to PDF - Active Spectrum
Contents
1. Extended Range 70 6 960 0 3 6 9631 0 60 X Y X Y 0 1 and 0 5 Ferrofluid in Toluene 1 5 and 10 Ferrofluid in Toluene Antioxidant Radicals in Lubricants ESR is a very effective way to monitor and identify antioxidants in lubricants Peroxy and other radicals formed as thermal degradation products react with antioxidants often forming stable radicals which are visible by ESR Flucidate reaction mechanisms through radical adducts ET I I I I I I I i 3420 3430 3440 3450 3460 3470 3480 3490 3500 Butylated Hydroxy Toluene BHT Loses the OH proton to free radicals py OH Med Q SPECTRUM O PES rum 3442 3 0 A Y 0 7 I I I I i 1 I I 1 I U I I 3420 3425 3430 3435 3440 3445 3450 3455 3460 3465 3470 3475 3480 l i CH t Bu SD o t Bu H3C CH3 ea OH de O Ors CH3 t Bu t Bu uch CH3 CH3 Galvinoxyl radical 4 4 methylenebis 2 6 Di tert butylphenol Loses the OH proton to free radicals Optically Polarized Nitrogen Vacancies in Diamond NV m 1 to m 1 NV m 0 to m 1 BW p Pl 4 at Pi r P1 lines 7 2 Naturally abundant NV VA BC hyperfine lines 160 200 240 280 320 360 400 440 mT NV m 1 to m 0 Special mirror allows laser light to be shown in to the resonator cavity to induce optica2. 3510 3520 3530 3540 3550 a ae Flat Cell Capillary Imm ID Signal to Noise 70 1 Signal to Noise 30 1 64 scans 4k points 15 mW 100 G sweep width O SPE rum Resolution Q Perylene Radical Cation Rad 3 3 1 EF 1 f i ae WT 344193445 3450 3455 3460 3465 3470 3475 3481 ACTIVE SPECTRUM Q stCrum Semiquinone Radical Anions 5 4 i I I I 1 1 1 1 I 1 3450 3452 3454 3456 3458 3460 3462 3464 3466 3468 3470 catechol ep 3444 3446 3448 3450 3452 3454 3456 3458 3460 3462 3464 34i 2 butylbenzosemiquinone 2 28 B 2 01 1 67 1 38 C 3 38 0 74 ACTIVE Some Applications OS rem Spin Trapping Kinetics Coordination Chemistry Antioxidant Radicals in Lubricants Dosimetry Crystal Defects Education DMPO as a Spin Trap For OH Electron spin resonance spectroscopy is a well established technique for measuring the signal from hydroxyl radicals that are spin trapped by DMPO These hydroxyl radicals are generated via the Fenton Reaction Fei H O gt Fes OH OH DMPO OH gt DMPO OH Micro ESR provides a portable cost effective and sensitive spectrometer that can measure DMPO OH radicals from this reaction DMPO OH Spin Adduct Q SPECTRUM PTIO as a Spin Trap for Nitric Oxide 1 ESR signal of a Phenyltetramethylnitronly nitroxide PTIO gt PAPA NONOate NO source is added to the tube 2 The ESR signal changing from the nitronyl nitroxide to the imino nitroxide 3 The imino nit
3. 853 Ct MY V DeltaY g I I I 3480 3490 3500 H el LUN Y axis First Derivative Load as many or few files as needed into the Micro ESR processing software WF X axis Magnetic field G f AXIS OPTIONS SAVE Display a single spectrum or overlay as many spectra as needed VA ALL ON OFF NORMALIZE lv Iiv v iiv vila viiv viiv ACTIVE SPECTRUM V FiteNames Concentrations Spectra Manipulation l Tempoldil l Concentrations l GrowthDecayvs Time Three Line Spectra SNR l PAChristine At A PiChristineiLAE v iv et AE Mu PAChristineiLAE Auto Center Center Field ho LOAD DELETE Se A 17 6 Frequency MHz 9731 39 i Power im P 5 No of Points 2048 0 No of Sweeps 1 0000 Scan AVERAGED Sa i COUT RAGE ANG IE 10 12 14 16 18 20 ADD VALUE TLS Double Integral ADD ALL 1042 14 CLEAR PAChristineiLABS fi 2019 11 S PAChristineiLABS 10828 54 PAChristineiLABS 3491 73 a Processing softvvare automatically calculates the double integral of all selected spectra and displays the values in a bar graph Ocean Spray Diet Blueberry Juice Data is saved is csv format so can D easily be read into other i S processing programs if desired KATE RE ia ma CE El ACTIVE Transition Metal Compounds CO scrum Extended Range 526 2 i i 2355 59 2750 3000 3250 3500 3750 3293 4 4268 Ferrofluids GES
