Horiba Scientific Quanta-phi F-3029 Скачать руководство пользователя страница 7

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Quanta-

rev. C (23 Apr 2010)

Introduction

0-1

Note:

Keep this and the other reference manuals near the system.

: Introduction

About the Quanta-

φ integrating sphere

This manual explains the theoretical and practical issues of operating and maintaining
the Quanta-



integrating sphere. The Quanta-



is used with the Fluorolog

-3, Fluoro-

Max

-3 and -4, and Fluorolog

-Tau-3 spectrofluorometers to study fluorescence from

solid, powder, thin-film and liquid samples. The main purpose of the Quanta-



is the

measurement of photoluminescence quantum yields of such materials.

The Quanta-



integrating sphere accessory is external to the spectrofluorometer. Light

from the sample compartment is directed into the sphere via a fiber-optic cable and the
F-3000 Fiber-Optic Adapter, and returned to the sample compartment (and then to the
emission monochromator) via a second fiber-optic cable and the F-3000.

Содержание Quanta-phi F-3029

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Страница 3: ...Quanta rev C 23 Apr 2010 i Quanta F 3029 Integrating Sphere Operation Manual rev C http www HORIBA com scientific...

Страница 4: ...ording without prior written permission from HORIBA Jobin Yvon Inc Requests for permission should be requested in writing Information in this manual is subject to change without notice and does not re...

Страница 5: ...t of method for data acquisition 1 14 Additional references 1 15 2 Requirements Unpacking 2 1 Environmental requirements 2 1 Software requirements 2 1 Unpacking 2 2 3 Installation Use 3 1 Method 3 1 C...

Страница 6: ...Quanta rev C 23 Apr 2010 iv...

Страница 7: ...d Fluorolog Tau 3 spectrofluorometers to study fluorescence from solid powder thin film and liquid samples The main purpose of the Quanta is the measurement of photoluminescence quantum yields of such...

Страница 8: ...g from your use or misuse of any such products including without limitation to persons injured directly or indirectly in connection with your use or operation of the products The foregoing indemnifica...

Страница 9: ...f use loss of data or loss of profits arising out of or in connection with our products or the use or possession thereof HORIBA Jo bin Yvon is also in no event liable for damages on any theory of liab...

Страница 10: ...t in personal injury or death Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met HORIBA Jobin Yvon Inc is not responsi ble for damage arising out of imp...

Страница 11: ...ne who has had sunburn However the UV light level around some UV equipment greatly exceeds the level found in nature Acute short term effects include redness or ulceration of the skin At high levels o...

Страница 12: ...NORMAL EYEGLASSES OR CONTACTS OFFER VERY LIMITED PROTECTION Training For the use of UV sources new users must be trained by another member of the labora tory who in the opinion of the member of staff...

Страница 13: ...ury to the retina This type of injury can occur during a single prolonged ex posure Excessive exposure to visible light can result in skin and eye damage Visible light sources that are not bright enou...

Страница 14: ...the heat deposited in the cornea may be conducted to the lens of the eye This heating of the lens is believed to be the cause of so called glassblow ers cataracts because the heat transfer may cause c...

Страница 15: ...t with an area A2 of defi nite size With geometrical considerations we can integrate the differentials to get sphere A A r A F 2 2 2 4 2 Equation 2 tells us that the fraction of light F that A2 receiv...

Страница 16: ...rminations The impulse response of an integrating sphere takes the form t e where is the time constant of the integrating sphere and is c d sphere ln 1 3 2 6 Equation 6 considers also the diameter of...

Страница 17: ...elated to events such as quenching and thermal dissipation or energy transfer kT processes including F rster Resonance Energy Transfer FRET will decrease both the quantum yield and fluo rescence lifet...

Страница 18: ...file from an empty integrating sphere without the sample only a blank Here Ea is the integrated luminescence from an empty integrating sphere only a blank For integration of function L over the wavele...

Страница 19: ...mple and blank s fluorescence spectral region intensities were measured us ing a 4 second integration time under otherwise the same instrument conditions as the La and Lc Integration of the emission s...

Страница 20: ...are performs an error propagation analysis to help evaluate when signal levels are not properly balanced This may occur with dilute concentrations of the sample or when samples exhibit very low quantu...

Страница 21: ...ger source of error is in the denominator Self absorption and inner filter effects The measurement of as an absolute value is strongly influenced by the sample con centration Relative changes and obse...

Страница 22: ...excitation black and emission red spectra to illustrate the overlap ping regions responsible for self absorption Clearly the overlap is much larger in rho damine 101 than in quinine sulfate The middl...

Страница 23: ...e right de picts the observed rela tionships between the in tegrated fluoresence area the absorbance and quan tum yield of fluo rescein in 0 1 N NaOH Clearly as the OD in creases beyond 0 1 units the...

