453E UV visible Spectroscopy System U
44. V Lamp UV Lamp Ignition Failed No UV Lamp Heater Current Blank has higher absorbance than sample spectrum Sticky Bubbles or floating particles in cell deflect and obscure light beam Blank or and sample medium is are not mixed homogeneously enough Impurity in blank medium Variation of Absorbance during blank sample measurement due to photodegradation or evaporation or thermal expansion of medium Deuterium lamp is defective Electronics and or optics defective Deuterium lamp is disconnected Deuterium lamp is defective Electronics failed see error No Current Through UV Lamp see error No Current Through UV Lamp see error No Current Through UV Lamp Ensure sample and blank use same solvent or chemical matrix Clean and passivate cells see Good Measurement Practices on page 23 Wait till blank sample medium equilibrates or stir blank sample medium Clean cell blank medium Use topped cells for blank sample measurement and or use UV cut off filter for blank sample measurement Screw down or replace deuterium lamp Replace SPM main board and or SDA data acquisition board and or optical unit Reconnect Deuterium lamp Replace Deuterium lamp Replace SLS lamp power supply board and or SPM main board see error No Current Through UV Lamp see error No Current Through UV Lamp see error No Current Through UV Lamp for detailed
45. ad Samples Standards with the vertical arrow keys and press Enter 2 Use the vertical arrow keys to select your samples standards and press Enter 3 To load your samples standards press F6 Done If you want to exit a dialog without loading your samples standards press Esc Loading a Timetrace only in Kinetics Press the F3 key File Print select Load Timetrace with the vertical arrow keys and press Enter Use the vertical arrow keys to select your timetrace and press Enter To load your timetrace press F6 Done 65 Operating your HP 8453E UV visible Spectroscopy System Saving Loading and Deleting Your Samples Standards and Timetraces Deleting Your Samples Standards and Timetraces Deleting Samples Standards only in Quantification from the PC card Press the F3 key File Print select Delete Samples Standards with the vertical arrow keys and press Enter Use the vertical arrow keys to select the samples standards you want to delete and press Enter To delete your samples standards press the F8 key Delete Deleting a Timetrace only in Kinetics from the PC card Press the F3 key File Print select Delete Timetrace with the vertical arrow keys and press Enter Use the vertical arrow keys to select the timetrace you want to delete and press Enter To delete your timetrace press the F8 key Delete Deleting Your Samples Standards and Timetraces from the volatile memory of the control
46. allation date all others from the ship date If buyer schedules or delays installation more than 30 days after delivery then warranty period starts on 31 day from date of shipment 60 and 61 days respectively for products shipped internationally HP warrants that its software and firmware designed by HP for use with a CPU will execute its programming instructions when properly installed on that CPU HP does not warrant that the operation of the CPU or software or firmware will be uninterrupted or error free Limitation of Warranty Onsite warranty services are provided at the initial installation point Installation and onsite warranty services are available only in HP service travel areas and only in the country of initial purchase unless buyer pays HP international prices for the product and services Warranties requiring return to HP are not limited to the country of purchase For installation and warranty services outside of HP s service travel area HP will provide a quotation for the applicable additional services If products eligible for installation and onsite warranty services are moved from the initial installation point the warranty will remain in effect only if the customer purchases additional inspection or installation services at the new site The foregoing warranty shall not apply to defects resulting from 1 improper or inadequate maintenance adjustment calibration or operation by buyer 2 buyer supplie
47. ard of the Handheld Controller 75 Triggering the Spectrophotometer from an External Device 76 Troubleshooting An overview over how you do a logical troubleshooting when your system fails 79 Troubleshooting Your Spectrophotometer 81 Troubleshooting Your Handheld Controller 83 Troubleshooting Your HP 8453E UV visible Spectroscopy Sys tem Error Messages 85 Service and Maintenance An overview over service and maintenance features of the HP S453E UV visible spectroscopy system and accessories 8 amp 9 Handheld Controller and Spectrophotometer Logbooks 91 Appendix A Contents Spectrophotometer Lamp History and Limits 95 Spectrophotometer Tests 96 Spectrophotometer Recalibrating the Wavelength Scale 99 Printer Printer Configuration 100 Accessories Recalibrating the Multicell Transport 101 Replacement Parts 102 Compatibility 104 Installing Accessories How to install accessories that are available to enhance the ca pabilities of your HP 8453 spectrophotometer 105 Thermostattable Cell Holder 107 Cell Stirring Module 109 Long Path Cell Holder 112 Optical Filter Wheel 115 Eight position Multicell Transport 119 Sipper System 127 Software and Firmware Upgrade How to upgrade the software of the handheld controller and firmware of the spectrophotometer 135 Upgrading the Software of the Handheld Controller 137 Upgrading the Firmware of the Spectrophotometer 138 Appendix B Contents Data Export
48. ating your HP 8453E UV visible Spectroscopy System Kinetics Task Kinetics Task Select Kinetic from the task list box Type ina Run Time total time of analysis a Cycle Time time between successive measurements using the numerical keys and select a Timescale For Cycle Times below 3 seconds plus twice the integration time the shutter will be kept open during the kinetic run Thus the samples will be irradiated with the full lamp light during the complete Run Time For Cycle Times below 2 seconds plus twice the integration time the stray light correction will not be applied This can lead to a decrease in instrument linearity in the UV region 3 Type in a Wavelength using the numerical keys and select a Rate Calculation 4 When a Rate Calculation has been selected specify a Calculation Time mane a 11 12 13 Range a Factor and if necessary a new unit to convert to Press the F6 key Done to save your settings and exit the screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Start to start your kinetic run The result of your measurement is automatically displayed on the screen After the kinetic run has finished press the F6 key to view the timetrace If you want to recalculate your rate coefficient based on the actual timetrace go to F2 Settings and select Recalculation Select a Rate Calculation specify a Calculation Time Range a Factor and if necessary a new un
49. bout This Edition First edition 05 98 Second edition 11 98 The publishing date indicates the current edition This date changes when a new edition is published Cz HEWLETT PACKARD In This Book This handbook describes what you have to do to install your HP 8453E UV visible spectroscopy system Most of the handbook deals with installing a complete system that is spectrophotometer handheld controller and printer However in the second half of this handbook you will find additional information about installing mecahnical and optical accessories accessory boards HP IB connections and configuration and software installation Printed in Germany 11 98 G1819 90003 IMAM G1819 90003
50. c acid 96 Water Acetonitrile 200 210 nm Cyclopentane n Hexane Glycerol 2 2 4 Trimethylpentane Methanol 210 220 nm n Butyl alcohol Isopropyl alcohol Cyclohexane Ethyl ether 245 260 nm Chloroform Ethyl acetate Methyl formate 265 275 nm Carbon tetrachloride Dimethyl sulfoxide Dimethyl formamide Acetic acid 280 290 nm Benzene Toluene m Xylene Above 300 nm Pyridine Acetone Carbon disulfide WARNING Many of the solvents in Table 1 are hazardous Be sure you fully understand their properties before using them When using volatile solvents such as acetone or methylene chloride make sure that the sample cell is stoppered Evaporation of a solvent can change 31 Good Measurement Practices General Considerations the solute concentration or cause solution noise due to solute convection currents Both of these will affect the accuracy of your measurements We also recommend stirring and temperature control when you use volatile solvents When using water as solvent we recommend using UV grade or HPLC grade water to reduce unwanted absorbance from the water If you are using the sipper sampler system the water should be degassed to avoid bubble formation in the flow cell especially if the water comes from a pressurized water supply Sample Preparation The sample cell should be rinsed three to five times with your intended solvent before you fill it with the pure solvent that will be used in the measureme
51. ch as paper disks magnetic tapes ribbons inks pens gases solvents columns syringes lamps septa needles filters frits fuses seals detector flow cell windows and so on 156 Warranty Statement Responsibilities of Hewlett Packard Hewlett Packard will provide warranty services as described in the following table Table 21 Warranty Services Services During Warranty Warranty Period Type HP PCE instruments 1 Year Onsite HP 1100 Series LC modules HP 8453 UV visible spectrophotometers CE LC UV visible supplies and accessories 90 Days Onsite Columns and consumables 90 Days Return to HP Gas discharge and tungsten lamps 30 Days Return to HP Repairs performed onsite by HP 90 Days Onsite This warranty may be modified in accordance with the law of your country Please consult your local HP office for the period of the warranty for shipping instructions and for the applicable wording of the local warranty Warranty services are included as specified for chemical analysis products and options purchased concurrently provided customer is located within a HP defined travel area HP warranty service provides for 8 a m to 5 p m onsite coverage Monday through Friday exclusive of HP holidays Columns and consumables are warranted to be free from defects for a period of 90 days after shipment and will be replaced on a return to HP basis if unused un HP repair warranty is limited to only the item repaired or r
52. d software hardware interfacing or consumables 3 unauthorized modification or misuse 155 Warranty Statement 4 operation outside of the environmental and electrical specifications for the product 5 improper site preparation and maintenance or 6 customer induced contamination or leaks THE WARRANTY SET FORTH IS EXCLUSIVE AND NO OTHER WARRANTY WHETHER WRITTEN OR ORAL IS EXPRESSED OR IMPLIED HP SPECIFICALLY DISCLAIMS THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE Limitation of Remedies and Liability THE REMEDIES PROVIDED HEREIN ARE BUYER S SOLE AND EXCLUSIVE REMEDIES IN NO EVENT SHALL HP BE LIABLE FOR DIRECT INDIRECT SPECIAL INCIDENTAL OR CONSEQUENTIAL DAMAGES INCLUDING LOSS OF PROFITS WHETHER BASED ON CONTRACT TORT OR ANY OTHER LEGAL THEORY Responsibilities of the Customer The customer shall provide 1 access to the products during the specified periods of coverage to perform maintenance 2 adequate working space around the products for servicing by HP personnel 3 access to and use of all information and facilities determined necessary by HP to service and or maintain the products insofar as these items may contain proprietary or classified information the customer shall assume full responsiblity for safeguarding and protection from wrongful use 4 routine operator maintenance and cleaning as specified in the HP operating and service manuals and 5 consumables su
