Advantage Series User Manual NuSpec Software 532
Contents
1. This tells the software where to locate the spectrometer If the correct port number is not initially displayed in the pull down menu then follow the instructions that are given on the screen to add the correct port to the list so that it can be selected i Select Spectrometer Port Sek Please select the port number of the spectrometer IF you do not know the port number turn off the spectrometer refresh the selector box and the spectrometer s port will disappear Then turn on the spectrometer refresh again and it will reappear Spectrometer Port gt Select if asort Fig 6 Select spectrometer port The first time the spectrometer is connected to a computer the Create Spectrometer Parameter File window will display Fig 7 Follow the onscreen instructions to continue This window is used to specify the range of wavenumbers for the system the imager temperature and the firmware version By simply clicking on the button that corresponds to your system 1 e ExamineR 532 the default parameters of that system will be automatically loaded on this screen Note This step is only required the first time the spectrometer is connected to the computer This window will not appear on subsequent connections gt Create Spectrometer Parameter File E This appears to be the first time this spectrometer has been connected to this computer You must create a file to describe certain parameters of the spectrometer For most system2. but the Busy light will stay on while the software takes a reference Busy Fig 22 Busy light Advantage Series User Manual DeltaNu May 2009 18 4 15 Laser Warning The laser warning symbol is shown next to the busy light only when the laser is ON Laser Warning Fig 23 Laser warning 4 16 Continuous Clicking the Continuous button allows the laser to run continuously until stopped This mode is used to focus or position the laser on the sample with the optimum signal collection To stop the continuous mode click the Continuous button again Continuous Fig 24 Continuous 4 17 Abort The ABORT button will cancel a reference an acquire or a continuous function when clicked ABORT Fig 25 Abort 4 18 Resolution The Resolution setting can be changed from Low Medium Low Medium Medium High or High using the pushbuttons on the left of the box The benefit of using a low resolution setting is that you get less background noise However high resolution allows one to see spectral features that would not be separated at lower resolution Note It is recommended that all library spectra be saved at a low resolution setting Resolution ru Low a Fig 26 Resolution Advantage Series User Manual DeltaNu May 2009 19 4 19 Baseline The Baseline feature can be turned ON or OFF Yes or No using the pushbuttons on the left When the baseline feature 1s ON the fluorescence 1s subtracted f
3. many samples do not require high resolution and the best spectra are obtained in the low resolution mode 8 0 Ambient Light We recommend that you characterize the ambient light conditions in the environment that you are working in This test will provide you peaks that could possibly interfere when a poor reference 1s obtained As an example we have provided a spectrum that was obtained by referencing with a shroud or black optical cloth covering the sample vial attachment After a reference was taken a fluorescent light turned on was placed in front of the attachment and a sample of the light was obtained Figure 39 200 400 600 800 1000 1200 1400 1600 1800 2000 Wavenumbers cm Fig 39 Ambient Light Example 785nm Advantage Series User Manual DeltaNu May 2009 26 9 0 Glass Interference Another issue that may arise when acquiring spectra is glass interference For example the manual adjustments on the focusing knob for the sample vial attachment allow minimal glass interference however certain experimental conditions may cause glass interference One common mistake is not filling the vial full enough with sample Consequently Raman is collected on the glass above the sample Interference due to fluorescence impurities in the glass may be observed near 1400 cm Figure 40 for the 8mm glass HPLC vials This spectrum may vary based upon the type of glass material used 200 400 600 800 1000 1200 1400 1600 1800 2000 Wav
4. Allen Wrench o 5 64 Allen Wrench Please note section 13 0 Changing the Desiccant It is important to the overall performance of the instrument that the desiccant is checked every 3 6 months Advantage Series User Manual DeltaNu May 2009 6 1 2 Laser Safety Warnings Fig 1 Laser safety label Aperture warning for Advantage 532 When acquiring data the system will emit up to 100mW at 532 nm of radiation through its output optics Aperture warning for Advantage 633 When acquiring data the system will emit up to 3mW at 633 nm of radiation through its output optics Aperture warning for Advantage 785 When acquiring data the system will emit up to 60mW at 785 nm of radiation through its output optics This hazard is specified by the Nominal Ocular Hazard Distance NOHD The Advantage NIR has an NOHD of 36 inches 91 4 cm This represents the distance at which the radiation has decreased to 2mW cm Caution use of controls or adjustments or performance of procedures other than those specified herein may result in hazardous radiation exposure Only trained authorized personnel should be allowed to use this instrument Occasional maintenance may be required to keep the output optics clean All maintenance should be performed with the system off DANGE PES IEA E LASER FANIA Tc AVON CAREC T ER PSUR 10 HE RAM ETE PROTEC TION A OUR O Fig 2 Laser Warning Label Advantage Series User Manual DeltaNu May 2009
5. Settings mfox My Documents Chemistry Advantage 200A4 spectra 200a cyclohexane2 s C Documents and Settings mfox My Documents Chemistry advantage 2004 spectra 200a ibuprofen basel Add ff Delte ff Delete al ABORT Fig 30 Load library The spectra or libraries that you selected will now be displayed on the main software screen Fig 31 To view the actual spectra click on the Library Entry Name at the bottom of the screen and the spectra will be displayed in the corresponding color of the highlighted entry name To de select the spectrum click on the entry name again It is also possible to view multiple spectra at once by clicking on multiple entry names Each spectrum will be displayed in a different color The library spectrum list can be sorted by correlation match or library entry name by clicking on the corresponding title bars at the top of the spectrum list 1 e Correlation or Library Entry Name The comment window allows further description of a sample spectrum to be added and saved with the spectrum The user can type in both the Comment and Spectrum Name fields and the changed values will be saved with the spectrum Advantage Series User Manual DeltaNu May 2009 22 Serial Number 120117 aA N u S p ec Imager Temperature Expert Interface lo Polarization PATA J Not Polarized Integration Time An Referencing Mode Software Retake Software Refere
