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Optics Express

Optics Express

  • Editor: Andrew M. Weiner
  • Vol. 22, Iss. 9 — May. 5, 2014
  • pp: 11244–11253
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Novel gas sensor combined active fiber loop ring-down and dual wavelengths differential absorption method

Yanjie Zhao, Jun Chang, Jiasheng Ni, Qingpu Wang, Tongyu Liu, Chang Wang, Pengpeng Wang, Guangping Lv, and Gangding Peng  »View Author Affiliations


Optics Express, Vol. 22, Issue 9, pp. 11244-11253 (2014)
http://dx.doi.org/10.1364/OE.22.011244


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Abstract

A novel active fiber loop ring-down gas sensor combined with dual wavelengths differential absorption method is proposed. Two Distributed Feedback Laser Diodes (DFB LDs) with different wavelengths are employed. One LD whose wavelength covered with the absorption line of target gas is used for sensing. Another LD whose wavelength is centered outside the absorption line is used for reference. The gas absorption loss can be obtained by differencing the reference signal and sensing signal. Compared with traditional method of one wavelength employed, it can eliminate the influence of the cavity loss variety and photoelectric device drift in the system efficiently. An Erbium Doped Fiber Amplifier (EDFA) with Automatic Gain Control (AGC) is used to compensate the loss of the light in the ring-down cavity, which will increase the cavity round trips and improve the precision of gas detection. And two fiber Bragg gratings (FBGs) are employed to get rid of amplified spontaneous emission (ASE) spectrum noise as filters. The calibrating ethyne samples of different concentrations are measured with a 65 mm long gas cell in order to evaluate the effect of reference. The results show the relative deviation is found to be less than ± 0.4% of 0.1% ethyne when a certain additional loss from 0 to 1.2dB is introduced to the cavity and the relative deviation of measured concentration is less than ± 0.5% over 24 hours.

© 2014 Optical Society of America

1. Introduction

Since the first demonstration of the high sensitivity of cavity ring-down spectroscopy (CRDS) by O’Keefe and Deacon in 1988 [1

1. A. O’Keefe and D. A. G. Deacon, “Cavity ring-down optical spectrometer for absorption measurements using pulsed laser sources,” Rev. Sci. Instrum. 59(12), 2544–2551 (1988). [CrossRef]

], CRDS has attracted more and more interests and been widely used for weak gas detection [2

2. J. B. Dudek, P. B. Tarsa, A. Velasquez, M. Wladyslawski, P. Rabinowitz, and K. K. Lehmann, “Trace moisture detection using continuous-wave cavity ring-down spectroscopy,” Anal. Chem. 75(17), 4599–4605 (2003). [CrossRef] [PubMed]

,3

3. D. B. Atkinson, “Cavity ring-down spectroscopy: techniques and applications,” J. Am. Chem. Soc. 132(13), 4972 (2010). [CrossRef]

]. Unlike conventional direct measurement schemes [4

4. J. S. Ni, J. Chang, T. Y. Liu, Y. F. Li, Y. J. Zhao, and Q. Wang, “Fiber methane gas sensor and its application in methane outburst prediction in coal mine,” J. Electron. Sci. Technol. China 6(4), 373–376 (2008).

], in which the attenuation of transmitted light through the target gas is measured, CRDS measures the intensity decay rate of an optical pulse as it is ringing down within a high-finesse optical cavity while interacting with the target gas [5

5. H. Waechter, J. Litman, A. H. Cheung, J. A. Barnes, and H.-P. Loock, “Chemical sensing using fiber cavity ring-down spectroscopy,” Sensors (Basel) 10(3), 1716–1742 (2010). [CrossRef] [PubMed]

]. The absorption loss of the target gas can be deduced from the pulse 1/e ring-down time [6

6. P. Zalicki and R. N. Zare, “Cavity ring-down spectroscopy for quantitative absorption measurements,” J. Chem. Phys. 102(7), 2708–2717 (1995). [CrossRef]

]. Within the past ten years, high-finesse optical cavities have been extensively used to increase the sensitivity of gas detection with several obvious advantages, such as a longer effective interaction length of light and gas sample [7

7. G. Berden, R. Peeters, and G. Meijer, “Cavity ring-down spectroscopy: Experimental schemes and applications,” Int. Rev. Phys. Chem. 19(4), 565–607 (2000). [CrossRef]

], an ultra-sensitive detection capability, and a simple experimental setup [8

8. T. von Lerber and M. W. Sigrist, “Cavity-ring-down principle for fiber-optic resonators: experimental realization of bending loss and evanescent-field sensing,” Appl. Opt. 41(18), 3567–3575 (2002). [CrossRef] [PubMed]

,9

9. S. Pu and X. J. Gu, “Fiber loop ring-down spectroscopy with a long-period grating cavity,” Opt. Lett. 34(12), 1774–1776 (2009). [CrossRef] [PubMed]

].

High reflection of mirrors and the stability of precision mechanism are crucial to CRDS. Compared with the conventional cavity ring-down (CRD) structure [10

10. J. Y. Lee, J. W. Kim, Y. S. Yoo, J. W. Hahn, and H. W. Lee, “Spatial-domain cavity ringdown from a high-finesse plane Fabry–Perot cavity,” J. Appl. Phys. 91(2), 582–594 (2002). [CrossRef]

13

13. Y. Chen, K. K. Lehmann, J. Kessler, B. S. Lollar, G. L. Couloume, and T. C. Onstott, “Measurement of the 13C/12C of atmospheric CH4 using near-infrared (NIR) cavity ring-down spectroscopy,” Anal. Chem. 85(23), 11250–11257 (2013). [CrossRef] [PubMed]