53. d with the system Connecting the Peristaltic Pump to the Line Power Your peristaltic pump draws power from an external source It operates at a line voltage of 100 120 V or 220 24 V AC 10 with a line frequency of 50 or 60 Hz 5 respectively The appropriate power cord is supplied with the sipper system It plugs into the power input socket at the rear of the pump see Figure 37 The male end of each power cord is different and designed to match the wall socket of a piraticular country or region 127 Figure 37 Remote connector CAUTION Installing Accessories Sipper System Rear View of Peristaltic Pump 250V LINE T200mA 100 120V T100mA 220 240V X R EMOTE QW law RS 4 A A WV g EN ieee E l y Line power connector Installing the Pump Cables Read the label on the rear panel of your pump to check the pump has the correct voltage option 100 120 V 60 Hz or 220 240 V 50 Hz for operation from your line power supply It is not possible to select a line voltage different from that on the label of your pump Push the connector of the power cord into the line power connector on the rear panel of the pump see Figure 37 3 Push the other plug of the power cord into the line power source Push the connector of the sipper GPIO cable G1103 61609 or sipper sampler GPIO cable part number G1103 61608 into the remote control
54. description of how to install the multicell system is given here For more detailed information e g technical specifications refer to the documentation that is shipped with the eight position Multicell Transport The Eight position Multicell Transport Fixing screw Fixing screw Installing the Eight position Multicell Transport The power for the multicell transport is supplied by the multicell transport interface of the spectrophotometer As soon as the multicell transport connector is plugged in and the spectrophotometer turned on the multicell transport will be powered on and does a self calibration No additional power connection is needed 119 Installing Accessories Eight position Multicell Transport 1 Place the multicell transport in the sample compartment of the spectrophotometer See step Figure 31 Figure 31 Top View of the Multicell Transport in Spectrophotometer Right fixing screw 2 Move the cell holder of the multicell transport manually to the left most position and tighten the screw at the right side Move it now to the right most position and tighten the screw at the left side 3 Plug in the connector of the multicell transport at the rear of the spectrophotometer See Figure 32 NOTE Turn the HP 8453 spectrophotometer off before plugging in the connector of the multicell transport Plugging the multicell connector in while the instrument is running
55. e g Single WL 2 Press the F5 key System and then press the F4 key Records 3 Inthe Records screen press the F1 key EMF select Setup Limits and press Enter Press the F7 key Reset You will be prompted for resetting the lamp usage of the Deuterium and Tungsten lamp separately 95 Table 7 No to fF WO NH Service and Maintenance Spectrophotometer Tests Spectrophotometer Tests Tests checking the optical and electronic performance of the HP 8453 UV visible spectrophotometer can be carried out from the software The list of tests that can be done are e Dark Current test e Intensity test e Stability test Dark Current Test To check the electronic performance of the diode array do the dark current test Choose a task e g Single WL Press the F5 key System Press the F3 key Tests select Diagnostics amp Maintenance and press Enter In the Tests screen press the Fl key Dark Current and the test will start By pressing the F8 key Take you can redo the test Press the F6 key Print to print out your results Press Escape to exit the dark current test The dark current test recommendations are listed in Table 7 Recommended values for the Dark Current Test Lower Limit of Counts Upper Limit of Counts 0 12 000 Intensity Test To check the performance of the lamp the optical system the A D converter and the diode array do the intensity test 96 pe U DN
56. e info logbook e firmware software update interface Math F4 key only in Equation task The Math key allows you to choose one of the following mathematical operations e Absorbance e Transmittance e Derivative e Add 45 Operating your HP 8453E UV visible Spectroscopy System Software Overview e Add Scalar e Subtract e Multiply Scalar Samples Standards F4 key only in Quantification task In Quantification you can change from the Calibration screen to the Evaluation screen In Calibration you setup your calibration curve In Evaluation you analyze your samples by means of your calibration curve The concentrations of your samples are displayed on the screen Context Menu m key Depending on the Task you are in you have direct and easy access to the following actions when you press the m key e Lamps on off e Clear sample measurement s e Clear standard measurement s only Quantification task e Clear timetrace measurement s only Kinetic task e Export sample standard as wav file e Export timetrace as csv file When you go to System the definition of the Context Menu actions changes to e Date amp Time set date and time e About show system revision e Restart restart the control module Under Records which is an item under System you will have the actions e Info Log show latest instrument messages e About show system revision In the Graphic screen you can excep
57. e switch to the resident system the fan of the spectrophotometer will speed up and run at a higher speed Press the F4 key Records F5 key FW Update and choose the appropriate dlb file in the list box using the vertical arrow keys and press Enter Now press the F8 key Execute to start the firmware upgrade The system will display the current status of the upgrade process 138 Software and Firmware Upgrade Upgrading the Firmware of the Spectrophotometer 12 When the upgrade process is finished press the F7 key Transfer to restart the handheld controller and the spectrophotometer NOTE After the firmware upgrade has been completed the fan will slow down and the spectrophotometer will do a self test 139 Software and Firmware Upgrade Upgrading the Firmware of the Spectrophotometer 140 Appendix B Data Export How you can export data of the HP 8453E UV visible spectroscopy system to other software applications Data Export This chapter describes how you can export data of the HP 8453E UV visible spectroscopy system in ASCII format to other software applications The ASCII data format can be read for example by the HP ChemStation UV visible software and so allows you to load data e g sample spectra measured with the HP 8453E UV visible spectroscopy system into the HP ChemStation software for further evaluation 142 Table 18 Data Export Exporting Data Exporting Data Fi
58. ell holder to its base Remove the cell holder and turn it upside down Insert the cell stirring module into the cavity in the base of the thermostattable cell holder see Figure 22 109 Figure 22 Installing Accessories Cell Stirring Module Installing the Cell Stirring Module 4 Tighten the four screws flathead M3x6 mm that will hold the cell stirring module in place 5 Attach the thermostattable cell holder to its base 6 Mount the thermostattable cell holder back in the sample compartment Tubing Connections and Operation The cell stirring module can be driven by either water or air Water is probably the fluid of choice because it is more easily controlled Water temperature can be up to 100 C 212 F with a maximum allowable back pressure of 4 bar approximately 60 psi If air is used to drive the cell stirring module the pressure should be less than 0 3 bar approximately 5 psi when the stirrer is started Again the maximum pressure is 4 bar approximately 60 psi There are several ways you can connect a water or air supply to the cell stirring module see Figure 23 In all cases we recommend using 3 16 inch i d silicon tubing between the water supply and the stirring module e The stirring module can be used alone without the thermostattable functions of the cell holder 110 Installing Accessories Cell Stirring Module e The same water supply can be used to regulate sample cell temperature
59. eplaced 157 Safety Information Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Hewlett Packard assumes no liability for the customer s failure to comply with these requirements General This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards Operation Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses
60. er In the appropriate task e g kinetics for Timetrace press the m key Use the vertical arrow keys to select either Clear all samples standards timetraces or Clear selected samples standards timetraces To delete your samples standards timetraces press Enter 66 NOTE Operating your HP 8453E UV visible Spectroscopy System Saving Loading and Deleting Your Methods Saving Loading and Deleting Your Methods The method file holds information on the settings of your system during measurement like e Wavelength range of the instrument e Integration time of the instrument e Used wavelength s e Data type e Graphic settings In Quantification you will have additionally e Unit e Calibration curve e Analyte name In Kinetics you will have additionally e Kinetic timing e Kinetic Calculation e Rate unit When a multicell transport or a peristaltic pump is connected to the instrument the method furthermore holds the e Measurement sequence for the multicell transport and the e Pump parameters e g pump time for the peristaltic pump When you save a method it is always saved to the instrument To save it to the PC card you have to download it from the instrument to the card 67 NOTE Operating your HP 8453E UV visible Spectroscopy System Saving Loading and Deleting Your Methods Saving a Method Press the F3 key File Print select Method with the vertical arrow
61. ett Packard GmbH Hewlett Packard Strasse 8 D 76337 Waldbronn Germany Your Comments Are Welcome We welcome your evaluation of this book Your comments and suggestions help us improve our publications Please attach additional pages of comments if necessary 1 Please circle Yes or No for each of the 2 Please rate the following features of the book following for their usefulness Is it easy to find the information you 1 Inadequate 2 Adequate 3 Superior need when you need it Yes No Table of contents I 2 3 Is the information technically Index 1 2 38 accurate Yes No Tabs 1 2 3 Are the instructions clear and complete Yes No Glossary 1 2 3 Are there enough examples and Illustrations 1 2 3 illustrations Yes No Ar iiaed eben Yes N Examples 1 2 3 e concepts explained clearly es No Readability 1 2 3 Comments Name Title Company Address City and State Country Postal Code Phone Please tear out and mail or fax Hewlett Packard Company Publications Department 2850 Centerville Road Wilmington DE 19808 Fax 302 633 8911 HP 8453E UV visible Spectroscopy System User Manual G1819 90003 Second edition 11 98 Printed in Germany Hewlett Packard has the right to use submitted suggestions without obligation ode pue ploy se jd Ides you og PUT POSTAGE HERE Hewlett Packard Company Publications Department 2850 Centerville Road Wilmington DE 19808 A
62. ette 129 replacing 130 with pump tubing 130 Turning on the HP 8453E UV visible Spectroscopy System 19 Turning the Lamps on and off 74 turning the lamps on and off 44 Turning the Lamps on and off Short cut 74 turn on self test 22 type in names 48 U unions 131 133 Unit 57 59 67 Unpack the handheld controller 14 152 Index npack the printer 14 npack the spectrophotometer 14 pgrading the Firmware 138 pgrading the Software 137 sed wavelength s 67 seful wavelength range of solvents 31 ser Id 68 ser Manual 103 UV grade water 32 UV Vis ChemStation 104 UV vis ChemStation 142 Ges 4eeeaa vV vertical arrow keys 48 viscous solutions 33 volatile solvents 31 voltage line power 11 voltage option 128 Ww Wait time 73 waste container 15 133 waste tubing 133 Waste Tubing Connection 133 water 31 Wavelength 59 61 Wavelength range 67 Wavelength Recalibration 53 99 Wavelength s 56 Wavelengths 57 wedge shaped cells 26 153 Index 154 Warranty Statement Warranty Statement All Chemical Analysis Products Hewlett Packard HP warrants its chemical analysis products against defects in materials and workmanship For details of the warranty period in your country call HP During the warranty period HP will at its option repair or replace products which prove to be defective Products that are installed by HP are warranted from the inst