6. and install them When it is finished the USB Serial Converter will be installed Click Finish Found New Hardware Wizard Completing the Found New Hardware Wizard The wizard has finished installing the software for USE Serial Converter Click Finish to close the wizard Vance Fig 56 USB serial converter screen Advantage Series User Manual DeltaNu May 2009 37 The second portion of the driver package will now be installed Follow the same steps as above for the USB Serial Converter This time you do NOT need to browse for the USB Driver file it is now stored in the installer s memory Upon completion you will see the USB Serial Port screen appear Fig 57 Click Finish and your spectrometer s USB link will be installed You should only have to perform this installation once However if your computer contains multiple USB ports it may be necessary to repeat this operation for every USB port that you intend to use for the spectrometer Found New Hardware Wizard Completing the Found New Hardware Wizard The wizard has finished installing the software for F USE Serial Port Click Finish to close the wizard E lancel Fig 57 USB serial port screen Advantage Series User Manual DeltaNu May 2009 38 13 0 Replacing the Desiccant Extra desiccant containers come with your instrument They will store dry in the containers provided We recommend that the desiccant is changed every
7. has a fluorescence background the following procedure is suggested Select yes under the baseline menu option and then click on continuous Carefully adjust the sample position In many cases it is possible to find a position that maximizes the Raman signal while minimizing fluorescence The baseline feature is very useful as it often allows for observation of a Raman feature that would normally be hidden in a more spurious baseline Once the position has been optimized select an integration time that produces a good signal to noise ratio and if needed average over several spectra Advantage Series User Manual DeltaNu May 2009 25 7 0 Resolution The Resolution feature can be used to improve spectra As a rule of thumb in any dispersive spectroscopy spectroscopy where a grating or prism spreads the spectrum across the exit plane of the spectrograph the signal to noise is inversely proportional to the resolution The Advantage series allows the user to select three resolution levels to improve signal to noise ratio At low resolution the signal to noise ratio is optimal but the spectral resolution is lower This can be readily observed with a sample such as toluene At the low resolution setting the two large peaks around 1000 cm are not resolved However note the excellent signal to noise ratio even at one second As the resolution is improved the two peaks are resolved at the cost of adding noise to the background As a rule of thumb
8. of energies Otherwise you Il never be able to distinguish the shifted ones from the source photons The laser produces quasi monochromatic light that forms a very narrow band of frequencies Lasers also produce this light in a small concentrated beam that 1s very intense A second technological advance that has revolutionized Raman spectroscopy 1s the Charge Coupled Device CCD The CCD is millions of times more sensitive than the eye and 1s able to record a complete Raman spectrum in less than a second Let s look back at the history of Raman spectroscopy to understand the advantage that the CCD affords Not long after Raman s first experiments scientists started using a photographic plate to record the Raman spectrum This provided the first hardcopy of a Raman spectrum The problem was that it didn t have a softcopy version that could be used for data analysis and spectral manipulation Early Raman spectroscopy was also like shooting in the dark The plates were exposed for hours to get a spectrum and you didn t know if the optics were properly aligned until the plate was developed The next big advance was the photomultiplier tube This is a sensitive optical transducer that converts photons into electrons They are sensitive enough to detect a single photon and a whole technology of single photon counting grew around them Now a Raman spectroscopist could set his instrument to view energy where Raman scattering should be observe
9. on your PC 1 Open library builder software Fig 43 2 Select the folder next to the top box to add the files that you wish to include in the new library gt Library Builder TER Destination Library File 4 Library Entries pc Range pa Old lib Files Progress Fig 43 Library builder software 3 Once you have added your files you can select the file name to save your new library under using the folder next to the bottom box on the display window 4 Click Start 5 The progress bar indicates the library development status To load up an existing library select the library under destination library file this loads that file and displays all the entries in the dropdown listbox selector To delete select the entry you want to delete in the dropdown listbox and click delete entry Note When you load up an old format library lib file you need to tell it the wavenumber range of the spectrometer that took those spectra in order for it to interpret the data correctly Advantage Series User Manual DeltaNu May 2009 29 11 0 Sampling Attachments The standard attachments for the Advantage are the Vial Sample Holder Melting Point Tube Adapter and NMR Tube Adapter There are also several optional attachments for the Advantage series The XYZ Stage Extension Tube Right Angle Input Optics and the NuScope microscope 11 1 Vial Sample Holder The Vial Sample Holder comes standard with the instrument It is
10. power of the energy This means that Compton s experiments with x rays with a wavelength of 0 7 nm and the observation of Raman scattering Advantage Series User Manual DeltaNu May 2009 39 with visible light at 500 nm will differ by 11 orders of magnitude Raman was able to observe the weak Raman effect by using the most intense light source available at the time the sun He focused a large telescope on the sun and placed a green filter in the intense beams of sunlight When he used a yellow filter to observe this beam of green light passing through a solution of chloroform he could see a weak yellow light The origin of the yellow light was the Raman effect A small amount of the green light from the sun had inelastically scattered from the chloroform molecules and shifted its energy so that the photons fell within the yellow part of the spectrum Today Raman spectroscopy has become much more sophisticated and much simpler to measure Major technological advances have transformed Raman spectroscopy from telescopes and visual observation to a highly sensitive spectroscopic technique The first technological advance was the laser The sun is pretty bright but it is sending its energy in all directions and over a very broad range of wavelengths The Raman effect is observed as a shift in energy of a photon and the shift can be related to a vibrational state of the sample To observe the shift one needs all of the photons to be a very narrow band
