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MICROX TX3 - Loligo Systems

1. 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 Stan Measurement Sampling Rate TER Stop Measurement The measurement is ended by 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 Description of Microx TX3 Software e amplitude phase E ambient light ss Dishlay Raw Valles 33 amplitude red Amplitude is too low the sensor tip may be damaged or 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 ra
2. The effect of increasing the salt concentration on the vapor pressure is neglectible small as shown in Table 13 5 Table 13 5 Variation of solution vapor pressure pw with salt concentration CI g 10009 O 9 1 t8 26 TIC Vapor pressure of solution torr D he 5 CY 44 no be pi fo lbs o hie 814 os 804 The dependence of oxygen solubility on salt concentration can also be obtained from equation 21 except that now values calculated from either equation 28 or 29 have to be used 10 a 2a cb 0 c 0 d 0 e 6 CI p amp q 0r 0 amp s 0 4 t 07 28 where 0 is the temperature in C a e are the coefficients used in equation 23 and p t are new constants given in Table 13 6 The values of these new constants obtained by fitting the polynomial to experimental data in the ranges 0 lt 0 x 30 C and O lt CI x 20 To obtain an oxygen solubility from the Bunsen absorption coefficient the same procedure as described previously is used An alternative equation to compensate the Bunsen absorption coefficient by the salt concentration displays equation 29 Appendix 94 10 EE EEN 29 where T is the temperature in Kelvin and A D and P S are the coefficients also given in Table 13 6 They are based on measurements for 273 1 lt T lt 308 18 K and 0 lt CI x 30 and is therefore more extensive than equation 28 Both equations give values of 10 o
3. Length of Stainless Needle Glass Fiber Length mm diameter mm Needle Type ES m 20 04 Housing 10m EC Optical Isolation m f Y with optical isolation EE E N without optical isolation Coating 120 0 8 f P eee as Shape of Sensor Tip S sharp tip lt 50 um F flat broken tip 140 um Example vm H esn Fels ris H skolos ior 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 5 2 2 Flow Through Cell Housed Oxygen Microsensors We offer 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 Fiber Optic Oxygen Microsensors Sensors and Housings Features e Easy to handle and robust e Online monitoring e Very fast response time e Sterilizable autoclave 130 C 1 5 atm EtO EtOH H202 e Measuring range from 0 to 250 air saturation 0 22 6 mg L e Limit of detection 0 2 96 air sat 20 umol L Schematic drawing of flow through cell housed microsensors Luer Lock a
4. 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 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 PT100 temperature sensor Raw data can be used for user defined recalculations according to the formulas and tables listed in the appendix Description of Microx TX3 Software Akti DESCRIPTION EEEE EEE EEEE test measurement INSTRUMENT INFO IDENTIFICATION PHIboard number 20020069 PM number 20020032 Serial number TX3 AOT 2003 0001 MUX channel ON 01 PARAMETERS Signal LED current 160 Ref LED c
5. 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 Calibration of Oxygen Sensitive Microsensors 63 Presens T Pression Teese sree cal 100 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 calibration 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 100 to the 4 pin connector in front 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 and click the cal button calibrate with temperature sensor calibrate without temp sensor Calibration of Oxygen Sensitive Microsensors 64 6 Enter the actual atmospheric pressure Th
6. 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 of Oxygen Sensitive Microsensors 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 Fix the microsensor with a clip to a laboratory support or a similar stable construction 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 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 male fiber plug Calibration of Oxygen Sensitive Microsensors 50 7 2 3 Calibration without Automatic Temperature Compensation Using the software you
7. LOLIGOSYSTEMS COM Instruction Manual MICROX TX3 fiber optic oxygen meter Loligo Systems ApS Niels Pedersens All 2 DK 8830 Tjele Denmark Phone 45 89 99 25 45 Fax 45 89 99 25 99 e www lolieosvstems com mail lolisosvstems com es VAT no 2746 7849 e Bank 5984 0004001376 Instruction Manual Microx TX3 Software Version TX3v531 January 2005 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 Table of Contents Table of Contents DES ZC 1 2 Safety ET E 2 3 Description of the Microx TX3 Device eeeeeeeeeeereeeeneeeee 4 4 Required Basic Equlpmebl ioiiaicihrr vias ra nias a ead a a a Ra e RE PIA Ria aa 7 5 Fiber Optic Oxygen Microsensors Sensors and Housings 8 5 1 Oxygen Sensitive Microsensors eeeeeeeeeee eene 8 5 1 1 Sensor Characteristics 3 2 2 ante heo eme ce pd be ia Ep rep e eege e cte 8 5 1 2 Design oftthe Sensor Tips etarsen teipio tee pacte Lern fe te e paths 11 5 1 3 Wl le RE E TEE 13 5 2 Housings of Oxygen Sensitive Microsensors eeeeeeeeeeneeeeee 14 5 2 1 Needle Type Housing Oxygen Microsensors nene 15 5 2 2 Flow Through Cell Housed Oxygen Microsensors esesseeseesiresieettsittitstrestrnrrn
8. are the respective luminescence intensities O2 the oxygen concentration and Kay the overall quenching constant 014 Koy IM l f O 1 t f O I Luminescence intensity in presence of oxygen l Luminescence intensity in absence of oxygen T Luminescence decay time in presence of oxygen To Luminescence decay time in absence of oxygen Ksy Stern Volmer constant quantifies the quenching efficiency and therefore the sensitivity of the sensor O2 oxygen content Appendix 82 1 04 6 Na 0 83 5 e P Ba 3 e 4 7 edi N SU 5 7 a E No 8 0 44 lt d z 1 e 2 TEE 0 2 4 d P dd 0 20 40 60 80 100 oxygen content 406 Figure 13 2 A Luminescence decrease in the presence of oxygen B Stern Volmer plot Indicator dyes quenched by oxygen are for example polycyclic aromatic hydrocarbons transition metal complexes of Ru ll Oe and Rh Il and phosphorescent porphyrins containing Pt II or Pd Il as the central atom 13 1 2 Major Components of Fiber Optic Microsensors 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 polarisation Light acts as the carrier of the information The major components of a typical fiber optical sensing system are a light source to illuminate the sensor laser light emitting
9. mg L uU Ww CO oO 0 5 10 15 20 23 6 C Figure 13 9 Dependence of the oxygen solubility in air saturated fresh water on temperature 91 30 35 40 45 50 Appendix 92 Table 13 3 Oxygen solubility in air saturated fresh water mg L TLC cs T 0 14 64 60 55 51 47 143 39 35 3 27 23 1 23 19 15 10 06 03 999 99 91 87 83 2 13 83 79 75 71 68 64 60 56 52 49 45 3 45 41 38 34 30 27 23 20 16 12 09 4 09 05 02 98 95 92 88 85 a 78 75 5 12 75 71 68 65 61 58 55 52 48 45 42 6 42 39 36 32 29 2 23 2 17 14 1 7 11 08 05 02 99 96 93 90 87 84 81 8 11 81 78 75 72 69 67 6 amp 4 e 58 55 53 9 53 50 47 44 42 39 36 33 31 28 25 10 25 23 20 18 15 12 10 07 05 0 99 11 on 97 ou 92 89 87 84 82 79 7 75 12 75 72 70 67 65 63 60 58 55 53 Si 13 51 48 46 44 41 39 37 435 32 30 28 Hy 28 26 23 B io 17 15 12 10 08 06 15 06 04 02 9 97 95 93 91 89 87 85 16 9 85 83 81 70 76 74 72 70 68 66 64 17 64 62 60 58 56 54 5 51 4 47 45 18 45 43 41 39 37 35 33 8 30 28 26 19 26 24 22 20 19 17 15 13 11 09 08 20 08 06 04 02 o 99 97 95 94 92 90 21 8 90 88 87 85 83 82 80 78 7 75 73 22 73 71 70 68 66 65 63 62 60 58 57 23 57 55 53 52 50 49 47 446 44 42 A 24 41 39 38 36 35 33 32 30 28 27 25 25 25 24 22 21 19 18 16 15 14 12 11 26 11 09 08 06 05 03 02 00 99 98 96 27 7 96 95 93 092 90 89 88 86 85 83 8 28 82 81 79 78 7 75 7 73 71 70 69 29 69 67 66 65 63 62 e 59 58 57 55 30 55 54 53 51 50 49 48 46 45 44 42 31 42 41 40 39 37 36 35 34 322 39
10. correlation coefficient R of this fit was higher than 0 999 1 tan 0 89 0 11 7 tan 1 Kg JO The oxygen content in air saturation can be calculated according to equation 8 1 tan tan d kol ndi tano A second model which also is based on equation 5 can be used for describing the oxygen calibration plot In this model Raus is set to be x Ksy f was determined to be 0 805 and x was determined to be 1 22 9 The correlation coefficient R of this fit was higher than 0 9999 0 8 1 tan _ 0 804 5 0 196 tn 1 K IO 1 SV 2 e eer 9 Appendix 86 The oxygen content in air saturation can be calculated according to equation 10 _ B VB 4 A C 9 10 rad SES 10 with the coefficients tan X K 10a tan SS 10a tan tan E tan 5 Fe tan X K aie Koo Kea FEE 10b tan RT 10c tan ch 13 3 Oxygen Conversion Formulas Please note These conversion formulas are only valid in aqueous solutions and humidified air These formulas have to be modified if measurements are performed in organic solvents or solutions with high salinity Saturation 6 air saturation Default Setting of the instrument see equation 10 in 13 2 oxygen saturation O air saturation 20009 11 100 0 2095 volume content of oxygen in air ppm in the gaseous phase 20 ppm O air saturation we 10000 12 1 i
11. 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 salt sve Wait about 30 sec 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 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 ES This will overwrite the exsisting calibration values X Cancel Afterwards wash the sensor tip with distilled water to clean it from sodium sulfite Don t retract the glass fiber 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 glass fiber 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 Also wash the temperature sensor by dipping it into water Now you have to record the second calibration value water vapor saturated air Place the calibration standard 100 containing wet cotton wool below the
