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High-sensitivity infrared attenuated total reflectance sensors for in situ multicomponent detection of volatile organic compounds in water

Nature Protocols volume 11, pages 377–386 (2016)Cite this article

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Abstract

In situ detection of volatile organic compounds (VOCs) in aqueous environments is imperative for ensuring the quality and safety of water supplies, yet it remains a challenging analytical task. We present a high-sensitivity method for in situ analysis of multicomponent VOCs at low concentrations based on the use of infrared attenuated total reflection (IR-ATR) spectroscopy. This protocol uses a unique ATR waveguide, which comprises a planar silver halide (AgClxBr1−x) fiber with cylindrical extensions at both ends to increase the number of internal reflections, and a polymer coating that traps VOCs and excludes water molecules. Depending on the type of VOC and measurement scenario, IR spectra with specific frequency windows, scan times and spectral resolutions are obtained, from which concentration information is derived. This protocol allows simultaneous detection of multiple VOCs at concentrations around 10 p.p.b., and it enables accurate quantification via a single measurement within 5 min without the need for sample collection or sample pretreatment. This IR-ATR sensor technology will be useful for other applications; we have included a procedure for the analysis of protein conformation changes in Supplementary Methods as an example.

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Figure 1: Illustration of the IR-ATR sensor setup.
Figure 2: Workflow of fiber fabrication.
Figure 3: IR absorption spectra.
Figure 4: Calibration function with high sensitivity and wide linear range (100–1,000 p.p.b.) for the detection of two groups of multiple VOCs in 5 min.

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Acknowledgements

The authors thank the National Natural Science Foundation of China (NSFC) and the Research Grants Council (RGC) of Hong Kong Joint Research Scheme (21261160489), and the Program for Changjiang Scholars and Innovative Research Team at the University of Science and Technology of China for partial support of this study. We also acknowledge The Natural Science Foundation of China (21505074), the Natural Science Foundation of Jiangsu Province (BK20140781), and the Priority Academic Program Development of Jiangsu Higher Education Institutions.

Author information

Author notes

  1. Rui Lu and Wen-Wei Li: These authors contributed equally to this work.

Authors and Affiliations

  1. Department of Chemistry, Chinese Academy of Sciences (CAS) Key Laboratory of Urban Pollutant Conversion, University of Science and Technology of China, Hefei, China

    Rui Lu, Wen-Wei Li, Guo-Ping Sheng & Han-Qing Yu

  2. Jiangsu Key Laboratory of Chemical Pollution Control and Resources Reuse, School of Environmental and Biological Engineering, Nanjing University of Science and Technology, Nanjing, China

    Rui Lu

  3. Institute of Analytical and Bioanalytical Chemistry, University of Ulm, Ulm, Germany

    Boris Mizaikoff

  4. School of Physics, Tel Aviv University, Tel Aviv, Israel

    Abraham Katzir

  5. Department of Applied Physics, Ariel University Center of Samaria, Ariel, Israel

    Yosef Raichlin

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Contributions

R.L., W.-W.L., B.M. and H.Q.Y. designed the experiments; R.L. conducted the experiments; A.K. and Y.R. fabricated and provided the fiber; R.L. and G.-P.S. conducted the data processing; R.L., W.W.L., B.M. and H.-Q.Y. wrote and edited the manuscript. All authors contributed to discussion on the results and implications of the manuscript.

Corresponding authors

Correspondence to Boris Mizaikoff or Han-Qing Yu.

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Competing interests

The authors declare no competing financial interests.

Integrated supplementary information

Supplementary Figure 1 (a) Curve fitting for BSA solution IR-ATR spectra in the amide I region together with the respective best-fitted individual band components, and (b) BSA secondary structure represented as a function of temperature.

Supplementary Figure 2 Synchronous (a) and asynchronous (b) two-dimensional IR-ATR correlation spectra of BSA.

Supplementary Figure 3 Schematic of the custom-made stainless mold for planar silver halide fabrication.

Supplementary Figure 4 Construction of the flow-cell with dimensional details.

Supplementary Figure 5 Changes of IR absorbance for 300 ppb (v/v) MAHs in aqueous solution with time.

Supplementary Figure 6 Calibration profiles of low-concentration VOC mixtures (10 to 70 ppb).

(a) Four monoaromatic hydrocarbons (toluene (TL), o-xylene (OX), m-xylene (MX), and p-xylene (PX), benzene is not shown for low correlation coefficient), and (b) six chlorinated hydrocarbons (monochlorobenzene (MCB), 1,2-dichlorobenzene (o-DCB), 1,3-dichlorobenzene (m-DCB), chloroform (CF), trichloroethylene (TCE), and perchloroethylene (PCE)).

Supplementary information

Supplementary Text and Figures

Supplementary Figures 1–6 and Supplementary Methods (PDF 824 kb)

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Lu, R., Li, WW., Mizaikoff, B. et al. High-sensitivity infrared attenuated total reflectance sensors for in situ multicomponent detection of volatile organic compounds in water. Nat Protoc 11, 377–386 (2016). https://doi.org/10.1038/nprot.2016.013

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