Full-field surface plasmon resonance sensor for high resolution refractive index measurement using common-path heterodyne interferometer

This study presents a full-field surface plasmon resonance (SPR) sensor induced by attenuated total reflection (ATR)-couple for liquid refractive index measurement. The system adopts a common-path heterodyne interferometer to measure the phase difference between P- and S-wave after passing through the SPR sensor. In order to realize the full-field measurement, it adopts a three-frame integrating-bucket method. The experimental results show great consistency profile between single point and full-field liquid refractive index measurement from 1.330 to 1.340 RIU. It shows that the best sensitivity and resolution of a single pixel in charge couple device (CCD) for liquid refractive measurement are 3.3 × 10⁴ (deg/RIU) and 3.53 × 10⁻⁶ (RIU), respectively. As compared with traditional single-point method, the proposed method with a regular CCD has no degradation. Therefore, the system has many applications in chemistry and biology.     

Surface plasmon resonance based fiber optic sensor for the detection of low water content in ethanol

A fiber optic sensor utilizing surface plasmon resonance (SPR) has been fabricated for the detection of low content of water in ethanol. The sensor utilizes spectral interrogation technique for operation. The resonance wavelength has been found to vary linearly with water content in the range 0-10% with sensitivity of 1.149 nm per percentage of water. The results are in agreement with the refractive index variation of ethanol-water mixture. The sensor has a water resolution of 0.145% which is better than the evanescent wave absorption sensor reported for the similar study. The sensor will find application in determining the low water content in ethanol which is used as a bio-fuel and in the field of medicine and organic chemistry.     

SPR传感芯片的理论与实验研究

针对光纤SPR(表面等离子体共振)传感器制作工艺复杂的问题,提出了一种光纤先固定后部分镀膜的SPR传感芯片的制作方法.依据电磁场和射线理论,分析并讨论了此种波长调制部分镀膜SPR传感芯片的工作原理,采用MEMS制作工艺对探测光纤进行封装固定以后,再对光纤进行部分镀膜,其结构简单,工艺性好,易于实现批量化.最后,搭建了一套基、于波长检测的光纤SPR测试系统对其进行测试.实验结果表明:在折射率范围为1.33～1.36时,共振波长同折射率具有良好的线性关系,光谱仪分辨率为0.1 m时,其分辨率可达到3×10-5折射率单位.     

Tethered DNA scaffolds on optical sensor platforms for detection of hipO gene from Campylobacter jejuni

DNA biosensors have gained increased attention over traditional diagnostic methods due to their fast and responsive operation and cost-effective design. The specificity of DNA biosensors relies on single-stranded oligonucleotide probes immobilized to a transduction platform. Here, we report the development of biosensors to detect the hippuricase gene (hipO) from Campylobacter jejuni using direct covalent coupling of thiol- and biotin-labeled single-stranded DNA (ssDNA) on both surface plasmon resonance (SPR) and diffraction optics technology (DOT, dotLab) transduction platforms. This is the first known report of the dotLab to detect targeted DNA. Application of 6-mercapto-1-hexanol as a spacer thiol for SPR gold surface created a self-assembled monolayer that removed unbound ssDNA and minimized non-specific detection. The detection limit of SPR sensors was shown to be 2.5 nM DNA while dotLab sensors demonstrated a slightly decreased detection limit of 5.0 nM (0.005 μM). It was possible to reuse the SPR sensor due to the negligible changes in sensor sensitivity (∼9.7 × 10⁻⁷ ΔRU) and minimal damage to immobilized probes following use, whereas dotLab sensors could not be reused. Results indicated feasibility of optical biosensors for rapid and sensitive detection of the hipO gene of Campylobacter jejuni using specific ssDNA as a probe.     

Study on design and application of fully automatic miniature surface plasmon resonance concentration analyzer

A fully automatic miniature surface plasmon resonance (SPR) concentration analyzer having high performance and low cost and developed using a Spreeta™ sensor was designed for field applications and concentration analysis. As in the case of Biacore™ instruments, the automatic sampling system of this device can introduce air segments between the sample/regeneration solution and buffer solution in the pipeline, which effectively prevents mixing of the solutions. A temperature sensor (AD 590) and temperature compensation method are used, which make the device insensitive to temperature fluctuations. A real-time data-smoothing algorithm for the SPR detection data is adopted; this can reduce the noise level to 5 × 10⁻⁷ RIU (refractive index units). The noise level of the sensorgram is 3.5% of the original level. Two types of self-prepared sensing chips—SMX-BSA (bovine serum albumin coated with sulfamethoxazole) and SMX-CM5 (carboxymethyl dextran coated with sulfamethoxazole)—are used to analyze the concentrations of sulfamethoxazole (SMX) standard solutions. Each chip's SMX calibration curve is established within the measurement range of 0-2000 ng/ml, and both limits of detection (LOD) are 2 ng/ml. One cycle of assay time is less than 15 min.     

