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MICROX TX3 - Loligo Systems

1. esssssseeeneeneennenenenen nennen 65 8 4 4 Performance proOte cis ue cote cet aw ttt a a e e tet flt te etu e cte e 66 9 General Instr ctiOris iiuoiue rs annman nnna rx e cts exo Eheu ex ro cx xm anro EEx ex FO CUFE HER EEEEEEE CREE EEEEE 67 9 1 Warm Up TIME sc ccct enc cccn nec DL E 67 9 2 Malntenan P E 67 9 3 EA H PEDE 67 10 Technical Data nio eiit rcr aeui eire rale ros ee 68 10 1 General Data eiaeaen a aaa aaan Ean ec EU Nee eR RENE RUD ERU Eger EP E NM CUN Ne chutes 68 10 2 Analog Output and External Trigger eese eeeneeen enne nennen 70 10 3 Technical Notes E A Ire ret eerte meis cede snsescucnterctenenadesuennte cove suasscuestecasds 71 10 4 Operation Notes 5 cei inrer aaea aa a nsec see uso cet uoi secu ae aaa aaan paeo aiaa 71 TT Trouble Shooting nore io cee alee eee es eee eal 72 12 Concluding Remarks iccnsce cscnccesccendenascencctscceadnnnccnceesenendesnaceecetceetsdevanncnccenecnedesecxens 73 13 Append qe ee ee ee a ae ee ee ee es 74 13 1 Basics in Optical Sensing of Oxygen esses eseeeee enenatis 74 13 1 1 Dynamic Quenching of Luminescence sssssssssssseeeeeeeneeneneen eene neret 74 13 1 2 Major Components of Fiber Optic Minisensors seseeeeeeneenenneneenn 75 13 1 3 Advantages of Optical Oxygen Sensitive Minisensors esee 76 1
2. 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 l 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 l A microoptode array for fine scale measurement of oxygen distribution 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 78 13 2 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 air saturation Default setting of the instrument oxygen saturation 20 95 O air saturation 100 0 2095 volume content of oxygen in air ppm in the gaseous phase 2095 1 0 100 10000 10000 ppm O air saturation 1 Img luL 1 aq O 1000000 Ikg 1L 10000 Ippm Partial press
3. calibrate without temp sensor by clicking the cal button Measurement Calibration librate with t erature se EET calibrate without temp sensor ca calibrate manually 5 Enter the actual atmospheric pressure and the temperature of the calibration standards 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 umol L Please note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentration units mg L umol L but the oxygen units 96 air saturation and 96 oxygen saturation have to be corrected for air pressure changes Calibration Menu 2 Point calibration without temperature sensor atm pressure i013 H mbar 1st point phase temperature 0 air sat fs fo ra jo le af Store current value 2nd point phase temperature 100 air sat fpr f Y zlpo fo de amplitude phase Lv Einish X Cancel 6 Place the vessel with the label cal 0 underneath the microsensor Please ensure that the glass fiber with its sensor tip is in the protective glass housing Locate the glass housing carefully about 5 mm above the water surface Calibration 56 7 The glass fiber with its sensing tip is prevented from slipping using a protection tubing Slacken the protection tubing from the glass
4. LOLIGOS I YSTEMS COM Instruction Manual MICROX TX3 Fiber optic oxygen meter L oii o LOLIGOSYSTEMS COM Instruction Manual Microx TX3 Software Version TX3v531 March 2006 Specification of Microx TX3 PC controlled one channel fiber optic oxygen meter for oxygen microsensors excitation wavelength of 505 nm quartz quartz glass fibers of 140 um outer diameter connected by ST fiber connectors Manufacturer PreSens Precision Sensing GmbH Josef Engert StraBe 9 D 93053 Regensburg Germany Phone 49 0 941 942 720 Fax 49 0 941 942 7227 Email info presens de Internet www presens de LETS MOTO ay CTS Table of Contents UM ICI etm 1 2 Safety Gulden iie tr reet urgere Fo i Ee EIE aui Ein BED IN IS HAE tUe EDS 2 3 Description of the Microx TX3 Device eeeeeeeeeeeeeeeeeeeeeennnnn nnns 4 4 Required Basic Equlpment eine ener rere nennen te tno tnn nnmnnn nenna 7 5 Fiber Optic Oxygen Microsensors Sensors and Housings 8 5 1 Sensor Chara cteristiCs 31 ee cvestecececctecueyconctedecccesecteasetesscctecesudesetecsvistesccesteadeets 8 5 2 Housings of Oxygen Sensitive Microsensors ceeeeeeeeeneeeeeereeenne nnne 13 5 2 1 Needle Type Housing Oxygen Microsensors NTH seeeeneenme 14 5 2 2 Needle Type Housing with Fixed Oxygen Microsensor NFSx PSt1
5. Replace oxygen sensor send the sensor back to PreSens for re coating service Check connection of the microsensor Replace microsensor Reduce false light Use optically isolated microsensors Calibrate again Check calibration solutions Immerse Sensor in calibration vessel the proper Prepare fresh sulfite solution Remove air bubbles by carefully tapping Completely extend the sensor Check amplitude Concluding Remarks 73 12 Concluding Remarks Dear customer With this manual we hope to provide you with an introduction to work with the Microx TX3 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 presens de With best regards Your PreSens Team Appendix 74 13 Appendix 13 1 Basics in Optical Sensing of Oxygen 13 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 ES p L emission of light 1 0O 6 x absorption of light d zn excited state energy transfer ns 3 by collision RE s 2 0 x 1 I gt no emission of light Figure 13 1 Principle of dynamic quenching of luminescence by molecular oxygen 1
6. 3 1 mm or a cable length of more than 10 m maximum 60 m please contact our service team info presens de e Penetration probe for insertion into semisolids like sediments or biofilms e Sterilizable H202 EtO EtOH e Not autoclavable since the syringe is made out of polypropylene for autoclavable needle type probe housings please contact our service team e Easy to handle and robust e Measuring range from 0 to 250 air saturation 0 22 6 mg L e Limit of detection 0 2 air saturation 20 umol L Fiber Optic Oxygen Microsensors Schematic drawing of a needle type housing microsensor male fiber optic plug spring safety nut fiber cable syringe plunger gt gt needle plastic base syringe housing syringe needle transport block needle plastic base i lass fiber protective plastic cap sensor tip syringe needle 15 Fiber Optic Oxygen Microsensors 16 Ordering information EFC HDHUHEUUHIT Length of Glass Stainless Needle Fiber Length mm diameter mm 25m Needle Type 2 Um 20 0 4 Housing 40 04 Optical Isolation 40 08 y with optical isolation Oxygen Sensitive Coating 40 12 N without optical isolation PSt1 0 250 air sat 120 0 8 Shape of Sensor
7. 50 um e Fastresponse time better than 1 s e Measures oxygen in both liquids and the gas phase e On line temperature compensation of the oxygen content Therefore they are ideally suited for the examination of very small sample volumes and for measuring oxygen gradients with high spatial resolution in heterogeneous systems Their small dimensions even allow measurements in living systems A set of different microsensors is available to make sure to meet your requirements for your applications Please feel free to contact our service team to find the best solution for your application Your PreSens Team Safety Guidelines 2 2 Safety Guidelines PLEASE READ THESE INSTRUCTIONS CAREFULLY BEFORE WORKING WITH THIS INSTRUMENT This device has left 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 fthe instrument is moved from cold to warm surroundings co
8. C amplitude 1 20 e g 1110 mV 22200 relative units phase 1 0 025 e g 1100 mV 27 50 d Analog Choice S Software 28 6 2 2 Control Bar Numerical display OXYGEN OXYGEN 100 3 oisour sj 100 3 aso airsatur jes umol L c hPa mbar Be RS see The actual oxygen content in the chosen unit here air saturation is displayed in the oxygen window The oxygen unit can be changed by clicking the pull down menu Tables and formulas for the calculation of different concentration scales are given in the appendix Please note It is also possible to change the oxygen unit during the measurement Temperature measurement The actual temperature value of the sample in the case of temperature compensated measurements is displayed in the temperature window If measurement is performed without temperature compensation the manually inserted temperature is displayed with the hint that temperature measurement is off line Control buttons The way to start a measurement is A Calibration of the microsensor with the Calibration Assistant B Start Measurement with the Measurement Assistant A Calibration The calibration assistant is opened see chapter 7 Calibration B Measurement By clicking Start Measurement the measurement assistant opens for entering the measurement settings If you haven t performed sensor calibration yet the following window appears Software 29 d Meas
9. PreSens offers the following standard designs Needle type housing NTH Flow through cell housing Implantable IMP oxygen oxygen microsensor FTCH oxygen microsensor microsensor 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 Fiber Optic Oxygen Microsensors 14 5 2 1 Needle Type Housing Oxygen Microsensors NTH syringe housing ransport block needle plastic E base protective plastic cap Features e High spatial resolution PreSens offers highly flexible needle type oxygen microsensors Needle type oxygen microsensors are miniaturized chemo optical oxygen sensors designed for all research applications were a small tip size 50 um to 140 um and fast response time too up to 1s are necessary Needle type oxygen microsensors are ideal for measuring oxygen distribution profiles in sediment and biofilms with a high spatial resolution of less than 50 um The glass fiber with its oxygen sensitive tip is protected inside a stainless steel needle and can be extended for measurement If the sensor tip is sheltered inside this needle it can be easily penetrated through a septum rubber or any other harsh material A 1 mL syringe tube made from polypropylene is used as the probe housing Fiber cables with a length up to 10 m and an outer diameter of 0 9 mm are available If you need a more robust cable o d
10. RJ11 4 4 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 red instrument off green instrument on orange stand b length 185 mm width 110 mm height 45 mm weight 630 g Technical Data 70 10 2 Analog Output and External Trigger The TX3 instrument version is supplied with a dual programmable 12bit analog output with galvanic isolation and an external trigger input e ANALOG OUTPUT GENERAL SPECIFICATION ANALOG OUTPUT Channels 2 Connector BNC Resolution 12 bit Output range 0 to 4095mV 2mV max error Galvanic isolation 500V rms Shortcut protection Yes Programmable to oxygen temperature amplitude phase by software Equivalence coefficients oxygen 1 0 1 ie 973 mV 97 3 air saturation temperature 1 0 1 ie 208mV 20 8 C amplitude 1 10 i e 2220 mV 22200 relative units phase 1 0 025 i e 1100 mV 27 50 Update rate The update rate is dependent on the sampling rate of the software If an external trigger is used the update rate is equivalent to the trigger pulse rate DC SPECIFICATION ANALOG OUTPUT Resolution oxygen 2mV gt 0 2 air saturation temperature 2mV gt 0 2 C amplitude 2mV 3
11. ssesssssss 17 5 2 3 Flow Through Cell Housed Oxygen Microsensors FTCH cccsceseeeeeeeeeeeeeseeeeeneeeeseeeeneeens 18 5 2 4 Implantable Oxygen Microsensors IMP c cceeeceeeeceeeseeeeeeeeeeeeeaeeseaeeseeaeesaeeesaeseeeeeeeeeneeee 20 WEE o Ln a 22 6 1 Software Installation and Starting the Instrument eee 22 6 2 Function and Description of the Microx TX3 Program eren 23 6 2 1 ML ii rrigee ce Rm 24 6 2 2 GontroL Bar ein menie eir EUREN EIC ERE RT EMI 28 6 2 3 Graphical WindOoW 3 cen eoe nuance E HH d eo E e cere ei 32 6 2 4 Status Bal 2 ee Ra AS i EU ERI Se T 32 6 3 Subsequent Data Handling eeeeseeeeeeeese essen eee enn nennt nena annnm annt nnns 33 EE rumpeec ER 34 7 1 Calibration of Needle Type Oxygen Microsensors eene 34 7 1 1 Preparation of the Calibration Standards 34 7 1 2 Mounting the Needle Type Microsensors ssssm mener 35 7 1 8 Calibration without Automatic Temperature Compensation seen 37 7 1 4 Calibration with Automatic Temperature Compensation seen 40 7 1 5 Ma al Caliprat oN i ei Ree er e ERE B ERU Ea 44 7 2 Calibration of Flow Through Housed Oxygen Microsensors 45 7 2 1 Preparation of the Calibration Standards 45 7 2 2 Mounting the Flow Through Housed Oxygen Microsens
12. temperature sensor compensated measurements here Description of the Microx TX3 Device 6 Rear Panel of the Microx TX3 device The Microx TX has two standard BNC connectors A1 and A2 for analog output channels 1 and 2 another one T1 fore xternal trigger input see figure below The electrical specifications of all rear panel connectors are given in technical specification sheet Please read echnical notes to avoid mistakes also the t ELEMENT DESCRPTION C2 Line adapter for power supply C3 RS232 interface male A1 Analog out channel 1 A2 Analog out channel 2 T1 External trigger input Features FUNCTION Connector for 9 36 V DC power supply Connect the device with a RS232 data cable to your PC Notebook here Connect the device with external devices e g a data logger Connect the device with external devices e g a data logger Connect the device with external devices e g data logger with a trigger output pulse generator microsensor oxygen meter with temperature compensation 2 x 12bit programmable analog channels with galvanic isolation measuring range 0 250 air saturation 9 36 V supply voltage or 220 110V AC adapter RS 232 interface robust metal box Required Basic Equipment 7 4 Required Basic Equipment e Oxygen meter Microx TX3 e Software for Microx TX3 e PC Notebook System requirements Windows 95 98 2000 Millenium NT 4 0 XP Pentium processor at least