63. ew of definitions of keys on the control module definitions of the keys on the spectrophotometer software features navigating through the tasks setting the parameters in a task saving loading and deleting of data saving loading and deleting of a method printing your results setting up parameters for your accessories switching the lamps on an off changing your PC card and triggering the HP 8453E UV visible spectroscopy system from an external device 38 Operating your HP 8453E UV visible Spectroscopy System Handheld Controller Overview Handheld Controller Overview Figure 14 Description of Control Module Keys Status Bar gle WL TEI duk Spee By Action Bar C Use Wavelength Zz nm D Data Type Absorbance t Q Menu Bar Context Menu GD GG CG CF CD OnlineHelp Q Exit Screen Confirm without saving Re Settings Typing of numbers Screen navigation and characters and typing of numbers and manual control of accessories characters NOTE Press the i key of the handheld controller for online help NOTE The actual definitions of the keys change with task and context 39 Operating your HP 8453E UV visible Spectroscopy System Spectrophotometer Overview Spectrophotometer Overview The front view of the spectrophotometer is shown in Fig
64. g up the Printer 1 For more detailed instructions how to setup the printer refer to the documentation that comes with the printer e Remove all safety shipping material from the printer e Put in the ink cartridge s that come with the DeskJet printers nn he printer le with th rial en Pin he RS 232 interf f the HP 84 hotometer and with th lel en ntroni interface to the ne See Figure 4 Figure 4 Connecting the Printer Cable to the HP 8453 Spectrophotometer D as B o O 1 Connect the printer to line power using the power module and switch it on Installation and Start Up Starting the HP 8453E UV visible Spectroscopy System Before you turn on your spectrophotometer make sure the light path through the sample compartment is clear All filters should be removed from the light path Anything blocking or absorbing part of the light beam could cause an error indication when you turn on the spectrophotometer Turning On 1 Turn on your spectrophotometer with the pushbutton at the lower left part of the instrument The pushbutton will stay pressed in and light green if power is present Figure 5 Turning on the HP 8453E UV visible Spectroscopy System Indicator 89 Blank button Sample button Line power switch 2 The fan will start turning 3 The indicator at
65. gs you into the Control Module Firmware Update screen In the list box select the appropriate file and press the F8 key Execute to start the update process At the end of the software update process the module will automatically restart with the new software loaded 137 NOTE No ao FF WO DH NOTE 10 11 Software and Firmware Upgrade Upgrading the Firmware of the Spectrophotometer Upgrading the Firmware of the Spectrophotometer As outlined in the last section of this chapter Compatibility on page 104 the software of the handheld controller and the firmware of the spectrophotometer have to match This section describes the procedure how the firmware of the spectrophotometer is upgraded Prerequisite for this task is a PC card with the new spectrophotometer firmware loaded Disconnect the handheld controller from the HP 8453 spectrophotometer Insert the PC card into the PC card slot of the handheld controller Reconnect your handheld controller to the HP 8453 spectrophotometer Choose a task e g Single WL Press the F5 key System Press the F4 key Records Select HP 8453 Module in the Records list box using the vertical arrow keys and press Enter Press the F5 key FW Update which brings you into the Module Firmware Update screen Press the F7 key Transfer and wait until the system swaps to the resident system This will be indicated by a message on the screen During th
66. ice YES wrong firmware gt load new firmware Fan slows down low speed No main board defective call service YES check position of 3 shutter and move it shutter is blocked manually spring of shutter is z Shutter clicks P L gt reconnect spring No spring of shutter is il R broken call service YES LED is Orange ei irnam n Front panel LED lamps off 7 ea LED ts Hed gt Call service No instrument defective System OK refer to the Reference Manual of the HP 8453 82 Troubleshooting Troubleshooting Your Handheld Controller Troubleshooting Your Handheld Controller Resetting the Software If your handheld controller does not work correctly disconnect the handheld controller CAN connector from the rear of the spectrophotometer and reconnect it This will restart the software of the handheld controller If the problem still remains then power off the spectrophotometer and wait 1 minute then power the spectrophotometer on again check if the LED at the front of the spectrophotometer turned Green after the boot up sequence In case the LED stays Orange or Red refer to the Troubleshooting Your Spectrophotometer on page 81 for more help If the problem still remains call your service representative PC card not Recognized by the Controller When your PC card is not recognized by the handheld controller either the card is defective or the card has not been inserted
67. inetics The wavelength range displayed can be changed when you choose Graphic in the Settings menu Miscellaneous Menus and Key Definitions The action keys are not only used in the Task menus but also in various different contexts like the Settings menu or other sub menus 47 Operating your HP 8453E UV visible Spectroscopy System Software Overview The definition of the keys changes with context and sub menu Their meaning can be easily deduced from the icon displayed and the action to be carried out Only the most important definitions are given here Done F6 key In the Settings menu screens are displayed allowing you to enter parameters for your task To save your entries and exit the screen press the Done key Whenever you want to exit a screen without saving your entries press the Escape key Print F6 key In the Records sub menu you can list the log book entries of several logbooks To get a hardcopy of these logbooks select the appropriate logbook and press F6 In the Test submenu you can printout the test results by pressing the F6 key Navigation Keys Arrow keys In all dialogs where you can e edit entryboxes e select options e select items from a list box e select and unselect check boxes e turn fields on and off the arrow keys and alphanumeric keys are activated and help in setting up your parameters For all edit boxes where you have to e type in names of samples standards files me
68. ing in the hole in the front cover of the spectrophotometer and push in the tubing until it comes out at the top part of the front panel of the spectrophotometer Figure 45 Installing Tubing in the Spectrophotometer Hole for tubing 7 Adjust the length of the sipper tubing that comes out of your front panel until it meets with the requirements of your sample containers 132 Installing Accessories Sipper System Waste Tubing Connection To install waste tubing choose the 1 5 m long tubing with the two hexagonal fitting on either end On one end of the tubing connect the fitting and ferrule to a union Figure 46 Connecting Waste Tubing to Pump Fitting Ferrule Union ae Conical Adapter Pump Tubing oo Connect the conical adapter to the union and insert the conical adapter in the pump tubing at the outlet side right side of the pump 3 Put the other end of the waste tubing in your waste container To verify proper installation use the numerical keys of the handheld controller to start and stop the pump See Table 17 for key numbers and related pump actions Table 17 Key Numbers and Related Pump Actions Key Number Pump Action 1 pump clockwise 2 pump counterclockwise 0 stop pumping For controlling the peristaltic pump from the software of the handheld controller refer to Setting the Parameters for the Sipper System on page 73 133
69. ion 54 Run Time 61 S Sample 25 47 76 sample 25 34 151 Index sample cell 25 32 sample degradation 116 Sample measurement 47 Sample Name 59 sample pushbutton 40 Sample return 73 Sample sequence 76 Samples 46 samples 50 save methods 44 save results 44 Saving a Method 68 Saving a Timetrace 64 Saving Your Samples Standards and Time Traces 64 Saving Loading Deleting of Methods 67 Search F8 key 50 sensitivity 27 serial number 104 Serial Parallel Printer Cable 102 Serial parallel printer cable 14 setting the language 20 Setting the Pump Parameters 73 Settings 44 Setup Sequence 71 shipping container contents 14 short cell fittings 131 shutter 81 signal to noise ratio 33 single beam instrument 25 Single Wavelength 42 Single Wavelength Task 55 Sipper System 127 Sipper system 106 sipper system 28 73 102 sipper system components 127 sipper tubing adjusting length 132 sipper sampler system 32 sipper sampler GPIO cable 128 sipper GPIO cable 128 snap lock lever 129 software 90 137 138 software language 20 software of the handheld controller 136 Software Overview 42 Software Tasks 43 solute convection 32 Solution 34 solution noise 32 solvent 25 solvent suitability 30 Solvents 30 Spectrophotometer Firmware 104 Spectrophotometer Hardware 104 Spectrophotometer Logbook 91 spectrophotometer settings
70. ion the filter wheel assembly clamp as shown in Figure 29 Replace the two screws but do not tighten them Installing the Optical Filter Wheel Assembly Bae Screw Clamp 4 Tilt the outer edge of the clamp up slightly 5 Bring the filter wheel assembly against the cell holder so that the clamp fits in the slot of the filter wheel assembly The mounting ridges on the filter wheel assembly should fit into the holes in the clamp The base of the filter wheel assembly should be against the base of the cell holder 6 Tighten the screws that hold the clamp 117 Installing Accessories Optical Filter Wheel Removing the Filter Wheel Assembly Loosen but do not remove the two screws that hold the clamp Separate the filter wheel assembly from the cell holder The filter wheel clamp may be left in place or removed In either case retighten the two screws Store the filter wheel in a clean plastic bag 118 Figure 30 Installing Accessories Eight position Multicell Transport Eight position Multicell Transport The eight position Multicell Transport part number G1120A is an accessory for the HP 8453 spectrophotometer It is a multi sample holder with multiple position capability see Figure 30 The multicell transport cell holder holds eight cells in a rack which can be held at a constant temperature with water circulated from a thermostatic bath provided by the user and not by Hewlett Packard A brief
71. it to convert to Press the F6 key Done to save your settings and exit the screen The result of your recalculation is automatically displayed on the screen 61 Operating your HP 8453E UV visible Spectroscopy System Kinetics Task NOTE How you save your results and your measurement parameters is described in Saving Loading and Deleting Your Samples Standards and Timetraces on page 64 and Saving Loading and Deleting Your Methods on page 67 62 Operating your HP 8453E UV visible Spectroscopy System Displaying of Data on the Screen Displaying of Data on the Screen You can display spectra or timetraces on the screen of your handheld controller The maximum number of spectra you can overlay on the display is three You cannot overlay several spectra in Single WL task and you cannot overlay several timetraces in Kinetics Displaying a Spectrum or Timetrace on the Screen Select a task from the task list box e g Single WL After you did the appropriate settings in the task dialog measure a blank Then measure a sample standard or timetrace depending on the task you are in Select the data you want to display by highlighting the appropriate item in the list box of the screen using the vertical arrow keys Press the F6 key Graphic to display the data Displaying Multiple Spectra on the Screen Select a task from the task list box except for Single WL and Kinetics After you did the appr
72. ively going you back into the screens you have been before Related F7 key Because the context sensitive help brings you always to topics directly linked to the screen you are in or the topic you highlighted your access to the help system is limited With the Related key the help system leads you through starting from your context sensitive help screen new help topics which have similar or related contents Search F8 key The help system not only includes topics on how to operate the handheld controller but also information on e installing your HP 8453E UV visible spectroscopy system e maintaining your HP 8453E UV visible spectroscopy system e configuring your HP 8453E UV visible spectroscopy system e spectroscopic idioms e g background correction 50 Operating your HP 8453E UV visible Spectroscopy System Software Overview e good measurement practice e g cell selection sample handling e task related information e g Single Wavelength Quantification e hardware related information e g installing accessories e error messages from the handheld controller message boxes like lamp door open to high current through Tungsten lamp appear e error messages from the spectrophotometer e g Red LED instrument does not turn on e troubleshooting e g how to do a blank measurement or a sample measurement e tests e g multicell transport test calibration dark current intensity Pressing
