Develop and characterize a flow metering standard down to 1 nl/min

Transcription

1 Develop and characterize a flow metering standard down to 1 nl/min Martin Ahrens FH Lüebeck, Germany EMRP Researcher Grant HLT07- REG2 1

2 Project aims HLT07- REG2 develop and characterize of a flow metering standard down to 1 nl/min uncertainty lower than 0.5 % under standard environmental conditions evaluate existing microfluidic devices with focus on their behavior for pulsating flow 2

3 Measurement priciple: front tracking system B C A x 0 x 1 3

4 Measurement priciple: front tracking system B C x 1 - x 0 : traveling distance t 1 - t 0 : measurement time R: radius of the capillary A x 0 x 1 3

5 Measurement priciple: front tracking system B C x 1 - x 0 : traveling distance t 1 - t 0 : measurement time R: radius of the capillary A x 0 x 1 3

6 Measurement priciple: front tracking system 3

7 Experimental set- up 4

8 Experimental set- up capillary 4

9 Experimental set- up fluidic connections capillary 4

10 Experimental set- up temperature chamber fluidic connections capillary 4

11 Experimental set- up camera, lens and light source temperature chamber fluidic connections capillary 4

12 Experimental set- up camera, lens and light source temperature chamber fluidic connections capillary linear stage 4

13 Calibration of the position measurement linear stage - meniscus position - meniscus drift > evaporation > leackage gage blocks 5

14 Calibration of the position measurement linear stage - meniscus position - meniscus drift > evaporation > leackage image processing - pixel noise > software > random disturbance gage blocks glass scale 5

15 Calibration of the position measurement linear stage - meniscus position - meniscus drift > evaporation > leackage image processing - pixel noise > software > random disturbance gage blocks glass scale 5

16 Calibration of the position measurement linear stage - meniscus position - meniscus drift > evaporation > leackage image processing - pixel noise > software > random disturbance gage blocks glass scale 5

17 Calibration of the position measurement linear stage - meniscus position - meniscus drift > evaporation > leackage image processing - pixel noise > software > random disturbance gage blocks glass scale 5

18 Calibration of the position measurement linear stage - meniscus position - meniscus drift > evaporation > leackage image processing - pixel noise > software > random disturbance gage blocks glass scale 5

19 Calibration of the linear stage Mitutoyo gage block, grad 1 6

20 Calibration of the linear stage Mitutoyo gage block, grad 1 u all, mm = u gage block + u temperature + u linear stage + u oil = (± 2.2) + (± 1.1) + (± 0.2) + (+ 0.2) µm = / µm 6

21 Uncertainty- pixel noise drift and oscillation of the meniscus in a 150 µm capillary relative front position [mm] time [h] 7

22 Uncertainty- pixel noise drift and oscillation of the meniscus in a 150 µm capillary relative front position [mm] time [h] 7

23 Uncertainty- pixel noise drift and oscillation of the meniscus in a 150 µm capillary relative front position [µm] time [h] 7

24 Uncertainty- pixel noise drift and oscillation of the meniscus in a 150 µm capillary counts sec. sec. 15 sec 60 sec Häufigkeit counts counts distribution [µm] Verteilung [µm] 4.0 Verteilung [µm] sec. sec. 300 sec 600 sec Häufigkeit counts distribution [µm] distribution [µm] distribution [µm] 7

25 Uncertainty- pixel noise drift and oscillation of the meniscus in a 150 µm capillary counts sec. sec. 15 sec 60 sec Häufigkeit counts counts distribution [µm] Verteilung [µm] 4.0 Verteilung [µm] sec. sec. 300 sec 600 sec Häufigkeit counts distribution [µm] distribution [µm] distribution [µm] 7

26 Uncertainty- pixel noise drift and oscillation of the meniscus in a 150 µm capillary counts sec. sec. 15 sec 60 sec Häufigkeit counts counts distribution [µm] Verteilung [µm] 4.0 Verteilung [µm] sec. sec. 300 sec 600 sec Häufigkeit counts distribution [µm] distribution [µm] distribution [µm] 7

27 Calibration of the radius measurement microscope - capillary diameter glass scale 8

28 Calibration of the radius measurement microscope - capillary diameter glass scale microct - variance capillary diameter CT scale 8

29 Calibration of the microct 9

30 Uncertainty - diameter 70 radii, every 50 µm at 4 different positions native maximum CT resolution 330 nm * sub pixeling 1/10 of the native resolution * depends on voltage, current of the cathode and the distance between target and object 10

31 Uncertainty - diameter 70 radii, every 50 µm at 4 different positions native maximum CT resolution 330 nm * sub pixeling 1/10 of the native resolution * depends on voltage, current of the cathode and the distance between target and object 10

32 Uncertainty - diameter 70 radii, every 50 µm at 4 different positions native maximum CT resolution 330 nm * sub pixeling 1/10 of the native resolution radius variation ± 0.6 µm * depends on voltage, current of the cathode and the distance between target and object 10

33 Uncertainty - diameter 70 radii, every 50 µm at 4 different positions native maximum CT resolution 330 nm * sub pixeling 1/10 of the native resolution r 75 = 76.7 ± 0.6, r 150 = ± 0.5 (2σ) radius variation ± 0.6 µm * depends on voltage, current of the cathode and the distance between target and object 10

34 Uncertainty - diameter 70 radii, every 50 µm at 4 different positions native maximum CT resolution 330 nm * sub pixeling 1/10 of the native resolution r 75 = 76.7 ± 0.6, r 150 = ± 0.5 (2σ) > counts radius [µm] * depends on voltage, current of the cathode and the distance between target and object radius variation ± 0.6 µm 10