13. 133 MHz 16 MB RAM e RS 232 Cable e Line adapter 110 220 V AC 12 V DC e Temperature sensor PT 1000 e Oxygen sensitive microsensor The microsensors 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 VWR International ordering number 215L1515 e Laboratory support with clamp micro manipulator scope of supply 5 Fiber Optic Oxygen Microsensors Sensors and Housings 5 1 Sensor Characteristics The principle of the sensor operation is based on the quenching of luminescence caused by collision between molecular oxygen and luminescent dye molecules in the excited state Figure 5 1 shows a typical response curve of an oxygen sensitive microsensor In the presence of oxygen the signal in our case the phase angle decreases The phase angle can be related to the oxygen content as shown in Figure 5 2 The theoretical aspects are explained more detailed in the appendix 60 0 O29 eO 0 Oj mI 5 8 aso 5 e e 20 2 oO 2 E wo 30 J o o 3 8 201 2 amp amp 2 T 0 t 0 200 t r t t r t t t 400 600 800 0 20 60 80 100 40 time s O Figure 5 1 Response of an oxygen microsensor toward Figure 5 2 Effect of the phase angle of an oxygen changes in the oxygen
14. 20 relative units phase 2mV gt 0 05 Accuracy error 10mV Technical Data 71 e EXTERNAL TRIGGER INPUT GENERAL SPECIFICATION EXTERNAL TRIGGER INPUT Channels 1 Connector BNC Input voltage range TTL compatible up to 24V Trigger mode Low High Low Input must be kept Low for at least 50us Normal state no current Isolation 500V rms Timing Specifications Min rise amp fall time for trigger 15ns see TTL specification Max rise amp fall time for trigger 2 ms Min pulse length 3 ms Min pause length 10 ms Min period length 13 ms 10 3 Technical Notes Power Adapter Microx TX3 should always be used with the original power adapter 110 220VAC 12VDC As an alternative power source a battery can be used that meets the DC input voltage given in technical specification The battery adapter cable is available as an additional accessory Analog Outputs WARNING The analog outputs are not protected against any input voltage Any voltage applied to the analog outputs can cause irreversible damage of the circuit RS232 Interface The unit uses special interface cable Another cable can cause the unit s malfunction Optical Output ST The ST 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 4 Operation Notes Oxygen Measurement To achieve the highest accuracy Microx TX3 should be warmed up for 5min before starting the mea
15. 3 Service Balancing maintenance and repair work may only be carried out by the manufacturer PreSens Precision Sensing GmbH Josef Engert StraBe 9 D 93053 Regensburg Germany Phone 49 0 941 942720 Fax 49 941 9427227 E mail info presens de Internet www presens de Please contact our service team should you have any questions We look forward for helping you and are open for any questions and criticism Technical Data 68 10 Technical Data 10 1 General Data oxygen range 0 250 air saturation resolution 1 0 05 air saturation 30 0 13 air saturation 100 0 44 air saturation 250 1 8 air saturation accuracy t 196 at 100 air saturation temperature range resolution accuracy CALIBRATION PROCEDURE 2 point calibration in oxygen free water and humidified air or air saturated water OPTICAL OUTPUT INPUT peu ST compatible Core Center 100 140 Wavelength 505 nm 0 1596 at 1 96 air saturation TEMPERATURE SENSOR INPUT PT1000 1 Nc N c PT1000 2 BRON Lemo Connector Size 00 Connector for PT 1000 temperature sensor DC INPUT De Range 12 V 1250mA up to 18V 900mA GND 18VDC GND 18VDC RJ11 6 4 Technical Data 69 DIGITAL OUTPUT communication protocol serial interface RS232 19200 Baud Databits 8 Stoppbits 1 Parity none Handshake none instrument output on RJ11 4 4 plug aum 1 4
16. 3 gives oxygen solubilities in mg L for temperature intervals of 0 1 C from 0 40 C The calculated value for cs at a temperature of 20 0 C agrees with the tabulated value of 9 08 mg L Figure 13 9 shows the temperature dependent oxygen solubility in air saturated fresh water Cg Oz mg L pw pw T py 0 2095 o 0 10 Moa Viy c O mg L nN Ww CO oO 0 5 10 15 20 25 0 C Figure 13 9 Dependence of the oxygen solubility in air saturated fresh water on temperature Appendix 83 Table 13 3 Oxygen solubility in air saturated fresh water mg L T C es T 1 2 3 4 5 6 7 8 9 1 0 0 14 64 6 55 51 47 43 39 35 8 27 28 1 28 19 15 10 06 03 99 S A 87 8 2 13 88 79 75 71 68 64 60 56 52 49 45 3 45 41 88 34 30 27 23 20 16 12 4 09 05 02 98 95 9 88 85 8 78 75 5 12 75 71 68 65 61 58 55 52 148 45 42 6 42 39 436 32 29 2 23 20 17 14 m 7 11 08 05 02 99 96 938 90 487 8 amp 8 amp 8 i 81 78 7 72 69 67 64 61 58 55 58 9 53 50 47 44 42 39 36 33 3 28 25 10 25 23 20 48 15 12 10 07 05 02 99 11 10 99 97 94 92 89 87 84 82 79 7 5 12 75 72 70 67 65 63 60 58 55 58 5 13 51 48 46 44 y 39 37 35 32 30 28 14 28 2 23 2i 19 17 15 12 10 08 15 06 04 02 99 97 95 93 A 89 837 8 6 ENS s 81 70 76 74 72 70 68 66 64 17 64 62 J 60 58 56 54 53 51 49 47 45 18 45 43 41 839 37 4235 338 31 30 28 26 19 26 24 22 20 19 17 15 13 11 09 08 20 WE os o o o 99 97 95 9
17. C 06 01 03 13 12 09 0 000 101 510 27 90 20808 20 00 06 01 03 13 12 10 0 017 101 410 27 91 20797 20 00 06 01 03 13 12 11 0 034 101 370 27 92 20785 20 00 06 01 03 13 12 12 0 051 101 960 27 85 20776 20 00 06 01 03 13 12 13 0 069 101 640 27 89 20776 20 00 06 01 03 13 12 14 0 085 101 530 27 90 20761 20 00 06 01 03 13 12 15 0 102 101 710 27 88 20774 20 00 06 01 03 13 12 16 0 119 101 730 27 88 20754 20 00 06 01 03 13 12 17 0 136 101 710 27 88 20747 20 00 06 01 03 13 12 18 0 154 102 080 27 84 20738 20 00 06 01 03 13 12 19 0 170 101 460 27 91 20739 20 00 06 01 03 13 12 20 0 188 101 790 27 87 20736 20 00 06 01 03 13 12 21 0 205 101 760 27 88 20717 20 00 06 01 03 13 12 22 0 222 101 920 27 86 20738 20 00 06 01 03 13 12 23 0 239 101 820 27 87 20718 20 00 06 01 03 13 12 24 0 256 101 990 27 85 20714 20 00 06 01 03 13 12 25 0 273 102 560 27 79 20711 20 00 Calibration 34 7 Calibration 7 1 Calibration of Needle Type Oxygen Microsensors 7 1 1 Preparation of the Calibration Standards Calibration of microsensors is performed using a conventional two point calibration in oxygen free water cal 0 and water vapor saturated air cal 100 Preparation of calibration solution 0 oxygen free water 1 Add 1 g of sodium sulfite Na SOs 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
18. 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 its 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 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 bL 514K 0 T I f O 1 1 f O5 I Luminescence intensity in presence of oxygen lo Luminescence intensity in absence of oxygen t 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 75 2 2 10 0 20 40 60 80 100 oxygen content 46 Figure 13 2 A Luminesce
19. Microsensors 10 Design of the Sensor Tips All the sensors mounted in different housings are available with two different glass fiber tips A a 50 um tapered tip and B a 140 um flat broken tip A Tapered sensor tip B Flat broken sensor tip Advantages of microsensors with a tapered tip Advantages of microsensors with a flat broken tip e high spatial resolution lt 50 um e more photostable than tapered sensor tips e very fast response times tso up to 1 s 2 long term stable e more robust Disadvantages of microsensors with a tapered tip Disadvantages of microsensors with flat broken tip uis e response times too in the order of 30 s e display photobleaching Fiber Optic Oxygen Microsensors 11 Response time The response time tgo 90 of the signal change has occurred in water is dependent from the sensor tip size and typical ranges from 1 s for a sensor tip tapered lt 50 um to about 20 s for a flat broken 140 um tip see figure 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 4 80 z J 5 60 flat broken EE J sensor tip 2 5 F 407 i s 50 um tapered 20 s
20. 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 Na2SOs and to ensure that the water is oxygen free Keep the vessel closed after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S204 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 a vessel and label it cal 100 2 Drill two holes for inserting the microsensor and the temperature sensor in the screw top and close the vessel with it 3 Wait about 2 minutes to ensure that the air is water vapor saturated Calibration 7 3 2 Mounting the Implantable Microsensors 1 Remove the microsensor carefully from the protective cover The microsensor is protected with a glass housing during the transport 2 Fixthe glass housing microsensor with a clip to a laboratory support or a similar stable construction fiber cable j d glass housing E glass fiber with its ST connector Be sensitive tip We strongly advise you not to handle the microsensors without the support especially when the sensor tip is extended 3 Remove the pr
21. Tip S sharp tip 50 um F flat broken tip 140 um Example Dm Hes Held sd H s lol lash on With this code you will order a microsensor type PSt1 mounted in a needle type housing NTH with a glass fiber length of 5 m L5 a sharp tapered sensor tip of smaller than 50 um TS mounted in a stainless needle of 40 mm length and 0 8 mm diameter NS 40 0 8 containing the oxygen sensitive fiber tip with additional isolation YOP Fiber Optic Oxygen Microsensors 17 5 2 2 Needle Type Housing with Fixed Oxygen Microsensor NFSx PSt1 Specifications This type offers an oxygen microsensor for all applications where a fixed sensor tip is necessary The fixed sensor tip is advantageous for measurements in packages The fiber optic oxygen microsensor is based on 140 um silica waveguides The sensor tip is fixed inside the small needle This sensor comes in two different versions One version is designed for measurement in gas phase order code NFSG The other one is for measurements in the liquid phase order code NFSL Fiber cables with a standard length of 2 5 m and an outer diameter of 0 9 mm are available If you need a more robust cable o d 3 1 mm or a cable length of more than 5 m maximum 60 m please contact our service team Features e Measuring range from 0 to 250 air saturation 22 6 mg L e Limit of detection 0 2 air sat 0 02 mg L e High spatial resolution e Used for soft and hard package contain
22. adapter female T connector ST connector fiber cable microsensor tip J 900 um 900 um male fiber plug Teflon sleeve with Luer Lock adapter integrated glass fiber female tightened with a silicone rubber Fiber Optic Oxygen Microsensors 19 Ordering information rons esa LL IptrE IHE loe t t t Needle Length of Optical isolation Type Glass Fiber Y with opt isolation Housing 2 5m N without opt isolation 5m Oxygen sensitive Shape of Sensor Tip coating PSt1 S sharp tip lt 50 um 0 250 air sat F flat broken tip 140 um Example With the ordering code FTCH PSt1 L5 TS YOP you will order a flow through cell FTCH with an integrated microsensor type PSt1 with a glass fiber length of 5 m L5 a sharp tapered sensor tip of smaller than 50 um TS containing the optically isolated oxygen sensitive fiber tip YOP Fiber Optic Oxygen Microsensors 20 5 2 4 Implantable Oxygen Microsensors IMP PreSens offers highly flexible implantable oxygen microsensors The microsensor tip is not housed in any additional housing The bare glass fiber tip can be mounted to your own custom made housing home made steel tubes custom made micro respirometer chambers etc It can be deployed in soil or implanted into the blood circuits of living animals or the liquid circuits of trees to measure oxygen online and in real time Small outer diameters of 900 or even 600 um allow insertion into implante
23. 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 measured by PT 1000 temperature sensor Raw data can be used for user defined recalculations according to the formulas and tables listed in the appendix DESCRIPTION test measurement INSTRUMENT INFO IDENTIFICATION PHlboard number 20020069 PM number 20020032 Serial number TX3 AOT 2003 0001 MUX channel ON 01 PARAMETERS Signal LED current 160 Ref LED current 075 Ref LED amplitude 106091 Frequency 005 Sending interval 0001 Averaging 71 SYSTEM SETTINGS APL function ON Temp compensation OFF Analog out chA o chB o RS232 echo ON Data logger OFF 0 800 Oxygen unit 96a s CALIBRATION Sensor type 1 0 a s phase 1 56 00 at 21 0 C amp 000000 100 a s phase 2 28 07 at 20 0 C amp 021100 Date ddmmyy 060103 Pressure mBar 1013 FIRMWARE Code ver 1 077 12 12 02 12 50 57 Xilinx built 20 08 02 MM DD YY Reset condition CONTINUOUS SOFTWARE INFO OxyView TX3 B2 V5 00 12 2002 by PreSens 06 01 03 13 12 08 MEASURE MODE SETTINGS Dynamic Aver 1 measure mod 1 sec start time 12 50 01 date time hh mm ss logtime min oxygen 26 airsatur phase amp temp