], in-fiber ring-down cavity [14

14. M. Jiang, W. G. Zhang, Q. Zhang, Y. P. Liu, and B. Liu, “Investigation on an evanescent wave fiber-optic absorption sensor based on fiber loop cavity ring-down spectroscopy,” Opt. Commun. 283(2), 249–253 (2010). [CrossRef]

16

16. G. Stewart, K. Atherton, H. B. Yu, and B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]

], can be made very robust and inexpensive, avoiding alignment of any free-space components as well as other complications such as the effects of input beam quality and interference [17

17. Z. Q. Tan and X. W. Long, “A developed optical-feedback cavity ring-down spectrometer and its application,” Appl. Spectrosc. 66(5), 492–495 (2012). [CrossRef] [PubMed]

]. Light can be coupled into the loop in a variety of different ways using commercial fiber–fiber couplers [18

18. K. M. Zhou, D. J. Webb, C. B. Mou, M. Farries, N. Hayes, and I. Bennion, “Optical fiber cavity ring down measurement of refractive index with a microchannel drilled by femtosecond laser,” IEEE Photon. Technol. Lett. 21(22), 1653–1655 (2009). [CrossRef]

,19

19. Y. Zhang, M. Zhang, and W. Jin, “Sensitivity enhancement in erbium-doped fiber laser intra-cavity absorption sensor,” Sensor. Actuat. A-Phys 104(2), 183–187 (2003).

], or custom interfaces [20

20. H. Waechter, K. Bescherer, C. J. Dürr, R. D. Oleschuk, and H.-P. Loock, “405 nm absorption detection in nanoliter volumes,” Anal. Chem. 81(21), 9048–9054 (2009). [CrossRef] [PubMed]

], etc.

In order to improve the measurement precision effectively, some works have been done on CRDS with active fiber loop. The active fiber, as the gain medium, is used to compensate the power loss of the laser in CRD and increase the cavity round trips [16

16. G. Stewart, K. Atherton, H. B. Yu, and B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]

,17

17. Z. Q. Tan and X. W. Long, “A developed optical-feedback cavity ring-down spectrometer and its application,” Appl. Spectrosc. 66(5), 492–495 (2012). [CrossRef] [PubMed]

,19

19. Y. Zhang, M. Zhang, and W. Jin, “Sensitivity enhancement in erbium-doped fiber laser intra-cavity absorption sensor,” Sensor. Actuat. A-Phys 104(2), 183–187 (2003).

,21

21. G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

]. Ring-down time of tens of microseconds can readily be achieved and extended to several hundred microseconds [21

21. G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

]. But gain fluctuations noise and amplified spontaneous emission (ASE) spectrum noise will limit the accuracy and repeatability to a certain extent. Some means have been employed to eliminate the noises. For example, G. Stewart et al. [16

16. G. Stewart, K. Atherton, H. B. Yu, and B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]

,21

21. G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

] applied gain clamp compensation to stabilize the gain of the EDFA. N Ni et al. [22

22. N. Ni, C. C. Chan, T. K. Chuah, L. Xia, and P. Shum, “Enhancing the measurement accuracy of a cavity-enhanced fiber chemical sensor by an adaptive filter,” Meas. Sci. Technol. 19(11), 115203 (2008). [CrossRef]

] proposed a digital least-mean-square (LMS) to reduce the ASE noise.

The cavity loss can be deduced from the pulse 1/e ring-down time. Then the concentration of target gas is obtained from the variation of the cavity loss, which is a key factor to measurement precision. In general, it is supposed that the cavity loss is a constant except for the gas absorption loss [16

16. G. Stewart, K. Atherton, H. B. Yu, and B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]

,21

21. G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

,23

23. K. L. Yu, C. Q. Wu, and Z. Wang, “Optical methane sensor based on a fiber loop at 1665 nm,” IEEE Sens. J. 10(3), 728–731 (2010). [CrossRef]

]. In fact, it is inevitable that some external factors (draw, pressure, twist, etc.) will bring a certain loss into the system and cause serious measurement errors especially in remote sensing. It is necessary to select an appropriate signal as reference for the cavity loss in real time.

Differential optical absorption method [24

24. T. Brauers, M. Hausmann, U. Brandenburger, and H. P. Dorn, “Improvement of differential optical absorption spectroscopy with a multichannel scanning technique,” Appl. Opt. 34(21), 4472–4479 (1995). [CrossRef] [PubMed]

29

29. B. Kaldvee, C. Brackmann, M. Aldén, and J. Bood, “Highly range-resolved ammonia detection using near-field picosecond differential absorption lidar,” Opt. Express 20(18), 20688–20697 (2012). [CrossRef] [PubMed]

] gives a good way to obtain reference signal (baseline) for system. Generally, it employs two light sources, one of which is tuned to the absorption line peak to measure the absorption, and another that measured the baseline. It has already been investigated for its merit, such as in remote sensing of atmosphere [24

24. T. Brauers, M. Hausmann, U. Brandenburger, and H. P. Dorn, “Improvement of differential optical absorption spectroscopy with a multichannel scanning technique,” Appl. Opt. 34(21), 4472–4479 (1995). [CrossRef] [PubMed]

,25

25. A. Merten, J. Tschritter, and U. Platt, “Design of differential optical absorption spectroscopy long-path telescopes based on fiber optics,” Appl. Opt. 50(5), 738–754 (2011). [CrossRef] [PubMed]

], especially in lidar system [26

26. S. Kameyama, M. Imaki, Y. Hirano, S. Ueno, S. Kawakami, D. Sakaizawa, and M. Nakajima, “Development of 1.6 μm continuous-wave modulation hard-target differential absorption lidar system for CO2 sensing,” Opt. Lett. 34(10), 1513–1515 (2009). [CrossRef] [PubMed]

29

29. B. Kaldvee, C. Brackmann, M. Aldén, and J. Bood, “Highly range-resolved ammonia detection using near-field picosecond differential absorption lidar,” Opt. Express 20(18), 20688–20697 (2012). [CrossRef] [PubMed]

