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OXY-10 - Loligo Systems

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1. 50 PME TUDIN 51 12 1 Basics in Optical Sensing of Oxygen eeeeeseeeeeeeseseeeeeeeene nennen nennen nnn nnnnn nnne nenne nnn 51 12 1 1 Dynamic Quenching of LUMINESCENCE sessssssssssssssssseeeeeeeee eene nennen 51 12 1 2 Major Components of Fiber Optic Minisensors eeenenennenennenenn 52 12 1 3 Advantages of Optical Oxygen Sensitive Minisensors eesseeeneeeenens 53 12 1 4 Luminescence Decay Tilme 2 cei ee ie len pan rad RAS n ERR EC MERI ES EAR kd ma paideia 53 12 1 5 Literature ic tne e VERE etude S 54 12 2 Determination of the Oxygen Concentration Using a Modified Stern Volmer Equation 55 12 3 Oxygen Conversion Formulas eeeeeeeeeieeeeesiseeeeee eene n enn nmn nnn nn nnn annnm nnns mannen annen nanenane 56 12 4 Temperature Dependent Constants Affecting the Oxygen Content ess 58 12 4 1 Water Vapor Pressure ete en exerted cete Ct e Ere Ut d roe esee xoi eee is 58 12 4 2 Bunsen Absorption Coefficient sess nnne 59 12 4 3 Dependence on the Salt Concentration sssssssssseeeeeenee nennen 62 12 5 Temperature Compensation of the Response of Oxygen Sensors eee 63 1 Preface Congratulations You have chosen a new innovative techn
2. sseeeeennnne 23 6 3 5 Graphical and numerical display of the respective channel ssseeeeeee 25 6 4 Data Handling E kit 26 7 Calibration kite P 28 7 1 Calibration of Oxygen Dipping Probe DP PSt3 eeeeseeeeeeeeeeeeeeeneeenn ennt nennt nnn 29 7 1 1 Calibration with two Calibration Standards sese 29 7 1 2 User defined calibrations inire RI Ete tee deed dat eee 32 7 2 Calibration of Flow Through Cell FTC PSt3 eeeeeeeeeeeeeeeee esee enne nennen nnne nnn nnn 33 7 2 1 Calibration with two calibration Standards sssseseeeeeneeeenenen enne 33 7 2 2 User defined calibrations 5 iere E patet e e dm eie ada Un bi al 37 7 3 Calibration of Planar Oxygen Sensitive Foils PSt3 Integrated in Glass Vials 38 7 3 1 Calibration with two calibration Standards ssssseseseeeeneneneneneneen een 38 7 3 2 User defined calibration iecore reU eU ect T ee eec ih 42 8 Measurement with Oxygen Sensor PSIt3 esses eeeeeee enne nnnnnnnnnnnnn nnt n ns nnn nsn n ns tnn nnne 43 8 1 Starting the measuremernit 5 cric ok abi ont aneka kone eer ane kanon Ca ko De dans kone eie anka ninatoa sesinin aaan 43 8 1 1 Scanning call Channels 2 1t ee ote E EH EPIRI Rt 43 8 1 2 Scanning selected Channel s c cccesceeseeceneeeeceseaeeee
3. 2 Inthe appearing save as window specify filename without extension and its location The PC software automatically creates one to ten different files The filename consists of the specified filename and the extensions ch1 txt ch2 txt to ch10 txt respectively All filenames are displayed in the section Created files ALL CHANNELS CREATED FILES MAIN PATH SINGEL CHANNEL Description ch 1 Description ch 2 Description ch 3 Description ch 4 Description ch 5 Description ch 6 Description ch 7 Description ch 8 Description ch 9 Deseription ch 10 Measurement with Oxygen Sensor PSt3 45 8 2 Some Advice for Correct Measurement 8 2 1 Signal drifts due to oxygen gradients Please keep in mind that the sensor only measures the oxygen content near its surface In unstirred solutions an oxygen concentration gradient often occurs Please check if air bubbles are on the sensor tip whenever unexpected drifts gradients or unstable measurement values occur Critical conditions for bubble formations are for example purging with air or other gases and increasing temperature during measurement The formation of a bio film during long term measurements or the accumulation of other sample components like oil or solid substances may lead to an oxygen gradient 8 2 2 Signal drifts due to temperature gradients A further source of imprecise measurement is insufficient temperature compensation Please bear in mind that the OXY 10
4. LOLIGOSYSTEMS COM Instruction Manual OXY 10 10 Channel Fiber Optic Oxygen Meter Loligo Systems ApS Niels Pedersens All 2 DK 8830 Tjele Denmark Phone 45 89 99 25 45 Fax 45 89 99 25 99 e www lolieosvstems com mail lolisosvstems com e VAT no 2746 7849 e Bank 5984 0004001376 LOLIGOSYSTEMS COM Instruction Manual OXY 10 Software Version OXY10v3 33FB April 2005 Loligo Systems ApS Niels Pedersens All 2 DK 8830 Tjele Denmark Phone 45 89 99 25 45 Fax 45 89 99 25 99 e www lolieosvstems com mail lolisosvstems com e VAT no 2746 7849 e Bank 5984 0004001376 Table of contents Table of Contents 1 MALI 1 2 Safety Guidelines 3s memes 2 3 Description of the OXY 10 DeViCe ccssseseessseesseeeeseeesseeeseeesseeeesaeesseeeeseeeaseeseseeensnaeaseeeaenesaseeeaeneeaseeeaes 3 3 1 DENIM R 3 3 2 Front Panel of the OXY 10 Device eseessesseeeeeee eene enne tnnt tnn nnne nnns annt anna tna tn sana tna aa 3 3 3 Rear Panel of the OXY 10 Device aksan eka ciere critt erect feat pipe pen toc tee unc annee k gan annus 4 4 Required Basic Equipment leeeeeeeeee esses eeeeee eese enn enne nnnn nennt nnne nnna nas ntn nass sam r asse nnns aset tnn s asas nass enn 5 5 Planar Oxygen MihiSensolrs de tice etr recepere ete eee ere ide ree cere kn esed gon kab enn kasek ao 6 5 1 Sensor Characteri
5. 58 9 58 4 0 05 2 4 10 2 20 4 30 4 40 3 temperature C Figure 12 13 Effect of the temperature on Po and the Stern Volmer constant Ksyv Consequently variations in the temperature cause variations in the measuring value at a constant oxygen content see Figure 12 11 Table 12 7 displays the deviation of the measuring value from the real oxygen content depending on temperature and the oxygen content Table 12 7 Deviations in the measured oxygen content A 96 air saturation at a constant oxygen content and variations in temperature by 1K 96 air saturation 25 Yo air sat 100 96 air sat 250 air sat 50 9 hPa 203 6 hPa 508 9 hPa A air saturation K 0 43 0 88 hPa t 1 62 3 30 hPa t 3 91 7 96 hPa Example If the temperature is measured with a precision of 0 2 C there is a variation in the measuring value at 100 Yo air saturation of 100 0 7 air saturation
6. e g if the instrument e is visibly damaged e no longer operates as specified e has been stored under adverse conditions for a lengthy period of time e has been damaged in transport If you are in doubt the instrument should be sent back to the manufacturer for repair and maintenance The operator of this measuring instrument must ensure that the following laws and guidelines are observed when using dangerous substances e EEC directives for protective labor legislation e National protective labor legislation e Safety regulations for accident prevention e Safety data sheets of the chemical manufacturer The OXY 10 is not protected against water spray The OXY 10 is not water proof The OXY 10 must not be used under environmental conditions which cause water condensation in the housing The OXY 10 must not be opened We explicitly draw your attention to the fact that any damage of the manufactural seal will render all guarantee warranties invalid Any internal operations on the unit must be carried out by personnel explicitly authorized by Loligo and under antistatic conditions The OXY 10 may only be operated by qualified personnel This measuring instrument was developed for use in the laboratory Thus we must assume that as a result of their professional training and experience the operators will know the necessary safety precautions to take when handling chemicals Keep the OXY 10 power supply and optical sensors out of the r
7. ethanol ethylene oxide H202 Oxygen sensor immobilized onto a polyester support Optical receive signals to analyzer e stands CIP Cleaning In Place conditions e sterilizable ethanol ethylene oxide H202 e not autoclavable e flexible Planar Oxygen Minisensor A polymer optical fiber is used as a light guide between the OXY 10 oxygen meter and a sensor foil SP PSt3 which was glued inside a glass vial to read out the analyte concentration non invasively and non destructively from outside through the transparent wall of the flask Ordering information Oxygen Sensor Spot Optical Isolation Spot Diameter in mm Y with optical isolation 5 N without optical isolation i a Oxygen Sensitive Coating Support PSt3 0 250 Yo air saturation PE polyester support G al rt standard e re Example akite DE Aa With this code you will order a planar oxygen sensor spots type PS 3 0 250 air saturation with optical isolation YOP immobilized onto a glass support G SUP The spot diameter is 5 mm Planar Oxygen Minisensor 13 5 2 2 Flow Through Cell with Integrated Planar Oxygen Sensor FTC PSt3 The flow through oxygen minisensor FTC PSt3 is a miniaturized fiber optic chemical sensor integrated in a T shape flow through cell The flow through cell is connected to the oxygen meter OXY 10 by a polymer optical fiber with 2 mm diameter as a light guide A glass tube with 2 mm inner diameter 4 mm
8. only measures correctly if the sample temperature is constant during measurement and the temperature is the same as you typed in at the beginning of the measurement Please also refer to Chapter 12 5 Temperature Compensation of the Response of Oxygen Sensors 8 2 3 Signal drift due to photodecomposition The oxygen sensitive material may be subject to photodecomposition resulting in a signal drift Photodecomposition takes place only during illumination of the sensor tip and depends on the intensity of the excitation light Therefore the excitation light was minimized Continuous illumination of a DP PSt3 oxygen sensor over a period of 24 hours may lead to a phase drift of up to 0 4 96 air saturation measured at 100 air saturation at 20 C However this effect of photodecomposition can even be minimized by changing the measuring mode to the second or minute interval mode In these modes the software switches off the excitation light after recording the data point and switches it on after the interval you have chosen Please use the interval method whenever it is possible to increase the shelf life of the sensor Drift in air saturation at 10096 air saturation when illuminating the oxygen sensor PSt3 for 1 12 and 24 hours in the continuous mode Drift per hour Drift per 12 hours Drift per 24 hours PSt3 lt 0 4 air saturation Measurement with Oxygen Sensor PSt3 46 0 Yo air saturation phas
9. 2 1 The second possibility is described in chapter 7 2 2 7 2 1 Calibration with two calibration standards For the calibration with current values you need calibration standards and your mounted sensor 7 2 1 1 Preparation of the Calibration Standards Calibration of oxygen minisensors is performed using a conventional two point calibration in oxygen free water cal 0 and water vapor saturated air or air saturated water cal 100 In the sub window Calibration cal 100 is denoted as 2 cal point Preparation of calibration standard cal 0 oxygen free water 1 Add 1 g sodium sulfite Na2SO3 to the vessel and label it cal 0 2 Dissolve Na SOs in 100 mL water The water becomes oxygen free due to a chemical reaction of oxygen with Na2SOs Additional oxygen diffusing from air into the water is removed by surplus of Na2SOg 3 Close the vessel with a screw top and shake it for approximately one minute to dissolve Na2SO3 and to ensure that the water is oxygen free Close the vessel after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S2O4 The shelf life of cal 0 is about 24 hours provided that the vessel has been closed with the screw top Preparation of calibration standard cal 100 air saturated water 1 Add 100 mL water to a suitable vessel and label it cal 100 2 To obtain air saturated water blow air into the water using an air pump with a glass
10. 4 description of the measurement if a content is added to the File description section max 3 lines Line 5 9 Identification information of the hardware only useful for service Line 11 18 Set parameters of the hardware only useful for service Line 20 25 System settings only useful for service Line 27 32 Information about the calibration which was used for the measurement useful if a mistake during calibration is supposed Line 34 36 Information about the firmware only useful for service Line 38 Pressure at which calibration was performed Line 39 xx The following rows separated by semicolons list the measuring data The first two rows contain the date and time the third the log time in minutes the fourth the oxygen content in the chosen unit The raw data phase angle in and the amplitude in mV are stored in the fifth and sixth row respectively The seventh row contains the temperature in C as given by the user Raw data can be used for user defined recalculations according to the formulas and tables listed in the appendix The data can be processed with any text editor The use of Microsoft Excel is possible by importing the file Software 27 MWN 58 C B E FE J 9 4 05 04 05 1 0 569 SW ver OXY10v3 28 Header Ch 6 PHiboard number vi210259 PMnumber 00000000 8 Serial number 00000000000000000000 9 MUXchannel ON 01 11 PARAMETERS 12 Signa