12. 20808 20797 20785 20776 20776 20761 20774 20754 20747 20738 20739 20736 20717 20738 20718 20714 20711 temp C 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 20 00 35 Calibration of Oxygen Sensitive Microsensors 36 7 Calibration of Oxygen Sensitive Microsensors 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 one gram sodium sulfite Na SO3 to the vessel and label it cal 0 2 Dissolve NazSO3 in 100 mL water Water becomes oxygen free due to a chemical reaction of oxygen with NazSO3 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 NaSO and to ensure that water is oxygen free Close the vessel after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S2O0 The shelf life of cal 0 is about 24 hours provided that the vessel has been closed with the screw top Preparation of calibration standard 100 water vapor saturated air 1 Place wet cotton wool in the vessel with
13. 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 7 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 GLASS FIBER WITH ITS SENSOR TIP IS PUSHED OUT HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK Calibration of Oxygen Sensitive Microsensors 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 salt E 9 Wait about 30 sec 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 0 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 ca
14. 8 Measurement Calibration of the microsensor is recommended before each measurement see chapter 7 Calibration of Microsensors If you don t want to recalibrate the microsensor you can use the calibration values of your last measurement see User Defined 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 positioned 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 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 to perform temperature compensated measurement Fix the tempe
15. A Store current value 2nd point phase temperature 100 air sat 7 br Seo do vie amplitude phase 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 Ensure that the sensor tip is dipped about 4 mm into the calibration solution 0 but not the protective syringe needle Calibration of Oxygen Sensitive Microsensors 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 ee Wait about 30 sec 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 0 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 of Oxygen Sensitive Microsensors Calibration Menu 2 Point calibration without temperature sensor atm pressure
16. 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 10096 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 Calibration of Oxygen Sensitive Microsensors Calibration Menu 2 Point calibration with temperature sensor atm pressure 1013 mbar 4st point phase temperature D air sat ps ba ok SC wi Store current value 2nd point phase temperature 100 Yair sat E d po Ye C amplitude phase temperature This will overwrite the exsisting calibration values X Cancel 13 Now calibration with temperature compensation is complete Confirm the calibration values by clicking the Store button 14 Pull the glass fiber with its sensor tip back into its protective glass housing before removing the microsensor from the calibration vessel 7 3 5 Manual Calibration A manual ca
17. at 100 values 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 of Oxygen Sensitive Microsensors 43 10 Now calibration is complete Confirm the calibration values by clicking the Finish button 11 Pull the sensor tip back into its protective syringe needle before removing the microsensor from the calibration vessel 12 Protect the syringe plunger against slipping out by inserting the transport block back into the syringe housing and don t remove it again until just before measurement 7 1 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 in front of the Microx TX3 Fix the temperature sensor and make sure that neither the temperature sensor nor its cable can touch the microsensor 6 Calibration of Oxygen Sensitive Microsensors 44 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 1 2 Mounting the Needle Type Microsensors 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 Measurement Calibration calibrate with temperature sensor
18. 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 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 Start the Microx TX3 software on your computer and click the calibration menu item Select the calibration routine calibrate without temp sensor and click the cat button Measurement Calibration calibrate with temperature sensor 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 concentrations units mg L umol L Please note that changes
19. 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 23 10 a2a cb 0 c 0 d 0 ce 0 23 where 0 is the temperature in C and a e the coefficients calculated by standard curve fitting procedures a 48 998 b 1 335 c 2 755 10 d 3 220 10 e 1 598 10 The square of the correlation coefficient is 0 999996 50 a 0 10 48 998 1 335 0 2 755 10 9 3 220 10 9 1 598 10 9 0 0 5 10 15 2 Figure 13 8 Variation of Bunsen absorption coefficient o 6 with temperature Appendix 90 The other form of equation to describe the variation of with temperature can be derived from a thermodynamical correlation and gives an equation of the form ite 2 B InT C 24 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 23 and 24 for the same temperature agree within 0 5 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 pa44 0 in air
20. may lead to a phase drift of up to 1 6 air saturation measured at 10096 air saturation at 20 C However this effect of photo decomposition 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 80 60 40 air saturation 96 20 0 2 4 6 8 10 12 14 16 18 20 22 24 time h Photostability of a tapered oxygen microsensor Measurement 73 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 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 0 air saturation immersing the sensor tip into the cal 0 solution and 100 air saturatio
21. 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 one gram sodium sulfite NazSO3 to the vessel and label it cal 0 2 Dissolve Na SOsin 100 mL water 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 NaSO 3 Close the vessel with a screw top and shake it for approximately one minute to dissolve NaSO and to ensure that water is oxygen free Close the vessel after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S2O0 The shelf life of cal 0 is about 24 hours provided that the vessel has been closed with the screw top Preparation of calibration standard 100 water vapor saturated air 1 Place wet cotton wool in the vessel and label it cal 100 2 Drill two holes for inserting the microsensor and the temperature sensor in the screw top and close the vessel with it 3 Wait about 2 minutes to ensure that air is water vapor saturated Calibration of Oxygen Sensitive Microsensors 58 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 Fi
22. of the special sensor 1 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 and click the manual button Calibration of Oxygen Sensitive Microsensors 56 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 0 air sat temp at 0 and 100 air sat temp at 100 Calibration Menu 2 Point calibration user defined atm pressure f 013 mbar 1st point phase temperature Larne bah coe Lu 2nd point phase temperature Do ainsa 2428 Ja feo je ze 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 Calibration of Oxygen Sensitive Microsensors 7 3 Calibration of Implantable Oxygen Microsensors 7 3 1 Preparation of the Calibration Standards Calibration of
23. oxygen free environment nitrogen sodium sulfite and air saturated environment ENVIRONMENTAL CONDITIONS Operating Temperature C 0 to 50 Storage Temperature C 10 to 65 Relative humidity up to 95 Dimensions DxWxH mm 185 x 110 x 45 Weight kg 0 63 Fiber Optic Oxygen Microsensors Sensors and Housings Temperature Microsensors can be used in the temperature range of 10 to 80 C We offer a Pt1000 temperature sensor in combination with the Microx TX3 to record temperature variations which are compensated using the Microx TX3 software see Chapter 7 Calibration of Microsensors and Chapter 8 Measurement In the appendix you will find a detailed description of the Temperature Dependent Constants Affecting the Oxygen Content chapter 13 4 and Temperature Compensation of the Response of Oxygen Sensors chapter 13 5 Cross sensitivity There exists no cross sensitivity for carbon dioxide CO hydrogen sulfide H2S ammonia NH3 pH any ionic species like sulfide Sz sulfate SO chloride Cl 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 d
24. range resolution accuracy CALIBRATION PROCEDURE 2 point calibration in oxygen free water and humidified air or air saturated water OPTICALOUTPUT INBUT ST compatible Core Center 100 140 Wavelength 505 nm TEMPERATURE SENSOR INPUT Lemo Connector Size 00 Connector for Pt 1000 temperature sensor PT1000 1 N C N C PT1000 2 SS GO MM A DC INPUT De anaes GND 18VDC GND 18VDC RJ11 6 4 Technical Data 76 DIGITAL OUTPUT communication protocoll serial interface RS232 19200 Baud Databits 8 Stoppbits 1 Parity none Handshake none instrument output on RJ11 4 4 plug a 1 4 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 o Operating temperature 0 to 50 C 10 to 65 Storage temperature 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 77 10 2 Analog Output and External Trigger The TX3 AOT 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