]. Y.Chen et al. [13

13. Y. Chen, K. K. Lehmann, J. Kessler, B. S. Lollar, G. L. Couloume, and T. C. Onstott, “Measurement of the 13C/12C of atmospheric CH4 using near-infrared (NIR) cavity ring-down spectroscopy,” Anal. Chem. 85(23), 11250–11257 (2013). [CrossRef] [PubMed]

] used a light at a reference wavelength to measure the baseline as reference signal of cavity loss. And a semiconductor optical amplifier (SOA) worked as an optical amplifier as well as a switch to control injection of the laser light into the cavity. But there was no gain in the cavity to compensate cavity loss. Hence, its ring down cavity was consisted of superhigh reflectivity mirrors (over 99.9993%), which was very complicated and needed the alignment of free-space components as well as other complications.

We designed a novel active fiber CRD system based on dual wavelengths differential absorption method. Two lasers of different wavelengths were modulated by taking pulse signal and injected into a same fiber loop alternately. By introducing dual wavelength reference technology, it can eliminate the influence of the cavity loss variety and photoelectric device drift in the system effectively. Two fiber Bragg gratings (FBGs) were employed to get rid of ASE spectrum noise as filters. And then, different concentration ethyne samples were tested in order to further evaluate the effect of reference.

2. Principle

The fiber gas measurement method of CRDS is based on absorption spectrum. When a narrow pulse light is injected into the fiber loop and as the pulse rings around the cavity, a decaying pulse train will be coupled out. The initial intensity of the light is I0. The intensity of the light after one cavity round trip is I [30

30. G. Stewart, K. T. V. Grattan, and B. T. Meggitt, in Optical Fiber Sensor Technology, Kluwer (Academic, 1998).

].
I=I0exp(δ10loge).
(1)
Here δ is the round-trip total loss for the pulse light, which is in the unit of decibel. loge is the logarithm with base 10. The intensity of the light after m times cavity round trips is:
Im=I0exp(mδ/4.343).
(2)
The round-trip time of the pulse light is represented as τ. And the 1/e ring-down time is tr, which is ring-down time constant. Equation (2) can be written:

trτ=4.343δ.
(3)

The round-trip loss for the pulse light contains the total loss and the gain in the cavity, which can be written as [21

21. G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

]:
δ=δt+δin+δc+δgas+δoth-G=δ'+δgas.
(4)
where δt is the fiber loss, δin is the insertion loss of the devices in the cavity, δcis the collimators loss, δgasis gas absorption loss, δothis the other components loss in the cavity, G is the gain in the cavity, δ' is inherent loss of the fiber loop, and δ'=δt+δin+δc+δothG. In Eq. (4) all losses are in the unit of decibel. So the gas absorption loss is

δgas=δδ'
(5)

When δgas is zero, the inherent loss δ' is equal to the round-trip loss with 0% target gas in gas cell.

In general, δgas can be obtained by:
δgas=δδ0
(6)
where δo is the round-trip loss with 0% target gas in gas cell.

The inherent loss δ' doesn’t change ideally, but it is inevitable that some external factors (draw, pressure, twist, etc.) will bring a certain loss into the cavity especially in long distance sensing. That is to say the inherent loss δ' is not constant in fact. So the expression of Eq. (6) is not identical always. It is necessary to calibrate the inherent loss δ' in real time in some practical applications.

The wavelength λ1 locates in an absorption line of target gas. When a narrow pulse light at wavelength λ1 is injected into the fiber loop, a portion of the light will be absorbed by the target gas. So the fiber round-trip loss δ(λ1)will include the target gas absorption loss. To the opposite, the wavelength λ2 is not covered with the target gas absorption line, so the light is not absorbed by the target gas. That is to say, the gas absorption loss is equal to zero at wavelength λ2. According to Eq. (4), the round-trip loss δ(λ2) is always equal to the inherent loss δ'of the fiber loop. When the inherent loss δ' is changed by the external factors, the round-trip loss δ(λ2)will be changed synchronously. The variations of them are equal. So the round-trip loss δ(λ2)can be used as reference of the inherent loss in real time in the system.

By selecting the wavelength λ1 and λ2 to be very close to each other, the inherent losses under these two wavelengths will be the same. So the revised gas absorption loss at wavelength λ1 is
δgas=δ(λ1)δ(λ2)
(7)
where δ(λ1)and δ(λ2) is the round-trip loss at wavelength λ1 and λ2, respectively. So it can efficiently eliminate the influence of the inherent loss variety in the system, by comparing the sensing signal (λ1) with reference signal (λ2).

The absorption relationship between the light power and concentration of target gas is governed by the Beer-Lambert law [30

30. G. Stewart, K. T. V. Grattan, and B. T. Meggitt, in Optical Fiber Sensor Technology, Kluwer (Academic, 1998).

]:
I'=I'0eαLC
(8)
where I' is the intensity of transmitted light, I'0 is the initial intensity of light, α represents the absorption coefficient of the gas, L represents the path length that the light travels through the gas, and C is the gas concentration.

The gas absorption loss can be obtained:

δgas=4.343αLC
(9)

Then the gas concentration can be obtained:

C=δgas4.343αL
(10)

Once the output pulse train is acquired, the 1/e ring-down time and the total loss can be reached. And the gas concentration can be obtained by the value of the gas absorption loss.

3. Experiment system

The configuration of the proposed dual wavelengths active fiber CRD gas detection system was shown in Fig. 1
Fig. 1 Configuration of the proposed dual wavelengths active fiber ring-down gas detecting system (DFB LD: Distributed Feedback Laser Diode; FBG: fiber Bragg grating; PD: photo diode; EDFA: Erbium Doped Fiber Amplifier)
. In this system, the fiber loop is composed with coupler2, coupler3, delay line, gas cell, circulator, FBG1, FBG2 and an EDFA.