11. the information is utilized The Instruments have high energy lasers that may burn some samples and targets It 1s the user s responsibility to verify that the Instruments will not damage the sample or target DeltaNu makes no recommendations nor does it assume any liability for how the Instruments are utilized or any damage they may cause The Instruments may come with software allowing the user to adjust the laser power settings These settings are approximate and may change over time and with repeated use DeltaNu makes no warranties or representations as to the accuracy or stability of the laser settings For precise determinations a laser power meter should be used As with all emissive scattering spectrometry technologies no reference beam is used and the Instruments are not intended for absolute or relative quantification of substances Use of the Instruments is at the user s own risk e U S Customers These products and technologies are for domestic use Any export must comply with United States Export Administration Regulations e Customers Outside U S The use sale re export or re transfer of DeltaNu s products and technologies directly or indirectly in any activities related to the design production use or stockpiling of chemical biological or nuclear weapons or missiles is strictly prohibited Contact DeltaNu with questions comments or concerns at www DeltaNu com or call us toll free at 1 866 301 6328 Copyrigh
12. 7 2 0 Diagram of Advantage system Looking at the back of an Advantage series spectrometer in the top left corner is the ON OFF switch and the serial number plate Further to the right locate the 12 volt DC connector and the USB connection Fig 3 Back of Advantage Series Spectrometer On the front of an Advantage series spectrometer there are two small LED s On the left a laser cooling light and on the right a laser ON light Advantage Fig 4 Front of Advantage NIR Spectrometer Advantage Series User Manual DeltaNu May 2009 8 3 0 Taking a Raman Spectrum The Advantage series spectrometers are specifically designed for ease of use Spectra of liquids or solids in standard sample vials are obtained by placing the vial in the sample holder It is recommended that the sample vial contain approximately 1 2 sample material to ensure detection by the laser beam in the first few weeks of use As the instrument becomes more familiar to the user it 1s possible to use very small amounts of sample material Simply adjust the sample vial vertically within the sample holder to ensure alignment of the sample and the laser beam Cyclohexane or toluene provides an excellent liquid sample to practice adjusting the sample holder Acetaminophen Tylenol or benzoic acid are good solid materials to use for practice in focusing Once the sample is in place ensure that the integration time is on second and press the Continuous but
13. Advantage Series User Manual NuSpec Software 532 633 785 DeltaMu Advantage Series User Manual DeltaNu May 2009 l A a 226 A a OP Tae eee eT EAE EL A Ree nn O O de cee 3 TES CF GC fear detest o A II O ERNE E ERNE FE does 3 PANTO ea a EREE E E EAT I TA E EEA IAE PE I EE AT 5 tt Unpacking and Checklist is 6 L BE salci A EE E E EE 7 20Diasram Of Advantage SV Stc itl eioen i e N E E E E Ea 8 XO Takina a Raman Spee U eraa O aE docs 9 A ONUS SOLE oc 10 A t Spectrometer Specie Ser INTERAC E raki a a a a a tee 10 Aa TIS COMME od INI OCG eens a a a 12 SP O 12 SP a a ERE PETE ERE REE 13 NAAA A 13 EI A a eo e OO E O 14 AS Basie ys Expert Usera 15 AO EAS CE OW iS 15 OLA AO ad dd di 16 Ate ow MIESTA ONIE COC O OPD RE eee Tee eee ener T eee ee eer eee ee Reenter 16 AD REFERERE Mode old een 16 4 tO Number Or Spectra 0 AC ios eee Bones eae aia ew sees 17 A In 17 A AA E ctesien su uses ooo anaes aS 18 A esta sz cleo aera estan Saco az on snes Senet ese use eee eS 18 QA Ni BU Yah yale cetacean Sst stale Sasa A 18 dto NAS CU WV AE IVI ias 19 A iG OMUIMUOUS ais 19 O 19 A VS IRC SO MIAO M cascada csscae r a a a cobeldabcagaidiveebeeekeebededandal sav sael eovendeeeehaueddss 19 AsV OS AS CMMI A E ad 20 a a eee ee ee ee 20 Dl TANG Ty CS acc seede selen eN E sb ONE A A E E E A A EE teatre ES 20 S S VIMO AVES PEA A AAA Aci 21 Si MA a A AN A eee 21 y o ere I AP A o In 21 A A O ER ERNE En 22 30 SVAGE IDEA Y LOS DOCUM
14. ENT A 23 A A REO 23 A A A A e 24 A A A A ES ERE RESEN EDER 25 A E 25 OO TEM OT eS Cc E E E O 25 POR So UO DERES rat he tt sue ocemed OO 26 ro Owe 110 or 01 AS 10 0 cae eee ne eee N Eee 26 SM E CRASS NG A a o E AE AATE TA A E EAER 24 10 0 Library Matching and Library Development ccccccccecseeseeeseeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeees 29 TEO Sample Attac IMENS id ee es 30 jl RS o MA rer enedes ree erm eee ee ec ee 30 MEZAN O en ee en ee ee ee ee eee 30 RREAN EPI Opies AA A AA A A AS LEE 31 F TRE Obie EXC a 32 ME su Saad E E E 33 120 Lordi WS Diy ei sc ER EU a 35 LS O Replacing the DESC A a 39 AO Raman Tutora ga eee ad dla ada 39 Advantage Series User Manual DeltaNu May 2009 2 Trademarks GRAMS Viewer is a registered trademark of Galactic Industries Corporation and Thermo Galactic Advantage 633 Advantage 785 Advantage 532 NuSpec NuScope and WatchDog are trademarks of DeltaNu Disclaimer The Advantage Inspector RockHound Responder Investigator and all Raman spectrometers and accessories made sold or repaired by DeltaNu Instruments are intended to provide initial determinations and be used as information resources and tools and not absolute or conclusive identifications of unknown substances The results provided by the Instruments should be verified by using other appropriate techniques DeltaNu makes no recommendations nor does it assume any liability for how
15. Nu May 2009 20 5 2 Saving Averaged Spectra An averaged spectrum can be obtained to minimize the noise in the spectra Typically no more than 10 acquired spectra are needed to minimize noise An average file is sometimes used as a library entry First select the number of spectra to be averaged by using the arrow keys next to the Number of Spectra to Acquire function and then click on the Acquire button Note You can use the Retake Software Reference Every N Spectra function to force it to retake a reference for every N number of spectra acquired by choosing a value for N 1 After the analysis is complete select Average in the Display window using the arrow keys on the top box Fig 19 2 Select the desired resolution level low medium or high If Save Raw Data is selected the spectra is automatically saved at high resolution If Save Display is selected it saves at whatever resolution setting is currently chosen We recommend that library entries be saved at low resolution 3 Select Save Display using the arrow keys under the Save Spectrum button Fig 28 Save the averaged spectra in a folder or as a single library entry 5 3 Saving a Multi file A multi file is a single file that contains more than one spectrum A multi file is not commonly used for anything other than repeatability tests It is NOT used for a library entry It can only be saved using the Save Raw Data selectio