25. slow down the sensor response Dissolved oxygen Gaseous oxygen Response time to for tapered sensors tip diameter lt 50 um 1 s lt 5 s with O I lt 0 5 s lt 1 s with O 1 flat broken sensors tip diameter 150 um lt 15 s lt 30 s with O 1 DS lt 10 s with O I O I Optical Isolation Fiber Optic Oxygen Microsensors Sensors and Housings 100 80 A 60 flat broken S sensor tip E d 40 an e lt 50 um tapered 20 sensor 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 lt 50 um and a microsensor with a flat broken sensor tip 140 um Sensor 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 H202 solution The oxygen sensitive material may be subject to photo decomposition resulting in a signal drift Photo decomposition takes place only during illumination of the sensor tip and depends on the intensity of the excitation light Drift in 6 air saturation at 10096 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 point
26. 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 Measurement 72 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 sensors 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 temperature is measured with a precision of 0 2 C there is a variation in the measuring value at 100 air saturation of 100 0 3 96 air saturation Please choose the measurement with temperature compensation to minimize temperature gradients 8 4 3 Signal drift due to photo decomposition The oxygen sensitive material may be subject to photo decomposition resulting in a signal drift Photo decomposition 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
27. 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 less influence on the measuring signal The decay time is not influenced by variations in the optical properties of the sample including turbidity refractive index and coloration 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 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 Il Ruckruh F Liebsch G Stangelmayer A Wolf
28. which agree to better than 1 Table 13 6 Values of the coefficients in equations 26 and 27 ESI AX e EATER oU o Um Pam kum Eqn 26 a 4 900 10 p 5 516 10 b 1 335 q 1 759 10 c 2 759 10 r 2 253 10 d 3 235 10 S 2 654 107 rM e 1614 107 t 15 362 108 Eqn 27 A 7 424 P 1 288 107 B 4 417 10 Q 5 344 10 C 2 927 R 4 442 10 D 4 238 10 S 7 145 107 Seawater has a salinity typically of 35 35g 1000g or a chloride content of about 19 o and therefore falls within the scope of both equations 13 5 Temperature Compensation of the Response of Oxygen Sensors Temperature affects the luminescence decay time as well as the luminescence intensity of the indicator dye The collisional frequency of the oxygen molecules with the indicator dye reflecting the diffusion coefficient of oxygen is also affected A typical oxygen response characteristic at different temperatures is shown in Figure 13 10 The phase angle 4 is a function of the oxygen content tan f O2 and decreases with increasing the oxygen content 0 0 60 19 5 2 5 ee 0 0 7 5 Aen 2 5 5 CO 7 596 a 13 15 SCH 7 5 CO e o7 50 1596 sx 25 15 e 25 ben 25 ep 40 25 E E 50 3o 2 Se 50 E 30 100 ioo i 50 e 100 100 20 250 2302 e 250 n M 0 C 10 C 20 C 30 C 40 C 10 mp a a a a a 0 1000 2000 3000 4000 5000 6000 time s Figure 13 10 Oxygen response characteristics
29. 0 Technical Data vis siisesceeceeweecssnsswvsatocecesecantaeas Wewcvcedecusvaaivavwecedeuesvasinavvenedocewees aks 75 10 1 General Data sini this Seti thn ei eee A ete ae eee E 75 10 2 Analog Output and External Trigger eese 77 10 3 Technical e 78 TOA Operation TE 78 11 Trouble Shooting hoo conii cocco da ihn Er runi E ER x C 79 12 Concluding Remarks eiii ei aa mrt ck e ead ari saa aS Exp E NER REIN USES MEME SERA NIE 80 DAE she qe S 81 13 1 Basics in Optical Sensing of Oxygen eene 81 13 1 1 Dynamic Quenching of Luminescence neret rens 81 13 1 2 Major Components of Fiber Optic Microsensors eene 82 13 1 3 Advantages of Optical Oxygen Sensitive Microsensors 83 13 1 4 Luminescence Decay TIime mise Terr eine Doe ce rne Be Ce ERAS a Ee CO 83 13 1 5 Literature cei ESA RIGEN RGB ch RARE 84 13 2 Determination of the Oxygen Concentration Using a Modified Stern Volmer Equaltlon nuege eset utr Le I DM EE 84 13 3 Oxygen Conversion Formulas eeeeeeeeeeeeeeeeennnen nennen nennen nnns 86 13 4 Temperature Dependent Constants Affecting the Oxygen Content 88 13 4 1 Water Vapor PressUre dE Reegele Lua ee o ed sib eee eo dava Tec e tian ecce cn 88 13 4 2 Bunsen Absorption Coefftcent nennen nnne nnne nnne 89 13 4 3 Dependence on the Salt Concentration essssessssseeeeneneenenen nennen 93 13 5 Temperatur
30. 00 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 10 Calibration of Oxygen Sensitive Microsensors Wait about 30 sec 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 temperature is constant the variation of the phase angle and temperature should be smaller than 0 05 and 0 2 C respective
31. 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 i e 973 mV 97 3 air saturation temperature 1 0 1 i e 208 mV 20 8 C amplitude 1 10 i e 2220 mV 22200 relative units phase 1 0 025 i e 1100 mV 27 509 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 t2mV gt 0 2 C amplitude t2mV 3 20 relative units phase t2mV gt 0 05 Accuracy error 10mV Technical Data 78 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 50uUs 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 2ms Min pulse length 3 ms Min pause length 10 ms Min periode 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 vo
32. 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 emission of LR d d light ES x S 1 I K absorption of light excited state energy transfer E E by collision 1 a Pd E SE C E P I 2 no emission of light Figure 13 1 Principle of dynamic quenching of luminescence by molecular oxygen 4 IN P e ms sn 1 Luminescence process in absence of oxygen 2 Deactivation of the luminescent indicator molecule by molecular oxygen The collision between the luminophore in its excited state and the quencher oxygen results in radiationless deactivation and is called collisional or dynamic quenching After collision energy transfer takes place from the excited indicator molecule to oxygen which consequently is transferred from its ground state triplet state to 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 t and t are the luminescence decay times in absence and presence of oxygen lo and
33. 30 32 30 29 28 26 25 24 23 21 20 19 18 33 18 17 15 14 13 12 1 09 08 07 06 34 06 05 04 0 o 00 99 98 97 96 29 35 6 94 93 092 91 90 89 88 87 85 84 83 36 83 82 81 80 79 78 77 75 74 73 72 37 72 71 70 69 68 67 66 6 64 63 e 38 61 60 59 58 57 56 55 54 53 52 5 39 51 50 49 48 47 46 45 44 43 4 4 40 41 40 39 38 37 36 35 34 33 32 3 Example cs 14 3 C 10 21 mg L Appendix 93 13 4 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 there is a decrease in the oxygen solubility This behavior is characteristic for the solubility of many nonelectrolytes it is the phenomenon known as the salting out effect Instead of chlorinity CI the amount of chloride in parts per thousand which was used as a measure of the amount of salt in water the term salinity is often used If salinity is preferred as a measure of salt concentration then the conversion from g L can be readily made using equation 27 S 1 805 CI 0 03 27 where S is the salinity in 0 or g 1000g Table 13 4 Solubility of oxygen in water as a function of temperature and salt concentration Total pressure 760 torr CI g 000g O 4 8 dR j6 120 T C Oxygen solubility mg L o as 139 133 126 n t3 19 0 HO Ji 3 j108 j 104 99 95
34. Assistant m Calibration Teeeeeneneneeeeeseneeseeseneeseananenenenenenene Start Measurement Measurement Sampling Rate Lounen RE A Calibration The calibration assistant is opened see chapter 7 Calibration of Oxygen Sensitive Microsensors B Measurement By clicking Start Measurement the measurement assistant opens to enter the measurement settings If you haven t performed sensor calibration yet the following window appears 5 Measurement Assistent ol x You did not calibrate the sensor after program start Date of last calibration Gan 1 02 Last calibration was made H days ago Ay 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 Cancef button If you have already performed sensor calibration the measuring assistant will be opened In this window you can choose the measurement settings Description of Microx TX3 Software 30 rN E x Measurement Assistent Choose the measurement settings Sampling Rate Dynamic Averaging 1 sec D 4 samples Tem
35. Please feel free to contact our service team to find the best solution for your application Your Loligo 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 If the instrument is moved from cold to warm surroundings condense 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 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 protect
36. al pressure in air saturated water and water vapor saturated air DO Te Pam Pw T 0 2095 20 Water vapor pressure is strongly affected by temperature variations and this of course influence the oxygen partial pressure as shown in equation 20 Table 13 1 Variation of water vapor pressure pw T with temperature e C o pw T mbar 6 1 A convenient fitting function is given by the Campbell equation 21 EE 21 where T is the temperature in Kelvin and A B and C constants given in Figure 13 7 120 p T exp 52 57 6690 9 T 4 681 InT R 1 100 H S 80 E pg 00 z E 40 20 EE a eH 272 277 282 287 202 297 302 307 312 317 322 T K Figure 13 7 Variation of water vapor pressure with temperature Appendix 89 13 4 2 Bunsen Absorption Coefficient The solubility of oxygen in water is temperature dependent and can be described using the Bunsen absorption coefficient 8 and the oxygen partial pressure p O according to equation 22 With increasing temperature the solubility of oxygen in water decreases c p 9 PO qo 22 N Cs p 0 temperature dependent solubility of oxygen in water p O5 oxygen partial pressure PN standard pressure 1013 mbar Table 13 2 Variation of Bunsen absorption coefficient a 0 with temperature ere jo s Ho fis fz20 25 30 35 40 50 The data in Table 13 2 can be described by two forms of equations The first form of equation to