Two DFB LDs (LD1 and LD2) are employed, whose wavelengths are λ1 (1530.37 nm) and λ2 (1530nm) respectively. And the output powers of LD1 and LD2 are 5.18mW and 5.23mW respectively under continuous-wave (CW) operation (driving current @50 mA; temperature @25°C). These two LDs are modulated by taking pulse signals and are controlled by a driver alternately. In another words, these two LDs work alternately to insure only one laser signal run in the loop. Temperature control is well done to keep the wavelengths of LDs stable.

The wavelength λ1 locates in an absorption line of target gas (ethyne in this paper). The higher target gas concentration is, the higher round-trip loss is. To the opposite, the wavelength λ2 is not covered with the target gas absorption line, and the light of LD2 is used as reference of the round-trip loss in the system.

The gas cell is formed with a pair of collimators at a distance of 65 mm, whose structure is very simple and stable [31

31. Y. Zhao, Y. Li, T. Zhang, C. Wang, and T. Liu, “Effect of temperature on methane gas concentration by tunable diode laser absorption spectroscopy,” Proc. SPIE 8421, 8421AP (2012). [CrossRef]

]. And its loss is 0.43dB. The split ratios of coupler1, coupler2 and coupler3 are 0.499, 0.987 and 0.989 at 1530nm. The insertion loss of the circulator is 0.7dB. The reflectivity of the FBG1 is 98% at 1530.39 nm and its full width at half maximum (FWHM) is 0.198nm, while the FBG2’s is 98% at 1530.02 nm and its FWHM is 0.203nm. The length of FBG1 and FBG2 is 1cm, and the fiber length between them is about 1cm, so the difference of round-trip time between the sensing signal (λ1) and reference signal (λ2) can be neglected. Temperature control is needed for the FBG when it is used as a filter. A TEC temperature control system is employed to keep the FBGs’ center wavelengths constant. The FBGs are placed on a thermoelectric cooler in free condition with thermally conductive silicone to conduct heat, to make sure the FBGs aren’t affected by any forces. Target temperature is set to 27 °C in this paper. The effect of temperature control is monitored in real time by PC using a RS232 interface. The temperature will keep stable after 2 minutes and the temperature fluctuation is about 0.01 °C.

EDFA with Automatic Gain Control (AGC) is used to compensate the power loss of the laser in the ring-down cavity, which will increase the cavity round-trips and improve the precision of gas detection. Pump (980nm) and controlling circuit are integrated in it. It provides excellent gain flatness with average gain accuracy of ± 0.5dB. As some researches [16

16. G. Stewart, K. Atherton, H. B. Yu, and B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]

,21

21. G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

] mentioned, the gain fluctuations would be observed when EDFA operated, and it would be more serious when the gain was close to the threshold condition. The gain fluctuation can be decreased significantly by AGC, but small signal fluctuations are still observed. It is an efficient way to sacrifice a fraction of sensitivity to get stability. The gain of the fiber loop is kept less than the cavity inherent loss. In order to eliminate the instability of ring-down cavity caused by ASE noise, two FBGs are employed to get rid of ASE spectrum noise as filters. Besides gain noise from EDFA, the photoelectric device drift noise is also a source to worsen sensitivity of the system. In our system, the sensing signal (λ1) and reference signal (λ2) are detected by a uniform detection circuit. Hence, some circuit noise can be eliminated efficiently by comparing the sensing signal (λ1) with reference signal (λ2).

As a note, the EDFA can be placed between port 1 of the circulator and the gas cell, or between the gas cell and the delay line, which is useful to filter the ASE noise by FBGs. But we found that some high frequency noise was brought into the system without optical isolation before the EDFA. In this paper, the EDFA is placed after circulator as shown in Fig. 1. The high frequency noise isn’t observed in this connection sequence. Of course, it is possible to bring a little ASE noise into the loop, but it can be filtered by FBGs before the light is amplified again when the light rings in the loop. Besides, we make the ASE noise leak to the detector as small as possible by adjusting the suitable gain of EDFA. Unlike high frequency noise, the ASE noise only produce a small direct current (DC) signal (offset) which is easier to remove, so that the influence can be neglected.

The DFB LDs emit a 900 ns wide pulse at a 10 kHz repeat rate into the fiber loop, alternately. A delay line (252m) enough long is absolutely necessary to separate two adjacent laser pulses in time domain. The output pulse train (ring-down signals) from port 2 of the coupler3 is received by a high-speed photo detector, and then the signal is averaged for 16 times by the oscilloscope (Agilent DSOX2014A) to reduce the noises.

4. Experiments and results

When a narrow pulse light is injected into the loop, it will ring around the cavity, and dozens of decaying pulses can be observed. The maximum values of all pulses are recorded, and the data are fitted to an exponential decay curve in the format of
y=y0+A1exp[-ttr]
(11)
where y is the output power of the pulse, y0 and A1 are the parameters which can be fixed in the fitting process, tr is the 1/e ring-down time, and t is time.

All the calibrating gases used in this paper were provided by the certified standard gas sample supplier. The test gas samples were filled in the gas cell at the standard atmospheric pressure. When the pure nitrogen (0% ethyne) was filled in the gas cell, the output ring-down signals and the fitted curves were shown in Fig. 2
Fig. 2 Output ring-down signals and the fitted curves of pure nitrogen
. Signal1 and signal2 were measured ring-down signals at wavelength λ1(1530.37nm) and λ2(1530nm) respectively. The dashed curves of fitting1 and fitting2 gave the fitting exponential decay curves of the peaks of signal1 and signal2 respectively. The first pulse of the train is coupled out directly, that is to say it doesn’t pass through the gas cell and doesn’t give any information about the gas concentration. Thus it should be unconsidered in calculating.