24. concentration microsensor on different oxygen contents Measuring range and limit of detection The optimal measuring range of PreSens oxygen sensitive microsensors is from 0 to 50 pure oxygen 250 96 air saturation However it is also possible to measure oxygen up to 10096 Please contact the PreSens service team to get the appropriate software when measuring up to 100 oxygen The measuring range 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 oxygen microsensors Dissolved Oxygen Gaseous amp Dissolved Oxygen Measurement range 0 250 air sat 0 22 5 mg L ppm 0 50 oxygen sat 0 700 umol 0 380 Torr 0 500 hPa Limit of Detection LOD 0 2 air saturation 0 41 hPa 20 ppb dissolved oxygen 0 30 Torr Fiber Optic Oxygen Microsensors 9 Resolution and accuracy Since the oxygen calibration plot displays a non linear 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 into different oxygen units Table 5 2 Oxygen resolution and accuracy of the oxygen microsensors at different oxygen contents at 20 C and 1013 mbar Dissolved Oxygen Gaseous amp Dissolved Oxygen Resolution 1 0 05 air sat at 20 C and 1013 hPa 30 0 13 air sat 0 09 0 005 mg L ppm 100 0 44 air s
25. continuous mode Mode Drift per hour Drift per 12 hours _Drift per 24 hours tapered sensor tip continuous mode 1 s 0 6 air saturation 1 air saturation 1 6 air saturation flat broken sensor tip 0 5 air saturation 0 5 air saturation lt 0 6 air saturation 8 4 4 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 096 air saturation immersing the sensor tip into the cal 0 solution and 100 96 air saturation measuring the cal 100 standard the sensor worked perfectly during the whole measurement General Instructions 67 9 General Instructions 9 1 Warm Up Time The warm up time of the electronic and optoelectronic components of the Microx TX3 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 ST fiber connector of the microsensor can be cleaned only with lint free cloth The sensor tip may be rinsed only with distilled water Please ensure that no sample residues are inside the syringe needle If necessary rinse the glass fiber with its oxygen sensitive tip with distilled water 9
26. housing extend the sensor tip about 1 cm from the glass housing and fix the glass fiber again with the protection tubing WHEN THE GLASS FIBER WITH ITS SENSOR TIP IS PUSHED OUT HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK 8 Ensure that the sensor tip is dipped about 4 mm into the calibration solution 0 but not the protective glass housing If the glass housing has been dipped into cal 0 by mistake please wash the glass fiber and the glass housing with distilled water to avoid salt crystallization within the housing Salt crystallization may seal the housing and the glass fiber with its sensor tip will break when extended Calibration 57 4 salt Ep 9 Wait about 30 s until the phase angle is constant the variation of the phase angle should be smaller than 0 055 and press the Store current value button to store the 096 air sat and temp at 0 values A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration Menu 2 Point calibration without temperature sensor atm pressure 1013 mbar 1st point D air sat 2nd point temperature phase 100 air sat aga zio fo aje af Store current value amplitude phase A Finish X Cancel This will overwrite the exsisting calibration values 10 Afterwards wash the sensor tip with distilled water to
27. into the vessel containing the calibration solution 100 cal 100 Connect a syringe to the other female Luer Lock adapter and fill the syringe slowly with calibration solution 100 Please ensure that there are no air bubbles located in the T connector around glass fiber with its sensitive tip Ensure that the temperature sensor has been dipped into the calibration solution cal 100 and that there are no temperature differences between the calibration vessel and the flow through cell Wait about 30 s until the phase angle and the temperature value is constant the variation of the phase angle and the temperature should be smaller than 0 05 and 0 2 C respectively and press the Store current value button to store both the 100 air sat and its temperature temp at 100 Afterwards press the calibration solution back the waste A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data 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 T connector around glass fiber with its sensitive tip Ensure that the temperature sensor has been dipped into the calibration solution cal 0 Wait about 30 s until the phase angle and the tem
28. of oxygen in air Oxygen partial pressure in air saturated water and water vapor saturated air p O Pam Pw T 0 2095 13 Temperature variations strongly affect water vapor pressure and thus influence the oxygen partial pressure as shown in equation 13 Table 13 1 Variation of water vapor pressure pw T with temperature 25 298 817 A convenient fitting function is given by the Campbell equation 14 B Pw T exp E ae 14 where T is the temperature in Kelvin and A B and C constants given in Figure 13 7 Appendix 80 120 T p T exp 52 57 6690 9 T 4 681 InT R 1 100 E t 80 A 52 57 B 6690 9 60 C 4 681 z a 40 20 0 272 217 282 287 292 297 302 307 312 317 322 T K Figure 13 7 Variation of water vapor pressure with temperature F is the square of the correlation coefficient 13 3 2 Bunsen Absorption Coefficient The solubility of oxygen in water is temperature dependent and can be described using the Bunsen absorption coefficient a 0 and the oxygen partial pressure p Oz according to equation 15 With increasing temperature the solubility of oxygen in water decreases p O5 pw TD N c p 0 o 0 15 Cs p 8 temperature dependent solubility of oxygen in water given in cm Oz cm p O2 oxygen partial pressure PN standard pressure 1013 mbar o 0 Bunsen absorption coefficient given in cm Oz cm Table 13 2 Variation of Bunsen a
29. problem with the Microx TX3 oxygen meter please contact our service team and have the software and instrument information ready To change back to the graphical window click the Measure Chart button Instrument Info MEASURE CHART INFO IDENTIFICATION PHIboard number 20020072 PM number 20020053 Serial number TX3 AOT opt18 03 004 MUX channel OFF 00 PARAMETERS Signal LED current 170 Ref LED current 175 Ref LED amplitude 73856 Frequency 005 Sending interval 0001 Averaging 3 Internaltemp 24 4 C SYSTEM SETTINGS APL function ON Temp compensation ON ch a Analog out chAtchBt R8232 echo ON Oxygen unit 96a s Print Info Software Info SOFTWARE VERSION OxyView TX3 V5 31 02 2004 PreSens Precision Sensing GmbH Josef Engert Strasse 9 D 93053 Regensburg Phone 49 0 941 94 2720 Fax 49 0 941 94 272 27 eMail info presens de Internet www presens de Software 26 LED Intensity With the current of the LED you can adjust the amount of light illuminating the sensor spot You can choose between an Auto Adjust of the LED where the Microx TX3 adjusts the optimal LED current itself or you can select Advanced where you can adjust the LED current yourself If you increase the LED current the signal amplitude increases since a higher light density illuminates the sensor spot Auto Adjust To make the adjustment of the LED intensity automatically j
30. 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 Undo Zoom button in the display menu under zoom 6 2 4 Status Bar COMI C Eigene Dateien Microx T gt lt 3 txt start 11 24 34 11 24 49 p Sw1 sw2 sw3 sw4 sw1 Displays the serial port which is used for communication of the Microx TX3 device with the PC Sw2 Displays the file name in which the measurement data are stored No storage file selected is displayed if no file was selected no data storage Sw3 Displays the start time of the measurement sw4 Displays the actual time 6 3 Subsequent Data Handling In the head of the ASCII file you find the description of your measurement which you have entered by storing the file Below you find the instrument info containing the data of the complete calibration routine and some more important settings of the instrument and firmware The software info below contains the version number of the Microx TX3 software date and time of the performed measurement If there is a problem with the Microx TX3 oxygen meter please contact our service team and have the software and instrument information ready Below you find the measure mode settings containing the dynamic averaging and the measuring mode The following rows separated by semicolons list the measuring data The first two rows contain the date
31. to store the 0 air sat value at the adjusted temperature A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration 39 Calibration Menu 2 Point calibration without temperature sensor atm pressure DE mbar 1st point phase D air sat f7 ps temperature 2nd point phase temperature i 100 air sat p p zo jo zie J Store current value amplitude phase A Finish X Cancel This will overwrite the exsisting calibration values X Cancel Afterwards wash the glass fiber with its sensor tip with distilled water to clean it from sodium sulfite Do not retract the sensor tip back into the protective syringe needle Exchange the calibration solution 0 with an identical vessel filled with distilled water Make sure not to touch the sensor tip Dip the sensor tip about 4 mm into the washing solution Afterwards retract the glass fiber back into the protective syringe needle without absorbing water To record the second calibration value water vapor saturated air place the calibration standard 100 containing wet cotton wool below the microsensor The vessel with the label cal 100 has to be closed by the screw top containing the two holes Make sure that the glass fiber is not extended Insert the syringe needle through one of the holes until it is about 1 cm deep insi
32. 2 Point calibration with temperature sensor atm pressure 1013 T mbar 4st point phase temperature 0 air sat fe fea j po p f Store current value 2nd point phase 100 air sat pes doo amplitude phase temperature a Einish 3 Cancel Calibration Message X This will overwrite the exsisting calibration values X Cancel 13 Now calibration with temperature compensation is complete Confirm the calibration values by clicking the Finish button 14 Pull the glass fiber with its sensor tip back into its protective glass housing before removing the microsensor from the calibration vessel Calibration 62 7 3 5 Manual Calibration A manual calibration should be applied if you do not want to calibrate your sensor again However this is only possible if you already know the calibration values of the special sensor Connect the Microx TX3 via the RS232 cable to your computer 2 Switch on the Microx TX3 oxygen meter 3 Start the Microx TX3 software on your computer and click the Calibration menu item 4 Select the calibration routine calibrate manually by clicking the manual button Measurement Calibration calibrate with temperature sensor calibrate without temp sensor calibrate manually 5 Enter the atmospheric pressure at which calibration was performed not the actual one and the respective calibration values 096 air sat temp at 096 a
33. 3 1 4 Luminescence Decay Time etti hee RR Hae 76 13 1 5 Literat r6 inue detenti e edente penu 77 13 2 Oxygen Conversion Formulas cccccccssecceeeceeeseeeseeeseseeeeneeeeseaeseseaeenseeeeeeeeeseaeseseeeeneeeeneas 78 13 3 Temperature Dependent Constants Affecting the Oxygen Content 79 13 3 1 Water Vapor Pressure in PR CREE Ee Ete pre Ras eo eres 79 13 3 2 Bunsen Absorption Coefficient esssessssssssseeseseeeee enne enne nnne nennen nnne nnne 80 13 3 3 Dependence on the Salt Concentration enne 84 1 Preface Congratulations You have chosen a new innovative technology for measuring oxygen The Microx TX3 is a precise single channel temperature compensated oxygen meter specially developed for very small fiber optic oxygen microsensors tip diameter 50 um The small outer dimensions low power consumption and a robust box make it ready for indoor and outdoor applications The Microx TX3 was specially developed for very small fiber optic oxygen microsensors It is based on a novel technology which creates very stable internally referenced measured values This enables a more flexible use of oxygen sensors in many different fields of interest Optical oxygen microsensors also called optodes have the following outstanding properties e They do not consume oxygen e Their signal does not depend on the flow rate of the sample e Diameter of the microsensor tip is lt
34. 4 92 90 21 8 90 88 87 8 83 8 80 7 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 4 24 41 39 438 36 835 33 32 30 28 27 25 25 25 4 22 1 19 18 1 15 4 12 N 26 11 09 08 06 05 03 02 00 99 98 96 27 7 96 95 9 92 90 89 88 86 85 83 8 28 8 8 79 B 77 75 74 BZB 7 70 29 69 67 66 6 63 6 amp 2 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 34 832 83 8 32 30 29 28 26 25 24 23 21 20 19 48 33 18 17 145 14 18 12 11 09 08 07 06 34 06 05 04 02 o 00 99 98 97 94 35 6 94 93 92 091 90 89 88 87 8 84 83 36 83 82 81 80 79 78 77 75 74 78 72 37 72 71 70 69 68 67 66 65 64 6 amp 3 6 38 61 60 59 58 57 56 55 54 53 52 5 39 51 50 49 48 47 46 45 44 43 42 y 40 41 40 39 38 37 36 35 34 33 32 8 Example cs 20 0 C 9 08 mg L Appendix 84 13 3 3 Dependence on the Salt Concentration Table 13 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