Sensitivity of surface plasmon resonance sensors based on metallic columnar thin films in the spectral and angular interrogations

Surface Plasmon Resonance (SPR) from metallic Columnar Thin Films (CTFs) of porosity as high as 0.5 was experimentally and theoretically investigated. The CTF layers were prepared by the Glancing Angle Deposition (GLAD) method. The SPR features were investigated in both the angular and the spectral modes. In the angular interrogation, increasing the porosity causes broadening to the dip width, shift to larger resonance angles, and increase of the sensitivity to analyte refractive index (RI) changes by about threefold compared with closed metal films. In the spectral interrogation, on the other hand, the resonance wavelengths are red-shifted for porous films; hence their spectral sensitivities are higher than those of closed films under the same experimental conditions. Nevertheless, the sensitivity behavior versus the resonance wavelength is similar to that of SPR sensors based on dense film layers. The shapes of the nanostructures constituting the CTF are described as ellipsoidal inclusions in which the effective permittivity dyadic of the composite material is calculated using the Bruggeman formalism with exact depolarization dyadics. The correlation between the sensitivity enhancement and the electromagnetic field intensity at the interface between the metallic film and the analyte was examined. Electromagnetic fields analyses were performed using the general 4 × 4 propagation matrices of general homogenous biaxial layers.     

Free chlorine sensing using an interferometric sensor

A waveguide interferometer based free-chlorine sensing technique has been developed. A polymer film for a specific free chlorine binding was designed, synthesized and applied on the surface of a waveguide. The material is based on cyanuric acid moieties along each repeating unit covalently tethered to poly(norbornene)s. Chlorine sensing was accomplished by measuring the refractive index change of the polymer, as a result of the reaction between cyanuric acid and free chlorine, interferometrically by the evanescent field extended above the waveguide surface. The free chlorine binding to cyanuric acid is reversible and a linear calibration curve from 0.1 to 10 mg L⁻¹ of HOCl concentration was obtained with the level of detection (LOD) and level of quantification (LOQ) of 0.047 and 0.328 mg L⁻¹ of HOCl, respectively. A free chlorine measurement with less interference from combined chlorine than DPD based colorimetric method was developed as a result of the different sensing responses of free and combined chlorine. Free chlorine residual was measured in samples collected from tap water and poultry processing waters by both optical sensor and DPD-based colorimetric method. Good agreement between both methods was observed although the levels for free chlorine measured by the optical sensor are systematically lower than the readings obtained from the DPD method. The difference might be the result of the interference from combined chlorine during the DPD measurement.     

Influence of woody elements of a Norway spruce canopy on nadir reflectance simulated by the DART model at very high spatial resolution

A detailed sensitivity analysis investigating the effect of woody elements introduced into the Discrete Anisotropic Radiative Transfer (DART) model on the nadir bidirectional reflectance factor (BRF) for a simulated Norway spruce canopy was performed at a very high spatial resolution (modelling resolution 0.2 m, output pixel size 0.4 m). We used such a high resolution to be able to parameterize DART in an appropriate way and subsequently to gain detailed understanding of the influence of woody elements contributing to the radiative transfer within heterogeneous canopies. Three scenarios were studied by modelling the Norway spruce canopy as being composed of i) leaves, ii) leaves, trunks and first order branches, and finally iii) leaves, trunks, first order branches and small woody twigs simulated using mixed cells (i.e. cells approximated as composition of leaves and/or twigs turbid medium, and large woody constituents). The simulation of each scenario was performed for 10 different canopy closures (CC = 50-95%, in steps of 5%), 25 leaf area index (LAI = 3.0-15.0 m² m^− 2, in steps of 0.5 m² m^− 2), and in four spectral bands (centred at 559, 671, 727, and 783 nm, with a FWHM of 10 nm). The influence of woody elements was evaluated separately for both, sunlit and shaded parts of the simulated forest canopy, respectively. The DART results were verified by quantifying the simulated nadir BRF of each scenario with measured Airborne Imaging Spectroradiometer (AISA) Eagle data (pixel size of 0.4 m). These imaging spectrometer data were acquired over the same Norway spruce stand that was used to parameterise the DART model.The Norway spruce canopy modelled using the DART model consisted of foliage as well as foliage including robust woody constituents (i.e. trunks and branches). All results showed similar nadir BRF for the simulated wavelengths. The incorporation of small woody parts in DART caused the canopy reflectance to decrease about 4% in the near-infrared (NIR), 2% in the red edge (RE) and less than 1% in the green band. The canopy BRF of the red band increased by about 2%. Subsequently, the sensitivity on accounting for woody elements for two spectral vegetation indices, the normalized difference vegetation index (NDVI) and the angular vegetation index (AVI), was evaluated. Finally, we conclude on the importance of including woody elements in radiative transfer based approaches and discuss the applicability of the vegetation indices as well as the physically based inversion approaches to retrieve the forest canopy LAI at very high spatial resolution.     