35 Calibration of the microscope/optical system Edmund optics, NIST- certificated 11

36 Calibration of the time measurement pc clock Time signal (PTB) GPS frequency counter 12

37 Calibration of the time measurement pc clock Time signal (PTB) GPS frequency counter not included 12

38 Results: measurement uncertainty (u) Source of uncertainty Value (±) Front`s displacement uncertainty u 1.2 µm/min 0.2 µm/mm 1.9 µm

39 Results: measurement uncertainty (u) Source of uncertainty Value (±) Front`s displacement uncertainty u for a sampling period Δt 15 s 4 µm for a sampling period Δt 60 s 5 µm for a sampling period Δt 300 s 8 µm for a sampling period Δt 600 s 9 µm 1.2 µm/min 0.2 µm/mm 1.9 µm

40 Results: measurement uncertainty (u) Source of uncertainty Value (±) Front`s displacement uncertainty u for a sampling period Δt 15 s 4 µm for a sampling period Δt 60 s 5 µm for a sampling period Δt 300 s 8 µm for a sampling period Δt 600 s 9 µm Sampling period uncertainty u 1.2 µm/min 0.2 µm/mm 1.9 µm 4 ms 3.6 ms

41 Results: measurement uncertainty (u) Source of uncertainty Value (±) Front`s displacement uncertainty u for a sampling period Δt 15 s 4 µm for a sampling period Δt 60 s 5 µm for a sampling period Δt 300 s 8 µm for a sampling period Δt 600 s 9 µm Sampling period uncertainty u 1.2 µm/min 0.2 µm/mm 1.9 µm 4 ms 3.6 ms Capillary`s radius uncertainty u 0.6 µm

42 Overall uncertainty 14

43 Overall uncertainty 2.6% 14

44 Syringe pump - Nexus

45 Syringe pump - Nexus 3000 oscillating volume flow 15

46 Syringe pump - Nexus 3000 oscillating volume flow correct dosage for extended periods (> 45 minutes) 15

47 Syringe pump - nemesys measurement with the tracking system and a the microskop 16

48 Syringe pump - nemesys measurement with the tracking system and a the microskop oscillating volume flow within minutes correct dosage for extended periods (> 45 minutes) 16

49 Syringe pump - nemesys measurement with the tracking system and a the microskop oscillating volume flow within minutes correct dosage for extended periods (> 45 minutes) 16

50 Flow sensor - LG16 LG16 shows lower flow rates than the front tracking system 17

51 Flow sensor - LG16 LG16 shows lower flow rates than the front tracking system correct measurement in compliance of the given uncertainty at 70 nl/min 6 % deviation at 10 nl/min 18 % deviation at 5 nl/min 17

52 Implantable infusion pump measurement with tracking system 18

53 Implantable infusion pump measurement with tracking system fluctuating volume flow within minutes (± 10 %) - the titanium bellows extends partially out with jerks in generell correct dosaging 18

54 Intercomparison VSL flow source good agreement between flow source and tracking set- up in the lower region (10-20 nl/min) no/bad agreement up from 50 nl/min 19

55 Intercomparison VSL flow source good agreement between flow source and tracking set- up in the lower region (10-20 nl/min) no/bad agreement up from 50 nl/min Possible reason: 19

56 Intercomparison VSL flow source good agreement between flow source and tracking set- up in the lower region (10-20 nl/min) no/bad agreement up from 50 nl/min Possible reason: bubbles 19

57 Intercomparison VSL flow source good agreement between flow source and tracking set- up in the lower region (10-20 nl/min) no/bad agreement up from 50 nl/min Possible reason: bubbles dissolving air in the tubes 19

58 Intercomparison VSL flow source good agreement between flow source and tracking set- up in the lower region (10-20 nl/min) no/bad agreement up from 50 nl/min Possible reason: bubbles dissolving air in the tubes thermal expansion of the connectors? 19

59 Summary the system is capable to measure with minutes AND hours 20

60 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 20

61 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min 20

62 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius 20

63 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius the minimum uncertainty u rel = 2.6 % 20

64 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius the minimum uncertainty u rel = 2.6 % 0.5 % 20

65 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius the minimum uncertainty u rel = 2.6 % 0.5 % the systen is capable to characterise various volume flow devices, such as syringe pumps, flow sensors and implantable infusion pump 20

66 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius the minimum uncertainty u rel = 2.6 % 0.5 % the systen is capable to characterise various volume flow devices, such as syringe pumps, flow sensors and implantable infusion pump Intercomparison with the primary flow source (VSL) SLG (METAS?) Nexus 3000 (VSL, DTI?) 20

67 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius the minimum uncertainty u rel = 2.6 % 0.5 % the systen is capable to characterise various volume flow devices, such as syringe pumps, flow sensors and implantable infusion pump ToDo Intercomparison with the primary flow source (VSL) SLG (METAS?) Nexus 3000 (VSL, DTI?) 20

68 Summary the system is capable to measure with minutes AND hours yet the lower measurement limit is 5 nl/min 1 nl/min the uncertainty is limited by the uncertainty of the capillary radius the minimum uncertainty u rel = 2.6 % 0.5 % the systen is capable to characterise various volume flow devices, such as syringe pumps, flow sensors and implantable infusion pump ToDo Intercomparison with the primary flow source (VSL) SLG (METAS?) Nexus 3000 (VSL, DTI?) Upload Data to BIPM 20

69 Many thanks for your attention The research leading to the results discussed in this report has received funding from the European Metrology Research Programme (EMRP). The EMRP is jointly funded by the EMRP participating countries within Euramet and the European Union. 21