Страница 24: ...that the sample is diluted to vary and minimize self absorption at the surface The solid dilution also serves to dilute the chromophoric sample to the point where its light scattering proper ties are...

Страница 25: ...cted in the figure on the right The regions of spectral overlap for the luminescence emission spectrum is eva luated by calculating the sum product of the emission spectrum with each of three observab...

Страница 26: ...rdinate at each wavelength value where xBar yBar and zBar are the intensity values from the three observable profiles at wavelength The corresponding xBA and yBA values are plotted against each other...

Страница 27: ...corresponding u BA and v BA values are plotted against each other to generate the closed semielliptical two dimensional area boundary plot for CIE 1976 blue right as shown in the sample plot for rhoda...

Страница 28: ...Quanta rev C 23 Apr 2010 Theory of Operation 1 14 Flowchart of method for data acquisition...

Страница 29: ...F Wittmann and R H Friend Adv Mater 9 230 1997 Measurement of Solid State Photoluminescence Quantum Yields of Films using a Fluorimeter L O P lsson A P Monkman Adv Mater 14 10 2002 757 758 Absolute M...

Страница 30: ...Quanta rev C 23 Apr 2010 Theory of Operation 1 16...

Страница 31: ...acking Environmental requirements Temperature 59 86 F 15 30 C Maximum temperature fluctuation 2 C Ambient relative humidity 75 Low dust levels No special ventilation Software requirements FluorEssence...

Страница 32: ...representatives of the receiving and carrier companies Once a location has been chosen unpack and assemble the equipment as described be low To avoid excessive moving and handling unpack the equipmen...

Страница 33: ...Sphere 1 Carefully open the shipping carton 2 Remove the foam injected top piece and any other shipping restraints in the carton 3 Carefully lift the integrating sphere from the car ton and rest it on...

Страница 34: ...Quanta rev C 23 Apr 2010 Requirements Unpacking 2 4...

Страница 35: ...phere Note Be sure to verify calibration for the instrument including Xe lamp scan and water Raman signal before using the Integrating Sphere accessory 3 Installation Use Method 1 Remove the cover of...

Страница 36: ...ers tood follow this procedure a Place the appropriate blank solvent in a firmly stoppered quartz cuvette with 12 mm 12 mm outer dimensions the same dimensions as a stan dard 4 mL 1 1 cm path length c...

Страница 37: ...th the pins on the sam ple holder Be sure the label IN is in the direc tion of the N2 purge ports and the scribed line on the lid matches the scribed line on the sphere d Rotate the liquid sample hold...

Страница 38: ...es or shapes con tact HORIBA Scientific f Tighten the set screw with the Allen key g Remove the protective cap from the emission port outward arrow Con nect the emission fiber optic bundle to the emis...

Страница 39: ...t drawer add the solid sample into the sample cup c Drop the coverslip on top of the sample d To avoid possible contamination be certain all traces of the sample material are removed from the outside...

Страница 40: ...ch the threaded thumbscrew on the lid to the threaded hole on the sphere g Place the solid sample cover on the integrating sphere h Tighten the thumbscrew to fix the lid in place i Raise the excitatio...

Страница 41: ...port Connect a fiber optic bundle to the integrating sphere emission port k Tighten the set screw with an Allen key l Remove the protective cap from the emission port Connect a fiber optic bundle to...

Страница 42: ...tion and emission bundles 5 Set up the F 3000 Fiber Optic Adapter drawer a Remove the standard sample drawer from the instrument s sample compartment b Insert the excitation and emission fiber optic b...

Страница 43: ...ta rev C 23 Apr 2010 Installation Use 3 9 e Tighten the screws to fix the drawer so lidly to the sample compartment The sample compartment drawer should look like this when installed 6 Start FluorEsse...

Страница 44: ...s We are trying to maximize but not saturate the excitation Rayleigh peak to ob tain an optimal luminescence signal to noise ratio a Place the solvent blank cuvette or blank solid material into the I...

Страница 45: ...h excitation light and the likely or expected range of sample luminescence In this case because the CCD correction factor was collected using the center wavelength of 700 nm we measure the range of 29...

Страница 46: ...s i Add the corrected signal with c subscript to the Formulas table j Give this file a Data Identifier k Choose 1 Accumulations If this is too noisy you will increase the accumulations later l Click...

Страница 47: ...ting it a Double click in the graph to open it b The same graph appears in a new window c Zoom with the Scale In button and select the luminescence to see its strength d Rescale and examine the Raylei...

Страница 48: ...periment In our case we will increase the Integration Time and Accumulations so that we have enough signal 106 counts s for analysis a In the FluorEssence toolbar click the Previous Experiment button...