37. allization within the housing Salt crystallization may seal the housing and the glass fiber with its sensor tip will break when extended salt EDEN Wait about 30 sec 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 0 air sat 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 sulfite 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 Now you have to record the second calibration value water vapor saturated air Place the calibration standard 100 containing wet cotton wool below the microsensor The Calibration of Oxygen Sensitive Microsensors 66 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 doesn t touch the microsensor
38. ase 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 1 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 100 to the 4 pin connector on the front panel of the Microx TX3 and carefully tighten the safety nut to perform temperature compensated measurement Immerse the temperature sensor in your sample and fix it with a laboratory support 4 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 User Defined calibration which is described in chapter 7 2 5 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 6 Please rinse the glass
39. at different temperatures Appendix 95 Figure 13 11 displays the oxygen dependence of the phase angle at different temperatures and Figure 13 12 the respective Stern Volmer plots These two figures and Table 13 7 displays that both the phase angle in absence of oxygen da and the Stern Volmer constant Ksy are temperature dependent du decreases with increasing temperature while KSV increases with increasing temperature 60 50 A phase angle S N 0 50 100 150 200 250 300 350 400 air saturation Figure 13 11 Effect of the temperature on the phase angle at different oxygen contents given in air saturation 5 5 40 C 5 30 C ae 4 5 et e 14 ke 3 5 e 3 ke el 2 5 2 tn 1 5 J 1 T 0 100 200 300 400 500 air saturation Figure 13 12 Effect of the temperature on the Stern Volmer constant Appendix 96 Table 13 7 Effect of the temperature on the phase angle in the absence of oxygen 4 and the Stern Volmer constant Rau TUS ep a S894 5644 Ka air sat 0 03678 0 03929 0 04257 0 04698 0 05085 1 a The Stern Volmer constant is determined via equation 9 Figure 13 13 displays the temperature dependence of du and Ksy From Table 13 7 and Figure 13 13 a decreases in du of about 0 08 can be calculated by increasing the temperature by 1 K On the other hand the Stern Volmer constant Ksy increases about 3 810 air sat by incr
40. ation temperature 1 0 1 e g 208mV 20 8 C amplitude 1 20 e g 1110mV 22200 relative units phase 1 0 025 e g 1100mV 27 50 Description of Microx TX3 Software 28 Analog Choice of x Please define the analog output ports analog channel 1 analog channel 2 C none C none oxygen airsat oxygen airsat C phase C phase C amplitude C amplitude C temperature C temperature sox g 6 2 2 Control Bar Numerical display OXYGEN OXYGEN RTS RTS airsatur TEMPERATURE a pa umol L off line 20 0 E an mg L ppm 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 manual inserted temperature is displayed with the hint that temperature measurement is off line Description of Microx TX3 Software 29 Control buttons The way to start a measurement is A Calibration of the minisensor with the Calibration Assistant B Start Measurement with Measurement
41. aturated 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 Fiber Optic Oxygen Microsensors Sensors and Housings 5 Fiber Optic Oxygen Microsensors Sensors and Housings 5 1 Oxygen Sensitive Microsensors 5 1 1 Sensor Characteristic 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 0360 54 0 0 O Ec s o 50 i n a e 404 o D o S 30 S o 1 O 3 G d S I amp Ke 10 0 t t t t t 0 200 400 800 0 20 40 60 80 100 time s O 96 Figure 5 1 Response of an oxygen microsensor Figure 5 2 Effect of the phase angle of an oxygen toward changes in the oxygen concentration microsensor on different oxygen contents Specifications of the oxygen microsensor and the Microx TX3 The optimal measuring range of the oxygen sensitive microsensor
42. beis O S Fast Response Oxygen Microsensors Based on Novel Soluble Ormosil Glasses Mikrochim Acta 131 35 46 1999 13 2 Determination of the Oxygen Concentration Using a Modified Stern Volmer Equation The Stern Volmer equation 4 displays a linear correlation between tan tan or t t and the oxygen concentration O tanc Tg z 14 Kgy O 4 sap hen El 4 Po phase angle of oxygen free water measured phase angle Ksy Stern Volmer Constant Oz oxygen content in air saturation The Stern Volmer plots of all our sensors show a distinct non linearity in their response behavior which is also observed for many other oxygen sensors described in literature This non linear response behavior can be described with a modified Stern Volmer equation Appendix 85 tan f n Lab tan I Ks O 1 Ksv 0 5 This model is based on the assumption that the indicator is distributed in the polymer matrix at two different sites and each fraction f4 1 f shows a different quenching constant Ksy Ksv For practical use this model is not very convenient since it has too many parameters which have to be calibrated Therefore two simplified models based on equation 5 can be used In the first model one fraction of the indicator is assumed to be non quenchable Ksy2 0 1 tan _ E xdi 6 tan o 1 K IO Equation 7 was used to describe the oxygen calibration plot of a microsensor type B2 The
43. calibrate without temp sensor calibrate manually Enter the actual atmospheric pressure The atmospheric pressure of the calibration is needed to convert the oxygen unit air saturation in partial pressure units hPa Torr or concentrations 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 concentrations 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 with temperature sensor atm pressure 1013 mbar 4st point phase temperature 0 air sat ps fea e of xe wi Store current value 2nd point temperature phase 100 96air sat s o2 d po fe C amplitude phase temperature 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 protective 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 10 Calibration of Oxygen Sensitive Microsensors 45 If the needle has been dipped into cal
44. cedure 3 times 7 2 4 Calibration with Automatic Temperature Compensation 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 in front of the Microx TX3 Switch on the Microx TX3 and connect the microsensor as shown in Chapter 7 2 2 Mounting the Flow Through Housed Microsensors Start the Microx TX3 software on your computer and click the calibration menu item Select the calibration routine calibrate with temperature sensor and click the cal button Measurement Calibration calibrate with temperature sensor calibrate without temp sensor calibrate manually Enter the actual atmospheric pressure The atmospheric pressure of the calibration is needed to convert the oxygen unit air saturation into partial pressure units hPa Torr or concentrations units mg L pmol L Please note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentrations units mg L umol L but the oxygen units 96 air saturation and oxygen saturation have to be corrected for air pressure changes Connect one of 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 1
45. dapter female T connector ST connector ke fiber cable microsensor tip gt 4 900 um 900 o_o SEN S male fiber plug Teflon sleeve with Luer Lock adapter integrated glass fiber female p tightened with a silicone rubber Ordering Information gel Ier HOHO Length of Glass Fiber Flow Through 25m Cell Housing EE Oxygen Sensitive Shape of Sensor Tip S p tip lt 50 um 0 250 a s F flat broken tip 140 um Example peres Hesu ls Hrs With this code you will order a flow through cell with FTCH an integrated microsensortype PSt1 with a glass fiber length of 5 m L5 a sharp tapered sensor tip of smaller than 50 um TS containing the optical isolated oxygen sensitive fiber tip Fiber Optic Oxygen Microsensors Sensors and Housings 5 2 3 Implantable Microsensors E Features e High spatial resolution e High flexibility We offer 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 costum made housing home made steel tubes costum 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 allows insertion into implanted Venflon tubes e Without any housings
46. diode lamps an optical fiber as signal transducer plastic or glass fiber a photodetector photodiode photomultiplier tube CCD array the optical sensor indicator immobilised in a solid matrix syringe needle glass fiber with its sensor tip i sensor housing mmm Figure 13 4 Scheme of a microsensor microoptode ST SPEDE Figure 13 3 Schematic drawing of the optical setup of a measuring system with microsensors LED light emitting diodes PMT photomultiplier OF optical filters ST fiber connector Appendix 83 13 1 3 Advantages of Optical Oxygen Sensitive Microsensors no oxygen is consumed during the measurement e the signal is independent of changes in flow velocity e high spatial 50 um and temporal resolution t lt 1 s 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 ppb range 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 polarisation information such as decay time or delayed fluorescence 13 1 4 Luminescence Decay Time The MICROX TX3 measures the luminescence decay time of th
47. e Compensation of the Response of Oxygen Sensors 94 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 lt 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 internal 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 Their signal does not depend on the flow rate of the sample Diameter of the micro sensor tip is 50 um Fast response time better than 1 s Measures oxygen in both liquids and the gas phase 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 you applications