16. The Right Angle Input Optics allows for horizontal sampling This positions the exit collection beam of the spectrometer at a 90 degree angle toward the sample The focal length of the Right Angle Input Optics is approximately 16 45 mm Advantage Series User Manual DeltaNu May 2009 31 1 Remove Sample Holder Using 1 8 Allen Wrench 3 Alach Right Angle lo Adaptor Using 5 64 Alien Wrench as Shown 4 Wilh Right Angle in place urn on instrument and open Advantage Softwa 5 Place a sample below the Right Angle Input Optics e ai Focus Adjustment With the Advantage Softwar In continuous mode adjust the focus until the y Sample desired signal is obtained Fig 48 Attachment of Right Angle Input Optics 11 4 Input Optics Extension The Input Optics Extension incorporates objectives that extend the exit beam and collection signal 5 inches beyond the instrument This allows the instrument to access a sample in congested locations The focal point is approximately 16 45 mm beyond the Input Optics Extension Advantage Series User Manual DeltaNu May 2009 32 Fig 49 Input Optics Extension 11 5 NuScope The Nuscope is a USB microscope attachment for imaging thin films microelectronic circuits mineral inclusions and pigments in art work identification of narcotics and plastic explosives and biological tissu
17. aNu May 2009 41 200 600 1000 1400 1800 2200 2600 3000 Intensity Wavenumber cm 1 Polystyrene 633nm 200 600 1000 1400 1800 2200 2600 3000 Intensity Wavenumber cm 1 Polystyrene 532nm Advantage Series User Manual DeltaNu May 2009 42
18. arization feature can only be found on Advantage 532 Advantage 633 and Advantage 785 software Raman spectra contain special information about the polarization of the scattered light Bands that are highly polarized correspond to totally symmetric modes This can be used to aid in the characterization of Raman features in a spectrum Polarization Not Polarized Fig 15 Polarization 4 8 Integration time The Integration Time feature has two modes Fig 16 Automatic and Manual Selecting the automatic feature means the integration time utilizes the same acquisition parameters as the device hardware The maximum default setting for the hardware is 60s In this mode the device selects the optimum exposure time based on the collection signal obtained in a 0 3s check of the sample It is recommended that library entries are saved using this automatic mode The manual feature allows the integration time to be changed In the manual mode the integration time cannot be set higher than 60 seconds The lowest setting is 0 01 seconds The integration mode and time can be changed using the arrow keys to select an option Integration Time ry 1 Manual J J Fig 16 Integration time 4 9 Referencing Mode Software referencing mode requires the manual Integration Time setting Automatic Integration Time cannot be used with Software referencing so that option is hidden when Software referencing mode is selected T
19. d and with an electronic display optimize the optical alignment When computers became commonly available it was possible to have them record this electronic signal and produce a software file that contained the spectrum This software file could be manipulated to remove artifacts that otherwise can distort Raman spectra However the photomultiplier s advantage came at a cost It was no longer possible to acquire a whole spectrum during a single integration period These instruments would take very small steps in energy and count the photons at each step A three Advantage Series User Manual DeltaNu May 2009 40 thousand point spectrum with photons counted for one second took three thousand seconds That s almost an hour The solution was to go back to the old concept of a photographic plate but this time use a digital camera The CCD does just that These little integrated circuit chips are extremely sensitive to light and they contain thousands of little picture elements called pixels that take the whole spectrum at once in less than a second Modern Raman spectroscopy with the Advantage is fun and educational The Advantage system uses a small laser to replace Raman s telescope and colored filters and a CCD detector to replace out dated photomultiplier tubes The result A spectrum in seconds 200 400 600 800 1000 1200 1400 1600 1800 2000 Intensity Wavenumber cm 1 Polystyrene 785nm Advantage Series User Manual Delt
20. d to match the wavenumbers with the correct peaks The colored bars can be selected and moved on the window by left clicking the mouse on the bars and dragging them over the correct peaks After you have correctly identified the peaks you can click the Save button to keep that calibration file or click Retake to obtain another calibration spectrum E Gpaelly Calibration Paaka Fig 11 Calibration parameters 4 4 2 Calibrate After you have saved your calibration peaks on the previous window you will now be redirected back to the software s main viewing window Fig 5 Now you are ready to calibrate the system to your polystyrene ASTM standard With the calibration standard still in the vial holder click on the Calibrate button When the calibration is complete a window will open with three selections Fig 12 Keep new calibration Keep old calibration and Retry calibration along with an rms error value The lower the rms error value the better the calibration If you choose to save this rms error number for your calibration 1t will be saved in the default sdb file This file 1s not readable but can be validated by the date stamp Re calibrate if the rms error value is greater than 2 0 New calibration rms error 1 7054 wavenumbers Old calibration rms error MaN wavenumbers ion Keep old calibration Retry calibration Fig 12 New calibration Advantage Series User Manual DeltaNu May 2009 14 4 5 Bas
21. dow The exact location of the cursor is numerically displayed X and Y axis coordinates below the spectra screen Clicking on the cursor icon in this box allows the user to manually enter X and Y coordinates for the cursor The hand icon Fig 33 on the lower right hand side of the viewing window allows the entire window to be pulled to a specific point After selecting the hand icon button Advantage Series User Manual DeltaNu 23 May 2009 left click the mouse cursor on the spectrum screen and drag the entire window without de pressing the mouse button where you want it Fig 33 Hand icon The magnifying glass icon Fig 34 allows the user to zoom in on the entire spectrum specific areas of the spectrum or specific peaks of interest A window with different options will open when the magnifying glass button is selected Fig 34 Magnifying glass options The cross icon Fig 35 allows the cursor to be moved to a specific location on the spectrum screen by clicking and dragging the cursor axis lines Fig 35 Cross icon The mouse can also be used to move the cursor on the screen While the cross icon is selected you can double click the left mouse button on the spectrum screen to center the screen on that point You can also click the middle mouse button or Alt left button on the screen to center the screen on the entire spectrum Clicking Ctrl left mouse button switches back and forth between the ma