35. 7 for the same temperature agree within 0 5 96 The Bunsen absorption coefficient however is not a very practical measure Values of a 0 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 9 in air saturated water at a temperature 0 of 20 C Equation 17 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 T and the vapor pressure pw T at the particular temperature are known Equation 16 or 17 can be used to obtain a and pw can be calculated from equation 14 The oxygen content cs of air saturated water can be calculated according to M c p 0 Pan Pw 95095 a9 18 Pn M In equation 18 pam is the actual atmospheric pressure corrected for the contribution of the water vapor pressure Pw and related to standard pressure pw The corrected pressure is multiplied by 0 2095 the volume content of oxygen in air by a 0 and by the molecular mass of oxygen Moz divided by the molar volume Vy Appendix 82 At a given atmospheric pressure of 1013 mbar Paim pn and a temperature of 20 C the oxygen content can be calculated according to equation 19 and results in 1013 23 3 32 g mol c 1013mbar 20 C 0 2095 0 031 0 009g L 9 06 mg L 19 1013 22414mol L Table 13
36. Select the calibration routine calibrate manually and click the manual button Measurement Calibration calibrate with temperature sensor calibrate without temp sensor calibrate manually 5 Enter the atmospheric pressure at which calibration was performed not the actual one and the respective calibration values 096 air sat temp at 096 and 100 96 air sat temp at 10096 Calibration Menu 2 Point calibration user defined atm pressure 1013 mbar 4st point phase temperature D air sat oe jea r jee je ze 2nd point phase temperature 100 airsat 2428 oz 2p Spo je iv 6 Now user defined calibration is complete Confirm the calibration values by clicking the Finish button A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration Message x This will overwrite the exsisting calibration values X Cancel Calibration 53 7 3 Calibration of Implantable Oxygen Microsensors 7 3 1 Preparation of the Calibration Standards Calibration of microsensors is performed using conventional two point calibration in oxygen free water cal 0 and water vapor saturated air cal 100 Preparation of calibration solution 0 oxygen free water 1 Add 1 g sodium sulfite Na2S03 to a vessel and label it cal 0 2 Dissolve Na SOsin 100 mL water
37. 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 water is not supersaturated 7 2 2 Mounting the Flow Through Housed Oxygen Microsensors 1 Remove the flow through housed microsensor carefully from the protective cover The microsensor is integrated in a sleeve consisting of Teflon tightened with a silicone rubber which is mounted to a T connector The sleeve is protected with a plastic cap screwed to the T connector The T connector has two female Luer Lock adapters for connection with plastic tubings Calibration 46 fiber cable protective cap Teflon sleeve with integrated glass fiber tightened with a silicone rubber male fiber plug end pieces connected to the female Luer Lock adapters of the T connector 2 Fix the microsensor with a clip to a laboratory support or a similar stable construction 3 Remove the two red end pieces from the T connector and connect the female Luer Lock adapters with the tubings of your flow through system 4 Remove the protective cap from the male fiber plug and connect it to the ST plug of the Microx TX3 device The female fiber plug of the Microx TX3 has a groove in which the spring of the male fiber plug of the microsensor has to be inserted The safety nut must be carefully attached while turning and is locked by turning slightly clockwise Be careful not to snap off t
38. a left click on the stop button in the control bar Warning Lights At the right bottom of the window you can find the amplitude phase angle and three warning lights The warning lights are explained below Ge amplitude Ge phase amplitude red Amplitude is too low the sensor tip may be damaged or the sensor cable may not be connected yellow Amplitude is critically low replacement of the sensor is recommended green amplitude is correct phase red phase angle is out of limits green phase angle is in normal range ambient light red background light e g direct sunlight lamp is too high Decrease of false light is recommended green ratio of sensor signal to false light is acceptable By clicking the Display Raw Values button the raw data of phase angle and amplitude are displayed next to the warning lights amp amplitude 31059 phase 27 66 ambient light 6 2 3 Graphical Window The respective sensor signal is displayed according to the selection of the 4 control buttons oxygen phase amplitude and temperature menu chart 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 can also be displayed by clicking the button Display Raw values 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
39. and fill the syringe Press the washing solution into the waste not back into the vessel Repeat this washing procedure 3 times 7 2 4 Calibration with Automatic Temperature Compensation 1 Connect the Microx TX3 via the RS232 cable to your computer 2 To perform temperature compensated measurement connect the temperature sensor PT 1000 to the 4 pin connector on the front panel of the Microx TX3 3 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 2 2 Mounting the Flow Through Housed Microsensors 4 Start the Microx TX3 software on your computer and click the calibration menu item 5 Select the calibration routine calibrate with temperature sensor by clicking the cal button Measurement Calibration calibrate with temperature sensor cal calibrate without temp sensor calibrate manually manual 6 Enter the actual atmospheric pressure 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 mol L Please note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentration units mg L umol L but the oxygen units 96 air saturation and 96 oxygen saturation have to be corrected for air pressure changes 10 Calibration 50 Connect one of female Luer Lock adapters with a plastic tubing which dips
40. asurement 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 e they are more sensitive than conventional electrodes up to ppt range e long term stability and low drift e using silica fibers it is possible to measure in samples while physically separate from the light source and detectors e light conducting fibers 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 13 1 4 Luminescence Decay Time The Fibox 3 measures the luminescence decay time of the immobilized luminophore as the oxygen dependent parameter t f O2 2 The Fibox 3 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 is shown by the following equation tan 2n T uod a tan 2r fma T 3b t tan O f O2 3c 1 luminescence d
41. at 2 72 0 01 mg L ppm 250 1 8 air sat 9 06 0 04 mg L ppm 0 21 0 01 oxygen 22 65 0 17 mg L ppm 6 3 0 03 oxygen 20 9 0 09 oxygen 52 4 0 38 oxygen 1 55 0 08 Torr 46 7 0 20 Torr 2 83 0 14 umol 155 5 0 65 Torr 85 0 0 3 umol 388 8 2 65 Torr 283 1 1 3 umol 2 0 1 hPa 798 0 5 2 umol 60 0 26 hPa 200 0 87 hPa 500 3 54 hPa Accuracy 20 C 1 at 100 air saturation 0 15 at 1 air saturation Temperature Microsensors can be used in the temperature range of 10 to 80 C PreSens offers a PT 1000 temperature sensor in combination with the Microx TX3 to record temperature variations which are compensated using the Microx TX3 software see Chapter 7 Calibration and Chapter 8 Measurement Cross sensitivity No cross sensitivity exists for carbon dioxide COz hydrogen sulfide H2S ammonia NHs pH any ionic species like sulfide S sulfate SO chloride CI or salinity Turbidity and changes in the stirring rate have no influence on the measurement The sensors can 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 Fiber Optic Oxygen
42. ble to set the right com port Please confirm your selection by clicking the OK button The information window disappears if the right com port is adjusted Select COM Port CINMNNENENN TN 6 2 Function and Description of the Microx TX3 Program The window shown below is displayed after starting the software TX3v531 exe The program has 4 main sections 1 Menu bar 2 Graphical window 3 Status bar 4 Control bar divided into numerical display control buttons and warning lights OxyView TX3 V5 31 File Charts Display Print Settings OXYGEN h airsatur v Measurement Calibration Start Measurement Sampling Rate Logging Status A Dianav Raw valies start time 00 00 00 warning lights numerical display amplitude phase control bar MEASURE CHART iNFO i i r i i i o M a MF a a d alae graphical window aA E E M SiL n measurement time Comi No File selected start 00 00 00 21 53 53 WS Software 24 6 2 1 Menu Bar File Charts Display Settings gt Exit gt Oxygen Zoom 2 Charts Com Port gt AutoScaleY1 gt Undo Zoom gt Phase gt Instrument Info gt Amplitude gt Clear Charts gt Analog settings gt Temperature Dimensions gt LED Intensit File Exit Closes the program Charts The respective charts of the measurement can be displayed Y o
43. bsorption coefficient a 0 with temperature epc o 5 20 30 so 50 a 0 10 49 01 42 94 38 11 34 17 31 01 28 43 26 30 23 16 20 85 The data in Table 13 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 13 2 A fourth degree polynomial fit can be chosen yielding equation 16 10a 2a cb 0 cc 0 d 0 amp e 0 16 where 0 is the temperature in C and a e the coefficients calculated by standard curve fitting procedures as given in Figure 13 8 Appendix 81 50 0 0 10 48 998 1 335 0 2 755 10 0 3 220 10 0 1 598 10 0 a 48 998 b 1 335 407 c 2 755 10 x d 3 220 104 fan e 1 598 10 4 3 30 20 0 5 10 15 20 30 35 40 45 50 25 0 C Figure 13 8 Variation of Bunsen absorption coefficient a 0 with temperature Ff is the square of the correlation coefficient The other form of equation to describe the variation of o with temperature can be derived from a thermodynamical correlation and gives an equation of the form nio S B InT C 17 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 of a in Table 13 2 that A 8 553 10 B 2 378 10 and C 1 608 10 Values of a calculated from eqns 16 and 1
44. can be readily made using equation 20 S 1 805 CI 0 03 20 where S is the salinity in o or g 1000g Table 13 4 Solubility of oxygen in water as a function of temperature and salt concentration Total pressure 760 torr T C Oxygen solubility mort CI g 1000g 0 7 0 14 5 13 9 13 3 12 6 10 11 3 11 3 10 8 10 4 8 5 8 1 Oo 78 7 0 6 7 6 4 The effect of increasing the salt concentration on the vapor pressure is negligible small as shown in Table 13 5 Table 13 5 Variation of solution vapor pressure pw with salt concentration Vapor pressure of solution torr The dependence of oxygen solubility on salt concentration can also be obtained from equation 14 except that now values calculated from either equation 21 or 22 have to be used for calculation of the Bunsen absorption coefficient Equation 21 differs from equation 16 by an additional forth degree polynomial term for chlorinity 10 a a b 0 c 0 d 0 e 6 Cl p q 0 r 0 s 6 t 6 21 where 0 is the temperature in C a e are the coefficients used in equation 16 and p t are new constants given in Table 13 6 The values of these new constants are obtained by fitting the polynomial to experimental data in the ranges 0 lt 0 lt 30 C and 0 lt CI lt 20 To obtain an oxygen solubility from the Bunsen absorption coefficient the same procedure as described previously is used s equation 18 page 74 An alternative equation to com
45. clean it from sodium sulfite Make sure not to touch the sensor tip Retract the glass fiber back into the protective glass housing without absorbing water 11 To record the second calibration value water vapor saturated air place the calibration standard 100 containing wet cotton wool below the microsensor The vessel with the label cal 100 has to be closed with the screw top containing the two holes Make sure that the glass fiber is not extended Insert the glass housing through one of the holes until it is about 1 cm deep inside the vessel Make sure that the glass fiber with its sensor tip does not touch the cotton wool when extended Slacken the protection tubing from the glass housing extend the sensor tip about 1 cm from the glass housing and fix the glass fiber again with the protection tubing Calibration 58 Wait about 30 s until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and click the Store current value button to store the 10096 air sat value at the adjusted temperature A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data 12 Now calibration is complete Confirm the calibration values by clicking the Finish button 13 Pull the glass fiber with its sensor tip back into its protective glass housing before removing the microsensor from the calibratio