48. e atmospheric pressure of the calibration is needed to convert the oxygen unit air saturation into partial pressure units hPa Torr or concentrations units mg L mol L Please note that changes in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentrations units mg L umol L but the oxygen units 96 air saturation and oxygen saturation have to be corrected for air pressure changes 7 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 sensor has been dipped about 1 2 cm into the calibration solution 8 The 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 GLASS FIBER WITH ITS SENSOR TIP IS PUSHED OUT HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK 9 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 of Oxygen Sensitive Microsensors 65 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 cryst
49. e immobilised luminophore as the oxygen dependent parameter 1 f Os 2 The MICROX TX3 uses the phase modulation technique to evaluate the luminescence decay time of the indicators If the luminophore is exited with a sinusoidally intensity modulated light its decay time causes a time delay in the emitted light signal In technical terms this delay is the phase angle between the exiting and emitted signal This phase angle is shifted as a function of the oxygen concentration The relation between decay time qt and the phase angle is shown by the following equation tan o 3 Jr fod Gg tano 21 f t 3b t tan P o sf O 3c t luminescence decay time phase angle fimog modulation frequency Lu max 1 0 0 9 0 8 0 7 0 6 0 5 0 4 4 0 3 0 2 4 0 1 4 0 0 5 0 5 10 15 20 25 30 time ys 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 Appendix 84 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
50. eY 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 23 Description of Microx TX3 Software 24 Clear Charts The graphs shown on the display is cleared Dimensions d Dimension Settings Choose the dimensions for the chart X axis ticks fi DU m Y axis minimum fo Y axis maximum iod X Cancel Pile Es You can adjust the number of measurements points on the x axis shown in the display maximum number of points are 5000 Furthermore you can adjust the minimum and the maximum of the y axis The AutoScaleY1 function is switched off Print Charts The charts shown in the display can be printed Settings ComPort The serial comport 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 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 Description of Microx TX3 Soft
51. easing the temperature by 1 K 59 4 y 59 77 0 08037 x T 0 0505 0 0485 e 58 9 E 4 w 0 0465 8 58 4 a E 0 0445 amp 57 9 L P 7 0 0425 57 4 i 0 0405 E 96 9 T 1 0 0385 y 20 0353 3 83 10 x i R 20 998 56 4 0 0365 3 5 10 4 20 5 30 4 40 4 temperature C Figure 13 13 Effect of the temperature on and the Stern Volmer consant Ksy Consequently variations in the temperature causes variations in the measuring value at a constant oxygen content see Figure 13 11 Table 13 8 displays the deviation of the measuring value from the real oxygen content depending on temperature and the oxygen content Tabelle 13 8 Variation of the measured oxygen content A 96 air saturation at a constant oxygen content and variations in temperature by 1K 96 air saturation 30 96 100 96 250 96 A air saturation K 0 56 1 72 96 t 4 68 96 Example If the temperature is measured with a precision of 0 2 C there is a variation in the measuring value at 10096 air saturation of 100 0 3 air saturation
52. ed against being put back into operation f 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 is visibly damaged no longer operates as specified has been stored under adverse conditions for a lengthy period of time has been damaged in transport f you are in doubt the instrument should be sent back to the manufacturer for repair and maintenance The operator of this measuring instrument must ensure that the following laws and guidelines are observed when using dangerous substances EEC directives for protective labor legislation National protective labor legislation Safety regulations for accident prevention Safety data sheets of the chemical manufacturer The Microx TX3 is not protected against water spray The Microx TX3 is not 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 Safety Guidelines 3 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 Loligo and under antistatic conditions Needle type sensors are housed in ex
53. etnnetnnetnneenne 17 5 2 3 Implantable Microsensors eese eene nennen nnne nnne eniti rennen ntt nnn ntn rennen 19 6 Description of Microx TX3 Software eeeeeeeeeeeeeeeeennnnnnene 21 6 1 Software Installation and Starting the Instrument 21 6 2 Function and Description of the Microx TX3 Program 22 6 2 1 uiri 23 6 2 2 referri 28 6 2 3 Graphical Window siet reU eto pere eR RI er in ete Ora 33 6 2 4 EE LEE 34 6 3 Subsequent Data Handling siiversecsiscccceissendeeiisatnessivandentascsesecadecestdivedanecivendvsdi sens 34 7 Calibration of Oxygen Sensitive Microsensors eese 36 7 1 Calibration of Needle Type Oxygen Microsensors 36 7 1 1 Preparation of the Calibration Standards nennen 36 7 1 2 Mounting the Needle Type Microsensors AAA 37 7 1 3 Calibration without Automatic Temperature Compensaton 39 7 1 4 Calibration with Automatic Temperature Compensation senes 43 7 1 5 Manual Calibtation oec tene heirs ae ree Yet Ee hie He Espere d sen E eee Even 46 7 2 Calibration of Flow Through Housed Oxygen Microsensors 48 7 2 1 Preparation of the Calibration Standards 48 7 2 2 Mounting the Flow Through Housed Oxygen Microsensors sseesseeeseeseeseerirerereresensernenn 48 7 2 3 Calibration with
54. fi 013 mbar 1st point phase temperature DU air sat f7 Ps i jez jo se 2nd point phase temperature 100 air sat p kr zo fo aje JA Store current value amplitude phase This will overwrite the exsisting calibration values Afterwards wash the glass fiber with its sensor tip with distilled water to clean it from sodium sulfite Don t retract the sensor tip 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 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 Now you have 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 inside 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 and temp
55. 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 Measurement 71 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 100 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 temperature sensor nor its cable can touch the microsensor 4 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 5 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 User Defined calibration which is described in chapter 7 3 5 6 The glass fiber with its sensing tip is prevented from slipping from the glass housin
56. g 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 don t touch the glass housing with the glass fiber tip WHEN GLASS FIBER WITH ITS SENSOR TIP IS EXTRACTED FROM THE PROTECTIVE HOUSING HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK 7 Becarefully by implanting the microsensor into your specially designed system Please contact our service team for custom desingned systems 8 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 4 Some Advice for Correct Measurement 8 4 4 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
57. he sensor tip that is flat broken TF containing the oxygen sensitive fiber tip with additional optical isolation YOP 6 Thi 6 1 1 Description of Microx TX3 Software 21 Description of Microx TX3 Software s software is compatible with Windows 95 98 2000 Millenium NT4 0 XP Software Installation and Starting the Instrument Insert the supplied disc CD into the respective drive Copy the file TX3v531 exe onto your hard disk for example create C MICROXTX TX3v531 exe Additionally you may create a link Icon on your desktop 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 Connect the power supply 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 If the 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 And choose the right com port With a right mouse click onto com port you are able 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 SR ss Descr
58. ibration 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 and temp at 0 values 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 Menu 2 Point calibration without temperature sensor atm pressure 11013 mba 4st point phase ee D air sat b pss pp ae iV S Store current value 2nd point phase temperature 100 air sat p p zo fo zie J Store current value amplitude phase A Einish X Cancel 10 Calibration of Oxygen Sensitive Microsensors 53 Calibration Message X This will overwrite the exsisting calibration values X Cancel Now calibration is complete Confirm the calibration values by clicking the Finish button Now you have 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 Repeat this washing pro
59. in the actual atmospheric pressure have no effect on the partial pressure units hPa Torr and concentrations 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 of Oxygen Sensitive Microsensors 51 Calibration Menu 2 Point calibration without temperature sensor be Ju spo RN ze _o Store current value Store current value amplitude phase X Cancel V Einish Connect one of 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 of Oxygen Sensitive Microsensors Wait about 30 sec 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 100 air sat and temp at 100 values 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 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 cal