11. C The calculated value for cs at a temperature of 20 0 C agrees with the tabulated value of 9 08 mg L Figure 12 9 shows the temperature dependent oxygen solubility in air saturated fresh water 15 14 13 12 11 10 Cg Oz mg L pw pw T pw 0 2095 o 0 10 Moz Vm c O5 mg L nN OW CO oO 0 5 10 15 20 25 6 C Figure 12 9 Dependence of the oxygen solubility in air saturated fresh water on temperature Table 12 3 Oxygen solubility in air saturated fresh water mg L Appendix 61 T 0 14 64 60 55 51 47 43 39 35 31 27 23 1 23 19 15 10 06 03 99 95 91 87 83 2 13 83 79 75 71 68 64 60 56 52 49 45 3 45 41 38 34 30 27 23 20 16 12 09 4 09 05 02 98 95 92 88 85 81 78 75 5 12 75 71 68 65 61 58 55 52 48 45 42 6 42 39 36 32 29 26 23 20 17 14 11 7 11 08 05 02 99 96 93 90 87 84 81 8 11 81 78 75 72 69 67 64 61 58 55 53 9 53 50 47 44 42 39 36 33 31 28 25 10 25 23 20 18 15 12 10 07 05 02 99 11 10 99 97 94 92 89 87 84 82 79 77 75 12 75 72 70 67 65 63 60 58 55 53 51 13 51 48 46 44 41 39 37 35 32 30 28 14 28 26 23 21 19 17 15 12 10 08 06 15 06 04 02 99 97 95 93 91 89 87 85 16 ig 85 83 81 70 76 74 72 70 68 66 64 17 64 62 60 58 56 54 53 51 49 47 45 18 45 43 41 39 37 35 33 31 30 28 26 19 26 24 22 20 19 17 15 13 11 09 08 EHI Er 06 04 02 01 99 97 95 94 92 90 21 8 90 88 87 85 83 82 80 78 76 75 73 22 73 71 70 68 66 65 63 62 60 58 57 23 57 55 53 52 50 49 47 46 44 42 41 24 41 39 38 36 35 33 32 30 28 27 25 25 25 24
12. Sensors and Actuators B 38 39 122 129 1997 e Klimant l Meyer V K hl M Fiber optic oxygen microsensors a new tool in aquatic biology Limnol Oceanogr 40 1159 1165 1995 e Klimant l Ruckruh F Liebsch G Stangelmayer A Wolfbeis O S Fast Response Oxygen Microsensors Based on Novel Soluble Ormosil Glasses Mikrochim Acta 131 35 46 1999 Appendix 55 12 2 Determination of the Oxygen Concentration Using a Modified Stern Volmer Equation The Stern Volmer equation 4 displays a linear correlation between tan o tan or t t and the oxygen concentration Oz tano To 1 Kg O 4 tanp sv 02 4 Po phase angle of oxygen free water o measured phase angle Ksv Stern Volmer constant O2 oxygen content in 96 air saturation The Stern Volmer plots of all our sensors show a distinct non linearity in their response behavior which is also observed for many other oxygen sensors described in literature This non linear response behavior can be described with a modified Stern Volmer equation 5 1 tan f 1 f ao 1__ 5 tan l K 0 1 Ky O This model is based on the assumption that the indicator is distributed in the polymer matrix at two different sites and each fraction fi 1 f1 shows a different quenching constant Ksv Ksvz For practical use this model is not very convenient since it has too many parameters which have to be calibrated Therefore two simplified
13. The software determines the minimum and maximum values to display all data 2 Autoscale Off The maximum and minimum value of the y axis can be defined by the user By clicking on the current value the minimum and or maximum value can be changed After typing the new value one has to click in the graphical window again to realize the change For the x axis only the starting value can be changed Zoom Function 1 Press the left mouse button and drag from left to right to enlarge a certain area of the graphical window The graphical window displays the selected data points and is not actualized with new data 2 Press the left mouse button and drag from right to left to recover the original display or click the Unzoom button The oxygen content is displayed in the chosen unit the temperature in C The raw values the phase angle in degrees and the sensor amplitude in mV are also displayed see Appendix for description of phase and amplitude Software 24 k UXY 10v3 33 Measurement Calibration Logging All channels Graphical window here to change values After that click somewhere inside the graphical window to make changes active Scale button Unzoom button GUI 2927 oj 200 6 3 5 Graphical and numerical display of the respective channel The measuring values and all raw values are displayed for each channel separately By clicking on the respective chann
14. diameter can be punched The sensor spots can be glued for example inside glass vials such as cell culture flasks bags and disposables The oxygen concentration can be measured non invasively and non destructively from outside through the wall Only prerequisite The wall has to be transparent and non fluorescent Please note Be sure to glue the sensor spots onto your vessel with the proper side The sensor support polyester foil or glass on which the sensor is spotted identifiable by its faint reflection is glued to the vessel while the sensor itself must look toward the sample The figure below shows how the highly enlarged sensor spot must be glued to the vessel Sample Optical isolation Sensor Sensor Support Vessel bottom Sensor spot SP glued into a vessel no optical isolation Optical isolated sensor spot SP glued into a vessel Canney Features foll inside e non invasive and non destructive measurement from outside A container through the wall of the flask excellent mechanical stability and long term stability more than 100000 data points without drift e online monitoring Cantainer wall Optical transmit signals to analyzer e response time teo in the order of 30 s e measuring range 0 250 a s e limit of detection 0 15 96 a s Oxygen sensor immobilized onto a glass support e stands CIP Cleaning In Place conditions e sterilizable autoclave 130 C 1 5 atm
15. frit airstone creating a multitude of small air bubbles while stirring the solution 3 After 20 minutes switch of the air pump and stir the solution for further 10 minutes to ensure that the water is not supersaturated 7 2 1 2 Mounting the Oxygen Sensitive Minisensors 1 Remove the flow through cell oxygen sensor carefully from the protective cover The oxygen sensitive material is immobilized to a glass tube which is located in a T connector with two female Luer Lock adapters The glass tube is tightened with a viton seal and two male Luer Lock connectors fix the glass tube in the T connector On request the seal can also be out of silicone Don t remove the two male Luer Lock adapters from the T connector You may loose the viton seal and the glass tube may be dislocated male Luer Lock connector containing a 2 mm POF located at the glass tube male Luer Lock connector male Luer Lock connector viton seal glass tube with viton seal integrated oxygen sensor 2 Fix the male Luer Lock adapter with the integrated 2 mm POF polymer optical fiber to the Luer T connector and ensure that the fiber is located close to the glass tube Calibration 34 Fix the flow through cell with a clip to a laboratory support or a similar stable construction Connect the two male Luer Lock connectors with the tubings of your flow through system Remove the protective cap from the male fiber plug and connect it to the SMA plug of the OXY 10
16. other channels by typing in the respective channel into the Channel Window to record the oxygen free calibration value cal 096 Rinse the sensor membranes gently with water after calibration to remove sulfite remaining on the surface Calibration 42 7 3 2 User defined calibration If temperature and phase angle of a former calibration of the same sensor are known the Calibration with constant values is possible 1 Switch on the OXY 10 and the PC software following chapter 6 2 Go to the window Calibration Select the channel to be calibrated in the section Channel of sub window Single channel or switch to the sub window All channels 3 Enter the respective calibration values a phase at 0 Yo air saturation temperature at 0 air saturation phase at 100 air saturation temperature at 100 air saturation pressure at which values a d were measured The atmospheric pressure of the calibration is needed to convert the oxygen unit air saturation into partial pressure units hPa Torr or concentrations units mg L pmol L oDAnv 2nd cal point E sat pressure 1013 Wie CHANNEL a EN temperature of cal0 standard C temperature of call00 standard S 05r E100 OO Sere gl 58 81 MR 26 59 l 4 To store the calibration values click the Calibrate button A dialog appears and informs you that you will program all channels in case the sub window All channels is chosen If sub window Single channel is chosen a dial
17. our works after careful testing of all functions and safety requirements The perfect functioning and operational safety of the instrument can only be ensured if the user observes the usual safety precautions as well as the specific safety guidelines stated in these operating guidelines Before connecting the device to the electrical supply network please ensure that the operating voltage stated on the power supply corresponds to the mains voltage The perfect functioning and operational safety of the instrument can only be maintained under the climatic conditions specified in Chapter 10 Technical Data in this operating manual If the instrument is moved from cold to warm surroundings condensate may form and interfere with the functioning of the instrument In this event wait until the temperature of the instrument reaches room temperature before putting the instrument back into operation Balancing maintenance and repair work should exclusively be carried out by a suitable qualified technician trained by us Especially in the case of any damage to current carrying parts such as the power supply cable or the power supply itself the device must be taken out of operation and protected against being put back into operation If there is any reason to assume that the instrument can no longer be employed without a risk it must be set aside and appropriately marked to prevent further use The safety of the user may be endangered
18. outer diameter is coated with oxygen sensitive dye at its inner wall The volume for liquid inside the FTC cell is about 100 10 ul The standard T shape flow cell can be easily connected via Luer Lock adapters to external tubings Liquids like water blood etc can be pumped through the cell Schematic drawing of flow through cell oxygen sensors Luer Lock adapter female POF polymer optical fiber L 2 5 m Luer Lock adapter female planar oxygen sensor SMA connector Features e very robust sensor with an excellent long term stability more than 100000 data points without drift online monitoring e sterilizable autoclave 130 C 1 5 atm ethanol ethylene oxide response time too in the order of 1 minute e measuring range 0 250 a s e limit of detection 0 15 Yo a s e stands CIP conditions cleaning in place 5 Yo NaOH 90 C Ordering Information E Flow Through Cell with integrated planar sensor Oxygen Sensitive Coating PSt3 0 250 Yo air saturation Order code for the Flow Through Cell FTC PSt3 Planar Oxygen Minisensor 5 2 3 Oxygen Dipping Probe DP PSt3 Schematic drawing POF polymer optical fiber L 2 5 m sensor spot es queam steel tube Features usable for process application This oxygen sensor consists of a polymer optical fiber with a polished distal tip which is coated with a planar oxygen sensitive foil The end of the polymer optical fi
19. partial pressure in air saturated water and water vapor saturated air P O Y Pan Pw T 0 2095 19 Temperature variations strongly affect water vapor pressure and thus influence the oxygen partial pressure as shown in equation 19 Table 12 1 Variation of water vapor pressure pw T with temperature LN s T D A convenient fitting function is given by the Campbell equation 20 pw sen A po Can 20 where T is the temperature in Kelvin and A B and C constants given in Figure 12 7 120 p T exp 52 57 6690 9 T 4 681 InT R 1 100 7 t SU A 52 57 en 1 B 6690 9 2 60 C 4 681 E A 40 20 0 T j T t T T j T T T t T H T T T 272 277 282 287 292 297 302 307 312 317 322 T K Figure 12 7 Variation of water vapor pressure with temperature F is the square of the correlation coefficient Appendix 59 12 4 2 Bunsen Absorption Coefficient The solubility of oxygen in water is temperature dependent and can be described using the Bunsen absorption coefficient a 8 and the oxygen partial pressure p O2 according to equation 21 With increasing temperature the solubility of oxygen in water decreases p O py D N c p 21 Cs p 9 temperature dependent solubility of oxygen in water given in cm Oz cm p O2 oxygen partial pressure PN standard pressure 1013 mbar a 8 X Bunsen absorption coefficient given in cm Oz cm Table 12 2