22. ene ASTM file It 1s recommended that you select Automatic for the Integration Time in order to get the best calibration Calibrating the system is only required if you have a lower correlation match than 0 95 between your polystyrene standard and the polystyrene calibration file stored in the library 4 4 1 Specify Calibration Peaks This is the first step in calibrating your polystyrene ASTM standard After you have placed a vial of the calibration standard in the vial holder select the Specify Calibration Peaks button on the lower left hand side of the software screen You will be redirected to a new screen and a spectrum of your standard will be displayed Four polystyrene peaks are pre selected and shown in the table and figure below Fig 10 The highlighted peak values will be used in this calibration step Mean Standard er Relative 12 ja bene Sample Frequency Deviation Points Intensity Polystyrene 6209 0 69 6 16 795 8 0 78 6 10 10074 0 54 6 100 1031 8 0 43 6 27 A 1155 3 0 56 6 13 1450 5 0 56 6 8 1583 1 0 86 6 12 1602 3 0 73 6 28 2 2852 4 0 89 5 9 2904 5 1 22 5 13 2 200 700 1200 i700 220 3054 3 1 36 6 32 Raman shift cm 4 Fig 10 Calibration Peaks Advantage Series User Manual DeltaNu May 2009 13 There are several colored bars on the calibration parameter screen Fig 11 Each color corresponds to a particular wavenumber 1 e red 620 9 Move the colored bars over the corresponding peaks as neede
23. enumbers cm Fig 40 Glass Vial Example 785nm Melting point tubes and NMR tubes may have different spectral impurities and acquiring a Raman spectrum of the sample container before each experiment 1s recommended Figure 41 illustrates glass fluorescence while sampling through a scintillation vial In all cases the maximum signal is achieved when the focal length is extended just beyond the glass interface Figure 42 illustrates glass interference while measuring an acetone solvent in a round bottom flask As the distance from the flask is increased glass interference is pronounced and eventually overwhelms the spectrum Advantage Series User Manual DeltaNu May 2009 2 100000 50000 500 1000 1500 2000 Wavenumber cm 1 Fig 41 Glass in Spectra Example 785nm lt Glass Interference from fla sk Po v QQ O ab O S 2 O 200 600 1000 1400 1300 Wavenumbers cm Fig 42 Round Bottom Flask Example 785nm Advantage Series User Manual DeltaNu May 2009 28 10 0 Library Matching and Library Development The NuSpec software comes with a basic library which is used to identify a wide variety of unknown samples You can ask your sales representative for a recent Excel list of the library samples or view them as spc or dnu files under the library directories The library builder software is used to create libraries for the spectrometer All library entries are saved in a folder that you designate
24. es The NuScope 1s attached with 7 64 Allen wrench Illumination of the sample surface 1s obtained with external white light sources or ambient light The surface image is viewed in real time with a color video camera using USB Shot software which allows movie and screen capture Coarse focus is achieved on the specimen with manual adjustment and fine focusing is obtained by a focus adjust knob to render a sharp image Third party rack and pinion microscope stages are used to assist in focusing and transversing the sample across the field of view FOV The field of view is approximately 1000um at 50x focal power Fig 50 NuScope Attachment Advantage Series User Manual DeltaNu May 2009 33 11 5 1 Installation of NuScope 1 Remove Sample Holder Using 1 8 Allen Wrench 3 Attach Nuacope to Adaptor Using 5 64 Allen Wrench as Shig 4 With Nuscope in place plug in USE cable into computer 5 Turn on instrument and open bolh the USE shat and Advantage software 6 Place a sample below the Focus Adjustment Nustope and focus the image in the USE Shot program Canoe the image is focused go to the Advantage sofware to run spectrum Fig 51 Installation of NuScope Advantage Series User Manual DeltaNu May 2009 34 12 0 Loading the USB Driver If your computer was not purchased with the spectrometer system the USB Drivers will need to be installed To ensure that the USB Driver is pro
25. gnifying glass tool and the cross tool 5 8 Print report The Print Report function will print a screen shot of the NuSpec software Select the printer and number of copies to be printed and select okay To close this feature select ABORT Print Report Fig 36 Print report Advantage Series User Manual DeltaNu May 2009 24 5 9 Imager temperature The imager temperature displays the temperature of the CCD This is updated every 30 seconds Imager Temperature Fig 37 Imager temperature 5 10 Exit To close or exit the NuSpec software click on the EX T button in the top right corner EXIT Fig 38 Exit 6 0 Fluorescence Challenges come when the sample has an inherent background due to fluorescence In this case background will also increase with the integration time and smaller improvements are gained by integrating longer The Advantage shows no improvement by integrating longer than 60 seconds the software does not allow integration longer than 59 seconds If the sample is fluorescing it may saturate the detector long before the 60 second integration period The best way to improve a spectrum in this case 1s to average over several spectra NuSpec offers a very unique feature that can also help with difficult samples This is the Baseline feature This feature performs a real time baseline correction to remove spurious features such as fluorescence from the spectrum If the sample is a poor Raman scatterer or
26. ic vs Expert User Interface Selecting Basic Interface allows the software to automatically use default settings for many of the basic controls These control buttons will be hidden on the viewing window Fig 13 This provides an easier to learn interface for casual users Selecting the Expert Interface gives access to all of the controls that are available for the current Spectrometer s a i E i i b i i i i i i i i wil m on Lt 3000 Eso 10 16000 1000 m H Ta Mob HI in Ln aa eee Durserr iz it mrs ADDED I i HE FL pone 100 a Time Reference one tl we Taken Stan Taken 7 lt lt lt _ aes Spectrum fio ey Ea APT E E 3 Ford Deport Fig 13 Basic user interface 4 6 Laser Power The Laser Power bar selects the power of the laser from five settings ranging from low to high Fig 14 It is normally best to use the High power setting for the laser This will provide the best signal to block out background noise However some samples may be burned or destroyed under High laser illumination When sample degradation is observed a lower power setting is suggested Laser Power Y High Fig 14 Laser power Advantage Series User Manual DeltaNu May 2009 15 4 7 Polarization This feature automatically subtracts molecule polarizations from the spectrum in order to provide information about the molecular symmetry The pol