4. 9 6 Delta x o Delta Y o Ta 12 I I I 1 I i a I I v I Detta Y 9 3420 3430 3440 3450 3460 3470 3480 3490 3500 3510 3520 8 I I 1 1 I 1 1 I H I 3420 3430 3440 3450 3460 3470 3480 3490 3500 3510 3520 The PBN CH spin adduct A third spin adduct MNP CH has formed remains and another spin and is superimposed on the PBN CH spin adduct is forming adduct Identifying Spin Adducts The hyperfine coupling constants help to identify the trapped radicals and give information about the electron spin density The hyperfine coupling constants are smaller both for the nitrogen and the proton in the PBN OCH spin adduct than the PBN CH spin adduct because the oxygen in the methoxy pulls spin density away from the nitrogen More direct information can be obtained about the radical from the nitroso spin adduct because the radical adds directly to the nitrogen atom We see coupling from the methyl protons only in the MNP CH spin adduct We know that it is the methyl not the methoxyl radical that had added to the MNP because MNP does not form oxygen centered radicals Q EE rum Kinetics and Spin Traps Stable radicals such as TEMPOL can be used to monitor reaction rates TEMPOL has an intense ESR signal and can react with other radicals to form ESR silent products The rate at which the TEMPOL signal disappears can be used to determine reaction rates and mechanism Active Spectrum s user friendly acquisition software allows for quick a
5. Q Stereum Active Spectrum s Benchtop Electron Spin Resonance Spectrometers Q SP rum Extended Range Benchtop ESR 4000G sweep range air cooled 6500 G sweep range water cooled Compact benchtop design Competitive pricing Variable temperature accessories available Technical Data Q EE rum 9 6 to 9 8 GHz Resonator Sample Tube Diameter Sweep Range Supply Voltage Data Interfaces Screen Dimensions Mass Cylindrical Dielectric Up to 5 8 mm Up to 6500 Gauss water cooled Up to 4000 Gauss air cooled 120 240 VAC Ethernet USB and 802 11 WiFi 21 cm Touch Panel display with Windows 7 Embedded DVI HDMI VGA 30 5 x 35 5 x56 cm 54 kg Q SERM Micro ESR Spectrometer Easily Transported Anywhere Plug In Power On Acquire Spectra Versatile Applications in Research Education and Industry Variable temperature accessories available Technical Data CD SE um Resonator Sample Tube Diameter Svveep Range Supply Voltage Data Interfaces Screen Dimensions Mass Cylindrical Dielectric Up to 5 8 mm Over 330 Gauss Centered at g 2 15 VDC 120 240 V Wall Adapter Included Ethernet and USB 21 cm Touch Panel display with Windows 7 Embedded DVI HDMI VGA 30 5 x 30 5 x 30 5 cm 10 kg O SE reum Online Benchtop ESR World s first industrial process monitoring instrument eProvides real time embedded non destructive measurements of free radicals and some tr
6. ansition metals Designed to work under harsh environmental conditions Easily transported to any site Hazardous location rated enclosures available Class 1 Div 1 and ATEX Technical Data CD SE rum 9 6 to 9 8 GHz Resonator Sample Tube Diameter Flow Mode Sample Tube Diameter Tube Mode Sweep Range Supply Voltage Data Interfaces Screen Dimensions Mass Operating Temperature Maximum Pressure Maximum Fluid Inlet Temperature Cylindrical Dielectric Up to 6 mm OD Up to 3 mm OD Over 300 Gauss centered at g 2 15 VDC 120 240 V wall adapter Included Ethernet and USB 21 cm Touch Panel display with Windows 7 Embedded DVI HDMI VGA 30 5 x 15 x 23 cm 10 kg 30 to 85 degrees C 100 psi 160 degrees C ACTIVE SPECTRUM Signal to Noise NOTE Signal and noise measurements are made using the same conditions The signal is calculated as the average of the amplitude of the three TEMPOL peak heights divided by two times the RMS noise in the Same spectrum Signal to Noise peak amplitude 2 RMS noise CD SERUM 50 uM TEMPOL in Water 1 scan 4k data points 15 mW GN gt 200 1 Extended Range Benchtop O SERUM 1 UM TEMPOL in Water Es e 0 5 3550 0 8959 3450 0 0 8 X Y 0 4 X Y 0 6 0 3 0 4 0 2 0 2 0 1 0 0 0 2 0 1 0 4 0 2 0 6 03 0 8 0 4 0 5 1 I I I I I I I I I i 3450 3460 3470 3480 3490 3500 3510 3520 3530 3540 3550 3450 3460 3470 3480 3490 3500