20. the file setup exe in folder installer and install the program to the desired folder 2 Thereafter Labview8 runtime engine is installed Please click Next in the following three windows without changing the chosen options 3 Finally click Finish in the next window EEEEENEEEENNS fanus EEEENEEENS 25 pen Chan dio Ma aoo bdt ti ae efi Digest Macer ere AU zyem ase ZAN Facit Poste ws cdi ndun ket ann trong re taa en eot on They htt mci rwn com eme on eet They tt ml omm c ow Dn Ret eT Processes oa me oa rem anes eta ice EARS ISO EIE RUBUS LA ssa adi MM tni Bt d LM AN Tae Tor pat ian 3 C iFragumr a nce remrernt Cifragumne Puticos remanent ue Com gan jen gt tm cum Danu pen cis tme e Figure 6 1 Screenshots of the windows appearing during the installation process of Labview8 Run time Engine Figure 6 2 Screenshot of the last window of the installation of Labview Run Time Engine Now the Software is properly installed and you will find a link in your Start menu Software 20 6 2 Starting OXY 10 and its Software 1 Connect the OXY 10 via the supplied serial cable to a serial port of your computer Tighten the cable with the screws on your computer and on the OXY 10 2 Connect the power supply 3 Please close all other applications as they may interfere with the software Start the program OXY10Qv3 22 in the Start menu The following information win
21. the software Consequently changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentration units mg L pmol L but the oxygen units 96 air saturation and 96 oxygen saturation have to be corrected for air pressure changes General Instructions 47 9 General Instructions 9 1 Warm Up Time The warm up time of the electronic and opto electronic components of the OXY 10 is 5 min Afterwards stable measuring values are obtained 9 2 Maintenance The instrument is maintenance free The housing should be cleaned only with a moist cloth Avoid any moisture entering the housing Never use benzine acetone alcohol or other organic solvents The SMA fiber connector of the minisensor can be cleaned only with lint free cloth The sensor tip may be rinsed only with distilled water 9 3 Service Balancing maintenance and repair work may only be carried out by the manufacturer Loligo Systems ApS Niels Pedersens All 2 DK 8830 Tjele Denmark Phone 44589992545 E mail mail loligosystems com Internet www loligosystems com Please contact our service team should you have any questions We look forward to helping you and are open for any questions and criticism Technical Data 48 10 Technical Data 10 1 General Data PSt3 oxygen sensor range 0 250 air saturation resolution 1 0 05 air saturation 30 0 1 Yo air saturation 100 0 5 96 air saturation 250 1 7 Yo a
22. 0 2 To obtain air saturated water blow air into the water using an air pump with a glass frit airstone creating a multitude of small air bubbles while stirring the solution 3 After 20 minutes switch off the air pump and stir the solution for further 10 minutes to ensure that water is not supersaturated 7 1 1 2 Mounting the Oxygen Sensitive Minisensors 1 Remove the oxygen sensor carefully from the protective cover Carefully remove the protective plastic cap covering the oxygen sensitive sensor spot Fix the oxygen sensor with a clip to a laboratory support or a similar stable construction Beo oq Remove the protective cap from the male fiber plug and connect it to one of the SMA plugs of the OXY 10 device The safety nut must be carefully attached while turning slightly clockwise 7 1 1 3 Performing the calibration Switch on the OXY 10 and the PC software following chapter 6 2 Goto window Calibration and enter the actual atmospheric pressure in hPa and the temperature of the calibration standards cal 0 and cal 100 The atmospheric pressure of the calibration is needed to convert the oxygen unit air saturation into partial pressure units hPa Torr or concentration units mg L umol L Please ensure that there are no temperature changes during the calibration of the oxygen sensor Besides it must be ensured that the temperature during later measurement is constant and already known However the temperatures during the m
23. 05 and press the CAL 0 button to store the 0 air sat and temp at 0 values Afterwards press the calibration solution into the waste A message window opens and informs you that you will change the last calibration values Click the OK button to store the new calibration data Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record the oxygen free calibration value cal 0 5 Rinse the sensor membranes gently with water after calibration to remove sulfite remaining on the surface 7 2 2 User defined calibration If temperature and phase angle of a former calibration of the same sensor are known the Calibration with constant values is possible 1 Switch on the OXY 10 and the PC software following chapter 6 2 Go to the window Calibration Select the channel to be calibrated in the section Channel of sub window Single channel or switch to the sub window All channels 3 Enter the respective calibration values a phase at 0 air saturation temperature at 0 96 air saturation phase at 100 air saturation temperature at 100 Yo air saturation pressure at which values a d were measured The atmospheric pressure of the calibration is needed to convert the oxygen unit 96 air saturation into partial pressure units hPa Torr or concentrations units mg L mol L pagg Measurement Calibration Logging All channels 2nd cal E00 00 k sat CHANNEL pressure
24. 22 21 19 18 16 15 14 12 11 26 11 09 08 06 05 03 02 00 99 98 96 27 7 96 95 93 92 90 89 88 86 85 83 82 28 82 81 79 78 77 75 74 73 71 70 69 29 69 67 66 65 63 62 61 59 58 57 55 30 55 54 53 51 50 49 48 46 45 44 42 31 42 41 40 39 37 36 35 34 32 31 30 32 30 29 28 26 25 24 23 21 20 19 18 33 18 17 15 14 13 12 11 09 08 07 06 34 06 05 04 02 01 00 99 98 97 96 94 35 6 94 93 92 91 90 89 88 87 85 84 83 36 83 82 81 80 79 78 77 75 74 73 72 37 72 71 70 69 68 67 66 65 64 63 61 38 61 60 59 58 57 56 55 54 53 52 51 39 51 50 49 48 47 46 45 44 43 42 41 40 41 40 39 38 37 36 35 34 33 32 31 Example cs 20 0 C 9 08 mg L Appendix 62 12 4 3 Dependence on the Salt Concentration Table 12 4 gives values of the concentration of dissolved oxygen at several temperatures in solutions with various chloride concentrations Increasing the salt concentration leads to a decrease in oxygen solubility This behavior is characteristic for the solubility of many nonelectrolytes it is the phenomenon known as the salting out effect Instead of chlorinity CI the amount of chloride in parts per thousand which was used as a measure of the amount of salt in water the term salinity is often used If salinity is preferred as a measure of salt concentration then the conversion from g L can be readily made using equation 26 S 1 805 CI 0 03 26 where S is the salinity in Zo or g 1000g Table 12 4 Solubility of oxygen in water as a function of temperature and sa
25. 6 1013 zi f EH temperature of cal0 standard CS temperature of cal100 standard e OZE 110000 004 AD 68 81 M 26 59 E 4 To store the calibration values click the calibrate button A dialog appears and informs you that you will program all channels in case the sub window All channels is chosen If sub window Single channel is chosen a dialogue appears informing you that you will change the last calibration values Click the Continue button to store the new calibration data Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record user defined calibration values Calibration 38 7 3 Calibration of Planar Oxygen Sensitive Foils PSt3 Integrated in Glass Vials There are two ways to calibrate the optical sensors One is the use of two calibration standards the other one is to type in known constants The first way needs two calibration standards Their preparation is described in chapter 7 3 1 The second possibility is described in chapter 7 3 2 7 3 1 Calibration with two calibration standards For the calibration with current values you need calibration standards and your mounted sensor Calibration of the minisensors is performed using conventional two point calibration in oxygen free water cal 0 and water vapor saturated air or air saturated water cal 100 In the sub window Calibration cal 100 is denoted as 2 cal point 7 3 1 1 Preparation of the Calibration
26. Bunsen absorption coefficient however is not a very practical measure Values of a 8 have therefore to be converted to mg L and the method for doing this is best illustrated by an example Example Calculation of the oxygen content Cs patm 0 in air saturated water at a temperature 0 of 20 C Equation 21 allows the solubility of oxygen in air saturated fresh water to be calculated for any temperature and pressure provided that the values of the Bunsen absorption coefficient a T and the vapor pressure pw T at the particular temperature are known Equation 22 or 23 can be used to obtain a and pw can be calculated from equation 20 The oxygen content cs of air saturated water can be calculated according to M c Pg 60 Pan Pw 9 5095 a 24 Pn M In equation 24 pam is the actual atmospheric pressure corrected for the contribution of the water vapor pressure Pw and related to standard pressure py The corrected pressure is multiplied by 0 2095 the volume content of oxygen in air by a 8 and by the molecular mass of oxygen Moz divided by the molar volume Vy At a given atmospheric pressure of 1013 mbar pam pn and a temperature of 20 C the oxygen content can be calculated according to equation 24 and results in 1013 23 3 32 g mol c 1013mbar 20 C _ 0 2095 0 031 0 009g L 9 06 mg L 25 1013 22 414mol L Table 12 3 gives oxygen solubilities in mg L for temperature intervals of 0 1 C from 0 40
27. P conditions cleaning in place 5 Yo NaOH 90 C as well as a 3 Yo H2O solution The oxygen sensitive material may be subject to photodecomposition resulting in a signal drift Photodecomposition takes place only during illumination of the sensor tip and depends on the intensity of the excitation light Table 5 4 Drift in air saturation at 100 air saturation when illuminating the oxygen sensor PSIS for 1 12 and 24 hours in the continuous mode 1 sec mode Drift per hour Drift per 12 hours Drift per 24 hours PSt3 lt a aes lt 0 4 air saturation Planar Oxygen Minisensor 10 5 2 Housings of Oxygen Sensitive Minisensors The fiber optic oxygen sensors are based on 2 mm polymer optical fibers POF Depending on the respective application we offer a set of different standard designs neg Planar oxygen sensitive sensor foils Flow through cell design connected to 2 mm Dipping Probe DP with coated SP a 2 mm POF FTC sensor foil Of course it is possible to build customer specific designs Please feel free to contact our service team to find the best solution for your application Planar Oxygen Minisensor 11 5 2 1 Planar Oxygen Sensitive Foils SP PSt3 Planar oxygen sensors SP PSt3 immobilized onto different supports polyester glass are available for customer specific applications Sensors based on a polyester support can be easily cut into small pieces using a razor blade Round spots Sensor spots of 3 mm in
28. Remarks 50 11 Concluding Remarks Dear customer With this manual we hope to provide you with an introduction to work with the OXY 10 fiber optic oxygen meter This manual does not claim to be complete We are endeavored to improve and supplement this version We are looking forward to your critical review and to any suggestions you may have You can find the newest version at www loligosystems com With best regards Your Loligo Team Appendix 51 12 Appendix 12 1 Basics in Optical Sensing of Oxygen 12 1 1 Dynamic Quenching of Luminescence The principle of measurement is based on the effect of dynamic luminescence quenching by molecular oxygen The following scheme explains the principle of dynamic luminescence quenching by oxygen ps a LI emission of ed light 1 O 6 i absorption of light excited E ki state energy transfer by collision 1 no emission of light ES AE 4 x 4 oa Figure 12 1 Principle of dynamic quenching of luminescence by molecular oxygen 1 Luminescence process in absence of oxygen 2 Deactivation of the luminescent indicator molecule by molecular oxygen The collision between the luminophore in its excited state and the quencher oxygen results in radiationless deactivation and is called collisional or dynamic quenching After collision energy transfer takes place from the excited indicator molecule to oxygen which consequently is transferred from its ground state triplet state to it