46. crosensors Start the Microx TX3 software on your computer and click the calibration menu item Select the calibration routine calibrate with temperature sensor by clicking the cal button Calibration 41 Measurement Calibration calibrate with temperature sensor oca calibrate without temp sensor cake calibrate manually manual 6 Enter the actual atmospheric pressure The atmospheric pressure of the calibration is needed to convert the oxygen unit 96 air saturation in partial pressure units hPa Torr or concentration units mg L mol L Please note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentration units mg L mol L but the oxygen units 96 air saturation and 96 oxygen saturation have to be corrected for air pressure changes Calibration Menu 2 Point calibration with temperature sensor atm pressure 1013 T mbar 1st point temperature phase D air sat ps fes 2 po fp C A Store current value temperature 2nd point phase s 100 air sat ps joo po foe amplitude phase temperature NE me SA Einish X Cancel 7 Place the vessel with the label cal 0 underneath the microsensor see picture below Please ensure that the sensor tip is not extended Locate the syringe needle carefully about 5 mm above the water surface Slowly press the syringe plunger and extend the sensor tip from its protectiv
47. d Venflon tubes Fiber cables with a length up to 10 m and an outer diameter of 0 9 mm are available If you need a more robust cable o d 3 1 mm or a cable length of more than 10 m maximum 60 m please contact our service team info presens de Features e High spatial resolution e High flexibility e Without any housings the microsensor is protected with a glass housing during the transport e Sterilizable H202 EtOH ethylene oxide EtO e Autoclavable 130 C 266 F 1 5 atm e Implantation into animal blood circuits e Soil implantation e Implantation in customer made housings e Measuring range from 0 to 250 air saturation 0 22 6 mg L e Limit of detection 0 2 air sat 20 umol L Schematic drawing of implantable microsensors ST connector sensor tip A sensor tip outer plastic cable male fiber plug 140 um bare glass outer plastic cable fiber inner plastic cable Fiber Optic Oxygen Microsensors 21 Ordering Information Limp H est uc Hec Lor IMPlantable Length of Bare glass fiter length Housing Glass Fiber 3 to customer request 2 5m Optical isolation 280 Y with opt isolation Oxygen sensitive Length of inner Shape of Sensor Tip N without opt coating PSt1 plastic cladding S sharp tip 50 um isolation 0 250 air sat 0 to customer request F flat broken tip 140 um Example With the order code IMP PSt1 L5 LIC 1 BGF 3 TF YOP you w
48. de the vessel Make sure that the glass fiber with its sensor tip does not touch the cotton wool when extended Extend the sensor tip wait about 30 s until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and click the Store current value button to store the 100 air sat value at the adjusted temperature Again a message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data 10 11 12 Calibration 40 Now calibration is complete Confirm the calibration values by clicking the Finish button Pull the sensor tip back into its protective syringe needle before removing the microsensor from the calibration vessel Protect the syringe plunger against slipping out by inserting the transport block back into the syringe housing and do not remove it again until just before measurement 7 1 4 Calibration with Automatic Temperature Compensation 1 2 Connect the Microx TX3 via the RS232 cable to your computer To perform temperature compensated measurement connect the temperature sensor PT 1000 to the 4 pin connector on the front panel of the Microx TX3 Fix the temperature sensor and make sure that neither the temperature sensor nor its cable can touch the microsensor Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 1 2 Mounting the Needle Type Mi
49. e sensor nor its cable can touch the microsensor Remove the microsensor carefully from the protective cover The microsensor is protected with a glass housing during the transport Fix the glass housing microsensor with a clip to a laboratory support or a similar stable construction Calibrate the sensor according to chapter 7 3 Calibration of Implantable Oxygen Microsensors If you do not want to re calibrate the sensor but use the calibration values of your last measurement choose Manual Calibration which is described in chapter 7 3 5 The glass fiber with its sensing tip is prevented from slipping from the glass housing using a protection tubing Remove the fiber cable from the glass housing for implantation Slacken the protection tubing from the glass housing and carefully extract the glass Be careful not to touch the glass housing with the glass fiber tip WHEN THE GLASS FIBER WITH ITS SENSOR TIP IS EXTRACTED FROM THE PROTECTIVE HOUSING HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK Be careful while implanting the microsensor into your specially designed system Please contact our service team for custom designed systems Please rinse the glass fiber with its sensor tip with distilled water after removing it from the sample to remove any sample residues Retract the sensor tip into the protective housing and insert the transport block to prevent the syringe plunger from slipping Measurement 65 8 4 Some Adv
50. e syringe needle Ensure that the sensor tip is dipped about 4 mm into the calibration solution 0 but not its protective syringe needle Ensure that the temperature sensor has been dipped about 1 2 cm into the calibration solution If the needle has been dipped into cal 0 by mistake please wash it with distilled water to avoid salt crystallization within the syringe needle Salt crystallization may seal the syringe needle and the glass fiber with its sensor tip will break when extended Calibration 42 salt Sedad 8 Wait about 30 s until the phase angle and the temperature value are constant the variation of the phase angle and the temperature should be smaller than 0 05 and 0 2 C respectively and press the Store current value button to store both the 0 air sat and the temperature temp at 0 A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration Message X This will overwrite the exsisting calibration values X Cancel 9 Afterwards wash the sensor tip with distilled water to clean it from sodium sulfite Do not retract the glass fiber back into the protective syringe needle Exchange the calibration solution O with an identical vessel filled with distilled water Make sure not to touch the glass fiber Dip the sensor tip about 4 mm into the washing solution Afterwards ret
51. ecay time o phase angle fmoa modulation frequency Appendix 77 I 5 0 5 10 15 20 25 30 time ps Figure 13 5 Schematic of the single exponential decay to gt t 5 0 5 10 15 20 25 30 time us Figure 13 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 measurement of the luminescence decay time an intrinsically referenced parameter has the following advantages compared to the conventional intensity measurement e The decay time does not depend on fluctuations in the intensity of the light source and the sensitivity of the detector e 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 gt photobleaching and leaching of the indicator dye has no influence on the measuring signal e The decay time is not influenced by variations in the optical properties of the sample including turbidity refractive index and coloration 13 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
52. eded to convert the oxygen unit air saturation into partial pressure units hPa Torr or concentration units mg L mol L Please note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentration units mg L umol L but the oxygen units 96 air saturation and 96 oxygen saturation have to be corrected for air pressure changes Calibration Menu 2 Point calibration without temperature sensor atm pressure 1013 mbar 1st point phase temperature O air sat po fo zo jo ze J Store current value 2nd point 100 air sat amplitude phase A Finish X Cancel 6 Connect one of the female Luer Lock adapters with a plastic tubing which dips into the vessel containing the calibration solution 100 cal 100 Connect a syringe to the other female Luer Lock adapter and fill the syringe slowly with calibration solution 100 Please ensure that there are no air bubbles located in the T connector around glass fiber with its sensitive tip Calibration 48 Wait about 30 s until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and press the Store current value button to store the 10096 air sat value at the adjusted temperature Afterwards press the calibration solution into the waste A message window opens and informs you that you will overwrite the existing calibration values Click the Co
53. ensor has been dipped about 1 2 cm into the calibration solution The glass fiber with its sensing tip is prevented from slipping using a protection tubing Slacken the protection tubing from the glass housing extend the sensor tip about 1 cm from the glass housing and fix the glass fiber again with the protection tubing WHEN THE GLASS FIBER WITH ITS SENSOR TIP IS PUSHED OUT HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK Ensure that the sensor tip is dipped about 4 mm into the calibration solution 0 but not the protective glass housing 10 11 12 Calibration 60 If the glass housing has been dipped into cal 0 by mistake please wash the glass fiber and the glass housing with distilled water to avoid salt crystallization within the housing Salt crystallization may seal the housing and the glass fiber with its sensor tip will break when extended salt EE Wait about 30 s until the phase angle and the temperature value are constant the variation of the phase angle and the temperature should be smaller than 0 05 and 0 2 C respectively and press the Store current value button to store both the 0 air sat value and its temperature temp at 0 A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Afterwards wash the sensor tip with distilled water to clean it from sodium sulf
54. ensor tip 0 0 20 40 60 80 100 120 140 time s Figure 5 3 Comparison of the response characteristics of a microsensor with a sensor tip tapered 50 um and a microsensor with a flat broken sensor tip Z 140 um Table 5 3 Response times teo of the oxygen microsensors Dissolved oxygen Gaseous oxygen Response time too for tapered sensors tip diameter lt 50 um 1 s lt 5 s with optical isolation 0 5 s 1 s with optical isolation flat broken sensors tip diameter 150 um 15 s 30 s with optical isolation lt 5 s 10 s with optical isolation Optical isolation Optically 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 optically 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 Optically 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 PreSens offers additional optical isolation for all types of oxygen sensors Fiber Optic Oxygen Microsensors 12 Sens
55. erature compensated measurement Immerse the temperature sensor in your sample and fix it with a laboratory support Calibrate the sensor according to chapter 7 2 Calibration of Flow Through Housed Oxygen Microsensors If you do not want to re calibrate the sensor but use the calibration values of your last measurement choose Manual calibration which is described in chapter 7 2 5 Connect the end pieces of the T connector with Luer Lock tubings obtained by novodirect B13323 B13312 B13316 B13303 or Luer Lock adapters for tubings obtained by novodirect B95900 B95908 B95919 and pump your sample through the flow through cell Please rinse the glass fiber with its sensor tip with distilled water after removing it from the sample to remove any sample residues Pump distilled water through the cell until all sample residues are removed 8 3 Measurement with Implantable Oxygen Microsensors 1 Please carefully read chapter 7 3 Calibration of Implantable Oxygen Microsensors in the manual instructions There you will find relevant information about the proper handling of microsensors They are the basic for the following chapter Connect the Microx TX3 via the RS232 cable to your computer Connect the temperature sensor PT 1000 to the 4 pin connector on the front panel of the Microx TX3 and carefully tighten the safety nut to perform temperature compensated measurement Fix the temperature sensor and make sure that neither the temperatur
56. fast sampling mode is about 250 ms when no temperature sensor is connected and decreases to about 350 ms when connecting a temperature sensor or activating the analog output channels Software 30 Please note The sensor shelf life can be increased using a slower measuring mode since the effect of photobleaching is reduced The illumination light is switched off between sampling A further advantage using a high measuring mode is that huge amounts of data for long time measurement can be avoided Dynamic averaging 5 The dynamic average defines the number of averaged measured Dynamic Averaging values The higher the running average the longer the time sampling time used for averaging The higher the running average is set the a samples smoother the measurement signal maximum 25 samples The default setting is 4 Temperature compensated oxygen measurements If you want to measure with temperature compensation click the orr button Please ensure that the temperature sensor PT 1000 is connected to the Microx TX3 before you click the Start button to continue The window where you can enter the temperature manually is disabled Temperature Compensation C off Enter the temperature during the measurement 4e fo ile If you want to measure without temperature compensation choose the off button Please enter the temperature of your measurement sample manually Click the Start button to start the meas