The parameters of fitting exponential decay curves were shown in Table 1

Table 1. Parameters of fitting exponential decay curves

table-icon
View This Table
. From Table 1, the 1/e ring-down time with pure nitrogen at wavelength λ1 is 10.27452μs. The correlation coefficient R2 of the fitting is larger than 0.998, which shows the fitting exponential decay curve with better accuracy. The round-trip loss is calculated as 0.52837 dB by the Eq. (3). The target gas absorption loss is zero in the condition. The 1/e ring-down time with pure nitrogen at wavelength λ2 is 10.26467μs. The round-trip loss is calculated as 0.52888 dB according to Eq. (3), which is consistent with the round-trip loss at wavelength λ1, with the relative deviation of 0.096%.

From Fig. 2 we can see that the measured round-trip time of the pulse light τ is 1.25 μs, which describes the interval between two adjacent output pulses. For SMF-28, the effective refractive index of the core neff is 1.468, so the total length of the loop l is calculated about 255.4m by the equationl=τc/neff, which is the length of the delay line and the connected optical fiber of other components in the loop. The length is enough to separate two adjacent laser pulses in time domain.

In the same way, the output ring-down signals and the fitted curves of 10% calibrating ethyne in nitrogen were shown in Fig. 3
Fig. 3 Output ring-down signals and the fitted curves of 10% ethyne
. Signal1 and signal2 are measured ring-down signals at wavelength λ1(1530.37nm) and λ2(1530nm) respectively. Fitting1 and fitting2 give the fitting exponential decay curves of the peaks of signal1 and signal2 respectively. Parameters of them are also shown in Table 1. From Table 1, the 1/e ring-down time with 10% ethyne in the gas cell at wavelength λ1 is 2.20208μs. Once more using Eq. (3), the round-trip loss is calculated as 2.46528dB, which contains the target gas absorption loss. The 1/e ring-down time with 10% ethyne at wavelength λ2 is 10.26025 μs from Table 1. The round-trip loss is 0.52911 dB. The target gas absorption loss is zero in the condition, because the wavelength λ2 is not covered with the absorption line of ethyne. According to Eq. (7), the absorption loss in 10% ethyne at 1530.37nm is about 1.93617dB.

Several different calibrating samples mixed by ethyne and nitrogen were tested. Measured 1/e ring-down time versus gas concentration was shown in Fig. 4(a)
Fig. 4 (a). the 1/e ring-down time versus ethyne concentration; (b). the round-trip loss versus ethyne concentration; (c). the ethyne concentration versus absorption loss.)
. The black-square and red-triangle curve represent 1/e ring-down time tr1) and tr2)of the output pulses at wavelength λ1 and λ2 respectively. 1/e ring-down time tr1) decreases with increasing of ethyne concentration, while 1/e ring-down time tr2) fluctuates slightly. The round-trip losses can be obtained by Eq. (3). The round-trip loss δ(λ1) at wavelength λ1 increases linearly with increasing of the ethyne concentration as the black-square curve shown in Fig. 4(b). If external factors don’t bring any loss into the cavity, the inherent loss of the loop is almost invariant. So the round-trip loss δ(λ2) at wavelength λ2 changes very slightly as red-triangle curve shown in Fig. 4(b). The gas absorption losses can be obtained by Eq. (7). The relationship between gas concentration and absorption loss is shown in Fig. 4(c). Experimental data are shown by black-square curve which can be fitted to a linear curve in the format ofy=kx+b.

The equation of the fitted line (red in Fig. 4(c)) can be described as
C=4.9994δgas0.00021
(12)
where C is the gas concentration (in percentage). The fitting correlation coefficient R2 using the linear model is 0.9996, which shows the excellent linearity between the ethyne concentration and the absorption loss. The slope of the fitted line is 4.9994%/dB. The constant term (−0.00021) is a measurement error.

In order to evaluate the effect of the reference in this method, an attenuator was employed to give an additional loss Δδ to the loop cavity. And a sample of 0.1% ethyne in nitrogen was tested. Both the round-trip loss δ(λ1) and δ(λ2) will synchronously change with the additional loss as shown in Fig. 5(a)
Fig. 5 (a). the round-trip loss versus additional loss; (b). the absorption loss versus additional loss; (c). the ethyne concentration versus additional loss.)
. The black-square and red-triangle curve represent the round-trip loss at wavelength λ1 and λ2 respectively. And the varieties of the round-trip loss δ(λ1) and δ(λ2) are equal to the additional loss Δδ. The measured absorption loss δgas of the sample gas can be obtained from Eq. (7) as Fig. 5(b) shown, which is less than 0.02dB. That is why the curves representing the round-trip loss δ(λ1) and δ(λ2) are very close to each other in Fig. 5(a). Because the round-trip loss δ(λ1) and δ(λ2) change with the additional loss synchronously, the measured absorption loss of definite gas is invariable according to Eq. (7). The measured concentration C can be obtained from Eq. (12) as shown in Fig. 5(c). And the relative deviation of measured concentration is found to be less than ± 0.4% of 0.1% ethyne when a certain additional loss from 0 to 1.2dB is introduced to the cavity. The results show it can efficiently eliminate the influence of the inherent loss variation in the system and maintain the measurement with a high accuracy by introducing dual wavelength reference technology.

In order to further evaluate the stability of the system, the 0.1% calibrating sample mixed by ethyne and nitrogen had been measured for 24 hours. The data was recorded per twenty minutes. And the concentration relative deviation is less ± 0.5% for 24 hours. The result in Fig. 6
Fig. 6 Ethyne concentration variation for 24 hours
shows that the system has a good performance in stability and sensitivity.