60. ioxide SO and gaseous chlorine Cl Both of them mimic higher oxygen concentrations Fiber Optic Oxygen Microsensors Sensors and Housings 5 1 2 Design of the Sensor Tips All the sensors mounted in different housings are available with two different glass fiber tips A a lt 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 Advantages microsensors with a tapered tip flat broken tip e high spatial resolution lt 50 um e more photostable than tapered ones e very fast response times tg up to 1 s in gt long term stable the liquids and 0 2 s in the gas phase e more robust Disadvantages of microsensors with a Disadvantages of microsensors with tapered tip flat broken tip e fragile e response times teo in the order of 30 s e display photobleaching Response time The response time oo 90 of the signal change has occurred in water is dependent from the sensor tip size and typical ranges from 1s 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
61. iption of Microx TX3 Software 6 2 Function and Description of the Microx TX3 Program The window shown below is displayed after starting the software microx 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 gt OxyView TX3 V5 31 File Charts Display Print Settings Measurement Calibration OXYGEN KN e Logging Status TEMPERATURE amp ambient light m off line C Display Raw Values MEASURE CHART INFO start time 00 00 00 numerical display measurement time start 00 00 00 21 53 53 22 Description of Microx TX3 Software 6 2 1 Menu Bar gt Oxygen gt Zoom gt AutoScaleyY1 gt Undo Zoom gt Amplitude gt Clear Charts gt Temperature mm Satins gt Charts gt Com Port gt Instrument Info gt analog settings gt LED Intensity File Exit Closes the program Charts The respective charts of the measurement can be displayed v or 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 AutoScaleY 1 Clear Charts Undo Zoom D Dimensions AutoScal
62. 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 e penetration probe for insertion into semisolids like sediments or biofilms e easy to handle and robust e sterilizable H2O EtO EtOH e not autoclavable since the syringe is made out of polypropylene For autoclavable needle type probe housings please contact our service team Measuring range from 0 to 250 air saturation 0 22 6 mg L e Limit of detection 0 2 96 air sat 20 umol L Fiber Optic Oxygen Microsensors Sensors and Housings Schematic drawing of a needle type housing microsensor male fiber optic plug L safety nut gt fiber cable gt syringe plunger gt syringe housing transport block gt needle plastic base protective plastic cap gt syringe needle uU spring needle plastic base syringe needle glass fiber sensor tip Fiber Optic Oxygen Microsensors Sensors and Housings Ordering information EXHECHCIHTIHSCOHS
63. libration data Calibration of Oxygen Sensitive Microsensors 62 Calibration Menu 2 Point calibration without temperature sensor atm pressure fi 013 mbar 1st point phase temperature D 95air sat ps i zl jo ze 2nd point phase temperature 100 96air sat p kr 2 zo fo aje Jf Store current value amplitude phase This will overwrite the exsisting calibration values X Cancel 10 Afterwards wash the sensor tip with distilled water to clean it from sodium sulfite Make 11 sure not to touch the sensor tip Retract the glass fiber back into the protective glass housing without absorbing water Now you have 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 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
64. libration should be applied if you don t 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 Switch on the Microx TX3 oxygen meter Start the Microx TX3 software on your computer and click the Calibration menu item e de D c Select the calibration routine calibrate manually and click the manual button Calibration of Oxygen Sensitive Microsensors 68 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 0 air sat temp at 0 and 100 air sat temp at 100 Calibration Menu 2 Point calibration user defined atm pressure f 013 mbar 1st point phase temperature Larne bah coe Lu 2nd point phase temperature Do ainsa 2428 Ja feo je ze 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 ES This will overwrite the exsisting calibration values X Cancel Measurement 69
65. ltage 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 measurement 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 79 11 Trouble Shooting Device does not work and LED Device is not switched on Switch on device with ON OFF on the front panel is not lit switch on the rear panel Connect power supply with No power supply device Device does not work and LED No connection to PC Check connection of the device on the front panel is on to your PC RS 232 Temperature compensation PT 1000 sensor is not connected Check connection failed no temperature properly measurement possible PT 1000 Sen
66. ly and click the Store current value button to store the 0 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 11 Calibration of Oxygen Sensitive Microsensors 55 Calibration Menu 2 Point calibration with temperature sensor atm pressure 1013 mbar 4st point phase temperature D air sat po fea s po fs SC f Store current value 2nd point phase temperature 100 air sat s Ak fo kr amplitude phase temperature S Einish _2 cance This will overwrite the exsisting calibration values X Cancel Now calibration with temperature compensation is complete Confirm the calibration values by clicking the Finish button Now you have 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 7 2 5 Manual Calibration A manual calibration should be applied if you don t want to calibrate your sensor again However this is only possible if you already know the calibration values
67. mg ul lppm o 1000000 1kg 1L 10000 Appendix 87 Partial pressure of oxygen in hPa po hPa p hPa pw T hPa 3 0 2095 13 in mbar Po mbar Pon bar py T mbar IE D 0 2095 14 in Torr Po Torr nm Py T mbar La 0 2085 0 75 15 Please note 1 mbar 1 hPa 0 750 Torr Oxygen Concentration in mg L T ir i M co mg L Pam Bal air saturation ou 5995 acr 1000 MG 16 Py 100 Va in ppm T ir i M co ppm Pam PwC 7b air saturation o 2095 acr 10 MO a7 Py 100 Vu in uumol L coU ir j M Co umol L Pam Bel air saturation o zue ery 1000 242 3135 as Pn 100 Vu Damm 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 o T Bunsen absorption coefficient at temperature T M O5 molecular mass of oxygen 32 g mol Vy molar volume 22 414 l mol Appendix 88 13 4 Temperature Dependent Constants Affecting the Oxygen Content 13 4 1 Water Vapor Pressure As shown in equation 13 18 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 19 p O2 oxygen partial pressure in dry air at a barometric pressure pam 0 2095 volume content of oxygen in air Oxygen parti
68. 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 doesn t touch the microsensor Extend the glass fiber with its sensor tip wait about 30 s until the phase angle and the temperature is constant the variation of the phase angle and 11 12 13 Calibration of Oxygen Sensitive Microsensors 46 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 Now calibration with temperature compensation is complete Confirm the calibration values by clicking the Finish button Pull the glass fiber with its 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 7 1 5 Manual Calibration A man
69. mpensation click the on 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 xd Enter the temperature during the measurement e kn zio d pe 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 measurement Temperature Compensation Eccl Enter the temperature during the measurement C on ze fo 3e Logging Setup To strat the measurement without logging data click Measure in the Logging setup and the Start button Logging Setup EE Measure C Measure amp Log File Desciption j 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 Dt Click the speichern button to confirm your settings Description of Microx TX3 Software 32 Data file selection Speichern 3 Eigene Dateien si e EI ex E3 adobe a Eigene Bilder a Eigene Musik my eBooks Dateiname Dateityp Data Files t t D Abbrechen He location file name File Desciption enter the description here
70. 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 Calibration of Oxygen Sensitive Microsensors 40 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 and click the cal button Measurement Calibration calibrate with temperature sensor cal 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 concentrations 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 concentrations 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 0 airsat s Tu zl jo a
71. n measuring the cal 100 standard the sensor worked perfectly during the whole measurement General Instructions 74 9 General Instructions 9 1 Warm Up Time The warm up time of the electronic and opto electronic 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 3 Service Balancing maintenance and repair work may only be carried out by the manufacturer Loligo Systems ApS Niels Pedersens All 2 DK 8830 Tjele Denmark Phone 45 8999 2545 E mail mail loligosystems com Internet www loligosystems com 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 75 10 Technical Data 10 1 General Data oxygen range 0 500 96 air saturation resolution 30 0 3 air aturation 100 0 9 96 air saturation 250 3 6 air saturation accuracy t 1 96 air saturation temperature
72. nd 2 another one for external trigger input See figure below The electrical specifications of all rear panel connectors are given in technical specification sheet Please read also the technical notes to avoid mistakes ELEMENT DESCRPTION FUNCTION Line adapter for power Connector for 9 36 V DC power supply supply C3 RS232 interface Connect the device with a RS232 data cable to your male PC Notebook here Analog out Connect the device with external devices e g a data channel 1 logger Analog out Connect the device with external devices e g a data channel 2 logger T1 External trigger input 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 0 500 air saturation 9 36 V supply voltage or 220 110V AC adaptor RS 232 interface robust metal box Features 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 133 MHz 16 MB RAM e RS 232 Cable e Line adapter 110 220 V AC 12 V DO 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 s