73. iven here For more details refer to the manual of the eight position multicell transport Stirring Module The stirring module part number G1120 60006 is an optional accessory for the eight position multicell transport The stirring module comprises the 122 Installing Accessories Eight position Multicell Transport stirring assembly four tubing clamps and 2 meters of 3 8 inch i d flexible tubing Two positions for mounting the stirring assembly are available One under the cell in the light path as shown in Figure 33 and one under the cell at the left side of the cell in the light path You can turn the stirring assembly by 90 degrees about the axis perpendicular to the base plate of the multicell transport thus bringing the fittings to three different positions Figure 33 Mounting the Stirring Assembly Inlet fitting D Outlet fitting E Stirring module mounted Second mounting position under the light path Cell holder screws Filter Kit Some compounds are photosensitive and may be decomposed during measurement This effect can be reduced or eliminated by using a filter to cut off the highly energetic low wavelength UV part of the spectrum The filter kit part number G1120 68707 comprises three threaded ring assemblies see Figure 34 having different filters The cut off wavelengths of the filters are different and absorb therefore varying amounts of the UV spectrum All threaded rings are labe
74. keys and press Enter 2 Press the F8 key Save As 3 Use horizontal and vertical arrow keys or alphanumeric keys to type in a file name for your method Confirm your method name by pressing Enter 5 As additional information you can mark the Protected check box type in a User Id and a Comment You can prevent your method from being changed by marking the Protected check box To save your method to the instrument press F6 Done 7 Ifyou want to copy a method to the PC card press the F2 key PC card 8 Press the F7 key lt lt Copy and the method will be stored on the PC card Loading a Method Press the F3 key File Print select Method with the vertical arrow keys and press Enter 2 Press the F2 key PC card 3 Select a method using the vertical arrow keys in the left list box and press the F8 key gt gt Copy The method will be automatically loaded to the instrument Deleting a Method on the Instrument Press the F3 key File Print select Method with the vertical arrow keys and press Enter 2 Press the Fl key Instrument 3 Press the F6 key Delete 4 Select whether you want to delete a Selected Method or All Methods and press Enter 68 Operating your HP 8453E UV visible Spectroscopy System Saving Loading and Deleting Your Methods Deleting a Method on the PC card Press the F3 key File Print select Method with the vertical arrow keys and press Enter 2 Press the F2 key
75. l the factors that affect your measurements If you decide that a filter is needed you should choose a filter that transmits the wavelengths needed for analytical information and that blocks the wavelengths that contribute to sample degradation Often your final choice will be a compromise since sometimes even the light at the wavelengths of analytical interest can affect your sample If you do not need a filter for a group of measurements you can move the filter wheel to position zero This permits full light transmission When you will not be using the filter wheel for an extended period of time you should remove the filter wheel assembly from the cell holder and store it in a clean plastic bag 116 Figure 29 Installing Accessories Optical Filter Wheel The optical filters of the filter wheel must be kept clean Dirty filters interfere with light transmission and lower the spectrophotometer performance These filters may be cleaned with isopropanol and photographic lens tissues Installing the Filter Wheel Assembly Installing the filter wheel assembly is fairly simple The procedure is the same for all three cell holders You will need a Phillips screwdriver to install the filter wheel assembly However if you install the filter wheel on the long path cell holder instead of a screwdriver a 2 5 mm hex wrench is required Remove the cell holder from the sample compartment 2 Remove the two screws shown in Figure 29 3 Posit
76. les created by the HP 8453E UV visible spectroscopy system can be exported as ASCII files to the PC card of the handheld controller From the PC card the ASCII files can then be retrieved into the HP ChemStation UV visible software or other software packages having an ASCII filter for data import There are different file types used by the HP 8453E UV visible Spectroscopy system in different tasks Accordingly different file types and extensions are used for data export to reflect the contents and data structure of the file File Extensions The file extension used by the HP 8453E UV visible spectroscopy system when saving timetraces in Kinetics is tr Data saved in all other modes will be stored under filenames having the extension sp When data is exported in ASCII format in Kinetics the files will have file extension esv whereas files exported in all other modes will have file extension wav This is summarized in Table 18 File Extensions used by the HP 8453E UV visible Spectroscopy System File extension for saving data File extension for exporting data Task internal format ASCII format Single WL sp wav Multi WL sp wav Equation sp wav Spectrum sp wav Quantification sp wav Kinetics tr CSV 143 Figure 47 Data Export Exporting Data File Structure of wav and csv Files File Structure of wav files All files stored under the extension wav contain e a header
77. lled with the corresponding cut off wavelength of the filters mounted Remove the multicell transport from the sample area Screw the threaded ring which holds the filter appropriate for your application in the circular 123 Installing Accessories Eight position Multicell Transport opening located at the rear part of the multicell transport If no threaded ring is screwed in the complete light coming from the lamps is let through Figure 34 Threaded Filter Ring for Multicell Transport Filter label Filter Thread Figure 35 shows the transmission characteristics of each filter Figure 35 Transmission Characteristics of Filters 100 80 60 40 IT T j T 1 190 200 300 400 500 600 700 800 820 124 Table 16 Installing Accessories Eight position Multicell Transport Table 16 shows the type of filters available Filter Types and Labels Label Filter 1 UV roll off 2 265 nm UV cut off at 50 T 3 295 nm UV cut off at 50 T Cell Holder The cell holder has a capacity for eight cells The outside dimensions of individual cells must be 12 5 x 12 5 mm and the height from base of the cell to the sample area 15 mm During an analysis the position of individual cells is maintained by a flat spring inside each of the cell compartments The spring alone fixes the cell No additional fixing mechanism is needed see Figure 36 The cell holder can be thermostated by an exte
78. ment Blank e sample measurements Sample or Standard When defining a sequence which includes a reference measurement the HP 8453 spectrophotometer acts as a pseudo dual beam instrument Defining a Measurement Sequence for Blank and Samples Choose a task If you are in Quantification task make sure you are in the Evaluation not in the Calibration screen In Calibration press the F2 key Samples to change to the Evaluation screen Press the F2 key Settings select Sequence with the vertical arrow keys and press Enter In the Setup Sequence user interface press enter to mark the box for defining the blank measurement Use the horizontal arrow key to activate the edit box for the cell number and use the numerical keys to type in a cell position number Press the horizontal arrow key again to highlight the check box for the sample measurements and press Enter to mark the check box Use the horizontal arrow key s to activate the edit box for the cell number s and use the numerical keys to type in cell position number s To save your settings press F6 Done 71 NOTE Operating your HP 8453E UV visible Spectroscopy System Defining a Sequence for the Multicell Transport Defining a Measurement Sequence for Blank and Standards only in Quantification The measurement sequence you will define under Calibration in the Quantification task Standards is completely independent of the measurement sequence you have defi
79. mentation that comes with your DeskJet or LaserJet printer If you connect your instrument to a line voltage that is higher than specified shock hazard or damage to your instrument can occur Power Cords Different power cords are offered as options with the spectrophotometer The female end of each of the power cords is identical It plugs into the power input socket at the rear of the spectrophotometer The male end of each of the power cords is different and designed to match the wall socket of a particular country or region 11 WARNING WARNING WARNING Installation and Start Up Site Requirements for Your HP 8453 Spectrophotometer Always operate your instrument from a power outlet which has a ground connection Always use the Hewlett Packard power cord designed for your region Space The spectrophotometer is 34 4 cm 13 5 inches wide 56 0 cm 22 0 inches deep and 18 5 cm 7 3 inches high see Figure 5 It weighs only 14 kg 30 86 lbs so it will fit on almost any desk or laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side to allow for the circulation of air for cooling and approximately 8 cm 3 1 inches in the rear for electrical connections Additional space is required for your printer and accessories like pumps Environment Your spectrophotometer will operate within specifications at ambient temperatures of 0 to 55 C 82 to 131 F If you use the in
80. ments 28 HOME position 121 homogeneity 33 horizontal arrow keys 48 HP 8453 spectrophotometer 102 HPLC grade water 32 humidity 12 I i key 50 improving productivity and reproduc ibility 127 Index item 51 indicator 19 Info Log 46 Info Logbook 92 inserting flow cell in cell holder 131 inserting tubing in hole in front cover of spectrophotometer 132 installing tubing in spectrophotometer 132 waste tubing 133 Installing a Thermostattable Cell Hold er 107 Installing the Cell Stirring Module 109 Installing the Eight position Multicell Transport 119 Installing the Filter Wheel Assembly 117 Installing the Long Path Cell Holder 112 Installing the Pump Cables 128 Installing the Pump Tubing 129 installing the waste tubing 15 installing your HP 8453E UV visible spectroscopy system 50 Integration time 67 Intensity Test 96 isopropyl alcohol 31 K Kinetic 42 Kinetic Calculation 67 Kinetic run 47 Kinetic timing 67 Kinetics 147 Kinetics Task 61 L lamp counters 90 Lamp History 95 Lamp Limits 95 Lamps on off 46 lamps start turning on 20 language settings 20 Laserjet 100 lens tissues 29 lever pressure control 129 snap lock 129 light beam 26 29 line frequency 11 line power consumption 11 line power supply 11 line power switch 41 150 Index line voltage 11 liquid samples 25 load method 44 load results 44 Loading wav Files int
81. n light is off the instrument is turned off 41 Operating your HP 8453E UV visible Spectroscopy System Software Overview Software Overview This section provides you with a general overview over the features of the software of the handheld controller and how you can get access to them All software features are grouped by the definition of the keys Tasks F1 key When booting up the system the software comes up with a screen giving the user the possibility to choose between six different software tasks Single Wavelength Multi Wavelength Equation 1 2 3 4 Spectrum 5 Quantification 6 Kinetics 42 Operating your HP 8453E UV visible Spectroscopy System Software Overview The general feature set of the individual tasks is shown in Table 2 Table 2 Feature Set of Software Tasks Number of Task Wavelengths Set of Readings Actions Task Specials Accessories Single WL 1 Absorbance Blank e Display of Sample Spectrum Multicell Transport Transmittance Sample or 1 Derivative Sipper 4 Derivative Multi WL 4 Absorbance Blank e Display of Sample Spectra Multicell Transport Transmittance Sample e Background Correction or 1 Derivative e Measurement Sequence Sipper Start ere SN Multicell Transp 4 Derivative Equation 4 Absorbance Blank e Display of Sample Spectra Multicell Transport Transmittance S e Measurement Sequence or oy ample an 1 Derivative Multicell Transp Sipper