27. mounted on the exit port with Allen screws and it is used for sampling liquids emulsions and powders through 8mm vials Inserts are provided for the analysis of liquids and crystals through NMR tubes and MP tubes The focusing knob is used to optimize the Raman signal The most intense Raman signal is obtained as the focal length is optimized 16 45 mm from the objective just beyond the glass interface 11 2 XYZ Stage The XYZ Stage is a manual positioning stage mounted directly on the instrument near the face of the exit collection port which minimizes disturbances and vibrations that may occur with externally mounted stages It 1s used to optimize and precisely position the beam on contaminants in thin films coatings and semiconductors inclusions in geological materials and on biomedical substrates The most popular method of securing the sample to the stage is two sided tape The XYZ stage allows the user to position traverse and adjust the focal position in micron steps Advantage Series User Manual DeltaNu May 2009 30 Le adh ata 3 Attach Magnetic SYSTEM IS OFF Interlock Override With Magnets Facing Towards Advantage System 2 Remove Sample Holder Using 1 8 Allen Wrench Sample Holder 4 Attach XYZ Stage To Bottom Of System Using 9 64 Allen Wrench Fig 46 Attachment of XYZ Stage 11 3 Right Angle Input Optics
28. n Fig 28 Another reason to save a multi file is to load the spectrum back into the NuSpec software and manipulate resolution etc If the file 1s saved at low resolution the smoothing effect 1s applied permanently and cannot be undone The integration time cannot be set higher than 10 seconds The lowest setting is 0 01 seconds 5 4 Load Spectrum This feature loads a spectrum spc or dnu file A new window will open when you click this button Fig 29 Select the spectrum that you wish to load from the appropriate folder Load Spectrum Fig 29 Load Spectrum Advantage Series User Manual DeltaNu May 2009 21 5 5 Load Library The Load Library feature loads a library of spectra from a specific folder Clicking on the Load Library button will open a new window that allows library or spectra files to be added selected or de selected or deleted Click on the Save button to continue after your final selections have been made To delete a spectra or library click on the file name to highlight it and click on the Delete button on the bottom of the screen To delete all the spectra libraries listed click on Delete All To exit this screen without making changes click on the ABORT button Select Library Files Y C Documents and Settings mfox My Documents Chemistry Advantage 2004 spectra 200a acetonitile spc C Documents and Settings mfox My Documents Chemistry Advantage 200A4 spectra 200a corn starch via C Documents and
29. nce Every N Spectra 0 for never em Number of Spectra to Acquire J Sequence Delay ln a LA A t A ine HO amp cat l I I l 1 1 1 1 1 I I 1 1 1 l 1 200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 3000 3200 3400 Wavenumber Cursors ix dY a FR ER HR vw BE CursorO 1004 1 1000 A a Spectrum Name Correlati Library Entry Name Library File 0 08 ibuprofen baseline _ C Documents and Settings mfox My Documents Chemistr 0 06 cyclohexanez C Documents and Settings mfox My Documents Chemistr x Time Reference Was Taken 1 42 56 539 PM 5 11 2009 Time Spectrum Was Taken 1 42 54 821 PM 5 11 2009 Color Specify E Calibration Peaks Calibrate z Copyright DeltaNu 2009 Fig 31 Library entry 5 6 Sync Library to Spectrometer DEK EXIT Connect to New Spectrometer Display J Spectrum a Resolution A J Low Baseline gt 150 Save Spectrum J Save Display J Save as dnu DeltaNu Load Spectrum Load Library Save Library Matches Print Report The Sync Library to spectrometer button loads the currently selected library to the system For the ReporteR model only Sync Library bo Spectrometer Fig 32 Sync library to spectrometer 5 7 Display Screen There are several features that allow the user to navigate the cursor on the spectrum viewing window zoom in on specific peaks and move the location of the viewing win
30. o a spectrometer and its clock is set different than the computer s clock it will ask you if you want to synch the spectrometer s clock to the computer Fig 8 Click OK to do so The clocks in the spectrometer and computer are different Spectrometer Clock 5 13 2009 11 52 AM Computer Clock 5 13 2009 10 53 AM Do you want to set the spectrometer clock Eo be the same as the computer clock Cancel Fig 8 Synch spectrometer clock 4 3 Serial Number The spectrometer is properly communicating with the software if the serial number of the device is displayed in the Serial Number box found in the upper right hand corner of the viewing window Fig 9 The software will automatically display the serial number in the box if the spectrometer is properly connected turned ON and the correct computer port was selected The user can select the Connect to New Spectrometer option to use another DeltaNu system while the software is running Serial Number 20117 Fig 9 Serial Number Advantage Series User Manual DeltaNu May 2009 12 4 4 System Calibration Each user should initially setup a calibration parameter file with the software Such parameters are used to correlate the pixels of the spectrum viewing window to a specific range of wavenumbers and to standardize the device to the polystyrene ASTM standard This feature allows the software to determine the peak windows in which to search for the polystyr
31. o use automatic Integration Time select either Hardware referencing or select None To take a new reference select retake software reference only and click acquire The reference spectrum will be displayed on Advantage Series User Manual DeltaNu May 2009 16 the graph and you can save it like a normal spectrum if you want to use it for further analysis A new reference spectrum is taken every time the integration time is changed Users should also take a reference when the ambient light has changed Referencing Mode i Software a T Fig 17 Referencing mode 4 10 Number of Spectra to Acquire This feature 1s used to acquire a specified number of spectrum consecutively that can then be averaged together Select the number of spectrum to acquire using the up and down arrows or the number pad on the keyboard Fig 18 Click the Acguire button to collect the spectra To view the averaged spectrum or the individual spectra use the Display feature to select the option of choice see Display section below Number of Spectra to Acquire h of Fig 18 Number of spectra to acquire 4 11 Display The Display feature allows the user to switch between showing the individual spectrum acquired or the averaged spectrum To view a specific spectrum in the averaged series select the display Spectrum option in the top box Fig 19 and use the arrows on the box below to scroll through the spectra n
32. perly installed please follow the steps below 1 Connect the USB cable to the PC and to the spectrometer 2 When prompted for on the New Device Recognized screen please browse for the file using automatic detection The system will automatically search for the file CDM 2 04 06 WHOL Certified in the spectrometer software folder If your PC is not able to detect the CDM 2 04 06 WHOL Certified folder automatically you can select this file manually The first screen to appear is the Welcome screen Fig 52 Select Yes this time only and click Next Found New Hardware Wizard Welcome To the Found New Hardware Wizard Windows will search for current and updated software by looking on pour computer on the hardware installation CO or on the Windows Update Web site vith your permission Read our privacy policy Can Windows connect to Windows Update to search for software es now and every time connect a device No not this time Click Next to continue Back Cancel Fig 52 Welcome screen The next screen is the USB High Speed Serial Converter screen Fig 53 Select Install from a list or specified location Advanced and click Next Advantage Series User Manual DeltaNu May 2009 35 Found New Hardware Wizard This wizard helps you install software for USB High Speed Serial Converter 9 IF your hardware came with an installation CD 2 or floppy disk insert it now What do pou