73. nsitive Microsensors 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 one gram sodium sulfite Na2SO3 to the vessel and label it cal 0 2 Dissolve NazSOz3 in 100 mL water Water becomes oxygen free due to a chemical reaction of oxygen with Na2SO3 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 Na SO and to ensure that water is oxygen free Close the vessel after calibration with a screw top to minimize oxygen contamination To prepare oxygen free water you also can use sodium dithionit Na2S2O 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 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
74. nt and the calibration process are allowed to be different 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 Start the Microx TX3 software on your computer and click the calibration menu item Select the calibration routine calibrate without temp sensor and click 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 concentrations 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 concentrations 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 of Oxygen Sensitive Microsensors 60 Calibration Menu 2 Point calibration without temperature sensor atm pressure 1013 Zi mbar 1st point phese temperature D air sat pe fso 2 rz fo zie A Store current value 2nd point temperature phase ioo sarsa pr Apo ze amplitude phase A Einish X Cancel
75. out Automatic Temperature Compensation sse 50 7 2 4 Calibration with Automatic Temperature Compensation sese 53 7 2 5 Manual GalibratiOri iar Dr je ben e egre oct b D e Ep A PED de eg 55 7 3 Calibration of Implantable Oxygen Microsensors eeeeeee 57 7 3 1 Preparation of the Calibration Standards AAA 57 7 3 2 Mounting the Implantable Microsensors AAA 58 7 3 3 Calibration without Automatic Temperature Compensaton 59 7 3 4 Calibration with Automatic Temperature Compensaton esee 63 7 3 5 Man al Galibr amp tioh iuo crie coe EE 67 Table of Contents 8 EE EE 69 8 1 Measurement with Needle Type Oxygen Microsensors 69 8 2 Measurement with Flow Through Housed Oxygen Microsensors 70 8 3 Measurement with Implantable Oxygen Microsensors 71 8 4 Some Advice for Correct Measurement esee eene nennen nnn 71 8 4 1 Signal drifts due to oxygen gradients eeseseeeeeeeeeeeeteeinttnttetttestrattnetnettnerntennnennnennsennce 71 8 4 2 Signal drifts due to temperature gradients 72 8 4 3 Signal drift due to Ghoto decompoeiton ee eeeeeeeteeeeeeeteneeeeeeeteaeeeeaeeseaeeseaeeseaeeseaeeteeeseeeteas 72 8 4 4 Performance proof tet i e E PP ID HC ERU CHEER CHRIS 738 GC E RE OT e EE 74 9 1 Warm Up TIME ste ei ee 74 9 2 Maintenances ecc 74 9 3 TEE 74 1
76. perature Compensation C off Enter the temperature during the measurement 2 zo jp pe Logging Setup Measure C Measure amp Log File Desciption er the di 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 measuring point is recorded The speed of recording a measurement point in the 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 Please note The sensor shelf life can be increased using a slower measuring mode since the effect of photo bleaching 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 The dynamic average defines number of averaged measured values The higher the running average the longer the time sampling time used for averaging The bh z samptes higher the running average is set the smoother the measurement signal maximum 25 samples The default setting is 4 Dynamic Averaging Description of Microx TX3 Software 31 Temperature compensated oxygen measurements If you want to measure with temperature co
77. rature 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 If 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 sensitive Avoid mechanical stress as far as possible Measurement 70 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 to your sample glass fiber sensor tip wrong position of the sensor tip syringe needle gas reservoir right position of the sensor tip There is an air reservoir inside the syringe needle The oxygen content inside the syringe needle is different to that of the sample since the gas exchange rate is slow Sensor tip must be outside for measurement and calibration 7 Ple
78. s The small outer dimensions low power consumption and robust box makes 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 exits the possibility to combine several single Microx TX3 oxygen meter to obtain a multichannel system It allows the mmm user to create a 2 3 4 or more channe 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 ST fiber connector Connect the fiber optic oxygen microsensor here red instrument off Li a green instrument on orange stand by Temp Connector for PT 1000 Connect the PT 1000 temperature sensor for temperature sensor temperature compensated measurements here Description of the Microx TX3 Device Rear Panel of the Microx TX3 device Two standard BNC connectors are added for analog output channels 1 a
79. s tapered sensor tip lt 0 6 air saturation 1 96 air saturation 1 6 air saturation flat broken sensor tip lt 0 5 air saturation lt 0 5 air saturation lt 0 6 air saturation Fiber Optic Oxygen Microsensors Sensors and Housings 100 80 60 40 air saturation 20 0 2 4 6 8 10 12 14 16 18 20 22 24 time h Figure 5 4 Photostability of a tapered oxygen microsensor 5 1 3 Optical Isolation Optical isolated sensor tips are required if your sample shows intrinsic fluorescence between 600 700 nm Consequently an optical isolation is recommended measuring in whole blood urine or chlorophyll containing samples Using optical isolated sensors exclude the impact of colored samples and ambient light on measurements Furthermore an additional optical isolation improves chemical resistance of the sensor membranes Optical isolated sensor tips of oxygen microsensors enable measurement in photosynthetically active samples since stimulation of photosynthesis due to emission of blue green light from the fiber tip is avoided We offer additional optical isolation for all types of sensor However using optical isolated sensor tips the tip diameter increases to 60 80 um whereas tip diameter of non isolated sensor tips is typically 30 to 40 uim for tapered microsensors Since the response time of the microsensor is dependent from the diffusion rate of oxygen through the sensor layer additional op
80. s is from 0 to 50 pure oxygen 250 air saturation However it is also possible to measure oxygen up to 100 Please contact the Loligo service team to get the appropriate software when measuring up to 100 oxygen Table 5 1 displays the measuring range of microsensors in different oxygen units Fiber Optic Oxygen Microsensors Sensors and Housings Table 5 1 Specifications of the OXY 4 micro device and the respective oxygen microsensors INSTRUMENT Channels 1 x optical channel ST connector Core Center 100 140 designed for micro sensors 1 x PT100 PT1000 con nector Dissolved Oxygen Gaseous Oxygen Measurement range 0 45 mg L ppm 0 500 air sat 0 100 oxygen sat 0 1 4 mmol 0 760 Torr 0 1013 hPa Limit of Detection LOD 0 2 air saturation 0 41 hPa 20 ppb dissolved oxygen 0 30 Torr Resolution at 20 C and 1013 hPa 0 09 0 005 mg L ppm 2 72 0 01 mg L ppm 1 0 05 96 air sat 30 0 13 96 air sat 100 0 44 air sat 250 1 8 96 air sat 9 06 0 04 mg L ppm 22 65 0 17 mg L ppm 0 21 0 01 96 oxygen 6 3 0 03 oxygen 20 9 0 09 oxygen 52 4 0 38 oxygen 2 83 0 14 umol 85 0 0 3 umol 1 55 0 08 Torr 46 7 0 20 Torr 155 5 0 65 Torr 388 8 2 65 Torr 283 1 1 3 umol 798 0 5 2 umol 2 0 1 hPa 60 0 26 hPa 200 0 87 hPa 500 3 54 hPa Response time tog for tapered sen
81. saturated water at a temperature 0 of 20 C Equation 24 allows the solubility of oxygen in air saturated fresh water to be calculated for any temperature and pressure provided that the values of the Bunsen absorption coefficient a T and the vapor pressure pw T at the particular temperature are known Equation 23 or 23 can be used to obtain o and pw can be calculated from equation 21 Table 13 3 gives oxygen solubilities in mg L for temperature intervals of 0 1 C from 0 40 C e M c P60 Pan Pw o 2995 9 9 25 Pn Nu In equation 25 pa is the actual atmospheric pressure corrected for the contribution of the water vapor pressure py and related to standard pressure py The corrected pressure is multiplied by 0 2095 the volume content of oxygen in air by 8 and by the molecular mass of oxygen Moz divided by the molar volume Vy At a given atmospheric pressure of 1013 mbar Pam py and a temperature of 20 C the oxygen content can be calculated according to equation 26 c 1013mbar 20 C 1013 23 3 0 2095 0 031 32 g mol E 0 009g L 9 06 mg L 26 1013 22414mol L Figure 13 9 shows the temperature dependent oxygen solubility in air saturated fresh water and Table 13 3 gives oxygen solubilities in mg L for temperature intervals of 0 1 C from 0 40 C as calculated via equation 25 and 23 for the Bunsen absorption coefficient Appendix 15 14 Gell mg L Py pw T Py 0 2095 o 0 10 Moy Viy 13 c O
82. sor is faulty Contact our service Warning light Amplitude red Microsensor is not connected Check connection of the ST properly connector ST Connector is contaminated Clean connector with a soft lint free cloth rag Sensor tip is damaged Replace oxygen sensor Send the sensor back to us for re coating service Warning light Phase red phase angle out of limits check connection of the microsensor replace microsensor Warning light overload red too much false light reduce false light use optical isolated microsensors calibration failed calibrate again check calibration solutions Sensor was not in the right Immerse Sensor in the proper calibration standard calibration vessel sulfite solution has aged Prepare fresh sulfite solution Strong signal fluctuations Air bubbles at sensor tip Remove air bubbles by carefully The glass fiber with its sensor tip tapping is not extended from the syringe Completely extend the sensor needle Concluding Remarks 80 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 loligosystems com With best regards Your Loligo Team Appendix 81