7. l polarization Data courtesy of Eric Scott Jeff Reimer s Lab UC Berkeley Extended Range Benchtop O FEE rum Dosimetry e Electron Spin Resonance can be used to measure radiation exposure e Signal amplitude of irradiated sample is proportional to the dose sample specific and true only for good dosimetry samples 225 i 20 17 5 15 12 5 10 i o gt 5 2 5 J TW 0 2 5 5 7 5 Delta x g Delta Y g l I 3500 3525 O FEE Rum Spectra of sample irradiated with 1 2 and 5 Gy from a Co source 1 5 Delta X p Delta Y g 3475 3500 3525 Doen y 0 7852x bi ose mesponse R2 0 9987 40 a Linear dose response of sample for 30 radiation doses from 1 to 50 Gy San lt x15 Cu 5 0 I 0 10 20 30 40 50 60 Dose Gy Crude Oil Analysis Q ser 704 3400 0 Vanadyl 20 10 ce qe Acer D PORE E 10 20 30 40 50 60 70 We 80 Asphaltene Asphaltenes contain radicals and vanadyl porphyrins are commonly found in crude oil Education Q run Active Spectrum s Micro ESR is an ideal undergraduate teaching tool It can easily be moved to labs classrooms or shared Easy to use so students can start to acquire data quickly Can be purchased with an Education Package Micro ESR Education Package Micro ESR Spectrometer Micro ESR Experiments Manual with Seven Labs Micro ESR Instr
8. nd easy set up of kinetics experiments Easy to use processing and analysis software allows for quick analysis of data Q SEE rum MMMM ETM Data Acquisition Sweep Settings Insert Sample into Spectrometer Comment Run Type EPI Single Run Continuous Runs Number of Multiple Runs with Delay Number of Auto minimum of points Number of Runs 10 Delay sec 15 2 Choose Multiple Runs with Delay O FEE Rum Sample Name vO acac 2 Comment Run Type Multiple Runs Number of Scans Number of Points Auto minimum of points Number of Runs dio Delay sec dis 3 Set up the Experiment a b d d e Enter the number of scans Enter the number of points per scan Enter number of runs Enter the delay time between runs Start acquisition VA VIFlleNames ALL ON OFF NORMALIZE v li e lv ily a v iiv i Iv iiv IE v iiv PAChristinei LA A P Christine LAe P Christine LAe P Christine LAE P Christine LAt Concentrations Array Operations Ad 397 30 vivim PChristineiLAE LR I PAChristineiLAE lv liv PAC hristineXLAE LOAD DELETE Frequency MHz 9731 9 Power mv 15 No of Points 2048 0 No of Sweeps 4 0000 Scan AVERAGED se DEL SCAN i ich I 3420 3430 j Spectra Manipulation Shift Wim I 3440 Data Processing Filtering F1 F2 F3 V d d V i I 3450 3460 Other Functions 881 852
9. roxide ESR signal Q SE um Determine Reaction Mechanisms by Observing Spin Adducts Using PBN t butyl a phenyl nitrone as a spin trap we follow a Fenton Reaction in DMSO The Fenton Reaction generates hydroxyl radicals which react with the PBN but also the DMSO The PBN OHe spin adduct is too short lived to observe directly but methoxyl OCH el radicals are also produced The PBN OCH spin adduct is long lived and easily observed by ESR As the reaction proceeds the major spin adduct changes from methoxyl to methyl MNP 2 methyl 2 nitrosopropane a spin trap itself is formed during the reaction MNP forms a third spin adduct with methyl radicals Q SEE rum 14 3420 10 3420 0 3420 0 12 A Y 25 X Y 20 A y 10 20 45 B 15 SR 10 4 10 GE 5 sa 0 Bs 0 SO ES NT NT A 0 4 5 5 8 10 10 10 15 SE DeltaX o ae DeltaX g 15 DeltaX o gen DeltaY 9 Delta Delta Y 16 i I I I I I I I i s K ch I I I I I I I I I ws 20 Eet 1 1 I 1 I 1 I I I 3420 3430 3440 3450 3460 3470 3480 3490 3500 3510 3520 3420 3430 3440 3450 3460 3470 3480 3490 3500 3510 3520 3420 3430 3440 3450 3460 3470 3480 3490 3500 3510 3520 PBN OCH Spin Adduct A second spin adduct Both PBN OCH and starts to form PBN CH Spin Adducts are present g m 3420 o ae 3420 0 T la X Y 6 ig 10 5 8 4 6 4 il 2 2 a o 0 M T a AE es A 41 er 4 3 6 4 8 5 Delta X p
10. uctor s Guide Lab Accessory Kit Micro ESR User s Manual Micro ESR Analysis and Processing Software with Manual http www activespectrum com Micro ESR_ Education Pkg2B Summary pdf CO PES RUM GEZ Contact e These are only a small number of ESR applications e For more information http www activespectrum com about us shtm Active Spectrum 1191 Chess Dr Foster City CA 94404 USA 650 212 2625 www activespectrum com
Download Pdf Manuals
Related Search