5. Conclusion

A novel active fiber loop CRD system based on dual wavelengths differential absorption method is designed. One wavelength centered within and another centered outside of the target gas absorption line. By introducing dual wavelength reference technology, it eliminates the influence of the cavity loss variety and photoelectric device drift in the system effectively. An EDFA with AGC is used to compensate the power loss of the laser in the ring-down cavity, in order to increase the cavity round trips and improve the precision of gas detection. And two FBGs are employed to filter ASE spectrum noise. And then, some calibrating mixed samples of ethyne and nitrogen are tested with a 65 mm long gas cell to further evaluate the effect of reference wavelength. The results show the relative deviation is found to be less than ± 0.4% of 0.1% ethyne when a certain additional loss from 0 to 1.2dB is introduced to the cavity. And the relative deviation of measured concentration is less than ± 0.5% over 24 hours.

Acknowledgment

This work was supported by Natural Science Foundation of China (60977058, & 61205083), Independent Innovation Foundation of Shandong University (2014YQ011), the key projects of Shandong Province (2011ZHZX1A0107), International Science and Technology Cooperation Program of China (2012DFA10730), Shandong Province Science Foundation (ZR2013FL028).

References and links

1.

A. O’Keefe and D. A. G. Deacon, “Cavity ring-down optical spectrometer for absorption measurements using pulsed laser sources,” Rev. Sci. Instrum. 59(12), 2544–2551 (1988). [CrossRef]

2.

J. B. Dudek, P. B. Tarsa, A. Velasquez, M. Wladyslawski, P. Rabinowitz, and K. K. Lehmann, “Trace moisture detection using continuous-wave cavity ring-down spectroscopy,” Anal. Chem. 75(17), 4599–4605 (2003). [CrossRef] [PubMed]

3.

D. B. Atkinson, “Cavity ring-down spectroscopy: techniques and applications,” J. Am. Chem. Soc. 132(13), 4972 (2010). [CrossRef]

4.

J. S. Ni, J. Chang, T. Y. Liu, Y. F. Li, Y. J. Zhao, and Q. Wang, “Fiber methane gas sensor and its application in methane outburst prediction in coal mine,” J. Electron. Sci. Technol. China 6(4), 373–376 (2008).

5.

H. Waechter, J. Litman, A. H. Cheung, J. A. Barnes, and H.-P. Loock, “Chemical sensing using fiber cavity ring-down spectroscopy,” Sensors (Basel) 10(3), 1716–1742 (2010). [CrossRef] [PubMed]

6.

P. Zalicki and R. N. Zare, “Cavity ring-down spectroscopy for quantitative absorption measurements,” J. Chem. Phys. 102(7), 2708–2717 (1995). [CrossRef]

7.

G. Berden, R. Peeters, and G. Meijer, “Cavity ring-down spectroscopy: Experimental schemes and applications,” Int. Rev. Phys. Chem. 19(4), 565–607 (2000). [CrossRef]

8.

T. von Lerber and M. W. Sigrist, “Cavity-ring-down principle for fiber-optic resonators: experimental realization of bending loss and evanescent-field sensing,” Appl. Opt. 41(18), 3567–3575 (2002). [CrossRef] [PubMed]

9.

S. Pu and X. J. Gu, “Fiber loop ring-down spectroscopy with a long-period grating cavity,” Opt. Lett. 34(12), 1774–1776 (2009). [CrossRef] [PubMed]

10.

J. Y. Lee, J. W. Kim, Y. S. Yoo, J. W. Hahn, and H. W. Lee, “Spatial-domain cavity ringdown from a high-finesse plane Fabry–Perot cavity,” J. Appl. Phys. 91(2), 582–594 (2002). [CrossRef]

11.

H. F. Huang and K. K. Lehmann, “Noise in cavity ring-down spectroscopy caused by transverse mode coupling,” Opt. Express 15(14), 8745–8759 (2007). [CrossRef] [PubMed]

12.

G. Totschnig, D. S. Baer, J. Wang, F. Winter, H. Hofbauer, and R. K. Hanson, “Multiplexed continuous-wave diode-laser cavity ringdown measurements of multiple species,” Appl. Opt. 39(12), 2009–2016 (2000). [CrossRef] [PubMed]

13.

Y. Chen, K. K. Lehmann, J. Kessler, B. S. Lollar, G. L. Couloume, and T. C. Onstott, “Measurement of the 13C/12C of atmospheric CH4 using near-infrared (NIR) cavity ring-down spectroscopy,” Anal. Chem. 85(23), 11250–11257 (2013). [CrossRef] [PubMed]

14.

M. Jiang, W. G. Zhang, Q. Zhang, Y. P. Liu, and B. Liu, “Investigation on an evanescent wave fiber-optic absorption sensor based on fiber loop cavity ring-down spectroscopy,” Opt. Commun. 283(2), 249–253 (2010). [CrossRef]

15.

M. Gupta, H. Jiao, and A. O’Keefe, “Cavity-enhanced spectroscopy in optical fibers,” Opt. Lett. 27(21), 1878–1880 (2002). [CrossRef] [PubMed]

16.

G. Stewart, K. Atherton, H. B. Yu, and B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]

17.

Z. Q. Tan and X. W. Long, “A developed optical-feedback cavity ring-down spectrometer and its application,” Appl. Spectrosc. 66(5), 492–495 (2012). [CrossRef] [PubMed]

18.

K. M. Zhou, D. J. Webb, C. B. Mou, M. Farries, N. Hayes, and I. Bennion, “Optical fiber cavity ring down measurement of refractive index with a microchannel drilled by femtosecond laser,” IEEE Photon. Technol. Lett. 21(22), 1653–1655 (2009). [CrossRef]

19.

Y. Zhang, M. Zhang, and W. Jin, “Sensitivity enhancement in erbium-doped fiber laser intra-cavity absorption sensor,” Sensor. Actuat. A-Phys 104(2), 183–187 (2003).

20.