29. S S J 20 0 0 20 40 60 80 100 120 140 160 180 time s Figure 5 3 Response characteristic of an optical isolated oxygen sensor PSt3 in a stirred and a non stirred sample solution and in the gas phase Table 5 3 Response times too of the oxygen sensors membrane PSt3 dissolved oxygen gaseous oxygen stirred not stirred oxygen sensor PSt3 too without optical isolation 20s 40s 6s too with optical isolation 30s 60s 10s Planar Oxygen Minisensor 9 Optical isolation Optical isolated sensor tips are required if your sample shows intrinsic fluorescence between 540 700 nm Consequently an optical isolation is recommended measuring in whole blood urine or chlorophyll containing samples Using optical isolated sensors excludes the impact of colored samples and ambient light on measurements Furthermore the optical isolation layer is applied to exclude strong ambient light to improve chemical resistance especially against oily samples as well as to reduce bio fouling on the sensor membrane Optical isolated sensor tips of oxygen sensors enable measurement in photosynthetically active samples since stimulation of photosynthesis due to emission of blue green light from the fiber tip is avoided We offer additional optical isolation for all types of oxygen sensors Sensor Stability The oxygen sensitive membrane stands gamma sterilization sterilization by ethylene oxide steam autoclavation 140 C 1 5 atm CI
30. Standards Preparation of calibration solution 0 oxygen free water 1 Add 1 g sodium sulfite Na2SO3 to the vessel and label it cal 0 2 Dissolve Na SOsin 100 mL water The water becomes oxygen free due to a chemical reaction of oxygen with Na2SOs Additional oxygen diffusing from air into the water is eliminated removed by surplus of Na2SOs 3 Close the vessel with a screw top and shake it for approximately one minute to dissolve Na2SO3 and to ensure that water the is oxygen free Close the vessel after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S2O4 The shelf life of cal 0 is about 24 hours provided that the vessel has been closed with the screw top Preparation of calibration standard 100 water vapor saturated air 1 Place wet cotton wool in the vessel and label it cal 100 2 Drill two holes for inserting the minisensor and the temperature sensor in the screw top and close the vessel with it 3 Wait about 2 minutes to ensure that air is water vapor saturated Preparation of calibration solution 100 air saturated water 1 Add 100 mL water to a suitable vessel and label it cal 100 2 To obtain air saturated water blow air into the water using an air pump with a glass frit airstone creating a multitude of small air bubbles while stirring the solution 3 After 20 minutes switch off the air pump and stir the solution for fur
31. Variation of Bunsen absorption coefficient 6 with temperature ep p p p Ts p p The data in Table 12 2 can be described by two forms of equations The first form of equation to describe the temperature dependent variation of the Bunsen absorption coefficient a 0 is obtained by fitting a general power series to the values in Table 12 2 A fourth degree polynomial fit can be chosen yielding equation 22 10 a a b 0 c 0 d 0 e 0 22 where 8 is the temperature in C and a e the coefficients calculated by standard curve fitting procedures as given in Figure 12 8 50 0 0 10 48 998 1 335 0 2 755 10 0 3 220 10 6 1 598 10 0 a 48 998 b 1 335 c 22 755 10 d 3 220 10 e 1 598 10 a 9 10 B 30 20 0 5 10 15 20 25 30 35 40 45 50 6 C Figure 12 8 Variation of Bunsen absorption coefficient a 8 with temperature F is the square of the correlation coefficient The other form of equation to describe the variation of a with temperature can be derived from a thermodynamical correlation and gives an equation of the form Appendix 60 Inl o 7 B InT C 23 where A B and C are constants and T is the temperature in K For oxygen dissolved in water we find by fitting the equation to the values ofain Table 12 2 that A 8 553 10 B 2 378 10 and C 1 608 10 Values of o calculated from eqns 22 and 23 for the same temperature agree within 0 5 Yo The
32. aeeteaeeeeaeeseaeeeeaeeseseeesaceseseeseaeeseeeeeeeteaes 44 8 1 3 Eoggling eL Eater EUR nati etm I Eee oie modd 44 8 2 Some Advice for Correct Measurement sees esee eene e nennen nennen nnn tnnt nnne 45 8 2 1 Signal drifts due to oxygen gradients sssssssseseseeeeeeeneneeen nennen 45 8 2 2 Signal drifts due to temperature gradients essssseseeeeeeenennenenennenns 45 8 2 3 Signal drift due to photodecomposition essssssseeeeeeeeeeennenennre nennen 45 8 2 4 Signal drift due to too much ambient light ssseseeeeenenenennneeens 46 8 2 5 Performance proof de ese Rec e ER ELE Lees 46 8 2 6 Correction for air pressure variations sssesesseeeeeeneeeeen nene nne 46 Table of contents 9 CI CB uei 47 9 1 Warm Up Aa aaa E ATEI TT 47 9 2 MaintenanCE saienisi naa aeaa maa E ara Eha pa anna aiaia aanas anana aain 47 9 3 ServiGe AA E TTT E do cec eed eic eko swelo de 47 10 Technic l Data riori riri eer nd e Ue aita ran konia og na D UY kan eka kenn e aa Van Ed kaa ayen EY a E SNR RE CE EARS RE ERR aa n ban 48 10 1 General Data iii E kwa a a 48 10 2 Technical rete M 49 10 3 Operation Notes E M 49 171 Concluding Remarks 25 oie citeccsc ces cncgsccde
33. all channels with the same value by clicking set all Please note By increasing the light intensity you increase the amplitude of the oxygen microsensor This leads to smoother phase signals However increasing the light intensity can increase photobleaching which decreases the shelf life of your sensor Software 26 Ten windows are used to display the data of each channel separately The windows named channel 1 to channel 10 show the data of the respective channel The oxygen unit is the same as specified in the window Measurement at the beginning of the measurement It is not possible to change the unit during the measurement The ast measured oxygen value is displayed in the marked field on the left The scale of the y axis and the starting point of the x axis can be set to different modes by clicking on the Scale button Two options are implemented 1 Autoscale On The software determines the minimum and maximum values to display all data 2 Autoscale Off The maximum and minimum value of y axis and the minimum of the x axis can be defined by the user By clicking on the current value the minimum and or maximum value can be changed The Clear graph button is used to clear the graphical window from all former data 6 4 Data Handling In the head of the ASCII file you find Line 1 time and date when the measurement has started software version Line 2 number of measured channel Line 3
34. an also be used in methanol and ethanol water mixtures as well as in pure methanol and ethanol We recommend to avoid other organic solvents such as acetone chloroform or methylene chloride which may swell the sensor matrix Interferences were found for gaseous sulfur dioxide SO2 and gaseous chlorine Cl Both of them mimic higher oxygen concentrations Planar Oxygen Minisensor 8 Response time The response time too 90 Yo of the signal change has occurred of the PSt3 oxygen sensor is less than 30 s in solution non stirred and even less than 8 s in the gas phase The response time too of the oxygen sensor is dependent from the diffusion rate of oxygen through the sensor layer and hence on the thickness of the sensor layer and the stirring rate A typical oxygen response curve of sensor membrane PSt3 in a non stirred and stirred sample solution is shown in Figure 5 3 below The response times tgo of sensor membrane PSt3 are listed in Table 5 3 below Unlike electrodes optical sensors do not consume oxygen and the signal is independent of changes in flow velocity which means that stirring decreases the response time but has no effect on the measured value Optical isolation of the oxygen sensitive layer which is applied to exclude ambient light and improve chemical resistance will slow down the sensor response 100 oxygen minisensor PSt3 8 801 5 J 60 stirred 5 too 40 s B J S non stirred Ka 40 T too 60
35. ber is covered with a high grade steel tube to protect both the sensor material and the POF Usually the fiber is coated with an optical isolated sensor material in order to exclude ambient light from the fiber tip SMA connector e very robust sensor with an excellent long term stability more than 100000 data points without drift e sterilizable H202 ethanol ethylene oxide e not autoclavable POF does not stand autoclaving conditions 130 C 1 5 atm e measuring range 0 250 a s e limit of detection 0 15 a s Ordering information KA Dipping Probe PST3 Oxygen Sensitive Coating PSt3 0 250 Yo air saturation Order code for the Oxygen Dipping Probe DP PSt3 Planar Oxygen Minisensor 15 5 2 4 Oxygen Probe for Inline Measurements in Fermenters OIM OIM consists of a fitting made from stainless steel The oxygen sensor is integrated in the top of the metal fitting as shown below The metal fitting is connected to the instrument via a polymer optical fiber The standard fiber cable length is 2 5 m OIM is available in different sizes 12 mm 25 mm and standard OIM fits to B Braun Biostat B and B Braun Biostat C fermenters Polymer optical fiber Steel housing diameter 12 mm DO Probe immobilized on a glass support This chemo optical DO probe has outstanding properties The system can be used after autoclavation without recalibration e The system is fully autoclavable up to 100 time
36. bration of oxygen minisensors is performed using a conventional two point calibration in oxygen free water cal 0 and water vapor saturated air or air saturated water cal 100 In the sub window Calibration constants cal 100 is denoted as 2 cal point Preparation of calibration standard cal 0 oxygen free water 1 Add 1 g sodium sulfite NapSOg3 to a vessel and label it cal 0 2 Dissolve Na SOsin 100 mL water The water becomes oxygen free due to a chemical reaction of oxygen with Na2SOs Additional oxygen diffusing from air into the water is removed by surplus of Na2SOs 3 Close the vessel with a screw top and shake it for approximately one minute to dissolve Na2SO3 and to ensure that the water is oxygen free Close the vessel after calibration with a screw top to minimize oxygen contamination The shelf life of cal 0 is about 24 hours provided that the vessel has been closed with the screw top Preparation of calibration standard cal 100 water vapor saturated air 1 Place wet cotton wool in the vessel with the label cal 100 2 Drill a hole for inserting the minisensor in the screw top and close the vessel If you want to calibrate several minisensors simultaneously drill as many holes as there are minisensors 3 Wait about 2 minutes to ensure that the air is water vapor saturated Alternatively Preparation of calibration standard cal 100 air saturated water 1 Add 100 mL water to a suitable vessel and label it cal 10
37. button Oxygen unit 4 Enter the sampling rates and the temperature for each channel By clicking locked the adjusted sampling rate of the first channel is also set for all other channels 5 Startthe measurement by clicking button A channels SINGLE SAMPLING CHANNEL CHANNEL RATE TEMPERATURE ALL CHANNELS oc Ls m M D ao M e a M ao NI a a OXYGEN UNIT M ao Tm M ao mm M ao 2 3 4 5 6 20 0 7 8 9 WARNINGS 1 T NI koz a Lg Tu M 3 a locked ml a a amp lt l Measurement with Oxygen Sensor PSt3 44 8 1 2 Scanning selected channels Switch on OXY 10 and PC software following chapter 6 Go to window Measurement Choose oxygen measurement unit from button Oxygen unit Enter the sampling rates and the temperature for each channel Please note If you want to adjust different scanning rates for the activated channels ensure that the locked field is not activated 5 Start the measurement by clicking the required channel button PON gt 8 1 3 Logging Measured data are logged during the measurement Add contents to the description fields in the File description section before starting logging This is not necessary but helpful as the description is later stored in the data file 1 Depending on the scan mode click on All Channels for logging all the selected channels in the measuring window or Single channel for single channel logging
38. device The safety nut must be carefully attached while turning slightly clockwise 7 2 1 3 Performing the calibration 1 Switch on the OXY 10 and the PC software following chapter 6 2 Go to window Calibration and enter the actual atmospheric pressure in hPa and the temperature of the calibration standards cal 0 and cal 100 The atmospheric pressure of the calibration is needed to convert the oxygen unit air saturation into partial pressure units hPa Torr or concentration units mg L pmol L Please ensure that there are no temperature changes during the calibration of the oxygen sensor Besides it must be ensured that the temperature during later measurement is constant and already known However the temperatures during the measurement and the calibration process are allowed to be different 3 Select the channel to be calibrated in the section Channel of sub window SINGLE CHANNEL or switch to the sub window ALL CHANNNELS Calibrate All Channels 1 For each sensor connect one plastic tubing with a syringe the other dip into the vessel containing the calibration solution 100 cal 100 Fill the syringes slowly with calibration standard cal 100 Please ensure that there are no air bubbles located in the glass tubes of the flow through cells Calibration 35 D 4100 00 2nd cal point CMs 1013 EP temperature of cal0 standard E GE temperature of cal100 standard ee 0 100 00 2 209 58 81 MA 2659 k Wait ab