Страница 49: ...to 0 1 s d Click the Run button The Intermediate Display appears e A Warning window may appear that the wavelength range includes val ues outside of the correction factor file s range Click the OK but...

Страница 50: ...here 10 Run the scan on the sample a Insert the sample cuvette into the liquid sample holder and replace the liquid sample holder into the integrating sphere Or place the sample in the solid sample ho...

Страница 51: ...sample and blank scans side by side helps c Change the Data Identifier field to acknowledge that the sample is now in the sphere d Click the Run button to rerun the scan with exactly the same parame t...

Страница 52: ...and blank s data Thus only two curves are used for analysis In the 4 curve method the Rayleigh lines and luminescence bands are in separate datasets for the sample and blank therefore there are four...

Страница 53: ...ection file name appears in the Sphere Cor rection field To run a 2 curve analysis see the method below d Browse with the Browse button for the combined sample data file The Graph Browser window opens...

Страница 54: ...g Enter the Start Excitation End Excitation Start Emission and End Emission values to find the correct Rayleigh line range yellow area in the preview and luminescence range blue area in the preview h...

Страница 55: ...e analysis except choose the four different datasets sample Ray leigh blank Rayleigh sample emission and blank emission and enter them into the HJY_PLQY window s fields as shown below In all cases con...

Страница 56: ...Quanta rev C 23 Apr 2010 Installation Use 3 22 b Choose Save As The Theme Save as window ap pears c Enter a Theme Name and click the OK button...

Страница 57: ...4 curve method for the sample and blank luminescence we in creased the integration time from 0 1 s to 1 s a factor of 10 to account for weak emission in comparison to the strong Rayleigh scattering A...

Страница 58: ...ues in the Start Wavelength and End Wavelength cells The software automatically recalcu lates values and replots You can view the integrated areas La and Lc Tabs show Data Sphere correction Control wh...

Страница 59: ...or a 2 curve analysis 1 Place the blank into the integrating sphere and properly close the sphere 2 Start FluorEssence run an emission scan 3 In the Experiment Setup window set the parame ters as show...

Страница 60: ...igh and luminescence regions e Click the Detectors icon to set the detector parameters f Enable the PMT detector checkbox here it is T1 g Set units to cps h Enable Correction and Dark Offset checkboxe...

Страница 61: ...us Experiment button b Click the Detectors icon to see the detectors page c Set the units to Counts d Set the Integration Time to yield 106 counts in the Rayleigh peak 7 Click the Run button to start...

Страница 62: ...click the Previous Experiment button to rerun the scan with the same pa rameters 10 In the Experiment Setup window change the Da ta Identifier field to indicate a sample scan 11 Click the Run button t...

Страница 63: ...4 curve analysis Follow the 2 curve analysis method but you may only adjust neutral density attenua tion and integration time to bring peak signals into the correct range You may scan on ly the lumin...

Страница 64: ...Integrating Sphere v 1 2 3 Jul 2008 Index 3 30...

Страница 65: ...g dry nitrogen or other pressurized gases 4 Maintenance Handling Wear clean gloves when handling the Integrating Sphere halves or the optional calibrated reflector in order to prevent the skin s natur...

Страница 66: ...Quanta rev C 23 Apr 2010 Maintenance 4 2...

Страница 67: ...are made for each of these po tential problems by generating and using radiometric correction factors for the Quanta For Quanta integrating spheres accompanying new instruments HORIBA Scientif ic s po...

Страница 68: ...s in the peak channel Step 8 Remove reflector from sample compartment and connect integrating sphere Step 9 Place cuvette reflector in integrating sphere at 45 between excitation and emission or powde...

Страница 69: ...rating correction factor files for the cuvette holder 1 Scan the reflectance spec trum in the sample com partment a On the standard sample compartment drawer attach the single cell sample holder b Pla...

Страница 70: ...artment e Place the sample compartment cover onto the sample compartment f In FluorEssence choose an emission experiment and click the Monos icon g Set the excitation monochromator to 0 nm zero order...

Страница 71: ...s Use counts per seconds cps units to adjust the peak intensity to be below the saturating limit 106 cps j Click the Run button to start the scan The Intermediate Display appears then the data k Evalu...

Страница 72: ...te sample holder Be sure the square top and bottom of the reflector are seated properly into the square depressions in the sample holder 2 Scan the reflectance spectrum in the integrating sphere a Ins...

Страница 73: ...Evaluate the peak intensity Increase the integration time or slightly change excitation bandpass to get at least 105 counts in the peak d Click the Run button The Inter mediate Display ap pears When t...

Страница 74: ...der 3 Calculate the sphere correction factor from the ratio of the reflec tance in the sphere to the sample compartment alone a In the toolbar choose Analysis A drop down menu appears b Choose HJY Too...