57. he fiber cable male fiber plug Calibration 47 7 2 3 Calibration without Automatic Temperature Compensation Using the software you can choose whether to perform the measurement and calibration with or without temperature compensation If you want to perform the calibration without automatic temperature compensation please ensure that the delivered temperature sensor PT 1000 is not connected to the Microx TX3 Please note Calibration without temperature compensation only makes sense if there is no temperature change during the calibration of the oxygen microsensor 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 1 Connect the Microx TX3 via the RS232 cable to your computer 2 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 2 2 Mounting the Flow Through Housed Microsensors 3 Start the Microx TX3 software on your computer and click the calibration menu item 4 Select the calibration routine calibrate without temp sensor by clicking the cal button Measurement Calibration calibrate with temperature sensor calibrate without temp sensor calibrate manually 5 Enter the actual atmospheric pressure and the temperature of the calibration standards The atmospheric pressure of the calibration is ne
58. he partial pressure units hPa Torr and concentration units mg L uimol L but the oxygen units 96 air saturation and oxygen saturation have to be corrected for air pressure changes Calibration Menu 2 Point calibration without temperature sensor atm pressure 1013 mbar 4st point phase temperature D air sat fs o d zl fo FC af Store current value 2nd point phase temperature 100 air sat p d i 20 jo aie amplitude phase A Finish X Cancel 6 Place the vessel with the label cal 0 underneath the microsensor Please ensure that the glass fiber with its sensor tip is not extended Locate the syringe needle carefully about 5 mm above the water surface Slowly press the syringe plunger and extend the glass fiber with its sensor tip from the protective syringe needle Calibration 38 Ensure that the sensor tip is dipped about 4 mm into the calibration solution 0 but not the protective syringe needle If the syringe needle has been dipped into cal 0 by mistake please wash the glass fiber and the syringe needle with distilled water to avoid salt crystallization within the syringe needle Salt crystallization may seal the syringe needle and the glass fiber with its sensor tip will break when extended salt E Wait about 30 s until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and press the Store current value button
59. ice for Correct Measurement 8 4 1 Signal drifts due to oxygen gradients Please take into account that the sensor has a high spatial resolution An oxygen gradient occurs most times in unstirred solutions which are in contact with ambient air In case of needle type sensors check first if the tip is completely extended from the needle or if air bubbles are on the sensor tip whenever unexpected drifts gradients or unstable measurement values occur In case of flow trough cells air bubbles located at the sensor tip cause signal drifts 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 also lead to an oxygen gradient 8 4 2 Signal drifts due to temperature gradients A further source of imprecise measurement is insufficient temperature compensation If you use the temperature compensation ensure that no temperature gradients exist between the microsensor and the temperature sensor If you measure without temperature compensation please bear in mind that the Microx TX3 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 13 5 Formulas for temperature compensation If the temperat
60. ill order an implantable IMP microsensor type PSt1 mounted in a glass housing The outer plastic cable with a diameter of 900 um is 5 m long L5 the inner plastic coating 600 uim 1 cm LIC 1 and a bare glass fiber length 140 um of 3 mm BGF 3 The sensor tip that is flat broken TF containing the oxygen sensitive fiber tip with additional optical isolation YOP 6 Software This software is compatible with Windows 95 98 2000 Millenium NT4 0 XP 6 1 Software Installation and Starting the Instrument 1 Insert the supplied disc CD into the respective drive Copy the file TX3v531 exe onto your hard disk for example create CAMICROXTX TX3v531 exe Additionally you may create a link Icon on your desktop 2 Connect the Microx TX3 via the supplied serial cable to a serial port of your computer Tighten the cable with the screws on your computer and on the Microx TX3 3 Connect the power supply 4 Please close all other applications as they may interfere with the software Start the program TX3v531 exe with a double click The following information window appears Connect the instrument to the PC waiting 5 Ifthe right com port is adjusted this information window disappears within a few seconds If the wrong com port is adjusted you are asked to set the right com port Connect the instrument to the PC waiting ss And choose the right com port With a right mouse click onto com port you are a
61. iption of the Microx TX3 Device The Microx TX3 is a precision temperature compensated oxygen meter designed for fiber optic oxygen microsensors The small outer dimensions low power consumption and a robust box make it ready for indoor and outdoor application For data visualization and storage the instruments have to be connected to a PC computer Microx TX3 instruments features e high precision e portable battery power optional e analog digital data output on request e temperature compensation There also exists the possibility to combine several single Microx TX3 oxygen meters to obtain a multichannel system It allows the user to create a 2 3 4 or more channel system up to 8 channels The Microx TX3 oxygen meter contains a dual 12 bit analog output and an external trigger input The analog output values can be programmed with the PC software included The user can choose between oxygen temperature amplitude or phase for each channel independently Microx TX3 can be used as a stand alone instrument when combined with an external data logger Description of the Microx TX3 Device 5 Front Panel ELEMENT DESCRIPTION FUNCTION S1 ON OFF switch Switches the device ON and OFF C1 ST fiber connector Connect the fiber optic oxygen microsensor here L1 Control red instrument off LED green instrument on orange stand by Temp Connector for PT 1000 Connect the PT 1000 temperature sensor for temperature
62. ite Make sure not to touch the sensor tip Retract the glass fiber back into the protective glass housing without absorbing water Also wash the temperature sensor by dipping it into water To record the second calibration value water vapor saturated air place the calibration standard 100 containing wet cotton wool below the microsensor The vessel with the label cal 100 has to be closed with the screw top containing the two holes Make sure that the glass fiber is not extended Insert the glass housing through one of the holes until it is about 1 cm deep inside the vessel Insert the temperature sensor through the other hole and make sure that it does not touch the microsensor Make sure that the glass fiber with its sensor tip does not touch the cotton wool when extended Slacken the protection tubing from the glass housing extend the glass fiber with its sensor tip about 1 cm from the glass housing and fix the glass fiber again with the protection tubing Wait about 30 s until the phase angle and the temperature is constant the variation of the phase angle and temperature should be smaller than 0 05 and 0 2 C respectively and click the Store current value button to store the 100 air sat and temp at 100 values A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data 61 Calibration Calibration Menu
63. ments e g blister packages beverage cans e Easy to handle and robust e Sterilizable H202 EtOH ethylene oxide EtO e Not autoclavable Ordering information esL JI ese Ht LH vL Ips L L HL orl 4 t t Needle Type Length of Stainless Needle Housing with Fixed Glass Fiber Length mm diameter mm oxygen Sensor 2 5m 20 0 4 G for gase phase 5m 40 0 4 Et Ror liquid phase Shape of Sensor Tip 40 0 8 Optical isolation Oxygen sensitive S sharp tip lt 50 um 720 12 _ v with opt isolation coating PSt1 F flat broken tip 140 um 120 0 8 _ N without opt isolation 0 250 air sat Order code for Needle Type Housing with Fixed Oxygen Microsensors NFSx PSt1 Fiber Optic Oxygen Microsensors 18 5 2 3 Flow Through Cell Housed Oxygen Microsensors FTCH PreSens offers miniaturized flow through cells with integrated oxygen microsensors They can be connected via Luer Lock adapters to tubings Liquids water blood can be pumped through the cell Online monitoring in real time is possible male fiber plug Luer Lock adapter sensor tip Luer Lock adapter Features e Easy to handle and robust e Online monitoring e Very fast response time e Sterilizable autoclave 130 C 1 5 atm EtOH H202 e Measuring range from 0 to 250 air saturation 0 22 6 mg L e Limit of detection 0 2 air saturation 20 umol L Schematic drawing of flow through cell housed microsensors Luer Lock
64. microsensor with a clip to a laboratory support or a similar stable construction We expressly warn you not to handle the microsensors without the support especially when the sensor tip is extended 4 Remove the protective cap from the male fiber plug and connect it to the ST plug of the Microx TX3 device The female fiber plug of the Microx TX3 has a groove in which the spring of the male fiber plug of the microsensor has to be inserted The safety nut must be carefully attached while turning and is locked by turning slightly clockwise Be careful not to snap off the fiber cable Calibration 36 male fiber plug 5 The glass fiber with its sensing tip is prevented from slipping using a transport block B Remove the transport block from the hole in the syringe housing Now it is possible to retract or extend the glass fiber with its sensor tip by pushing or pulling the plunger Before pushing out the sensor tip make sure that you have removed the protective plastic cap and have some space in front of the syringe needle 4 transport blocking sensor tip WHEN THE GLASS FIBER WITH ITS SENSOR TIP IS PUSHED OUT HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK Calibration 37 7 1 3 Calibration without Automatic Temperature Compensation Using the software you can choose whether to perform the measureme
65. n vessel 7 3 4 Calibration with Automatic Temperature Compensation 1 Connect the Microx TX3 via the RS232 cable to your computer 2 To perform temperature compensated measurement connect the temperature sensor PT 1000 to the 4 pin connector on the front panel of the Microx TX3 Fix the temperature sensor and make sure that neither the temperature sensor nor its cable can touch the microsensor 3 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 3 2 Mounting the Microsensors 4 Start the Microx TX3 software on your computer and click the calibration menu item 5 Select the calibration routine calibrate with temperature sensor by clicking the cal button Calibration 59 Enter the actual atmospheric pressure 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 note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentration units mg L mol L but the oxygen units air saturation and 96 oxygen saturation have to be corrected for air pressure changes Place the vessel with the label cal 0 underneath the microsensor Please ensure that the sensor tip is in the protective glass housing Locate the glass housing carefully about 5 mm above the water surface Ensure that the temperature s
66. nce 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 Il Os Il and Rh Il and phosphorescent porphyrins containing Pt II or Pd Il as the central atom 13 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 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 aphotodetector photodiode photomultiplier tube CCD array e the optical sensor indicator immobilized in a solid matrix POF polymer optical fiber sensor spot L 2 5 m p SMA connector amm LE gms steel tube Figure 13 3 Scheme of a minisensor Appendix 76 Glasfaser Koppler Minisensor ST LED Figure 13 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 13 1 3 Advantages of Optical Oxygen Sensitive Minisensors e no oxygen is consumed during the me