39. dow appears rou age m z initialization Ea Please connect the instrument to the PC and turn the power switch on Next please select the proper serial port number Serial Port 4 Choose the right com port with a left mouse click on Serial Port Then press OK The following window appears and all 10 channels are initialized Loading data from channel 1 If the wrong com port is adjusted the software gives an error message Please change the com port and press OK 6 3 Function and Description of the OXY 10 Software The window shown below is displayed after starting the software OXY 10 software The program has 5 main sections 1 Measurement Calibration Logging All Channels Graphical and numerical display of all channels a Fo DN Graphical and numerical display of the respective channel 6 3 4 Measurement With this software it is possible to start the measurement scanning all channels by clicking the All Channel button or selected channels by clicking the required single channel button Before starting the measurement you have to choose the oxygen unit air saturation hPa Torr mg L or pmol L the sampling rate fastest sampling max 15 s and enter the measurement temperature The button Warnings has the possible captions WARNINGS ON This caption indicates that the software will warn if no sensor is connected or if the sensor intensity is low If sensor intensity
40. e angle 1 100 air saturation 0 5 10 15 20 25 time h Photodecomposition test of PSt3 continuously illuminating the sensor membrane for 25 hours 8 2 4 Signal drift due to too much ambient light A source of error is the detector overload due to too much ambient or sensor light A detector overload can be recognized with appearing warning prospective the warnings are activated Please notify that your measurement is not reliable if the warning light overload is shining red A detector overload can affect both the amplitude and the phase angle Please decrease the LED intensity to reduce the amounts of photons reaching the photodetector 8 2 5 Performance proof If you want to prove the performance during the past measurement please check the calibration values by inserting the sensor tip in the cal 0 and cal 100 calibration standards when you have finished your measurement If the device shows 0 air saturation immersing the sensor tip into the cal 0 solution and the value of the second calibration point measuring the cal 100 standard the sensor worked perfectly during the whole measurement 8 2 6 Correction for air pressure variations The atmospheric pressure of the calibration is needed to convert the oxygen unit 96 air saturation into partial pressure units hPa Torr or concentration units mg L pmol L The partial pressure and the oxygen concentration units are calculated from air saturation by
41. e given in the technical specification sheet Please read also the technical notes to avoid mistakes a am PI Rz SerNo OXY 10 03001 Serwan Berar Cire Wagern surg Gernany a A a H 230 VAC ELEMENT DESCRPTION FUNCTION ON OFF switch Switches the device ON and OFF C1 Line adapter for power Connector for 230 V AC power supply supply C2 RS 232 interface Connect the device with a RS 232 data cable to your male PC Notebook here Required Basic Equipment 5 4 Required Basic Equipment e Oxygen meter OXY 10 e Software for OXY 10 e PC Notebook System requirements Windows 98 2000 XP Millenium NT 4 0 Pentium processor at least 166 MHz 64 MB RAM a RS 232 port or a USB port and a USB serial adapter is needed e RS 232 Cable e Line adapter 110 220 V AC 12 V DC e Oxygen sensitive minisensor The minisensors are mounted into different types of housings e Vessels for calibration standard 100 water vapor saturated air 100 air saturation and calibration solution 0 oxygen free water We recommend Schott laboratory bottles with a thread which can be obtained by Merck Eurolab ordering number 215L1515 scope of supply Planar Oxygen Minisensor 6 5 Planar Oxygen Minisensors 5 1 Sensor Characteristic of the Oxygen Sensitive Minisensors The principle of the sensor operation is based on the quenching of luminescence caused by collision between molecular oxygen and luminescent dy
42. e molecules in the excited state Figure 5 1 shows a typical response curve of an oxygen sensitive sensor In the presence of oxygen the signal in our case the phase angle 9 decreases The phase angle 9 can be related to the oxygen content as shown in Figure 5 2 The theoretical aspects are explained more detailed in the appendix 60 60 010 0 Op g 50 Fi 9 2 40 S o a o Ej 30 20 10 T A 10 0 2 4 6 8 10 12 14 16 18 20 0 20 40 60 80 100 120 140 160 180 200 220 240 time min air saturation Figure 5 1 Response of minisensor PSt3 toward Figure 5 2 Effect of the phase angle of minisensor changes in the oxygen concentration PSt3 on different oxygen contents Measuring range and limit of detection We offer an oxygen sensor membrane called PSt3 which is tailored for oxygen measurements up to 250 air saturation The measuring ranges and the limit of detection of this sensor are given in Table 5 1 Table 5 1 Measuring range and limit of detection of the PSt3 oxygen sensor membrane Dissolved Oxygen Gaseous amp Dissolved Oxygen Measurement range 0 22 mg L ppm 0 250 air sat 0 50 Yo oxygen sat 0 700 umol 0 380 Torr 0 500 hPa Limit of Detection LOD 0 15 air saturation 0 31 hPa 15 ppb dissolved oxygen 0 23 Torr Planar Oxygen Minisensor 7 Resolution and accuracy Since the oxygen calibration plot displays a non lin
43. each of children As the manufacturer of the OXY 10 we only consider ourselves responsible for safety and performance of the device if e the device is strictly used according to the instruction manual and the safety guidelines e the electrical installation of the respective room corresponds to the DIN IEC VDE standards The OXY 10 and the sensors must not be used in vivo examinations on humans The OXY 10 and the sensors must not be used for human diagnostic or therapeutical purposes 3 Description of the OXY 10 Device 3 1 Instrument The OXY 10 is a 10 channel oxygen meter for use with fiber optic oxygen minisensors based on a 2mm polymer optical fiber POF The OXY 10 system detects oxygen the oxygen partial pressure in both solutions dissolved oxygen as well as in the gaseous phase For operation a PC Notebook with RS 232 interface is required The OXY 10 is controlled using a comfortable software which also saves and visualizes the measured values OXY 10 does not contain temperature sensors temperature changes during the measurement are not compensated by the software 3 2 Front Panel of the OXY 10 Device ELEMENT DESCRIPTION FUNCTION CH1 CH10 SMA fiber connector Connect the fiber optic oxygen minisensor here on Line Blue Control instrument on LED off instrument off Description of the OXY 10 Device 4 3 3 Rear Panel of the OXY 10 Device The electrical specifications of all rear panel connectors ar
44. ear behavior the oxygen resolution is given for four different partial pressures at 20 C the accuracy for two different partial pressures The resolution in oxygen is also transformed in different oxygen units Table 5 2 Oxygen resolution and accuracy of the PSt3 oxygen sensor membrane at different oxygen contents at 20 C and 1013 mbar Resolution 1 0 05 Yo air sat at 20 C and 1013 hPa 30 0 1 airsat 0 09 0 005 mg L ppm 100 05 4 airsat 2 72 0 01 mg L ppm 250 1 7 air sat 9 06 0 05 mg L ppm 021 0 01 oxygen 22 65 0 15 mg L ppm 6 3 0 02 Yo oxygen 20 9 t 0 1 96 oxygen 52 4 0 35 oxygen 1 55 0 08 Torr 46 7 0 2 Torr 2 83 0 14 umol 155 5 0 75 Torr 85 0 0 28 umol 388 8 2 6 Torr 283 1 1 4 umol 2 0 1 hPa 798 0 4 7 umol 60 0 3 hPa 200 1 hPa 500 0 3 hPa Accuracy 20 C t 196 at 100 Yo air saturation 0 15 at 1 air saturation Temperature The oxygen sensors can be used in the temperature range of 0 to 50 C The OXY 10 does not contain temperature sensors Temperature changes during the measurement are not compensated by the software Cross sensitivity No cross sensitivity exists for carbon dioxide CO2 hydrogen sulfide H2S ammonia NH3 pH any ionic species like sulfide Sz sulfate SO4 chloride CI or salinity Turbidity and changes in the stirring rate have no influence on the measurement The sensors c
45. easurement and the calibration process are allowed to be different 3 Select the channel to be calibrated in the section Channel of sub window SINGLE CHANNEL or switch to the sub window ALL CHANNNELS Calibration 30 Calibrate All Channels Place the calibration standard 100 cal 100 containing wet cotton wool underneath the oxygen minisensors The vessel with the label cal 100 has to be closed with the screw top containing the holes Insert the plastic fibers carefully through the holes without touching the oxygen sensitive spots until they are about 3 cm deep inside the vessel Make sure that the plastic fibers with their sensor spots cannot touch the vessel and the cotton wool Measurement Calibration Logging All channels SINGLE CHANNEL 5 ALL CHANNELS Calibration constants 1100 00 Jl 20 0 Calibration with current values CAL 100 00 User defined calibration J 58 81 J 2659 Wait about 3 minutes until the phase angles are constant and press the CAL 100 button to store the 100 air sat calibration values at the adjusted temperature A message window opens and informs you that you will program all channels with the actual calibration values Click the OK button to store the new calibration data 7 a EI This will programm all channels Cancel To record the second calibration values oxygen free water cal 0 place the vessel with the label cal 0 underneath the oxygen minisen
46. el the actual measured oxygen concentration is shown in the unit you have adjusted in the menu bar measurement The raw values amplitude and phase value can be displayed by clicking on Raw values on in the Channel settings on the right side or they can be hidden by clicking on off Chameli Channel2 Chanels Channel4 channels Channel6 Channel channels Channel channel 10 Oxygen 10021 Channel 1 settings Amp Phase Temp Cleargraph Auto scale measurement time min Channel settings In the channel settings the user is able to configure each channel separately and to optimize the instrument performance 1 Raw values The raw values the phase angle in degrees and the sensor amplitude in mV can be displayed hidden by clicking the On Off button If the raw values are not displayed the signal amplitude is shown via a bar the longer the bar the higher the signal 2 Signal LED intensity Note After changing the intensity any sensor calibration for the changed channel has to be repeated With the current of the LED you can adjust the amount of light illuminating the sensor spot The LED current can be set manually between 10 and 100 If you increase the LED current the signal amplitude increases since a higher light density illuminates the sensor spot The channel settings can be adjusted for the respective chosen channel by clicking set one However it is also possible to set
47. ers are able to transport more information than power currents information can be simultaneously transferred e g intensity of light spectral distribution polarization information such as decay time or delayed fluorescence 12 1 4 Luminescence Decay Time The OXY 10 measures the luminescence decay time of the immobilized luminophore as the oxygen dependent parameter t f O2 2 The OXY 10 uses the phase modulation technique to evaluate the luminescence decay time of the indicators If the luminophore is excited with light with sinusoidally modulated intensity its decay time causes a time delay in the emitted light signal In technical terms this delay is the phase angle between the exciting and emitted signal This phase angle is shifted as a function of the oxygen concentration The relation between decay time t and the phase angle 9 is shown by the following equation TN tan o A tan P 27 f aoa T 3b t tan f O2 3c t luminescence decay time phase angle fmou modulation frequency Appendix 54 MI I I max max 5 0 5 10 15 20 25 30 time ys Figure 12 5 Schematic of the single exponential decay to gt ti 5 0 5 10 15 20 25 30 time us Figure 12 6 The luminophore is excited with sinusoidally modulated light Emission is delayed in phase expressed by the phase angle F relative to the excitation signal caused by the decay time of the excited state The