82. ned under Evaluation in the Quantification task Samples Choose the Quantification task Press the F4 key Standards if you are not already in the Calibration screen of the Quantification task Press the F2 key Settings select Sequence with the vertical arrow keys and press Enter In the Setup Sequence user interface press enter to mark the box for defining the blank measurement Use the horizontal arrow key to activate the edit box for the cell number and use the numerical keys to type in a cell position number Press the horizontal arrow key again to highlight the check box for the standard measurements and press Enter to mark the check box Use the horizontal arrow key s to activate the edit box for the cell number s and use the numerical keys to type in cell position number s To save your settings press F6 Done 72 Operating your HP 8453E UV visible Spectroscopy System Setting the Parameters for the Sipper System Setting the Parameters for the Sipper System For high precision measurements a sipper system part number 89068D has to be used with the HP 8453E UV visible Spectroscopy System It comprises a flow cell connectors and tubings and a peristaltic pump In the software of the handheld controller you can define parameters for the peristaltic pump like e Pump time ins e Wait time in s e Sample return in Setting the Pump Parameters 1 Choose a task 2 Press the F2 key Setti
83. ng with the light beam Make sure the tubing is securely attached it expands when heated and if it is not secure a leak will result Insert the sample cell and lower the lever down to lock the cell in place 107 Installing Accessories Thermostattable Cell Holder Begin pumping thermostatted water through the manifold Wait for the sample cell and sample to reach thermal equilibrium before you make any measurements The time required to reach thermal equilibrium will vary depending on the water temperature and the sample but generally should take about five minutes When the thermostattable cell holder is not in use it is best to disconnect the tubing and drain the manifold 108 Figure 21 Installing Accessories Cell Stirring Module Cell Stirring Module The HP 89055A cell stirring module shown in Figure 21 mounts inside the base of the thermostattable cell holder It provides the capability of magnetic induction stirring inside a standard 1 cm sample cell The cell stirring module contains a plastic encased magnetic impeller that can be driven by water or pressurized air When you put a magnetic stirring bar 9301 1161 into the filled sample cell the stirring bar rotates in tandem with the impeller magnet thus stirring the sample Cell Stirring Module Installing the Cell Stirring Module Remove the thermostattable cell holder from the sample compartment Remove the three screws that hold the thermostattable c
84. ngs select Sipper with the vertical arrow keys and press Enter 3 Inthe Sipper Settings user interface use the horizontal arrow key to activate the edit box for the Pump Time and use the numerical keys to type in your pumping time 4 Dothe same for the Wait Time and Sample Return 5 To save your settings press F6 Done 73 pe U DN Operating your HP 8453E UV visible Spectroscopy System Switching the Lamps On and Off Switching the Lamps On and Off Turning the Lamps On and Off in the System Menu Choose a task Press the F5 key System and then the F1 key Control In the Control list box select Lamps and press Enter Use the horizontal arrow keys to select a lamp and vertical arrow keys to turn it on or off To save your settings press F6 Done Turning the Lamps On and Off Shortcut Choose a task Press the m key select Lamps on off using the vertical arrow keys and press Enter Use the horizontal arrow keys to select a lamp and vertical arrow keys to turn it on or off To save your settings press F6 Done 74 Figure 18 Operating your HP 8453E UV visible Spectroscopy System Changing the PC card of the Handheld Controller Changing the PC card of the Handheld Controller Data like for example sample spectra can be saved to and retrieved from the PC card of the handheld controller How the PC card is changed is described in the following procedure Disconnect the control module from
85. nt Turning the cell upside down on a small stack of absorbent tissues will help remove any residual solvent This treatment will minimize contamination from previous experiments Samples which contain colloidal dispersions dust or other particulate matter should be filtered centrifuged or allowed to settle If not the overall attenuation of transmittance spectrum due to light scattering and or reflection will hide the spectral information from the analyte Photosensitive Samples A few substances are very photosensitive They degrade or undergo photochemical reactions if exposed to light This can be easily seen by a decrease of sample absorbance over time Use of Filters At shorter wavelengths higher energy UV light is most likely to degrade photosensitive samples If you have a problem you can selectively block portions of the UV spectrum with a UV cut off filter An optical filter wheel assembly with three cut off filters is available for the spectrophotometer The cut off wavelength of the filter you choose should be low enough that it does not eliminate important spectral information but high enough that it blocks the light that could degrade your sample If you use a filter with your samples you must use the same filter when you make your blank measurement For further information about the filter wheel see Optical Filter Wheel on page 115 32 Good Measurement Practices General Considerations Turning the Dy Lam
86. o the UV vis ChemStation Software 147 Loading a Method 68 Loading a Timetrace 65 Loading Your Samples Standards and Time Traces 65 logbook entries 90 Long path cell holder 106 M magnetic impeller 109 magnetic induction stirring 109 maintaining your HP 8453E UV visible spectroscopy system 50 Maintenance 99 101 maintenance and diagnostic tests 45 Maintenance Logbook 92 maintenance logbook 45 Making measurements 25 malfunction of the system 91 Math 45 58 mathematical operation 58 Measurement sequence 67 methanol 31 method file 67 methyl formate 31 m key 46 64 65 74 Mounting the Cell Holder 16 moving the multicell transport 44 Multi Wavelength 42 Multi Wavelength Task 56 Multicell Transport 76 Multicell transport 106 multicell transport 49 67 71 102 multicell transport interface 119 Multicell Transport Positions 122 Multiply Scalar 46 m xylene 31 N Navigation Keys Arrow keys 48 n butyl alcohol 31 n hexane 31 Numerical Keys 48 numerical keys 49 121 o online help 39 online Help i key 50 operating conditions 12 optical filter 32 Optical filters 106 optical self tests 20 Optical Specifications of Cells 26 optical surfaces 29 P parallelism 26 part numbers 102 particulate matter 32 Passivating new Cells 29 PC card not recognised by the Control ler 83 PCL file 70 peristaltic pump 67 127 photochemical
87. on on products and services visit our worldwide web site on the Internet at http www hp com go chem 162 Your Comments Are Welcome We welcome your evaluation of this book Your comments and suggestions help us improve our publications Please attach additional pages of comments if necessary 1 Please circle Yes or No for each of the 2 Please rate the following features of the book following for their usefulness Is it easy to find the information you 1 Inadequate 2 Adequate 3 Superior need when you need it Yes No Table of contents I 2 3 Is the information technically Index 1 2 38 accurate Yes No Tabs 1 2 3 Are the instructions clear and complete Yes No Glossary 1 2 3 Are there enough examples and Illustrations 1 2 3 illustrations Yes No Ar iiaed eben Yes N Examples 1 2 3 e concepts explained clearly es No Readability 1 2 3 Comments Name Title Company Address City and State Country Postal Code Phone Please tear out and mail or fax Hewlett Packard GmbH Chemical Analysis Group Europe Hewlett Packard Strasse 8 D 76337 Waldbronn Germany Fax 49 7243 602 501 HP 8453E UV visible Spectroscopy System User Manual G1819 90003 Second edition 11 98 Printed in Germany Hewlett Packard has the right to use submitted suggestions without obligation ode pue ploy se jd Ides you og PUT POSTAGE HERE Marketing Communications Group Hewl
88. opriate settings in the task dialog measure a blank Then measure a sample or standard depending on the task you are in Select the data you want to display by first highlighting the appropriate item in the list box of the screen and then marking it using the vertical arrow keys Do the same for the up to two additional samples or standards you want to overlay in the graphic window Press the F6 key Graphic to display the samples or standards you select 63 NOTE NOTE Operating your HP 8453E UV visible Spectroscopy System Saving Loading and Deleting Your Samples Standards and Timetraces Saving Loading and Deleting Your Samples Standards and Timetraces Saving Your Samples Standards and Timetraces When you save your data by selecting the save item in the File Print list box all data is always saved to the PC card of your handheld controller Saving data while no PC card is installed will lead to an error message Saving Samples Standards only in Quantification Press the F3 key File Print select Save Samples Standards with the vertical arrow keys and press Enter Use horizontal vertical arrow keys and alpha numerical keys to type in a file name for your samples standards The default file extension is sp 3 Confirm your file name by pressing Enter To save your samples standards press F6 Done If you want to exit a dialog without saving your samples standards press Esc Expo
89. oscopy system can be used to transfer data from the handheld controller to the HP ChemStation UV visible software This feature is not applicable to timetraces exported as csv files only to spectra exported as wav files The PC used for running the HP ChemStation software and loading the data of the handheld controller must have a PC card drive Apply the following procedure to export data to the HP ChemStation software Select a task e g Single WL Press the m key select Export and press Enter In the Dialog Box that comes up type in a file name by using horizontal and vertical arrow keys Press Enter to confirm your file name Press the F6 key to export a spectrum to the PC card wav file extension 5 Remove the PC card from the handheld controller and put it into the PC card drive of your PC Load the data into the HP ChemStation software by selecting the Import Samples Standards Auxiliary item from the File menu item The wav files can be loaded in all modes of the HP ChemStation except for Kinetics mode and Thermal Denaturation mode Auxiliary spectra can only be loaded in Advanced or Dissolution single bath and multi bath mode 147 Data Export Exporting Data 148 Index Numerics 2 2 4 trimethylpentane 31 4 MByte PC card 14 A Absorbance 45 accessories 44 accurate results 25 acetic acid 31 acetone 31 acetonitrile 31 Action Keys F6 F7 F8 key 47 adapter conical
90. ossible Cause s Action s Wavelength Calibration Failed Wavelength Recalibration Data Lost Raw Data Buffer Overflow Excessive Diode Dark Current Deuterium lamp disconnected Deuterium lamp is defective Filter assembly defective Optical components misalignment Processing of calibration data invalid Dip switch settings of 8 bit configuration switch are wrong Firmware has been updated SPM main board has been replaced Spectra acquired cannot be transferred fast enough to handheld controller SDA data acquisition board unable to set dark current Photo Diode s defective Reconnect deuterium lamp Screw down or replace deuterium lamp Replace shutter filter assembly Screw down lamps or replace optical unit Replace SPM main board Check dip switch settings and perform a wavelength recalibration Perform a wavelength recalibration Perform a wavelength recalibration Reduce number of spectra acquired or raise cycle time or reduce wavelength range or increase memory on SPM main board Replace SDA data acquisition board of spectrophotometer Replace optical unit 87 Troubleshooting Troubleshooting Your HP 8453E UV visible Spectroscopy System Error Messages Table 5 System Error Messages and Troubleshooting Procedures continued Error Message Possible Cause s Action s Invalid Data Points in Spectrum No Current Through UV Lamp No Voltage at U