67. nd 100 96 air sat temp at 10096 Calibration Menu 2 Point calibration user defined atm pressure 013 mbar 4st point phase temperature D air sat oc fes F 0 fp zie 2nd point phase temperature 100 air sat zlps jv r zo je zie X Cancel 6 Now user defined calibration is complete Confirm the calibration values by clicking the Finish button When doing so a message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration Message X This will overwrite the exsisting calibration values X Cancel Measurement 3 8 Measurement Calibration of the microsensor is recommended before each measurement see chapter 7 Calibration of Microsensors f you do not want to recalibrate the microsensor you can use the calibration values of your last measurement see Manual Calibration Each calibration is only valid for the corresponding microsensor and should be repeated before beginning a new measurement Especially after longer measurements more than 18000 measuring points or 5 h continuous sensor illumination the sensor should be re calibrated Ensure that the temperature of the sample is known and is constant during measurement if you do not use temperature compensation In the case of temperature compensated measurements the temperature sensor PT 1000 should be p
68. ndensate 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 must only be carried out by a suitable qualified technician trained by us A 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 e g if the instrument e is visibly damaged e nolonger operates as specified e has been stored under adverse conditions for a lengthy period of time e has been damaged in transport f you are in doubt the instrument should be sent back to the manufacturer PreSens 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 Microx TX3 is not protected against water spray The Microx TX3 is n
69. nsitive Avoid mechanical stress as far as possible 6 The sensor tip will only measure accurately if the glass fiber with its sensor tip has been completely extended from the syringe needle Inside the needle there is an air reservoir in which the oxygen content is different from your sample syringe needle glass fiber SRDIBOI up gas reservoir right position of the sensor tip wrong position of the sensor tip Sensor tip must be outside for measurement There is an air reservoir inside the syringe needle The oxygen and calibration content inside the syringe needle is different from that of the sample since the gas exchange rate is slow 7 Measurement 64 Please rinse the glass fiber with its sensor tip with distilled water after removing it from the sample to remove any sample residues Retract the sensor tip into the protective housing and insert the transport block to prevent the syringe plunger from slipping 8 2 Measurement with Flow Through Housed Oxygen Microsensors Please carefully read chapter 7 2 Calibration of Flow Through Housed Oxygen Microsensors in the manual instructions There you will find relevant information about the proper handling of microsensors They are the basic for the following chapter Connect the Microx TX3 via the RS232 cable to your computer Connect the temperature sensor PT 1000 to the 4 pin connector on the front panel of the Microx TX3 and carefully tighten the safety nut to perform temp
70. nt and calibration with or without temperature compensation If you want to perform the calibration without automatic temperature compensation please ensure that the delivered temperature sensor PT 1000 is not connected to the Microx TX3 Please note Calibration without temperature compensation only makes sense if there is no temperature change during the calibration of the oxygen microsensor 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 1 Connect the Microx TX3 via the RS232 cable to your computer 2 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 1 2 Mounting the Needle Type Microsensors 3 Start the Microx TX3 software on your computer and click the calibration menu item 4 Select the calibration routine calibrate without temp sensor by clicking the cal button Measurement Calibration calibrate with temperature sensor calibrate without temp sensor calibrate manually 5 Enter the actual atmospheric pressure and the temperature of the calibration standards 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 umol L Please note that changes in the actual atmospheric pressure have no effect on t
71. ntinue button to store the new calibration data 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 T connector around glass fiber with its sensitive tip Wait about 30 s until the phase angle is constant the variation of the phase angle should be smaller than 0 05 and click the Store current value button to store the 0 air sat value at the adjusted temperature Afterward press the calibration solution into the waste A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration 49 Calibration Menu 2 Point calibration without temperature sensor atm pressure 1013 mbar 1st point phase temperature 1 D air sat ps a zl Jo ze i 2nd point phase temperature 100 96air sat p pr 5 20 fo zie A Store current value amplitude phase 24681 57 286 af Finish X Cancel This will overwrite the exsisting calibration values 9 Now calibration is complete Confirm the calibration values by clicking the Finish button 10 To wash the glass fiber with its sensor tip with distilled water to clean it from sodium sulfite dip the plastic tubing into a vessel containing distilled water
72. or Stability The oxygen sensitive membrane stands sterilization by ethylene oxide steam autoclavation 140 C 1 5 atm CIP conditions cleaning in place 5 NaOH 90 C as well as a 3 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 microsensor with a tapered and flat broken sensor tip for 1 12 and 24 hours in the continuous mode 1 sec mode Mode Drift per hour Drift per 12 hours Drift per 24 hours 3600 measuring points 43200 measuring points 86400 measuring points tapered sensor tip 0 6 air saturation 1 96 air saturation 31 6 96 air saturation flat broken sensor tip 0 5 96 air saturation 0 5 96 air saturation 0 6 96 air saturation 100 S 80 c 4 9 1 S 6041 aZ 4 n 407 20 1 o He Iaa 0 2 4 6 8 10 12 14 16 18 20 22 24 time h Figure 5 4 Photostability of a tapered oxygen microsensor Fiber Optic Oxygen Microsensors 13 5 2 Housings of Oxygen Sensitive Microsensors PreSens fiber optic oxygen microsensors are based on 140 um silica optical fibers To protect the small glass fiber tip against breaking suitable housings and tubings around it depending on the respective application were designed
73. ors sse 45 7 2 8 Calibration without Automatic Temperature Compensation seen 47 7 2 4 Calibration with Automatic Temperature Compensation sene 49 7 2 5 Manual Galibratiori exe UE uelis 52 7 3 Calibration of Implantable Oxygen Microsensors eene 53 7 3 1 Preparation of the Calibration Standards 53 7 3 2 Mounting the Implantable Microsensors ssseenm nme 54 7 3 8 Calibration without Automatic Temperature Compensation sseeeeee 55 7 3 4 Calibration with Automatic Temperature Compensation eene 58 7 3 5 Manual Calibrationiiccc vee t eee cient eerie ie tere oder es Ghee ees 62 LETS MOTO ai CTS GS MeasuremerLb ie ee T retinal ee eevee 63 8 1 Measurement with Needle Type Oxygen Microsensors eee 63 8 2 Measurement with Flow Through Housed Oxygen Microsensors 64 8 3 Measurement with Implantable Oxygen Microsensors eene 64 8 4 Some Advice for Correct Measurement eee nunne nnnnnn nunne nnne 65 8 4 1 Signal drifts due to oxygen Qradient eecceeeceeeseeeeeeeeeneeeeeeeeaeeeeeeeeeeeeeeseaeeseaeeseaeeseeeteaees 65 8 4 2 Signal drifts due to temperature gradients essssseseeeeeeenene nens 65 8 4 3 Signal drift due to photodecomposition
74. ositioned as close as possible to the microsensor to avoid temperature differences 8 1 Measurement with Needle Type Oxygen Microsensors 1 Please carefully read chapter 7 1 2 Mounting the Needle Type Microsensors and chapters 7 1 3 7 1 4 Calibration of the Microsensor without with Automatic Temperature Compensation in the manual There you will find relevant information about the proper handling of microsensors They are the basic for the following chapter 2 Connect the Microx TX3 via the RS232 cable to your computer 3 Connect the temperature sensor PT 1000 to the 4 pin connector on the front panel of the Microx TX3 to perform temperature compensated measurement Fix the temperature sensor and make sure that neither the temperature sensor nor its cable can touch the microsensor 4 Calibrate the sensor according to chapter 7 1 Calibration of Needle Type Oxygen Microsensors lf you do not want to re calibrate the sensor but use the calibration values of your last measurement choose User Defined calibration which is described in chapter 7 1 5 5 Position the microsensor right above your sample The syringe needle with retracted glass fiber can be punched through a sept or immersed into a tissue Remove the transport block Extend the glass fiber with its sensor tip from the syringe needle by carefully pressing the syringe plunger Please take into account that the fine glass fiber with its sensor tip is mechanically quite se
75. ot water proof The Microx TX3 must not be used under environmental conditions which cause water condensation in the housing The Microx TX3 is sealed The Microx TX3 must not be opened We explicitly draw your attention to the fact that any damage of the manufactural seal will render of all guarantee warranties invalid Any internal operations on the unit must be carried out by personal explicitly authorized by PreSens and under antistatic conditions Safety Guidelines 3 The Microx TX3 may only be operated by qualified personal 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 Microx TX3 and the equipment such as PT 1000 temperature sensor power supply and optical sensors out of the reach of children As the manufacturer of the Microx TX3 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 Microx TX3 and the sensors must not be used for in vivo examinations on humans The Microx TX3 and the sensors must not be used for human diagnostic or therapeutical purposes Description of the Microx TX3 Device 4 3 Descr
76. otective cap from the male fiber plug and connect it to the ST plug of the Microx TX3 device The female fiber plug of the Microx TX3 has a groove in which the spring of the male fiber plug of the microsensor has to be inserted The safety nut must be carefully attached while turning and is locked by turning slightly clockwise Be careful not to snap off the fiber cable male fiber plug Calibration 55 7 3 3 Calibration without Automatic Temperature Compensation Using the software you can choose whether to perform the measurement and calibration with or without temperature compensation If you want to perform the calibration without automatic temperature compensation please ensure that the delivered temperature sensor PT 1000 is not connected to the Microx TX3 Please note Calibration without temperature compensation only makes sense if there is no temperature change during the calibration of the oxygen microsensor 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 1 Connect the Microx TX3 via the RS232 cable to your computer 2 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 3 2 Mounting the Implantable Microsensors 3 Start the Microx TX3 software on your computer and click the calibration menu item 4 Select the calibration routine
77. pensate the Bunsen absorption coefficient by the salt concentration displays equation 22 10 a ex A LC InT4 D T Cl p 24R InT S T 22 5 T T where T is the temperature in Kelvin and A D and P S are the coefficients given in Table 13 6 They are based on measurements for 273 1 x T lt 308 18 K and 0 lt CI lt 30 and is therefore more extensive than equation 21 Both equations give values of 10 a which agree to better than 1 Appendix 85 Table 13 6 Values of the coefficients in equations 21 and 22 Eqn 21 a 4 900 10 p 5 516 10 1 335 q 1 759 10 C 2 759 10 r 2 253 107 d 8 235 10 s 2 654 107 Em Bg ON aa haere alee se ere EO OU TRE Eqn 22 A 7 424 P 1 288 10 B 4 417 10 Q 5 344 10 C 2 927 R 4 442 10 D 4 238 10 S 7 145 10 Seawater has a typical salinity of 35 76 35 g 1000 g or a chloride content of about 19 o and therefore falls within the scope of both equations
78. perature are constant the variation of the phase angle and temperature should be smaller than 0 05 and 0 2 C respectively and click the Store current value button to store the 096 air sat and temp at 0 values Afterwards press the calibration solution into the waste Again a message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data Calibration Calibration Menu amplitude phase temperature Calibration Message 11 Now calibration with temperature compensation is complete Confirm the calibration values by clicking the Finish button 12 To wash the glass fiber with its sensor tip with distilled water to clean it from sodium sulfite dip the plastic tubing into a vessel containing distilled water and fill the syringe Press the washing solution to the waste not back into the vessel Please repeat this washing procedure 3 times Also wash the temperature sensor by dipping it into water Calibration 52 7 2 5 Manual Calibration A manual calibration should be applied if you do not want to calibrate your sensor again However this is only possible if you already know the calibration values of the special sensor Connect the Microx TX3 via the RS232 cable to your computer 2 Switch on the Microx TX3 oxygen meter 3 Start the Microx TX3 software on your computer and click the Calibration menu item 4