83. sors lt 1 s without optical isolation 5s with optical isolation 0 5 s without optical isolation 1 s with optical isolation Response time too for flat broken sensors lt 15 s without optical isolation lt 30 s with optical isolation lt 5 s without optical isolation 10 s with optical isolation Accuracy at 100 air sat 20 C t 196 at 100 96 air saturation 0 1596 at 1 96 air saturation Temperature PT1000 Range Resolution Accuracy 0 50 C 0 5 C 1 C Digital interface RS 232 interface with galvanic isolation 19200 Baud Databits 8 RJ connector RJ 6 4 SUB D 9 cable for RS232 PC port included Analog outputs Dual 12bit programmable outputs with BNC connectors galvanic isolation Specification Range Resolution Accuracy Analog output Oxygen 0 400 air sat 0 2 air sat 0 5 air sat Analog output Temperature PT1000 0 50 C 0 2 C 1 C External Trigger TTL compatible with galvanic isolation BNC connector Acquisition time Programmable default 1 second min 250 ms Power supply 12 VDC max 550 mA 110 240 VAC 50 60 Hz adapter SOFTWARE OxyView Oxygen units User selectable from air saturation oxygen saturation hPa Torr mg L ppm pmol Compatibility Windows 95 98 2000 Millenium NT4 0 2000 XP Calibration Conventional two point calibration with
84. t of the LED intensity is finished when in the status window the message Auto adjustment finished appears Click the Close button to confirm the settings LED Intensity Adjust Auto Adjust Advanced Description of Microx TX3 Software 27 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 Auto Adjust Advanced LED Intensity 45 Z amplitude 11092 Please note that 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 x The calibration values are no longer valid Please recalibrate the sensor af Calibration 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 Analogue 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 973mV 97 3 air satur
85. the label 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 air is water vapor saturated Calibration of Oxygen Sensitive Microsensors 37 7 1 2 Mounting the Needle Type Microsensors 1 Remove the microsensor carefully from the protective cover The needle type microsensor is housed in 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 H transport B A protective block plastic cap 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 H transport A protective blocking plastic cap Calibration of Oxygen Sensitive Microsensors 38 3 Fix the microsensor with a clip to a laboratory support or a similar stable construction We expressly warn you not to handle with 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
86. the microsensor is protected with a glass housing during the transport e Sterilizable autoclave 130 C 1 5 atm EtO EtOH H202 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 31 Jieoo um 7 tip outer Um cable sensor tip 140 um bare glass outer plastic cable fiber inner plastic cable ST connector male fiber plug Fiber Optic Oxygen Microsensors Sensors and Housings Ordering Information we Hesu Hat Tiet Tel TH or Shape of Sensor Tip implantable S sharp tip 50 um housing F flat broken tip 140 um outer plastic cable Diameter um length m length of bare glass fiber 900 um 0 10 Diameter um length mm Oxygen Sensitive 140 um 1 to customer request Optical Isolation Coating 0 250 a s inner plastic cable Y with optical isolation diameter um length cm N without optical isolation 600 um 0 to customer request Example With this code you will 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 900 5 the inner plastic coating 600 um 1 cm 600 1 and a bare glass fiber length 2 140 um of 2 mm 140 2 T
87. tical isolation of course increases the response time fol to 3 7 seconds while the response time ts of non isolated sensors is 1 3 seconds Fiber Optic Oxygen Microsensors Sensors and Housings 5 2 Housings of Oxygen Sensitive Microsensors The 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 Of course it is possible to build customer specific housings Please feel free to contact our service team to find the best solution for your application We offer the following standard designs Needle type housing NTH Flow through cell housing Implantable IMP oxygen oxygen microsensor FTCH oxygen microsensor microsensor Fiber Optic Oxygen Microsensors Sensors and Housings 5 2 1 Needle Type Housing Oxygen Microsensors transport block needle plastic gp base protective plastic cap Features e high spatial resolution We offer highly flexible needle type oxygen microsensors Needle type oxygen microsensors are miniaturized optical chemical oxygen sensors designed for all research applications were a small tip size lt 50um 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
88. tremely sharp syringe needles Avoid injury by handling the needle carefully Please pay attention to all safety guidelines for safe handling of sharp needles and syringes Beware of injuring with the needle as well as with the sensor tip The glass fiber can break if pricked into the skin and can cause inflammation 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 PT100 PT1000 temperature sensor power supply and needle type 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 microsensors must not be used in vivo examinations on humans The Microx TX3 and the microsensors must not be used for human diagnostic or therapeutically purposes Description of the Microx TX3 Device 4 3 Description of the Microx TX3 Device The Microx TX3 is a precision temperature compensated oxygen meter designed for fiber optic oxygen microsensor
89. ual calibration should be applied if you don t 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 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 and click the manual button Calibration of Oxygen Sensitive Microsensors 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 0 air sat temp at 0 and 100 air sat temp at 100 Calibration Menu 2 Point calibration user defined atm pressure f 013 mbar 1st point phase temperature D air sat foe fas r alpo je zc 2nd point temperature 100 air sat feo je zie 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 existing calibration values Click the Continue button to store the new calibration data Calibration Message ES This will overwrite the exsisting calibration values X Cancel Calibration of Oxygen Se
90. urrent 075 Ref LED amplitude 106091 Frequency 005 Sending interval 0001 Averaging 21 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 WW 096 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 airsatur 06 01 03 13 12 09 0 000 101 510 06 01 03 13 12 10 0 017 101 410 06 01 03 13 12 11 0 034 101 370 06 01 03 13 12 12 0 051 101 960 06 01 03 13 12 13 0 069 101 640 06 01 03 13 12 14 0 085 101 530 06 01 03 13 12 15 0 102 101 710 06 01 03 13 12 16 0 119 101 730 06 01 03 13 12 17 0 136 101 710 06 01 03 13 12 18 0 154 102 080 06 01 03 13 12 19 0 170 101 460 06 01 03 13 12 20 0 188 101 790 06 01 03 13 12 21 0 205 101 760 06 01 03 13 12 22 0 222 101 920 06 01 03 13 12 23 0 239 101 820 06 01 03 13 12 24 0 256 101 990 06 01 03 13 12 25 0 273 102 560 phase 27 90 27 91 27 92 27 85 27 89 27 90 27 88 27 88 27 88 27 84 27 91 27 87 27 88 27 86 27 87 27 85 27 79 amp
91. w data of phase angle and amplitude are displayed next to the warning lights 6 2 3 Graphical Window amplitude 31059 E phase 27 66 amp ambient light de Raw vale 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 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 Description of Microx TX3 Software 34 6 2 4 Status Bar COM1 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
92. ware Instrument Info IDENTIFICATION PHIboard number 20020072 PM number 20020053 Serial number TX3 AOT opt1 8 03 004 MUX channel X OFF 00 PARAMETERS Signal LED current 170 Ref LED current 175 Ref LED amplitude 73856 Frequency 005 Sending interval 0001 Averaging sa Internaltemp 24 4C SYSTEM SETTINGS APL function ON Temp compensation ON ch a chAtchBt ON Oxygen unit 96a s Software Info SOFTWARE VERSION OxyView TX3 V5 31 Se PreSens Se l 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 waw presens de Description of Microx TX3 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 just click the button Start Auto Adjust Please check that the oxygen microsensors has been connected to the instrument LED Intensity Adjust Auto Adjust Advanced Status The automatically adjustmen
93. 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 sl male fiber plug 74 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 Calibration of Oxygen Sensitive Microsensors 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 2 transport blocking sensor tip WHEN GLASS FIBER WITH ITS SENSOR TIP IS PUSHED OUT HANDLE WITH CARE THE GLASS FIBER IS UNPROTECTED AND MIGHT BREAK 7 1 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
94. x the glass housing microsensor with a clip to a laboratory support or a similar stable construction fiber cable protection tubing i j glass fiber with its ST connector Be sensitive tip We strongly advise you not to handle with microsensors without the support especially when the sensor tip is extended 3 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 male fiber plug Calibration of Oxygen Sensitive Microsensors 59 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 measureme

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