48. gen Sensitive Coating PSt3 0 250 air saturation Order code for the OxyFinger OFG PSt3 17 Planar Oxygen Minisensor 18 5 2 7 Coaster for Shaking Flasks and Spinner Flasks CSF Application Online control of oxygen in shaking flasks and spinner flasks Control amp Data Cbaster System set up for online DO measurement in shaking flasks Specifications The coaster for shaking flasks and Spinner flasks is a tool for online monitoring of dissolved oxygen concentration in shaking flasks The coaster for shaking flasks does not contain a sensor It redirects the light so that oxygen sensors in shaking flasks can be read out The coaster has a colored circle which makes it easy to position it right under the sensor The position of the optical read out is flexible and can be adjusted to different sizes of shaking flasks The standard cable length is 2 5 m The cable has an outer diameter of 2 6 mm Please note The coaster for shaking flasks and spinner flasks does not contain a sensing layer It is designed to read out sensor foils which are attached to the inner side of a shaking flask spinner flask or a similar vessel e g beaker Ordering Information Order code for the Coaster for Shaking Flasks CS Software 19 6 Software 6 1 Software Installation This software is compatible with Windows 98 2000 Millenium NT4 0 XP 1 Insert the supplied disc CD into the respective drive Start
49. hase angles are constant the variation of the phase angles should be smaller than 0 05 and click the CAL 100 button to store the 100 air sat calibration values at the adjusted temperature A message window opens and informs you that you will program all channels with the actual calibration values Click the OK button to store the new calibration data 3 To record the second calibration values oxygen free water cal 0 remove the cal 100 solution from the vessels and fill them with the calibration standard 0 cal O To minimize the response time slightly stir the solution Please note Vigorous stirring can lead to an oxygen contamination of the cal O solution Wait about 3 minutes until the phase angles are constant the variation of the phase angles should be smaller than 0 05 and press the CAL 0 button to store the 0 air saturation calibration values at the adjusted temperature A message window opens and informs you that you will program all channels with the actual calibration values Click the OK button to store the new calibration data 4 Rinse the sensor membranes gently with water after calibration to remove sulfite remaining on the surface Calibration 41 Calibrate Single Channels Place the calibration solution 100 cal 100 air saturated water or water vapor saturated air into the glass vessel To minimize the response time slightly stir the solution Please ensure that the cal 100 solution com
50. ir saturation accuracy 1 96 air saturation at 100 96 air saturation CALIBRATION PROCEDURE PSt3 oxygen sensor 2 point calibration in oxygen free water and humidified air or air saturated water Optical Connector SMA compatible 2 mm polymer optical fiber Wavelength 505 nm POWER INPUT 230VAC 50 60Hz 0 5A max DIGITAL INTERFACE Communication Protocol serial interface RS 232 38400 Baud Databits 8 Stoppbits 1 Parity none Handshake none Instrument output on RJ11 4 4 plug RJAT 4 4 Technical Data 49 Interface cable to PC RJ11 4 4 to DSub9 D Sub9 female 2 RXD 3 TXD 5 GND 1 4 6 7 8 9 N C ENVIRONMENTAL CONDITIONS Operating temperature 0 to 50 C Storage temperature 10 to 65 C Relative humidity up to 95 OPERATION CONTROL LED at the front panel length 300 mm width 250 mm height 140 mm weight 3600 g 10 2 Technical Notes The unit uses a special interface cable Another cable can cause the unit s malfunction Optical Output SMA The SMA connector is a high precision optical component Please keep it clean and dry Always use the rubber cap to close the output when not in use 10 3 Operation Notes To achieve the highest accuracy the OXY 10 should be warmed up for 5 min before starting the measurement Please see the details of the measurement process described in the OXY 10 manual Concluding
51. is either a change in the color absorbance or spectral distribution or the luminescence properties intensity lifetime polarization Light acts as the carrier of the information The major components of a typical fiber optical sensing system are e alight source to illuminate the sensor laser light emitting diode lamps e an optical fiber as signal transducer plastic or glass fiber e a photodetector photodiode photomultiplier tube CCD array e the optical sensor indicator immobilized in a solid matrix POF polymer optical fiber sensor spot En p SMA connector inn DEZAN steel tube Figure 12 3 Scheme of a minisensor Appendix 53 Glasfaser Koppler Minisensor ST LED Figure 12 4 Schematic drawing of the optical setup of a measuring system with minisensors LED light emitting diodes PMT photomultiplier OF optical filters ST fiber connector 12 1 3 Advantages of Optical Oxygen Sensitive Minisensors e no oxygen is consumed during the measurement e the signal is independent of changes in flow velocity e they are able to measure the oxygen content in dry gases e they are insensible towards electrical interferences and magnetic fields they are more sensitive than conventional electrodes up to ppt range long term stability and low drift using silica fibers it is possible to measure in samples while physically separate from the light source and detectors e light conducting fib
52. is low the ntensity check should be done by the user If the sensor intensity process fails the sensor must be replaced WARNINGS OFF This caption indicates that the software will show no warnings This is only recommended for advanced users On the right side you can find the version number of the software If you have questions regarding the OXY 10 software please contact our service team and have the software version number ready Furthermore the actual date time are presented on the right side 6 3 2 Calibration The detailed calibration process of oxygen sensors you can find in chapter 7 6 3 3 Logging Measured data are logged during the measurement Add contents to the description fields in the File description section before starting logging max 3 lines This is not necessary but helpful as the description is later stored in the data file 1 Depending on the scan mode click on All channels for logging all channels or Single channel for single channel logging 2 Inthe appearing save as window specify filename without extension and its location The PC software automatically creates one to ten different files The filename consists of the specified filename and the extensions ch1 txt ch2 txt to ch10 txt respectively ch stands for channel All filenames are displayed in the section Created files Please note Logging must be enabled before starting the measurement After the measurement i
53. l LED current 060 13 Ref LED current 075 14 Ref LED amplitude 117036 15 Frequency 006 Sending interval 0001 17 Averaging Wa 18 Intemaltemp 20 0 C 20 SYSTEM SETTINGS 21 APL function ON 22 Temp compensation OFF 23 Analogout OFF 24 RS232echo OFF 25 Oxygen unit a s CALIBRATION 28 Sensortype 3 28 096a sphase 1 58 29 at 020 0 C amp 142800 30 100 00 a s phase 2 26 50 at 020 0 C amp 061300 31 Date ddmmyy 050405 32 Pressure mBar 1013 33 FIRMWARE 35 Code 3 015 IAP 06 28 04 12 26 31 36 Xilinx built 01 05 04 MM DD Y Y 38 Pressure hPa 1013 39 Date dd mm Timeihh mm Logtime min Oxyi96 air sat Phasel Amp Tempi C Recalibration 41 05 04 05 10 39 29 0 99 91 26 51 61346 20 42 05 04 05 10 39 43 0 24 99 96 26 5 61421 20 43 05 04 05 10 39 58 0 49 100 01 26 49 61419 20 M4 M test ch1 Figure 6 3 Logged data of channel 1 displayed in Microsoft Excel Calibration 28 7 Calibration The second window in the menu bar of the OXY 10 software is named Calibration It consists of two sub windows The sub window SINGLE CHANNEL Figure 7 1 is used to calibrate each channel individually The sub window ALL CHANNELS Figure 7 2 calibrates all channels with one command Use this option if you want to calibrate all channels in one calibration procedure Please note For calibrating the sensor it is necessary to
54. left Set of four coasters for shaking flasks right Coaster with green positioning ring 7 3 1 3 Calibration 40 Performing the calibration Switch on the OXY 10 instrument and the PC software following chapter 6 Go to window Calibration and enter the actual atmospheric pressure in hPa and the temperature of the calibration standards cal 0 and cal 100 The atmospheric pressure of the calibration is needed to convert the oxygen unit 96 air saturation into partial pressure units hPa Torr or concentration units mg L pmol L Please ensure that there are no temperature changes during the calibration of the oxygen sensor Besides it must be ensured that the temperature during later measurement is constant and already known However the temperatures during the measurement and the calibration process are allowed to be different Select the channel to be calibrated in the section Channel of sub window SINGLE CHANNEL or switch to the sub window ALL CHANNNELS Calibrate All Channels 1 Place the calibration solution 100 cal 100 air saturated water or water vapor saturated air into the glass vessels To minimize the response time slightly stir the solution Please ensure that the cal 100 solution completely covers the sensor foils 2nd cal point C 100 00 BS pressure C 1013 ES temperature of cal standard C temperature of cal100 standard C ec 0969 100 00 2 ed 58 81 ME 26 59 IE Wait about 3 minutes until the p
55. lt concentration Total pressure 760 torr Oxygen solubility mg L CT 9 10009 D ICE T3 ow f m m wa pw 3s 399 35 NON ON L AN KL KL on The effect of increasing the salt concentration on the vapor pressure is negligible small as shown in Table 12 5 Table 12 5 Variation of solution vapor pressure pw with salt concentration Vapor pressure of solution torr Eme 3 RE The dependence of oxygen solubility on salt concentration can also be obtained from equation 21 except that now values calculated from either equation 27 or 28 have to be used for calculation of the Bunsen absorption coefficient Equation 27 differs from equation 22 by an additional forth degree polynomial term for chlorinity 10 a a b O c 0 c d 0 e 6 Cl p q 8 r 0 s 0 t 6 27 where 0 is the temperature in C a e are the coefficients used in equation 22 and p t are new constants given in Table 12 6 The values of these new constants are obtained by fitting the polynomial to experimental data in the ranges 0 lt 0 lt 30 and 0 lt CI lt 207 To obtain an oxygen solubility from the Bunsen absorption coefficient the same procedure as described previously is used s equation 24 page 60 An alternative equation to compensate the Bunsen absorption coefficient by the salt concentration displays equation 28 Q 10 a ea A p CMT D T Heri 2er 28 where T is the temperature in Kelvin and A D a
56. measurement of the luminescence decay time an intrinsically referenced parameter has the following advantages compared to the conventional intensity measurement The decay time does not depend on fluctuations in the intensity of the light source and the sensitivity of the detector The decay time is not influenced by signal loss caused by fiber bending or by intensity changes caused by changes in the geometry of the sensor e The decay time is to a great extent independent of the concentration of the indicator in the sensitive layer 2 photobleaching and leaching of the indicator dye has no influence on the measuring signal The decay time is not influenced by variations in the optical properties of the sample including turbidity refractive index and coloration 12 1 5 Literature If you want to find out more about this subject we recommend the following publications e Wolfbeis O S Ed Fiber Optic Chemical Sensors and Biosensors Vol 1 amp 2 CRC Boca Raton 1991 e Klimant l Wolfbeis O S Oxygen Sensitive Luminescent Materials Based on Silicone Soluble Ruthenium Diimine Complexes Anal Chem 67 3160 3166 1995 e Klimant I K hl M Glud R N Holst G Optical measurement of oxygen and temperature in microscale strategies and biological applications Sensors and Actuators B 38 39 29 37 1997 e Holst G Glud R N K hl M Klimant A microoptode array for fine scale measurement of oxygen distribution