91. own to the selected item When leaving a box you have to press the appropriate key connected to the line you follow For the Wavelength Recalibration example you will get the following path Select one of the tasks e g Single WL In the task screen press the System key In the system screen press Tests Then select Diagnostics amp Maintenance and press Enter In the Diagnostics amp Maintenance screen press the Maintenance key and select Wavelength Recalibration Follow the instructions on the screen 53 Operating your HP 8453E UV visible Spectroscopy System General Navigation Through the Tasks Roadmap for Software Navigation Figure 17 slusAq 4N A Y arepdn 607 Boq 100g 3wa 4 slinsey lUud GMW Jue w s ie ied Hae uoneinojesoy besn u wnnsul o 10924 due 10 Sw 5 ile wed poyan alejeq enes auey oul uonesqueoey uonesqieoey aoeneully 31120 ee SGA 74881 EOIN yGuajenen 08s B a reos w SOROS 9S l L z awl 21940 eve wl PLOT aw uny ueu queuing x weoghe Ayyiqe Aysuayuy ojeg 3 uoHIsinboy pieogiey aqureyy HIIQELS suau yeg SONOUIY
92. p off The short wavelength radiation leading to photodegradation comes from the light of the D Lamp For application where readings are taken at wavelengths above 400 nm the Do Lamp can be turned off The light intensity supplied by the Tungsten lamp is sufficient for a good signal to noise ratio over the wavelength range 400 nm 1100 nm When using cells with small apertures you should check the signal to noise ratio by making sample measurements under conditions of your application Stirring and Temperature Control Solution homogeneity can be a problem especially for viscous solutions There are cases where due to convection induced gradients rapid absorbance changes may give irreproducible data These changes can be observed spectroscopically by taking measurements with short integration times To minimize convection effects keep the temperature of your sample the same as the cell holder or environmental temperature Problems like these can also be minimized by using a thermostattable cell holder and or a stirring module A similar effect can occur in cases of incomplete mixing This is especially true where the specific gravities or miscibilities of the solvent and analyte are quite different Again stirring is a way to prevent this kind of problem In an unstirred cell it is sometimes possible to observe local photodegradation of sensitive analytes Because the actual volume of the sample in the light path is very small stirring
93. pability Make sure the power switch of the spectrophotometer is in the off position that is the pushbutton stands out Plug the female end of the power cord into the power input socket at the rear of the spectrophotometer Plug the male end of the power cord into your electrical outlet 16 Installation and Start Up Connecting the Handheld Controller Connecting the Handheld Controller Connect the flexible CAN cable of the handheld controller to the right CAN interface at the rear of the spectrophotometer See Figure 3 Figure 3 Connecting the CAN Cable of the Handheld Controller iS GS gees Spel E CEES Ea o 6o __ _ 0 wares Right Can interface O The handheld controller is powered by the CAN interface of the spectrophotometer It does not need any additional power supply The software of the handheld controller is started automatically as soon as the HP 8453 is powered on and the controller connected to the spectrophotometer 17 Installation and Start Up Installing the Printer Detailed instructions for installing your printer are specific to the type and configuration of the printer and are provided with it This section gives a checklist of the main installation steps refer to the documentation that was delivered with your printer for detailed information Settin
94. pe to exit the stability test The stability test recommendations are listed in Table 9 Table 9 Recommended Values for the Stability Test Allowed Range in Counts 100 98 pe U DH QO HN Service and Maintenance Spectrophotometer Recalibrating the Wavelength Scale Spectrophotometer Recalibrating the Wavelength Scale Changes of the wavelength scale of the HP 8453 are normally negligible This is mainly due to the fact that there are no moving parts in the spectrophotometer doing the wavelength selection After changing lamps or the shutter assembly or severe mechanical shock there may be a slight chance of a wavelength shift To check and if necessary recalibrate the wavelength scale of your spectrophotometer apply the following procedure Choose a task e g Single WL Press the F5 key System Press the F3 key Tests select Diagnostics amp Maintenance and press Enter In the Tests screen press the F4 key Maintenance select Wavelength Recalibration and press Enter Press the F8 key Execute to execute the test Select Adjust and press Enter to recalibrate the wavelength scale or select Cancel to leave the screen without recalibrating the wavelength scale Press the F6 key Done to leave the screen 99 Service and Maintenance Printer Printer Configuration Printer Printer Configuration This section provides you with a procedure how you select your printer and
95. ptical unit replaced The entries in the maintenance logbook are stored on the mainboard of the spectrophotometer They are reloaded when the system is booted up again LI Info Logbook m key in Records screen which logs maintenance tasks like e UV lamp ignition e UV lamp off e Multicell transport disconnected e Blank e Shutter open closed e Stray light filter open closed e Analysis making a Sample or Standard measurement 92 Service and Maintenance Handheld Controller and Spectrophotometer Logbooks e Method saved deleted e System parameters changed L EMF Logbook m key in Records screen which logs maintenance tasks like e Number of ignitions for UV Lamp exceeded e Number of ignitions for Vis Lamp exceeded e Lamp burn time for UV Lamp exceeded e Lamp burn time for Vis Lamp exceeded Handheld Controller Logbook Messages coming from the software of the handheld controller are logged in the following logbooks I System Logbook System Log which logs all actions carried out or seen by the handheld controller such as e Error during calculation e Memory consumed Viewing and Printing the System Logbooks 1 Choose a task e g Single WL 2 Press the F5 key System 3 Press the F4 key Records and select one of the logbooks by either pressing e F2 System Logbook e F3 Error Logbook e F4 Maintenance Logbook e m Info Logbook 4 Press F6 Print to print out the chosen logbook
96. r In general ablank measurement should be repeated as often as is practical Even in a thermally stable environment a blank measurement should be taken eryhalf hou to ensure accurate results ken n rater Chemically the only difference between the blank and the sample should be the presence of the analyte s For m rements with li blank should be a sample cell filled with the solven Sample Cell or Cuvette Material Quartz Sample cells Givettes or sample cells with quartz face plates are required if you want to use the full 1 1100 nm wavelength r of your spectrophotometer If you plan on working only in the visible and or short wave near infrared range of 350 to 1100 nm you can use good quality Disposable plastic sample cells for measurements in the range 400 1100 nm are also available The quality of these cells varies and they are generally not recommended 25 Figure 7 Good Measurement Practices General Considerations The accuracy of the readings of a diode array instrument is very sensitive to spatial shifts of the analysis light beam Cells having non parallel opposite faces or so called wedge shaped cells lead to a spatial shift of the light beam see Figure 7 Therefore the opposite cell walls illuminated by the analysis light beam have to very parallel The parallelism is measured in terms of the angle between the two opposite cell walls We recommend to use 10 mm path length cells with an angle
97. reactions 32 photodegradation 33 photographic lens tissues 117 photosensitive substances 32 pipette 30 plastic sample cells 25 poor linearity 26 poor photometric accuracy 26 power consumption 11 power supply 11 power switch 41 pressure wheel 129 pressure control lever 129 Previous F6 key 50 Print F6 key 48 Print Results 70 print your results 44 Printer 100 Printer Configuration 100 printer configuration 90 Printer Interface 102 printer settings 45 Printing your Results 70 pump 49 Pump Action 133 Pump parameters 67 Pump time 73 pump tubing 133 with tubing cassette 130 pushbuttons 40 pyridine 31 RAEN 42 59 Quantification Task 59 Quantification task 46 quartz sample cells 25 Quick Reference Guide 103 R rack 119 Range 61 rapid absorbance changes 33 Rate Calculation 61 Rate unit 67 ready to measure 20 Recalculation 61 recalculation 44 Recalibrating the Multicell Transport 101 recalibrating the multicell transport 90 Recalibrating the Wavelength Scale 99 recalibrating the wavelength scale 90 Recommended Cells 27 Records 45 46 Reference Wavelength s 56 59 Related F7 key 50 relative humidity 12 repeat ignition cycle 20 Replacement Parts 102 replacement parts 90 replacing tubing cassette 130 Resetting the Lamp Counters 95 Resetting the Software 83 Restart 46 restart the software 75 roadmap 53 Roadmap for Software Navigat
98. rnal water bath The tubing connectors for the water bath are shown in Figure 36 You can remove the cell holder very easily by loosening the two fixing screws as shown in Figure 36 The Multicell cell holders are manufactured to such a precision that you can exchange cell holders leaving the multicell transport base in place without readjusting the multicell transport at all Thus you can exchange very easily batches of up to eight cells 125 Installing Accessories Eight position Multicell Transport Figure 36 Removing the Cell Holder Assembly Cell holder screws 126 Installing Accessories Sipper System Sipper System The sipper system part number 89068D is an accessory for the HP 8453 spectrophotometer It comprises a flow cell connectors and tubings and a peristaltic pump By eliminating the handling of cuvettes and the errors that can result from cuvette repositioning the sipper system provides a simple method of improving the productivity and reproducibility of spectrophotometric analyses The sipper system comprises a single channel peristaltic pump quartz flow cell teflon tubing and remote cables In operation the sipper system aspirates a liquid sample into a flow cell where it is measured and then returned or pumped to waste A brief description of how to install the sipper system is given here For more detailed information e g technical specifications refer to the documentation that is shippe
99. rror Logbook 92 error logbook 45 Error Messages 85 error messages 51 Escape and Enter Keys 49 Escape Key 49 ethyl acetate 31 ethyl ether 31 export data 142 Export sample standard 46 Export timetrace 46 Exporting a selected Sample Standard as ASCII File 64 Exporting a Timetrace as ASCII File 65 Exporting Data 143 External Triggering 76 F Fl key 42 44 F2 key 44 45 F3 key 44 45 70 F4 key 45 46 F5 key 44 F6 key 47 F7 key 47 F8 key 47 Factor 61 fan 19 ferrules 131 File Extensions 143 File Structure 144 File Print 44 70 Filter 116 124 Filter Kit 122 123 filter wheel 123 filters 123 firmware 90 137 138 firmware and software revision 45 firmware of the spectrophotometer 136 firmware revisions 104 firmware software update interface 45 fittings 131 cell 131 flow cell 28 127 131 arrow mark on 131 flow cells 36 french language software 20 frequency line power 11 front panel LED 81 front panel pushbuttons 40 front view 40 fuses 11 FW Update 137 138 G glass cells 25 glycerol 31 good measurement practice 51 GPIO connector 129 GPIO interface 76 Graphic 63 graphic 44 Graphic F6 key 47 Graphic settings 67 ground connection 11 H handheld Controller Logbook 93 Handheld Controller Overview 39 Handling Cells 30 hardware related information 51 help screens 51 high precision measurements 73 highest precision measure