33. rom the spectra giving a smoothing effect to the spectra The number allows the user to fine tune the baseline algorithm to account for differences in the width of peaks for different spectra Baseline ca co Fig 27 Baseline 5 0 Saving Spectrum The Save Spectrum button allows the user to save spectra to specific library folders The spectrum can be saved as displayed on the screen Save Display or as raw data Save Raw Data by using the arrow keys next to the top box Fig 28 Next you can choose what type of file to save it as using the arrow keys on the second box Files can be saved as dnu spc or prn extensions Once you have chosen the file type click on the Save Spectrum button choose a library or folder in which to save the spectra file and give the file a name Note To save a library file it must be saved with the Save Display function Save Spectrum 7 Save Display Mave as onu DeltaMu Fig 28 Save spectrum menu 5 1 File Types Library entries used for the library builder may be saved as spc dnu or prn files However it is recommended that library entries are saved as spc files If you wish to be able to load a spectrum back into the NuSpec software then save it as a dnu file to preserve all of the metadata To be able to load a spectrum into GRAMS save it as a spc file To load it into Microsoft Excel it must be saved as a prn file Advantage Series User Manual Delta
34. rt the software Once the intensity is optimized and the background noise is minimized click the Continuous button again to stop the acquisition Now adjust the integration time to the desired time and click Acquire The integration time required to obtain a spectrum depends on the sample and the application The Advantage series detector begins to saturate around a signal greater than 65 535 counts per second To obtain the best signal to noise ratio keep the largest peak in the spectrum close to but under 65 500 counts per second Advantage Series User Manual DeltaNu May 2009 9 4 0 NuSpec Software A figure showing the software user interface window is illustrated below Fig 5 with a further explanation of all its features A DeltaNu system must be on and connected for the software to work properly 4 1 Spectrometer Specific User Interface Certain controls do not apply to some spectrometers For example not all spectrometers have the Polarization feature or automatic integration time When you connect to a spectrometer the software user interface hides the controls that do not apply to that Spectrometer gt NuSpec aag Battery Serial Number gt TM f Not Connected i EXIT NuSpec pee Volume eger Temperature f Connecta AR Jo o New Spectrometer Laser Power z 24000 Display high e Spectrum 21 22000 2 Polarization NH O PPI cal ot Polarize 5 z j Not Polarized 20000
35. s 3 Resolution 18000 Low Integration Time 16000 Baseline an No S r 1 A 160 ut j 14000 Referencing Mode a BES S R z J Software 12000 e Save Spectrum D S 10000 qseve Display Retake Software A Reference Every N Spectra 0 for never Jlo Save as dnu DeltaNu f y Y Number of Spectra to Acquire Sp A Sequence Delay o A Load Spectrum Load Library I I 1 1 I I I I I I 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 3000 3200 3400 Syne Library to Wavenumber Spectrometer Acquire E lt a ma vE Pa CT ath Cursors mer ee ee He 17 Save Library y E CursorO 1000 1000 1 Time Spectrum Time Reference rat t Matches Continuous ommen al gt Was Taken Was Taken Spectrum Name 00 00 00 000 PM 00 00 00 000 PM 3 MM DD YY YY IMM DD YYYY Print Report ABORT Color Correlation i Library Entry Name i Library File 4 A Specify Calibration Peaks i Calibrate t _ Copyright DeltaNu 2009 e Ps l gt gt gt _ Q _ _ _____________ ooo Fig 5 NuSpec software screen Advantage Series User Manual DeltaNu May 2009 10 Select the NuSpec software from C Program Files DeltaNu or from a Desktop shortcut that you may have created When the software is first opened the computer port that the spectrometer is plugged into must be selected before continuing Fig 6
36. s you can just click the button to load defaults for your model of spectrometer and then click save Systems with a Mosir camera require several extra parameters Consult our documentation for the necessary parameter values Save ABORT Has a Mosir Load defaults for Port 1 Get Mosir Advantage 532 E COM Serial Number AA Serial Number vantage i i g 20117 i Serial Number Advantage 785 Firmware Version 7 Advantage 633 i Mosir Type E 350 ExamineR 785 First Wavenumber Mosir Y Start it InspectoR r 200 Jlo Last Wavenumber Mosir End 113400 o Reporter Imager Temperature Mosir High Voltage ObserveR RockHound l Load defaults for A THU Fig 7 Create spectrometer parameter file Advantage Series User Manual DeltaNu May 2009 11 4 2 Disconnected Mode When the software prompts you to select the spectrometer computer port if you click ABORT the software will go into the disconnected mode It will also go into disconnected mode if there is an error while attempting to connect to a spectrometer In this mode the serial number display will read Not Connected While you are Not Connected you can still upload spectrum files and library files view the spectra and perform sample matching Any of the controls on the left that communicate with the spectrometer directly will be ignored This can be a useful mode to do off line data analysis Note If you connect t
37. t 2002 2009 DeltaNu All rights reserved Advantage Series User Manual DeltaNu May 2009 Manufacturer Model Type of Equipment Testing Provider and Certification by Tests CE Declaration of Conformity DeltaNu Inc 5452 Old Highway 130 Laramie WY 82070 307 745 9148 Fax 307 745 9152 www deltanu com sales deltanu com Advantage Systems Raman Spectrometers Communication Certification Laboratory Salt Lake City Utah Emissions EN 55011 1998 FCC Part 15 Subpart B ICES 003 Test Serial No 73 8004 Immunity EN 55024 1998 EN 61000 3 2 EN 61000 3 3 Test Serial No 83 0972 Safety EN 61010 1 1990 A1 1992 A2 1995 Test Serial No 89 0667 the undersigned hereby declare that the equipment above conforms to the above Directives and Standards when used in accordance with the manufacturer s specifications Place of Issue Laramie WY Ned ameno Date of Issue October 20 2004 Keith Carron General Manager Advantage Series User Manual DeltaNu May 2009 4 1 0 Introduction Congratulations on your purchase The Advantage series spectrometers are easy to use on solutions gels powders and coatings The Advantage series covers a wide spectral range for analysis of inorganic anions to aliphatic hydrocarbons It is used in industrial applications academic research and teaching labs This manual will lead you through initial set up steps for taking a spectrum and a thorough descrip