H. Waechter, K. Bescherer, C. J. Dürr, R. D. Oleschuk, and H.-P. Loock, “405 nm absorption detection in nanoliter volumes,” Anal. Chem. 81(21), 9048–9054 (2009). [CrossRef] [PubMed]

21.

G. Stewart, K. Atherton, and B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]

22.

N. Ni, C. C. Chan, T. K. Chuah, L. Xia, and P. Shum, “Enhancing the measurement accuracy of a cavity-enhanced fiber chemical sensor by an adaptive filter,” Meas. Sci. Technol. 19(11), 115203 (2008). [CrossRef]

23.

K. L. Yu, C. Q. Wu, and Z. Wang, “Optical methane sensor based on a fiber loop at 1665 nm,” IEEE Sens. J. 10(3), 728–731 (2010). [CrossRef]

24.

T. Brauers, M. Hausmann, U. Brandenburger, and H. P. Dorn, “Improvement of differential optical absorption spectroscopy with a multichannel scanning technique,” Appl. Opt. 34(21), 4472–4479 (1995). [CrossRef] [PubMed]

25.

A. Merten, J. Tschritter, and U. Platt, “Design of differential optical absorption spectroscopy long-path telescopes based on fiber optics,” Appl. Opt. 50(5), 738–754 (2011). [CrossRef] [PubMed]

26.

S. Kameyama, M. Imaki, Y. Hirano, S. Ueno, S. Kawakami, D. Sakaizawa, and M. Nakajima, “Development of 1.6 μm continuous-wave modulation hard-target differential absorption lidar system for CO2 sensing,” Opt. Lett. 34(10), 1513–1515 (2009). [CrossRef] [PubMed]

27.

J. R. Chen, K. Numata, and S. T. Wu, “Error reduction methods for integrated-path differential-absorption lidar measurements,” Opt. Express 20(14), 15589–15609 (2012). [CrossRef] [PubMed]

28.

R. E. Warren and R. G. Vanderbeek, “Online estimation of vapor path-integrated concentration and absorptivity using multiwavelength differential absorption lidar,” Appl. Opt. 46(31), 7579–7586 (2007). [CrossRef] [PubMed]

29.

B. Kaldvee, C. Brackmann, M. Aldén, and J. Bood, “Highly range-resolved ammonia detection using near-field picosecond differential absorption lidar,” Opt. Express 20(18), 20688–20697 (2012). [CrossRef] [PubMed]

30.

G. Stewart, K. T. V. Grattan, and B. T. Meggitt, in Optical Fiber Sensor Technology, Kluwer (Academic, 1998).

31.

Y. Zhao, Y. Li, T. Zhang, C. Wang, and T. Liu, “Effect of temperature on methane gas concentration by tunable diode laser absorption spectroscopy,” Proc. SPIE 8421, 8421AP (2012). [CrossRef]

OCIS Codes
(060.2370) Fiber optics and optical communications : Fiber optics sensors
(300.1030) Spectroscopy : Absorption
(300.6340) Spectroscopy : Spectroscopy, infrared
(280.4788) Remote sensing and sensors : Optical sensing and sensors

ToC Category:
Sensors

History
Original Manuscript: January 24, 2014
Revised Manuscript: March 28, 2014
Manuscript Accepted: April 22, 2014
Published: May 2, 2014

Citation
Yanjie Zhao, Jun Chang, Jiasheng Ni, Qingpu Wang, Tongyu Liu, Chang Wang, Pengpeng Wang, Guangping Lv, and Gangding Peng, "Novel gas sensor combined active fiber loop ring-down and dual wavelengths differential absorption method," Opt. Express 22, 11244-11253 (2014)
http://www.opticsinfobase.org/oe/abstract.cfm?URI=oe-22-9-11244