100. rting a selected Sample Standard as ASCII File Press the m key Select Export Selected Sample from the task list box Use horizontal vertical arrow keys and alpha numerical keys to type in a file name for your samples standards The default file extension is wav Confirm your file name by pressing Enter 5 To save your samples standards press F6 Done Saving a Timetrace only in Kinetics Press the F3 key File Print select Save Timetrace with the vertical arrow keys and press Enter Use horizontal vertical arrow keys and alpha numerical keys to type in a file name for your timetrace The default file extension is tr 64 NOTE NOTE Operating your HP 8453E UV visible Spectroscopy System Saving Loading and Deleting Your Samples Standards and Timetraces 3 Confirm your file name by pressing Enter 4 To save your timetrace press F6 Done If you want to exit a dialog without saving your timetrace press Esc Exporting a Timetrace as ASCII File Press the m key 2 Select Export Selected Timetrace from the task list box 3 Use horizontal vertical arrow keys and alpha numerical keys to type in a file name for your timetrace The default file extension is esv 4 Confirm your file name by pressing Enter To save your timetrace press F6 Done Loading Your Samples Standards and Timetraces Loading Samples Standards only in Quantification Press the F3 key File Print select Lo
101. s is described in Saving Loading and Deleting Your Samples Standards and Timetraces on page 64 and Saving Loading and Deleting Your Methods on page 67 56 a AeA WO N m mn Ss NOTE Operating your HP 8453E UV visible Spectroscopy System Equation Task Equation Task Select Equation from the task list box Type in the appropriate analytical Wavelengths using the numerical keys Select your Data Type using the horizontal arrow keys Select a Unit using the horizontal arrow keys Type in your equation for evaluation using the arrow F1 F2 F3 F4 and F5 keys Use the F7 key Delete to delete a single entry and the F8 key Clear to delete the complete equation Press the F6 key Done to save your settings and exit the screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Sample to make a measurement on your sample The result of your measurement is automatically displayed on the screen Select a sample by using the horizontal arrow keys and press the F6 key to display a sample spectrum on the screen How you save your results and your measurement parameters is described in Saving Loading and Deleting Your Samples Standards and Timetraces on page 64 and Saving Loading and Deleting Your Methods on page 67 57 a A Fk WO NS NOTE Operating your HP 8453E UV visible Spectroscopy System Spectrum Task Spectrum Task Select
102. ser Manual In This Book This handbook describes what you have to do to install and operate your new HP 8453E UV Visible spectroscopy system The first part of the handbook deals with installing a complete system that is the spectrophotometer the handheld controller and printer In the second part of this handbook you will find additional information about installing accessories and operating and maintaining your HP 8453 spectrophotometer In the last main part of the manual you will find information about the structure and contents of the software It also describes in brief how to use the software Use Chapter 1 Installation and Start Up if you need more detailed information to begin with Use Chapter 2 Good Measurement Practices if you require information about general operating conditions to perform accurate and reliable measurements e g handling samples solvents and cuvettes Other chapters contain the following information Chapter 3 Operating your HP 8453E UV visible Spectroscopy System gives you detailed informations about the features of the software and how to operate the handheld controller Chapter 4 Troubleshooting gives you hints and tips how you can resolve technical problems of the HP 8453E UV visible Spectroscopy System In Chapter 5 Service and Maintenance you will find information on service and maintenance features supported by the HP 8453E UV visible Spectroscopy System
103. ssories with electronic components are available to enhance the functionality and capabilities of your spectrophotometer These accessories are described in the second part of this chapter e Multicell transport e Sipper system Detailed information on the multicell transport and the sipper system are included with the accessories in separate handbooks 106 Figure 20 Installing Accessories Thermostattable Cell Holder Thermostattable Cell Holder The HP 89054A thermostattable cell holder see Figure 20 is a single cell cell holder with a manifold around the cell Water from a thermostatted water bath can be circulated through the manifold to hold the sample cell at a uniform temperature Up to 1 cm open topped cells and flow cells can be used in a thermostattable cell holder Thermostattable Cell Holder Tubing connector Tubing restraint tab Installing a Thermostattable Cell Holder Loosen the hold down screws and remove the current sample holder from the sample compartment Orient the thermostattable cell holder the same way the standard cell holder was oriented and lower it onto the sample compartment mounting guides 3 Tighten the hold down screws Connect tubing silicon 3 16 inch i d to the inlet and outlet of the manifold It does not matter which side is used as the inlet and which side is used as the outlet If necessary route the tubing under the tubing restraint tab to keep it from interferi
104. stallation Checkout on page 22 use this section to check if your spectrophotometer in combination with the handheld controller software is in proper operating condition Optionally there are instrument tests which can be used for a quick check out of the spectrophotometer These instrument tests can only be executed after 45 minutes warm up time of the instrument 10 WARNING WARNING Installation and Start Up Site Requirements for Your HP 8453 Spectrophotometer Site Requirements for Your HP 8453 Spectrophotometer Power considerations Your spectrophotometer can operate on a line voltage of 100 120 or 220 240 V AC 10 with a line frequency of 50 or 60 Hz 5 Maximum power consumption is 220 VA The instrument power supply has wide ranging capability It accepts any line voltage supplied at the above mentioned range Consequently there is no voltage selector at the rear of the spectrophotometer There are no externally accessible fuses because automatic electronic fuses are implemented in the power supply To disconnect the instrument from line pull out the power cord The power supply still uses some power even if the power switch on the front panel is turned off No external power supply is needed for your handheld controller it is powered by the CAN interface The DeskJet printer accepts a nominal line voltage of 110 or 220 V AC witha line frequency of 60 or 50 Hz For more information see the docu
105. standards timetraces on the PC card e delete methods on the PC card e save methods to the instrument e copy methods from the instrument to the PC card e delete methods from instrument and PC card e load methods into the buffer of the instrument e print your results System F5 key The System key takes you into a new screen where all the F keys have new meanings Control F1 key Control provides access to e turning the lamps on and off e moving the multicell transport e starting the pump only pump and no multicell transport connected 44 Operating your HP 8453E UV visible Spectroscopy System Software Overview Configure F2 key Configure provides access to e spectrophotometer settings e g wavelength range integration time e system options e g prompt for task settings e display contrast e printer settings Tests F3 key Tests provides access to e performance tests for the spectrophotometer e g photometric accuracy e maintenance and diagnostic tests for the whole system e g dark current wavelength recalibration Records F4 key The Records key brings you into another screen where you can check e EMF limits e g lamp usage in hours e firmware revision of the spectrophotometer and software revision of the handheld controller e system logbook e g shutter open UV lamp on e error logbook e g visible lamp current e maintenance logbook firmware upgrade done lamp exchanged
106. strument at environmental temperatures higher than 50 C 122 F the rear of the instrument may get hot The spectrophotometer can be shipped or stored where the ambient temperature is between 40 and 70 C 4 and 158 F Do not store ship or use your instrument under conditions where temperature fluctuations could cause condensation within the instrument Condensation will damage the electronics If your instrument was shipped in cold weather leave it in its box and allow it to warm up slowly to room temperature to avoid condensation You can operate your spectrophotometer in environments with relative humidity up to 95 non condensing provided the temperature is between 25 and 40 C 77 to 104 F Avoid air circulation of varying temperatures like from refrigerators or air conditioners and exposure to direct sun light to ensure the instrument operates within performance specifications 12 Installation and Start Up Site Requirements for Your HP 8453 Spectrophotometer Your spectrophotometer can be stored at altitudes up to 4 600 m 14 950 ft and operated at altitudes up to 2 000 m 6 500 ft 13 Installation and Start Up Unpacking Your HP 8453E UV visible Spectroscopy System Unpacking Your HP 8453E UV visible Spectroscopy System Upon receipt of your spectrophotometer handheld controller and printer inspect the shipping containers for any signs of damage If the containers or cushioning material are
107. t for Single WL and Kinetics e overlay up to three spectra of same data type 46 Operating your HP 8453E UV visible Spectroscopy System Software Overview Action Keys F6 F7 F8 key Task Menu In all software tasks of the handheld controller the action keys start default or previously defined measurements F7 and F8 key The definition of key F6 is such that you can display a selected spectrum Single WL or timetrace Kinetics or up to three selected spectra all other tasks The spectra you want to overlay in the graphics screen are marked by using horizontal arrow keys Blank F8 key When pressing the Blank key a reference measurement is carried out You cannot view the blank spectrum but it is internally stored in the RAM of the HP 8453 spectrophotometer All sample or standard measurements always refer to the latest blank measured and there is always only one blank spectrum stored in the RAM Sample Standard Start Run F7 key Depending on the Task you are in pressing the F7 key starts either a e Sample measurement e Standard measurement only in Quantification e Measurement sequence defined for the multicell transport not in Single WL and Kinetics e Kinetic run only in Kinetics Graphic F6 key Displaying up to three spectra of the samples or standards taken over the complete or a defined wavelength range of the spectrophotometer can be achieved by pressing the F6 key not in Single WE and K
108. t your Data Type using the horizontal arrow keys Press the F6 key Done to save your settings and exit the screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Sample to make a measurement on your sample The result of your measurement is automatically displayed on the screen Press the F6 key to display the sample spectrum on the screen How you save your results and your measurement parameters is described in Saving Loading and Deleting Your Samples Standards and Timetraces on page 64 and Saving Loading and Deleting Your Methods on page 67 55 pe WO N 1 a A NOTE Operating your HP 8453E UV visible Spectroscopy System Multi wavelength Task Multi wavelength Task Select Multi WL from the task list box Type in the appropriate analytical Wavelength s using the numerical keys Select your Data Type using the horizontal arrow keys Select a Background Correction if necessary and type in the Reference Wavelength s Press the F6 key Done to save your settings and exit the screen Press the F8 key Blank to make a measurement on your solvent Press the F7 key Sample to make a measurement on your sample The result of your measurement is automatically displayed on the screen Select a sample by using the horizontal arrow keys and press the F6 key to display a sample spectrum on the screen How you save your results and your measurement parameter