38. three months in humid areas and every six months max in dryer areas The desiccant will turn from a blue to pink when it has adsorbed a significant amount of moisture If the desiccant is dark blue you do not have to change it Steps To Replace The Desiccant Remove Desiccant Holder Plug Using 3 16 Allen Wrench 2 Replace Old Desiccant With New Desiccant Attach Desiccant Holder Plug Figure 58 Desiccant replacement instructions 14 0 Raman Tutorial Raman spectroscopy finds its origins in Planck and Einstein s formulation that light is not only wavelike in nature but has the dual character of waves and particles Once scientists began thinking about the concept of light as particles the possibility of inelastic scattering of these particles became a method of proof of this new theory In 1923 Compton showed this with inelastic scattering of x rays from a graphite target That same year Smekal theoretically predicted that photons should inelastically scatter from molecular transitions Five years later in 1928 C V Raman and K S Krishnan published an article in the journal Nature with experiments that proved Smekal s prediction of inelastic scattering of light For his discovery Raman was award the Nobel Prize and the inelastic scattering of visible light from molecular transitions has been named after him One of the characteristics of inelastic scattering is that the intensity of the scattering scales to the fourth
39. tion of the DeltaNu software and features Other sections in this manual will help you improve spectra by describing the product software features in more detail provide basic troubleshooting for the most common problems seen while operating and contact information for problems not found in the manual Also included are pictures and descriptions of all attachments available for use with the Advantage series spectrometers along with guides for installation Advantage Series User Manual DeltaNu May 2009 1 1 Unpacking and Checklist Using the checklist found in the shipping container or the following list review and make sure all parts are accounted for The following items come standard with an Advantage series spectrometer Advantage series Raman Spectrometer Sample Holder Assembly Melting Point Tube Adapter NMR Tube Adapter Vials 250 8mm sample Jump Drive or CD o DeltaNu Software o SPC Viewer Instruction Manual Power Supply Power Cord USB Cable 1 8 Hex T Handle Wrench 3 16 Allen Wrench Extra Desiccants Laptop PC with Kensington Lock Library Management Software The following items are accessories for the Advantage series spectrometer XYZ Stage o Magnetic Interlock Override o 9 64 Hex Wrench Input Optics Extension Right Angle Input Optics NuScope o 5 32
40. ton The system will acquire a reference spectrum with a shutter blocking the laser beam and then continually acquire spectra with the reference subtracted out every second This real time mode allows the user to observe changes in the spectrum while manipulating the sample holder Now that the system is displaying real time spectra properly focus the laser beam onto the sample material by adjusting the silver knob on the front of the sample holder For liquids the focus is not critical and there is a large range over which the adjustment makes very little change in the spectrum When the sample is far away from the instrument there is a decrease in signal and perhaps an increase in background as the glass sample vial itself moves into focus Similarly if the sample is too close the sample vial will dominate the spectrum Once the laser is focused for optimal signal the user should not have to make adjustments However the distance is dependent on the index of refraction of the sample and may differ slightly with different samples Solids are optimized the same way If the solid is opaque the optimization 1s more critical than with liquids The ideal distance will be that at which the laser is focused just on the sample material and not the glass vial The Advantage series have an interlock that shuts the laser off if the sample holder is removed If the laser turns off while focusing because the interlock has been tripped focus back and resta
41. umbers To view the averaged spectrum simply select the Average display option in the top box Display Spectrum Js Fig 19 Display Advantage Series User Manual DeltaNu May 2009 17 4 12 Sequence Delay The Sequence Delay feature can be used when acquiring multiple spectra at once to insert a specified time delay in between acquiring each spectrum The time is set in seconds from the start of the first acquire to the start of the next acquire If the delay is less than the specified integration time then each spectrum is acquired for the full integration time and the next acquire starts as soon as the previous one is done Sequence Delay s Fig 20 Sequence delay 4 13 Acquire Clicking on the Acquire button turns the laser on and begins the acquisition of the spectrum At this point the software will collect as many spectra consecutively as you have specified Note When more than one spectrum is acquired it can be saved as a multi file or as a single averaged file The procedure to save a single file or a multi file 1s further described in the section below titled Save Spectrum Fig 21 Acquire 4 14 Busy The Busy light Fig 22 in the top right corner of the viewing window is on when the software is busy Note This light is not an indication of the laser being ON or OFF For example when an Acquire action is performed the Laser Warning indicator will turn off when the laser goes off
42. want the wizard to do Install the software automatically Recommended Click Next to continue Back Cancel Fig 53 USB high speed serial converter screen The search and installation options menu will now appear Found New Hardware Wizard j Please choose your search and installation options S f Search for the best driver in these locations Use the check boxes below to limit or expand the default search which includes local paths and removable media The best driver found will be installed Search removable media floppy CD ROM IM Include this location in the search JCD ocuments and Settings Compaq Owner Deskto Dont search will choose the driver to install Choose this option to select the device driver from a list Windows does not guarantee that the driver you choose will be the best match for your hardware lt Back Hest gt Cancel Fig 54 Search and installation options Select Browse and find the location of the USB Driver files Click Next after you have selected the appropriate file location from the Browse For Folder window Fig SS Advantage Series User Manual DeltaNu May 2009 36 Select the Folder that contains drivers For your hardware y My Network Places ED 3 1 06 DN 5 8 03 0014 3 builds O DeltaNu Software 9 Labview Prior fem Reporte Fig 55 Browse for folder window The software will now search for the driver files
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