79. r hidden Oxygen Oxygen content in the chosen unit Phase Phase angle the raw data Amplitude The magnitude of the sensor signal Temperature The measured temperature Display Zoom File Charts Display Print Settings Zoom d m AutoScaley1 Undo Zoom Clear Charts 0 Dimensions AutoScaleY 1 is the default setting AutoScaleY1 means that the y axis is scaled automatically Undo Zoom The original display is recovered see also graphical display Clear Charts The graph shown on the display is cleared Dimensions You can adjust the number of measurement M rreemempremm x points on the x axis shown in the display maximum number of points is 5000 Choose the dimensions for the chart Furthermore you can adjust the minimum and the maximum of the y axis X axis ticks 1000 si The AutoScaleY1 function is switched off Y axis minimum p Y axis maximum 104 X cs Print Charts The charts shown in the display can be printed Settings Com Port The serial com port com1 com20 for the serial interface RS 232 can be chosen in this window COM 1 is the default setting If you choose the wrong com port the information window Connect the instrument to the PC and choose the right com port does not disappear Instrument Info Here you can find the version of the software and some important settings of the instrument If you have a
80. ract the glass fiber back into the protective syringe needle without absorbing water Also wash the temperature sensor by dipping it into water 10 To record the second calibration value water vapor saturated air place the calibration standard 100 containing wet cotton wool below the microsensor The vessel with the label cal 100 has to be closed with the screw top containing the two holes Make sure that the glass fiber with is sensor tip is not extended Insert the syringe needle through one of the holes until it is about 1 cm deep inside the vessel Make sure that the glass fiber with its sensor tip does not touch the cotton wool when extended Insert the temperature sensor through the other hole and make sure that it does not touch the microsensor Extend the glass fiber with its sensor tip wait about 30 s until the phase angle and the temperature are constant the variation of the phase angle and temperature should be smaller than 0 05 and 0 2 C respectively and click the Store current value button to store the 100 air sat and temp at 100 values A message window opens and informs you that you will overwrite the existing calibration values Click the Continue button to store the new calibration data 11 12 13 Calibration 43 Now calibration with temperature compensation is complete Confirm the calibration values by clicking the Finish button Pull the glass fiber with its sen
81. sor tip back into its protective syringe needle before removing the microsensor from the calibration vessel Protect the syringe plunger against slipping out by inserting the transport block back into the syringe housing Calibration 44 7 1 5 Manual Calibration A manual calibration should be applied if you do not want to calibrate your sensor again However this is only possible if you already know the calibration values of the special sensor 1 Connect the Microx TX3 via the RS232 cable to your computer Switch on the Microx TX3 oxygen meter Start the Microx TX3 software on your computer and click the Calibration menu item Boo KN Select the calibration routine calibrate manually by clicking the manual button Measurement Calibration perature sensor calibrate without temp sensor calibrate manually 5 Enter the atmospheric pressure at which calibration was performed not the actual one and the respective calibration values 0 air sat temp at 096 and 100 air sat temp at 100 Calibration Menu 2 Point calibration user defined atm pressure 1013 mbar 1st point phase temperature D air sat oe fea r feo jp zc 2nd point phase temperature 100 air sat zlps joo a apo je ze X Cancel 6 Now user defined calibration is complete Confirm the calibration values by clicking the Finish button A message window opens and informs you that you will overwrite the exi
82. sting calibration values Click the Continue button to store the new calibration data Calibration Message x This will overwrite the exsisting calibration values X Cancel Calibration 45 7 2 Calibration of Flow Through Housed Oxygen Microsensors 7 2 1 Preparation of the Calibration Standards Calibration of microsensors is performed using conventional two point calibration in oxygen free water cal 0 and air saturated water cal 100 Preparation of calibration solution 0 oxygen free water 1 Add 1 g of sodium sulfite Na2S03 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 NazSOz and to ensure that the water is oxygen free Keep the vessel closed after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S204 The shelf life of cal 0 is about 24 hours provided that the vessel has been closed with the screw top 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
83. surement Please see the details of measurement process described in Microx TX3 manual Temperature Compensation No other than supplied temperature sensor could be used with the unit The use of any other temperature sensor can damage the oxygen meter Trouble Shooting 11 Trouble Shooting Error Device does not work and LED on the front panel is not lit Device does not work and LED on the front panel is on Temperature compensation failed no temperature measurement possible Warning light Amplitude red Warning light Phase red Warning light overload red No cal Strong signal fluctuations PT 1000 sensor is not connected Cause Device is not switched on No power supply No connection to PC properly PT 1000 sensor is faulty Microsensor is not connected properly ST connector is contaminated Sensor tip is damaged Phase angle out of limits Too much false light Calibration failed Sensor was not in the right calibration standard Sulfite solution has aged Air bubbles at sensor tip The glass fiber with its sensor tip is not extended from the syringe needle Amplitude is too low 72 Action Switch on device with ON OFF switch on the rear panel Connect power supply with device Check connection of the device to our PC RS 232 Check connection Contact our service Check connection of the ST connector Clean connector with a soft lint free cloth rag
84. surplus of Na2SOs 3 Close the vessel with a screw top and shake it for approximately one minute to dissolve Na SOs and to ensure that the water is oxygen free Keep the vessel closed with a screw top after calibration to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S204 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 a vessel and label it cal 100 2 Drill two holes for inserting the microsensor and the temperature sensor in the screw top and close the vessel 3 Wait about 2 minutes to ensure that the air is water vapor saturated Calibration 35 7 1 2 Mounting the Needle Type Microsensors 1 Remove the microsensor carefully from the protective cover The needle type microsensor is housed in a 0 4 x 40 mm syringe needle mounted to a 1 mL plastic syringe housing with integrated PUSH amp PULL IN amp OUT mechanism The syringe needle is protected with a protective plastic cap A protective plastic cap A transport B block 2 Carefully remove the protective plastic cap A covering the syringe needle When doing so grip the plastic base of the needle tightly The syringe needle must not be removed from the syringe housing Work carefully tightly grip the needle base 3 Fix the
85. ure is measured with a precision of 0 2 C there is a variation of 100 0 3 96 air saturation in the measuring value at 100 air saturation Please choose the measurement with temperature compensation to minimize temperature gradients 8 4 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 is minimized Continuous illumination of a tapered sensor tip over a period of 24 hours may lead to a phase drift of up to 1 6 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 microsensor 100 X 80 c 4 Q J S 604 3 M 5 J L 407 i 20 d 7 0 2 4 6 8 10 12 14 16 18 20 22 24 time h Photostability of a tapered oxygen microsensor Measurement 66 Drift in air saturation at 100 air saturation when illuminating the microsensor with a tapered and flat broken sensor tip for 1 12 and 24 hours in the
86. ure of oxygen in hPa po hPa Pam hPa py T hPa air saturation 0 2095 6 100 in mbar Po mbar Pan mbar Pw T mbar oy PD 0 2095 7 in Torr Po Torr i AE a i28 D 0 2095 0 75 8 Please note 1 mbar 1 hPa 0 750 Torr Oxygen Concentration in mg L T ir i M co mg L Pe Pwlt air saturation 9599s 7 1999 2 6 Px 100 Vu in ppm mg L Appendix 79 FT M co ppm co mg L Pas Pw D Pb air saturation 0 5995 acr 1999 MO 40 P 100 V in umol L 1000 Co umol L co mg L co mg L 31 25 o M Co mg L MO o mg L MOGLIE 2 Rant p0b Rar esistono 2058 aep 10000001 P 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 O2 cm M Oz molecular mass of oxygen 32 g mol Vu molar volume 22 414 L mol 13 3 Temperature Dependent Constants Affecting the Oxygen Content 13 3 1 Water Vapor Pressure As shown in equation 4 11 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 12 p Oz oxygen partial pressure in dry air at a barometric pressure patm 0 2095 volume content
87. urement Temperature Compensation Enter the temperature during the measurement C on ze fo 3e Logging Setup To start the measurement without logging data click Measure in the Logging setup and the Start button Logging Setup C Measure amp Log File Desciption X Cancel To store the data of your measurement click in the Logging Setup the Measure amp Log item and click the button Choose File Here you can select the location where you want to store the data Choose as file extension txt Click the speichern button to confirm your settings Software 31 Data file selection Speicher Eigene Dateien B ex E3 adobe B Eigene Bilder S Eigene Musik My eBooks Dateiname Dateityp Data Files txt Abbrechen file location File Desciption enter the description here You can enter a measurement description in the text field File description which is stored in the ASCII file To start the measurement click the Starf button In the Information windows Sampling Rate you can find the adjusted sampling rate To be sure whether you perform a measurement with or without logging the data the Logging Status window displays whether the actual measurement is stored to a file logging or not no logging Measurement Start Measurement Sampling Rate Stop Measurement The measurement is ended by
88. urement Assistent Iof x You did not calibrate the sensor after program start Date of last calibration 2871 1 02 Last calibration was made 7 days ago New Calibration X Cancel If you want to measure with the last sensor calibration you can find the date of the last calibration in the window click the Continue button To obtain reliable results we strongly recommend to perform a sensor calibration before measurement by clicking the New calibration item when connecting a new sensor Follow the instructions given in chapter 7 to calibrate the respective microsensor To leave this menu click the Cancel button If you have already performed sensor calibration the measurement assistant will be opened In this window you can choose the measurement settings D x Measurement Assistent Choose the measurement settings Sampling Rate Dynamic Averaging 1 sec a samples Temperature Compensation S450 Enter the temperature during the measurement on a ze m Measure C Measure amp Log File Desciption fienterthe description here SSS X Cancel In the Sampling Rate window you can select the desired measurement mode with a drop down menu By clicking the drop down menu you can choose from fast sampling update rate each 250 350 ms to the 60 min mode where each hour a measurement point is recorded The speed of recording a measurement point in the
89. ust click the button Start Auto Adjust Please check that the oxygen microsensor has been connected to the instrument LED Intensity Adjust The automatical adjustment of the LED intensity is finished when the message Auto adjustment finished appears in the status window Click the Close button to confirm the settings LED Intensity Adjust Advanced Click the Advanced button to change the LED current manually Values between 10 and 100 are possible After clicking the confirm button you can see the change of the amplitude in the window below LED Intensity Adjust amplitude 11092 Software 27 Please note After changing the LED intensity you should re calibrate the oxygen microsensor A warning window points you to re calibrate the oxygen microsensor LED Adjust Warning 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 Analog output Here you can choose which data are exported via the analog output The Microx TX3 device has two analog outputs and one trigger input The desired data sources oxygen temperature amplitude phase can be chosen via the dialog box Equivalence coefficient oxygen 1 0 1 e g 973 mV 97 3 air saturation temperature 1 0 1 e g 208 mV 20 8

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