109. th Cell Holder Loosen the hold down screws and remove the current sample holder from the sample compartment Orient the long path cell holder so that the clamps that hold the sample cell in place are on the right Lower the cell holder onto the sample compartment mounting guides 112 Figure 25 Installing Accessories Long Path Cell Holder Tighten the hold down screws Installing a Sample Cell Position the cell stops according to the path length of the sample cell you will be using For example if your sample cell is a 1 cm cell Positioning the Cell Stops for a 1 cm Sample Cell Cell clamps Clamp screws Cell stops If your sample cell is not one of the standard lengths position the cell stops as for a long path sample cell i e move all cell stops in Figure 25 to the left Because the light beam is collimated absolute positioning of the sample cell is not important however consistent cell positioning gives more consistent results The cell stops make it easier to consistently position your sample cells Install the sample cell between the clamps Slide it against the cell stop If your sample cell is not one of the standard lengths position it so the clamps are gripping the mid point of the cell Allow the clamps to close against the sample cell see Figure 26 Tighten the four screws that hold the sample cell in place 113 Installing Accessories Long
110. th blank or sample solution Floating particles in the cell will deflect the light beam and so lead to a very poor quality of the measured spectrum Floating Particles in a Cell SP floating particles will deflect and scatter the light beam 29 Figure 11 Absorbance Good Measurement Practices General Considerations Spectrum Taken With Floating Particles in the Light Path 400 600 800 1000 Wavelength nm Lens tissues for glasses or other uses often contain detergents or lubricants which can affect your measurements If possible avoid cleaning the faces of your cell between blank and sample measurements Handling Cells Always install a cell so that it faces the same direction to minimize problems with cell non uniformity For best results with microcuvettes leave your sample cell clamped in position throughout the measurement sequence Solutions should be removed and replaced by pipette or use flow cells Solvents Your choice of solvents should be based primarily on the solvent s absorbance characteristics over the wavelengths of interest its suitability as 30 Good Measurement Practices General Considerations a solvent for the analyte and on experimental conditions Table 1 lists common solvents and the lower limit of their useful wavelength range Table 1 Lower Limit of UV Transmission for Some Common Solvents Lower Limit Solvent 180 195 nm Sulfuri
111. the Search key gives you access to the choice to enter the help either via the 1 Contents item or the Ll Index item Choosing Contents brings you to the Table of Contents of the help system How the table of contents is structured is shown in Figure 16 When you select Index you have the possibility to browse for words which are in the help system The words are grouped in alphabetic order and have links to help screens As soon as you choose one of the words from the list the appropriate help screen is displayed 51 Figure 16 Tasks Single WL Multi WL Equation Spectrum Quantification Kinetics Operating your HP 8453E UV visible Spectroscopy System Software Overview Table of Contents of the Help System Single WL 1 Wavelength Absorbance Transmittance Derivative Multi WL 4 Wavelengths Absorbance Transmittance Derivative Equation 4 Wavelengths Absorbance Transmittance Derivative User defined equation Spectrum Complete range Absorbance Transmittance Derivative Mathematical operations applied on spectra Quantification 1 Wavelength Absorbance Transmittance Derivative Quantitative Analysis Calibration Kinetics 1 Wavelength Absorbance Time resolved measurements System Control Configure Tests Records Context Menu m key Control Lamps on off Multicell move to position Pump start stop Configure
112. the sample will reduce the time any given analyte molecule is in the light path This minimizes the photodegradation and increases homogeneity Using a flow cell with continuous flow can yield similar results Checklist for Best Results Cell M Cell is made of quartz or glass Apertured cell has black sides Apertured cell has an aperture greater than or equal to 3 mm Cell windows are free of fingerprints and other contamination O O wu Flow cell used instead of an apertured standard cell 33 Figure 12 Absorbance Good Measurement Practices General Considerations Measurements m m m m m m m m Solution in cell is free of floating particles Solution in cell and cell walls are free of bubbles Solution in cell is mixed homogeneously Blank measured on same solvent as sample Blank measurement shows a flat baseline Figure 12 and Figure 13 show a good and a poor baseline Cell orientation of blank and sample measurements is the same Ideally the cell is not removed between the measurements which means the cell is filled rinsed using a pipette or a flow cell is used Time between blank and sample measurement should be short Example of a Blank on Water Showing a Good Baseline 200 0 0015 0 0010 0 0005 0 0000 0 0005 0 0010 400 600 800 1000 400 600 800 1000 Wavelength nm 34 Good Measurement Practices General Considerations Example of
113. the spectrophotometer before removing or inserting a PC card Insert the connecting side of the PC card into PC card slot of the handheld controller until you feel it will not go in nay further Reconnect the control module to the spectrophotometer to restart the software To remove the PC card press the card eject button Changing the PC card Card eject button 75 Table 4 NOTE Operating your HP 8453E UV visible Spectroscopy System Triggering the Spectrophotometer from an External Device Triggering the Spectrophotometer from an External Device External Triggering Unless the peristaltic pump is connected to the spectrophotometer through the GPIO interface the GPIO port can be used to trigger a measurement from an external device Three types of measurements can be triggered e Blank measurement e Sample measurement e Standard measurement only in Quantification The trigger lines use the GPIO connector pins as shown in Table 4 Trigger Inputs Pin Function 9 Trigger blank measurement 10 Trigger sample measurement 11 Trigger standard measurement only in Quantification task 15 Ground Measurements are activated on contact closure to ground pin 15 By default the trigger lines 9 10 11 are always active in all tasks except for Kinetics task External Triggering and Multicell Transport You can setup two separate sequences for the multicell transport e Sample sequence
114. the upper right corner of the front panel will light in three different colors The ellow Colop which means busy will stay on during the start up and self test routines until at least one of the lamps is ignited and the spectrophotometer is ready to operate 19 NOTE Installation and Start Up Starting the HP 8453E UV visible Spectroscopy System The turn on procedure including electronic self tests lasts about 20 seconds before the lamps start turning on Under cold ambient conditions the lamp may not ignite and the instrument will repeat the ignition cycle automatically The entire turn on and self test process will take about 1 2 minutes Optical self tests are performed which last a few seconds When the feem indicator at the upper right corner of the front panel comes on the instrument is ready to measure As soon as the handheld controller is connected to the spectrophotometer and the spectrophotometer is turned on the software of the handheld controller is started automatically If the front panel indicator remains yellow the system has been configured for both lamps to be off at start up If the indicator shows a d color there is an error condition Try turning on the spectrophotometer again If the red indicator persits check Chapter 4 Troubleshooting of this manual or the Service Manual of the HP 8453 spectrophotometer Selecting the Appropriate Language of the Software If you have 2 MB version
115. thods the arrow keys and alphanumeric keys are defined such that you can enter names The horizontal arrow keys allow you to move the cursor whereas the vertical arrow keys are used to select a letter Numerical Keys The keys of the numerical keyboard can have to different meanings depending on the menu or sub menu you are in e Inthe task menus you can control your accessories like moving the 48 Table 3 Operating your HP 8453E UV visible Spectroscopy System Software Overview multicell transport to different positions or starting the pump to turn clockwise counterclockwise or stop In screens with edit boxes e g file save analyte name where you enter names you can use the alphanumeric or arrow keys to type numbers and letters of the alphabet You can type names using the numeric keys 0 9 The 0 key contains zero and special characters Each other key contains its corresponding number and three letters Pressing 1 once gives you the number 1 pressing 1 twice gives the letter A pressing 1 three times gives B and pressing 1 four times gives C The 2 key continues with 2 then D E and F and so on Use the vertical arrow keys to move to the next position and the horizontal arrow keys to scan the alphabet and to find special characters Press Done function key F6 once you have finished to return to the main window Text
116. tinued Error Message Possible Cause s Action s UV Lamp Heater Overcurrent VIS Lamp Overcurrent Cooling Fan Defective Lamp Door Open Digital Signal Processor Error Ignition failed Deuterium lamp defective Lamp power supply defective Main board defective see error UV Lamp Heater Overcurrent Fan is disconnected Cycles per minute sensed at fan is too low Fan sticks or is defective Main board defective Lamp door is open Light switch is not covered by metal door Light switch is defective Communication error between the main processor and the digital signal processor on the SPM main board Communication error between SPM main board and SDA data acquisition board Flat ribbon cable defective Retry to start the lamp Replace Deuterium lamp Replace SLS lamp power supply board Replace SPM main board see error UV Lamp Heater Overcurrent but replace Tungsten lamp instead Reconnect cooling fan Move cooling fan manually and replace if necessary Replace SPM main board Close lamp door Reposition or replace metal door Replace SLS lamp power supply board Replace SPM main board Replace SDA data acquisition board Replace flat ribbon cable 86 Troubleshooting Troubleshooting Your HP 8453E UV visible Spectroscopy System Error Messages Table 5 System Error Messages and Troubleshooting Procedures continued Error Message P
117. ure 15 The spectrophotometer is shipped with the standard single cell holder Standard and accessory cell holders can be removed and replaced in seconds with few or no tools See Installing Accessories on page 105 for more details Figure 15 Front View and Keys of the Spectrophotometer Indicator Blank button Standard button Sample button Line power switch The four push buttons on the front panel cause the following actions to be performed and the resulting data to be sent to the handheld controller e blank the instrument takes a blank measurement that is a reference measurement of solvent without the analyte This is used in all subsequent sample measurements until a new blank measurement is taken e sample the instrument takes a sample measurement or starts a series of measurements This depends on the parameters set in your software e standard the instrument takes a measurement of a standard Additional information such as concentration and so on have to be entered in the 40 Operating your HP 8453E UV visible Spectroscopy System Spectrophotometer Overview operating software e stop this button is not active with the handheld controller The line power switch is located at the lower left part of the instrument Pressing it will turn on the instrument It stays pressed in and shows a green light when the instrument is turned on When the line power switch stands out and the gree

HP 8453E UV-VIS User Manual (G1819

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