57. models based on equation 5 can be used In the first model one fraction of the indicator is assumed to be non quenchable Ksy2 0 1 p f HO 1 f 6 tn I K 0 The oxygen content in Yo air saturation can be calculated according to equation 7 tanF I tanF 0 a 7 an L f anF g sv A second model which also is based on equation 5 can be used for describing the oxygen calibration plot In this model Ksv2 is set to be m Ksv1 I tanF f 1 f Qi 1 1 8 tanF IE Ks 0 1 m Ks 10 The oxygen content in Yo air saturation can be calculated according to equation 9 B NB 4 A C 2 A O with the coefficients Appendix 56 F A KE 92 tanF tanF tanF B Ky Kol in Ke Ka ti K 9b tanF tanF tano E tan Q 9c 12 3 Oxygen Conversion Formulas Please note These conversion formulas are only valid in aqueous solutions and humidified air These formulas have to be modified if measurements have to be performed in organic solvents or solutions with high salinity saturation 26 air saturation Default setting of the instrument see equation 9 in 12 2 Yo oxygen saturation 96 O air saturation uem 10 100 0 2095 volume content of oxygen in air ppm in the gaseous phase ppm O air saturation zak ee I 100 10000 10000 11 piae 1 E Img a luL 1 a 1000000 Ikg 1L 10000 Partial
58. nd P S are the coefficients given in Table 12 6 They are based on measurements for 273 1 T 308 18 K and 0 CI 3076 and is therefore more extensive than equation 27 Both equations give values of 10 a which agree to better than 1 96 Appendix 63 Table 12 6 Values of the coefficients in equations 27 and 28 cage peg ee ea Eqn 27 a 4 900 10 p 5 516 10 b 1 335 q 1 759 10 C 2 759 10 r 2 253 107 d 3 235 104 s 2 654 107 e 1 614 10 t 5 362 10 Eqn28 A 3 C404 5 0 077777777777p 7 88 4307 B 4 417 10 Q 5 344 10 C 2 927 R 4 442 10 D 4 238 10 S 7 145 107 Seawater has a typical salinity of 35 76 35 g 1000 g or a chloride content of about 19 Zo and therefore falls within the scope of both equations 12 5 Temperature Compensation of the Response of Oxygen Sensors A typical oxygen response characteristic at different temperatures is shown in Figure 12 10 The phase angle is a function of the oxygen content P tand f O2 and decreases with increasing the oxygen content 65 10 0 5 ge 0 5 ic 0 0 0 0 5 o 1 5 pos 0 5 1 5 5 55 a 1 5 on k 3 B i 1 5 pg O a 6 e 3 45 6 a E 690 ao 6 12 lo 35 12 2 1296 2 E 209 1296 amp 25 s 20 20 jd 7 50 50 15 50 50 50 2 C 10 C 20 C 30 C 40 C 5 i 0 1000 2000 3000 4000 5000 time s Figure 12 10 Oxygen response characteristics at different temperat
59. ndow Calibration Select the channel to be calibrated in the section Channel of sub window Single channel or switch to the sub window All channels 3 Enter the respective calibration values a phase at 0 air saturation temperature at 0 Yo air saturation phase at 100 air saturation temperature at 100 Yo air saturation pressure at which values a d were measured The atmospheric pressure of the calibration is needed to convert the oxygen unit 96 air saturation into partial pressure units hPa Torr or concentrations units mg L pmol L paap O en SRI de mas CEON E 4 To store the calibration values click the Calibrate button A dialog appears and informs you that you will program all channels in case the sub window all channels is chosen If sub window single channel is chosen a dialogue appears informing you that you will change the last calibration values Click the Continue button to store the new calibration data WARNING E This will change last calibration values Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record user defined calibration values Calibration 33 7 2 Calibration of Flow Through Cell FTC PSt3 There are two ways to calibrate the optical sensors One is the use of two calibration standards the other one is to type in known constants The first way needs two calibration standards Their preparation is described in chapter 7
60. nt via a polymer optical fiber The standard fiber cable length is 2 5 m If you need a cable length of more than 2 5 m up to 15 m available please contact our service team Response times of the oxygen sensor OEC PSi3 Response time Stirred Not stirred Gaseous Oxygen too 60s 1205s 20s Ordering information OIM Exchange Cap Order code for the OIM Exchange Cap OEC PSt3 Planar Oxygen Minisensor 5 2 6 OxyFinger Chemo Optical DO Probe for Mini Fermenters OFG PSt3 OxyFinger consists of a glass test tube glass finger which is coated with an oxygen sensitive foil The sensor signal is transmitted to the instrument via a polymer optical fiber Cable lengths between 2 and 15 meters are available OxyFinger will be manufactured following your specifications Please specify both length and diameter of the glass finger and the size of the vessel closure Please contact our service team The OxyFinger Chemo Optical DO Probe for Mini Fermenters has outstanding properties e The system can be used after autoclavation without recalibration e The system is fully autoclavable up to 100 times e In contrast to classical oxygen electrodes membrane cleaning and frequent replacement is not necessary e There are no electrolyte solutions to poison or replenish e No time for polarization is needed e Long shelf life e measuring range 0 250 a s e limit of detection 0 15 Yo a s Ordering information OXYFinger Oxy
61. ogue appears informing you that you will change the last calibration values Click the Continue button to store the new calibration data Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record user defined calibration values Measurement with Oxygen Sensor PSt3 43 8 Measurement with Oxygen Sensor PSt3 Calibration of the sensor is recommended before each measurement see chapter 7 If you don t want to recalibrate a sensor you can use the calibration values of your last measurement These values are stored in the hardware of OXY 10 Each calibration is only valid for the corresponding sensor Especially after longer measurements more than 10000 measure points or 3 h continuous mode the sensor should be re calibrated Ensure that the temperature of the sample is known and is constant during measurement 8 1 Starting the measurement Note Saving of data is explained in chapter 6 3 3 page 22 and in chapter 8 1 3 page 44 Logging Measurement is started either for selected one to ten channels or for all channels In both cases the scanning rate can be defined for each channel separately In both cases the channels are scanned sequentially Click the Measurement menu bar to adjust the measurement conditions 8 1 1 Scanning all channels 1 Switch on OXY 10 and PC software following chapter 8 1 3 2 Goto window Measurement 3 Choose oxygen measurement unit from
62. ology for measuring oxygen The OXY 10 is a compact easy to transport and completely PC controlled fiber optic oxygen meter The data evaluation is PC supported as well The OXY 10 was specially developed for small fiber optic oxygen sensors flow through cells and integrated sensor systems It is based on a novel technology which creates very stable internally referenced measured values This allows a more flexible use of oxygen sensors in many different fields of interest Optical oxygen sensors also called optodes have important advantages over common Clark type electrodes They are small e They do not consume oxygen Their signal does not depend on the flow rate of the sample e They have an excellent long term stability They can be physically divided from the measuring system which means a contactless measurement e They can be autoclaved and y sterilized Therefore they are ideally suited for the examination of small sample volumes long term measurements in difficult samples and for biotechnological applications A set of different oxygen minisensors flow through cells and integrated sensor systems is available to make sure you have the sensor which is ideally suited to your application Please feel free to contact our service team to find the best solution for your application Your Loligo Team 2 Safety Guidelines PLEASE READ THESE INSTRUCTIONS CAREFULLY BEFORE WORKING WITH THIS INSTRUMENT This device has left
63. out 3 minutes until the phase angles are constant the variation of the phase angles should be smaller than 0 05 and press the CAL100 button to store the 100 air sat calibration values at the adjusted temperature Afterwards press the calibration solutions into the waste A message window opens and informs you that you will program all channels with the actual calibration values Click the OK button to store the new calibration data To record the second calibration values oxygen free water dip the plastic tubings into the vessel containing the calibration solution 0 cal 0 and fill the syringes slowly with it Please ensure that there are no air bubbles located in the glass tubes of the flow through cells Wait about 3 minutes until the phase angles are constant the variation of the phase angles should be smaller than 0 05 and click the CAL 0 button to store the 0 air sat calibration values at the adjusted temperature Afterward press the calibration solutions into the waste A message window opens and informs you that you will program all channels with the actual calibration values Click the OK button to store the new calibration data Rinse the sensor membranes gently with water after calibration to remove sulfite remaining on the surface Calibration 36 Calibrate Single Channels 1 Connect one plastic tubing with a syringe the other dip into the vessel containing the calibration solution 100 cal 100 Fill the sy
64. pletely covers the sensor foil 2nd cal point f 100 00 EU sat CHANNEL el Li 1013 IZ 6 EB temperature of cal standard t C temperature of cal100 standard ec Oxygen 99 99 4 air sat pma 119411 Wait about 3 minutes until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and click the cal 10096 button to store the 100 Yo air sat calibration value at the adjusted temperature A message window opens and informs you that you will change the last calibration values Click the OK button to store the new calibration data Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record the 100 calibration value cal 100 To record the second calibration value oxygen free water cal 0 remove the cal 100 solution from the vessel and fill it with the calibration standard 0 cal 0 To minimize the response time slightly stir the solution Please note Vigorous stirring can lead to an oxygen contamination of the cal 0 solution Wait about 3 minutes until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and press the CAL 0 button to store the 0 air sat calibration value at the adjusted temperature A message window opens and informs you that you will change the last calibration values Click the OK button to store the new calibration data Repeat this procedure for all
65. pressure of oxygen in hPa po hPa p n hPa p T hPa 4 D 0 2095 12 in mbar po mbar p mbar p y T mbar LA ouem 0 2095 13 in Torr po Torr an bag epos Z D 022095 0 75 14 Please note 1 mbar 1 hPa 0 750 Torr Appendix Oxygen Concentration in mg L Spr ifs M e imaj Pas Bw airs Saturation ao 598 2a dag Dee 15 z P 100 V in ppm mg L SN OL Ta i M s kapital fye o PA PAD M AE ATANN a ry Ou pe z Pa 100 V in umol L 1000 c mol L c mg L c mg L 31 25 o M 7 eo mg L MO o mg L E T ir i Pam Pwi 96 air saturation 0 2095 a T 1000000 Pw 100 Vy Patm actual atmospheric pressure pn standard pressure 1013 mbar 0 2095 volume content of oxygen in air Pw T vapor pressure of water at temperature T given in Kelvin a T Bunsen absorption coefficient at temperature T given in cm Os cm M Oz molecular mass of oxygen 32 g mol Vu molar volume 22 414 L mol 57 Appendix 58 12 4 Temperature Dependent Constants Affecting the Oxygen Content 12 4 1 Water Vapor Pressure As shown in equation 12 17 the water vapor pressure py influences the oxygen partial pressure of air saturated water and water vapor saturated air Oxygen partial pressure in dry air p O Pam 0 2095 18 p Oz oxygen partial pressure in dry air at a barometric pressure pam 0 2095 volume content of oxygen in air Oxygen
66. ringe slowly with calibration solution cal 100 Please ensure that there are no air bubbles located in the glass tube of the flow through cell Measurement Calibration Logging All channels IER SINGLE CHANNEL J9 ALL CHANNELS Calibration constants 100 00 E No eo e Calibration with current values 99 99 CAL DZ 26 64 z 11941 2 Wait about 3 minutes until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and press the CAL 100 00 button to store the 100 air sat calibration value at the adjusted temperature Afterwards press the calibration solution into the waste A dialogue appears informing you that you will change the last calibration values Click the Continue button to store the new calibration data WARNING This will change last calibration values Cancel 3 Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record the 100 air saturation calibration value cal 100 4 To record the second calibration value oxygen free water dip the plastic tubing into the vessel containing the calibration solution 0 cal 0 and fill the syringe slowly with it Please ensure that there are no air bubbles located in the glass tube of the flow through cell Calibration 37 Wait about 3 minutes until the phase angle is constant the variation of the phase angle should be smaller than 0