Страница 75: ...roubleshooting 5 9 e In the Sample field browse for the sample data the last data collected using the Browse button f Click the OK button when found g Similarly find the sphere data using the Browse b...

Страница 76: ...Quanta rev C 23 Apr 2010 Troubleshooting 5 10 h Browse for the MCorrect file name using the Browse button The completed HJY_Sphere_Correction window looks something like this...

Страница 77: ...11 i Click the OK button when ready The ASCIIEXP window opens j Enter a name for the final ratio file in the File name field and click the Save button The Import and Export window appears k Click the...

Страница 78: ...ance spectrum in the sample compartment a Insert the powder reflector disk into the 1933 Solid Sample Holder b Place the Sample Holder on the sample drawer Keep a 45 angle between exci tation and emis...

Страница 79: ...Essence choose an emission experiment and click the Monos icon g Set the excitation monochromator to 0 nm zero order for white light transmission the emission scanning range to match the corrected reg...

Страница 80: ...nsity to be below the saturating limit 106 cps j Click the Run button to start the scan The Intermediate Display appears then the data k Evaluate the peak intensity in cps units change the units to co...

Страница 81: ...ubleshooting 5 15 b Pull solid sample support itself out c Insert the uncalibrated powder reflector into the support d Slide sample holder back in e Push sample drawer in so that the sample is raised...

Страница 82: ...ch the threaded thumbscrew on the lid to the threaded hole on the sphere f Place the solid sample cover on the integrating sphere g Tighten the thumbscrew to fix the lid in place h Raise the excitatio...

Страница 83: ...le to the integrating sphere emission outward arrow port j Tighten the set screw with an Allen key 3 Calculate the sphere correction factor from the ratio of the reflectance in the sphere to the sam p...

Страница 84: ......

Страница 85: ...rs and ob structions Wavelength settings are improperly calibrated or selected Correct calibration of excitation and emission monochromators and se lect appropriate grating Wrong detector or mirror se...

Страница 86: ...elect correct blank and sample graphs Use of inappropriate theme in PLQY tool Select appropriate theme for PLQY experimental conditions Sample and blank cuvette or powder holders are not optically mat...

Страница 87: ...et for com plete resolution of the spectral fea tures of the excitation bands and fluorescence signal areas Usually from 1 to 5 nm is sufficient Insufficient neutral density attenua tion Use neutral a...

Страница 88: ...properly confi gured and turned on as needed 3 Following the instructions in System Operation run a xenon lamp scan to make sure the system is properly calibrated Print the spectrum for each and note...

Страница 89: ...ton which saves the information to a file Zip Info button which com presses the information while sav ing it Print Info button which prints out the software information 11 Click the OK button to close...

Страница 90: ...660 160 or fax at 732 549 5125 Outside the United States call the local distributor You may also reach us at our web page http www HORIBA com scientific When you contact the Service Department have th...

Страница 91: ...iameter 25 4 mm 1 00 Side fiber hole diameter 5 08 mm 0 200 Port fraction in cuvette mode 1 043 Port fraction in solid sample mode 2 103 Optics head field of view diameter 25 4 mm 1 00 Integrating sph...

Страница 92: ...Quanta rev C 23 Apr 2010 Technical Specifications 7 2 Transmission curve of fiber optic bundles Software FluorEssence version 3 5 or higher with valid USB key Excel 2000 or later software...

Страница 93: ...c subscript 3 12 5 5 5 14 calibrated reflector 4 1 5 1 5 8 Cancel button 5 7 caution notice 0 4 CCD detector 1 4 3 10 11 3 25 5 1 6 3 CD ROM 2 2 5 1 Center Wavelength 3 11 chromaticity 1 11 3 24 Chro...

Страница 94: ...1 9 fluorescence decay 1 3 fluorescence lifetime 1 2 1 3 Fluorescence Main Experiment Menu 3 10 FluorEssence 2 1 3 9 10 3 14 3 18 3 25 5 4 5 6 5 13 6 4 5 7 2 Fluorolog 3 0 1 2 2 Fluorolog Tau 3 0 1 Fl...

Страница 95: ...r film holder 5 12 Previous Experiment button 3 14 3 16 3 27 28 Print Info button 6 5 Project Name window 3 13 3 26 27 5 7 protective gloves 0 4 purge ports 3 3 6 1 7 1 Q quantum yield 0 1 1 3 4 1 6 1...

Страница 96: ...citation 3 20 Start Wavelength cell 3 24 Summed Scans 3 15 support technical 6 4 Synapse OE 5 1 system configuration 6 5 T T1 3 26 technical support 6 4 Theme Name 3 22 Theme Save as window 3 22 theor...

Страница 97: ...up application images are collaged in the overall design Beginning from a nano size element the scale of the story develops all the way to the Earth with a gentle flow of the water 3880 Park Avenue Ed...

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