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References

  1. A. O’Keefe, D. A. G. Deacon, “Cavity ring-down optical spectrometer for absorption measurements using pulsed laser sources,” Rev. Sci. Instrum. 59(12), 2544–2551 (1988). [CrossRef]
  2. J. B. Dudek, P. B. Tarsa, A. Velasquez, M. Wladyslawski, P. Rabinowitz, K. K. Lehmann, “Trace moisture detection using continuous-wave cavity ring-down spectroscopy,” Anal. Chem. 75(17), 4599–4605 (2003). [CrossRef] [PubMed]
  3. D. B. Atkinson, “Cavity ring-down spectroscopy: techniques and applications,” J. Am. Chem. Soc. 132(13), 4972 (2010). [CrossRef]
  4. J. S. Ni, J. Chang, T. Y. Liu, Y. F. Li, Y. J. Zhao, Q. Wang, “Fiber methane gas sensor and its application in methane outburst prediction in coal mine,” J. Electron. Sci. Technol. China 6(4), 373–376 (2008).
  5. H. Waechter, J. Litman, A. H. Cheung, J. A. Barnes, H.-P. Loock, “Chemical sensing using fiber cavity ring-down spectroscopy,” Sensors (Basel) 10(3), 1716–1742 (2010). [CrossRef] [PubMed]
  6. P. Zalicki, R. N. Zare, “Cavity ring-down spectroscopy for quantitative absorption measurements,” J. Chem. Phys. 102(7), 2708–2717 (1995). [CrossRef]
  7. G. Berden, R. Peeters, G. Meijer, “Cavity ring-down spectroscopy: Experimental schemes and applications,” Int. Rev. Phys. Chem. 19(4), 565–607 (2000). [CrossRef]
  8. T. von Lerber, M. W. Sigrist, “Cavity-ring-down principle for fiber-optic resonators: experimental realization of bending loss and evanescent-field sensing,” Appl. Opt. 41(18), 3567–3575 (2002). [CrossRef] [PubMed]
  9. S. Pu, X. J. Gu, “Fiber loop ring-down spectroscopy with a long-period grating cavity,” Opt. Lett. 34(12), 1774–1776 (2009). [CrossRef] [PubMed]
  10. J. Y. Lee, J. W. Kim, Y. S. Yoo, J. W. Hahn, H. W. Lee, “Spatial-domain cavity ringdown from a high-finesse plane Fabry–Perot cavity,” J. Appl. Phys. 91(2), 582–594 (2002). [CrossRef]
  11. H. F. Huang, K. K. Lehmann, “Noise in cavity ring-down spectroscopy caused by transverse mode coupling,” Opt. Express 15(14), 8745–8759 (2007). [CrossRef] [PubMed]
  12. G. Totschnig, D. S. Baer, J. Wang, F. Winter, H. Hofbauer, R. K. Hanson, “Multiplexed continuous-wave diode-laser cavity ringdown measurements of multiple species,” Appl. Opt. 39(12), 2009–2016 (2000). [CrossRef] [PubMed]
  13. Y. Chen, K. K. Lehmann, J. Kessler, B. S. Lollar, G. L. Couloume, T. C. Onstott, “Measurement of the 13C/12C of atmospheric CH4 using near-infrared (NIR) cavity ring-down spectroscopy,” Anal. Chem. 85(23), 11250–11257 (2013). [CrossRef] [PubMed]
  14. M. Jiang, W. G. Zhang, Q. Zhang, Y. P. Liu, B. Liu, “Investigation on an evanescent wave fiber-optic absorption sensor based on fiber loop cavity ring-down spectroscopy,” Opt. Commun. 283(2), 249–253 (2010). [CrossRef]
  15. M. Gupta, H. Jiao, A. O’Keefe, “Cavity-enhanced spectroscopy in optical fibers,” Opt. Lett. 27(21), 1878–1880 (2002). [CrossRef] [PubMed]
  16. G. Stewart, K. Atherton, H. B. Yu, B. Culshaw, “An investigation of an optical fibre amplifier loop for intra-cavity and ring-down cavity loss measurements,” Meas. Sci. Technol. 12(7), 843–849 (2001). [CrossRef]
  17. Z. Q. Tan, X. W. Long, “A developed optical-feedback cavity ring-down spectrometer and its application,” Appl. Spectrosc. 66(5), 492–495 (2012). [CrossRef] [PubMed]
  18. K. M. Zhou, D. J. Webb, C. B. Mou, M. Farries, N. Hayes, I. Bennion, “Optical fiber cavity ring down measurement of refractive index with a microchannel drilled by femtosecond laser,” IEEE Photon. Technol. Lett. 21(22), 1653–1655 (2009). [CrossRef]
  19. Y. Zhang, M. Zhang, W. Jin, “Sensitivity enhancement in erbium-doped fiber laser intra-cavity absorption sensor,” Sensor. Actuat. A-Phys 104(2), 183–187 (2003).
  20. H. Waechter, K. Bescherer, C. J. Dürr, R. D. Oleschuk, H.-P. Loock, “405 nm absorption detection in nanoliter volumes,” Anal. Chem. 81(21), 9048–9054 (2009). [CrossRef] [PubMed]
  21. G. Stewart, K. Atherton, B. Culshaw, “Cavity-enhanced spectroscopy in fiber cavities,” Opt. Lett. 29(5), 442–444 (2004). [CrossRef] [PubMed]
  22. N. Ni, C. C. Chan, T. K. Chuah, L. Xia, P. Shum, “Enhancing the measurement accuracy of a cavity-enhanced fiber chemical sensor by an adaptive filter,” Meas. Sci. Technol. 19(11), 115203 (2008). [CrossRef]
  23. K. L. Yu, C. Q. Wu, Z. Wang, “Optical methane sensor based on a fiber loop at 1665 nm,” IEEE Sens. J. 10(3), 728–731 (2010). [CrossRef]
  24. T. Brauers, M. Hausmann, U. Brandenburger, H. P. Dorn, “Improvement of differential optical absorption spectroscopy with a multichannel scanning technique,” Appl. Opt. 34(21), 4472–4479 (1995). [CrossRef] [PubMed]
  25. A. Merten, J. Tschritter, U. Platt, “Design of differential optical absorption spectroscopy long-path telescopes based on fiber optics,” Appl. Opt. 50(5), 738–754 (2011). [CrossRef] [PubMed]
  26. S. Kameyama, M. Imaki, Y. Hirano, S. Ueno, S. Kawakami, D. Sakaizawa, M. Nakajima, “Development of 1.6 μm continuous-wave modulation hard-target differential absorption lidar system for CO2 sensing,” Opt. Lett. 34(10), 1513–1515 (2009). [CrossRef] [PubMed]
  27. J. R. Chen, K. Numata, S. T. Wu, “Error reduction methods for integrated-path differential-absorption lidar measurements,” Opt. Express 20(14), 15589–15609 (2012). [CrossRef] [PubMed]
  28. R. E. Warren, R. G. Vanderbeek, “Online estimation of vapor path-integrated concentration and absorptivity using multiwavelength differential absorption lidar,” Appl. Opt. 46(31), 7579–7586 (2007). [CrossRef] [PubMed]
  29. B. Kaldvee, C. Brackmann, M. Aldén, J. Bood, “Highly range-resolved ammonia detection using near-field picosecond differential absorption lidar,” Opt. Express 20(18), 20688–20697 (2012). [CrossRef] [PubMed]
  30. G. Stewart, K. T. V. Grattan, and B. T. Meggitt, in Optical Fiber Sensor Technology, Kluwer (Academic, 1998).
  31. Y. Zhao, Y. Li, T. Zhang, C. Wang, T. Liu, “Effect of temperature on methane gas concentration by tunable diode laser absorption spectroscopy,” Proc. SPIE 8421, 8421AP (2012). [CrossRef]

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