67. s e In contrast to classical oxygen electrodes membrane cleaning and frequent replacement is not necessary e There are no electrolyte solutions to poison or replenish e No time for polarization is needed e Long shelf life Please note The OIM is only ready for use together with the Optical Exchange Cap OEC see page 16 containing the oxygen sensor membrane Ordering information Oxygen Inline Steel Tube Measurements Diameter mm Length mm 12 120 12 140 12 215 12 325 12 425 Planar Oxygen Minisensor 16 5 2 5 OIM Exchange Cap OEC PSt3 Applications The OIM Exchange Cap OEC is the sensitive coating in a metal cap It is used to replace the old sensitive coating and has outstanding properties e The PSt3 coated OEC can be used after autoclavation without recalibration e The PSt3 coated OEC is autoclavable up to 100 times e In contrast to classical oxygen electrodes membrane cleaning and frequent replacement is not necessary e The PSt3 coated OEC can be easily exchanged e There are no electrolyte solutions to poison or replenish e No time for polarization is needed e Long shelf life e Optical isolation prevents cross sensitivity of the sensor towards turbid or fluorescent samples e measuring range 0 250 a s limit of detection 0 15 96 a s The OEC is coated with the oxygen sensitive material PSt3 It has to be integrated into the Oxygen Probe OIM The sensor signal is transmitted to the instrume
68. s excited singlet state As a result the indicator molecule does not emit luminescence and the measurable luminescence signal decreases A relation exists between the oxygen concentration in the sample and the luminescence intensity as well as the luminescence lifetime which is described in the Stern Volmer equation 1 Here to and t are the luminescence decay times in absence and presence of oxygen lo and are the respective luminescence intensities O2 the oxygen concentration and Ksy the overall quenching constant b ef et eKsy 04 t f O5 1 t f O l Luminescence intensity in presence of oxygen lo Luminescence intensity in absence of oxygen Ti Luminescence decay time in presence of oxygen To Luminescence decay time in absence of oxygen Ksv Stern Volmer constant quantifies the quenching efficiency and therefore the sensitivity of the sensor O2 Oxygen content Appendix 52 afr 10 1 1 0 20 40 60 80 100 oxygen content Figure 12 2 A Luminescence decrease in the presence of oxygen B Stern Volmer plot Indicator dyes quenched by oxygen are for example polycyclic aromatic hydrocarbons transition metal complexes of Ru ll Os Il and Rh Il and phosphorescent porphyrins containing Pt Il or Pd Il as the central atom 12 1 2 Major Components of Fiber Optic Minisensors In optical chemical sensors the analyte interacts with an indicator and changes its optical properties The result
69. sors Insert the plastic fibers about 2 cm deep into the cal 0 solution Make sure that the plastic fibers with their sensor spots cannot touch the vessel To increase the response time stir the cal 0 solution Wait about 3 minutes until the phase angles are constant the variation of the phase angles should be smaller than 0 05 and click the CAL 0 button to store the 0 calibration values at the adjusted temperature A message window opens and informs you that you will program all channels with the actual calibration values Click the OK button to store the new calibration data Rinse the sensor membranes gently with water after calibration to remove sulfite remaining on the surface Calibrate Single Channels 4 Calibration 31 Place the calibration standard 100 cal 100 containing wet cotton wool underneath the oxygen minisensor The vessel with the label cal 100 has to be closed with the screw top containing the hole Insert the plastic fiber carefully through the hole without touching the oxygen sensitive spot until it is about 3 cm deep inside the vessel Make sure that the plastic fiber with its sensor spot cannot touch the vessel and the cotton wool 2nd cal point t 100 00 hie 4 CHANNEL edi MA 1013 I7 a EN temperature of cal0 standard C a at temperature of cal100 standard C He Oxygen 99 99 airsat Amplitude 119411 A dialogue appears informing you that you will change the las
70. stic of the Oxygen Sensitive Minisensors eee 6 5 2 Housings of Oxygen Sensitive Minisensors eeeeeeeeeeeeeeeeee eene eene nnne nennen nennen 10 5 2 1 Planar Oxygen Sensitive Foils SP PSt3 essen 11 5 2 2 Flow Through Cell with Integrated Planar Oxygen Sensor FTC PSt3 ssssss 13 5 2 3 Oxygen Dipping Probe DP PSt sssssssesseseneeneeenenenneene nennen nennen nennen nnns 14 5 2 4 Oxygen Probe for Inline Measurements in Fermenters OIM 15 5 2 5 OIM Exchange Cap OEC PSI3 eere a aaee a aE Er aeaea nnne nennen restet reset enn 16 5 2 6 OxyFinger Chemo Optical DO Probe for Mini Fermenters OFG PSt3 ueussuuse 17 5 2 7 Coaster for Shaking Flasks and Spinner Flasks CSF sese 18 6 SOMWANG ei ki kn kep po wd ee iced A ELE kk pep a Len eben kd po 19 6 1 Software Installation 19 6 2 Starting OXY 10 and its Software ceeeseeeeseeeeeeeeneeeeeeeeenseeeneeeenseaenenaeaseesaeneeneeeeseeasneeaseeeeseseeeeeees 20 6 3 Function and Description of the OXY 10 Software ssccssesseneseesesseeesseeenseeeeeeaenseeeaseeenseeeaseaenee 20 6 3 1 MOJSUFO MON be indo eec o teet cita er etx red rite Ae sees reeset 22 6 3 2 Galibration zd 2 inen e DER REN RARE ARRIERE 22 6 3 3 Mere eee a ie te n 22 6 3 4 All Channels Graphical and numerical of all channel
71. stop the measurement Calibration during measurement is not possible To stop the measurement go to the window Measurement and click the All channel button if you perform a measurement with all channels or the respective active channel button During a measurement the calibration buttons are not active Figure 7 1 Figure 7 2 2nd cal point 100 00 ii sat CHANNEL pressure f 1013 hPa t Es temperature of call standard ees temperature of cal100 standard s epitude MENT 0969 100 00 KI sat sat 2 98 58 81 EU 2659 Screenshot of the sub window SINGLE CHANNEL of the window Calibration 2nd cal point f 100 00 EU sat E CHANNEL pressure A 1013 hPa t EN temperature of call standard C temperature of cal100 standard 0 100 00 43 sat sat Phase d Screenshot of the sub window ALL CHANNELS of the window Calibration Calibration 29 7 1 Calibration of Oxygen Dipping Probe DP PSt3 There are two ways to calibrate the optical sensors One is the use of two calibration standards the other one is to type in known constants The first way needs two calibration standards Their preparation is described in chapter 7 1 1 The second possibility is described in chapter 7 1 2 7 1 1 Calibration with two Calibration Standards For the calibration with current values you need calibration standards and your mounted sensor 7 1 1 1 Preparation of the Calibration Standards Cali
72. t calibration values Click the Continue button to store the new calibration data Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record the cal 100 value To record the second calibration value oxygen free water cal 0 place the vessel with the label cal 0 underneath the oxygen minisensor Insert the plastic fiber about 2 cm deep into the cal 0 solution Make sure that the plastic fiber with its sensor spot cannot touch the vessel To increase the response time stir the cal 0 solution Wait about 3 minutes until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and click the CAL 0 button to store the 0 calibration value at the adjusted temperature A message window opens and informs you that you will change the last calibration values Click the OK button to store the new calibration data Repeat this procedure for all other channels by typing in the respective channel into the Channel Window to record the oxygen free calibration value cal 0 Rinse the sensor membranes gently with water after calibration to remove sulfite remaining on the surface Calibration 32 7 1 2 User defined calibration If temperature and phase angle of a former calibration of the same sensor are known the Calibration with constant values is possible 1 Switch on the OXY 10 and the PC software following chapter 6 2 Qo to the wi
73. t is not possible to store the measured values Starting logging during the measurement is also possible but stores only the values from the beginning of logging on CREATED FILES MAIN FATH Description ch 1 Description ch 2 Description ch 3 Description ch 4 Description ch 5 api ren Ten SEEN EP 100 gt 02 gt 100 a s Description ch 6 Description ch 7 Description ch 8 Description ch 9 Description ch 10 6 3 4 All Channels Graphical and numerical of all channel NOTE The All channels window is only enabled when scanning times for all adjusted channels are measured with the same scanning time The graphical display shows all data since the measurement was started The oxygen unit is the same as specified in the window Measurement at the beginning of the measurement It is not possible to change the unit during the measurement With the data choice button it is possible to switch between the data a oxygen concentration in the unit specified in the window Measurement at the beginning of the measurement b phase see appendix for description of phase and amplitude c amplitude see appendix for description of phase and amplitude The Clear graph button is used to clear the graphical window from all former data The scale of the y axis and the starting point of the x axis can be set to different modes by clicking on the Autoscale button Two options are implemented 1 Autoscale On
74. ther 10 minutes to ensure that the water is not supersaturated Calibration 39 7 3 1 2 Mounting the Oxygen Sensitive Minisensors 1 Remove the oxygen sensitive foil carefully from the protective cover 2 Glue small spots of the oxygen sensitive foil into the desired glass vessel using transparent silicone The transparent silicone can be purchased from Loligo left Oxygen sensitive foil glued on the inner surface of a glass vial right Glass vial with integrated oxygen sensitive foil in appropriate adapter Please note Be sure to glue the sensor spots onto your vessel with the proper side The sensor support polyester foil or glass on which the sensor is spotted identifiable by its faint reflection is glued to the vessel while the sensor itself must look toward the sample The figure on page 11 shows how the highly enlarged sensor spot must be glued to the vessel 3 Remove the protective cap from the male fiber plugs of the delivered fiber cable and connect it to the SMA plugs of the OXY 10 and the holding device The safety nut must be carefully attached while turning slightly clockwise If the oxygen sensitive foil is used in shaking flasks we recommend the use of coasters for shaking flasks They are shown below During calibration and measurement the sensor spot has to be placed on top of the fiber optic of the coaster The fiber optic of the coaster is located in the middle of the green positioning ring See also page 18
75. ures Figure 12 11 displays the oxygen dependence of the phase angle at different temperatures and Figure 12 12 the respective Stern Volmer plots These two figures show that both the phase angle in absence of oxygen Po Figure 12 11 and the Stern Volmer constant Ksv starting slope in Figure 12 12 according to equation 4 are temperature dependent o decreases with increasing temperature while Ksy increases with increasing temperature Appendix 64 phase angle 3 3 Ow N 10 0 20 40 60 80 100 120 140 160 180 200 220 240 air saturation Figure 12 11 Effect of the temperature on the phase angle at different oxygen contents given in air saturation 6 m 40 C 30 C 20 C 10 C 5 2 C 2 S 4 N 2 a 0 20 40 6 80 100 120 140 160 180 200 220 240 260 air saturation 7 Figure 12 12 Effect of the temperature on the Stern Volmer constant Figure 12 13 displays the temperature dependence of Po and Ksv From Figure 12 13 decreases in o of about 0 09 can be calculated by increasing the temperature by 1 K On the other hand the Stern Volmer constant Ksv increases about 5 0 104 96 air sat by increasing the temperature by 1 K Appendix 65 61 9 y 62 14 0 08915 x 0 07 0 068 0 066 0 064 0 062 0 06 0 058 0 056 0 054 y 0 04899 4 965 10 x 0 052 R 0 99948 R 0 99914 61 4 60 9 60 4 o J 59 9 59 4 Koy air saturation

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