PROSPECT-4 and 5: Advances in the leaf optical properties model separating photosynthetic pigments

The PROSPECT leaf optical model has, to date, combined the effects of photosynthetic pigments, but a finer discrimination among the key pigments is important for physiological and ecological applications of remote sensing. Here we present a new calibration and validation of PROSPECT that separates plant pigment contributions to the visible spectrum using several comprehensive datasets containing hundreds of leaves collected in a wide range of ecosystem types. These data include leaf biochemical (chlorophyll a, chlorophyll b, carotenoids, water, and dry matter) and optical properties (directional-hemispherical reflectance and transmittance measured from 400 nm to 2450 nm). We first provide distinct in vivo specific absorption coefficients for each biochemical constituent and determine an average refractive index of the leaf interior. Then we invert the model on independent datasets to check the prediction of the biochemical content of intact leaves. The main result of this study is that the new chlorophyll and carotenoid specific absorption coefficients agree well with available in vitro absorption spectra, and that the new refractive index displays interesting spectral features in the visible, in accordance with physical principles. Moreover, we improve the chlorophyll estimation (RMSE = 9 µg/cm²) and obtain very encouraging results with carotenoids (RMSE = 3 µg/cm²). Reconstruction of reflectance and transmittance in the 400-2450 nm wavelength domain using PROSPECT is also excellent, with small errors and low to negligible biases. Improvements are particularly noticeable for leaves with low pigment content.     

Ultrasensitive immunosensing of tuberculosis CFP-10 based on SPR spectroscopy

An antigen (Ag), CFP-10, found in tissue fluids of tuberculosis (TB) patients may be an ultimate candidate for use as a sensitive TB marker with a sensing method for early simplified diagnosis of TB. In this study, chemical and optical optimizations were carried out using novel immuno-materials for establishment of a self-assembled surface plasmon resonance (SPR) optical immunosensor system for detection of CFP-10, which is valuable for pre-clinical work, prior to conduct of massive clinical observations. For creation of a simple sensing interface, a monoclonal antibody (anti-CFP-10) was immobilized directly on a gold surface, followed by blocking with cystamine. Orientation and accessibility of anti-CFP-10 were assessed by the selective binding of CFP-10. Recent results indicate that the reusability of the sensor chip adopting the cystamine method was found to be preferable to other immobilization methods. A linear relationship was well correlated between SPR angle shift and CFP concentrations in the range from 100 ng mL⁻¹ to 1 μg mL⁻¹. Modification of the SPR chip with antibody provides a simple experimental platform for investigation of isolated proteins under experimental conditions resembling those of their native environment.     

Searching for optimal sensitivity of single-mode D-type optical fiber sensor in the phase measurement

To improve the sensitivity of a single-mode D-type optical fiber sensor, we selected a D-type optical fiber sensor with 4 mm long and 4 μm core thickness made of a single-mode fiber, a Au-coating on the sensor with a thickness range of 15–32 nm, a light wavelength of 632.8 nm, and an incident angle of 86.5–89.5° for different refractive index (1.33–1.40) sensing. These simulations are based on the surface plasmon resonance (SPR) theory using the phase method which shows that the sensitivity is proportional to the refractive index, Au film thickness and lower incident angle on the sensing interface. The sensitivity is higher than 4000 (degree/RIU), and the resolution is better than 2.5 × 10⁻⁶(RIU) as the minimum phase variation is 0.01°. This device is used to detect the refractive index or gas or liquid concentration in real-time. The proposed sensor is small, simple, inexpensive, and provides an in vivo test.     

Dynamically modulated intensity interrogation scheme using waveguide coupled surface plasmon resonance sensors

An electro-optically modulated intensity interrogation method based on tunable waveguide coupled surface plasmon resonance sensors has been proposed. It has been theoretically and experimentally demonstrated that the proposed scheme can enable sensitive measurement of measurand variations. By modulating the refractive index in the waveguide layer, this interrogation method yields modulated signal whose amplitude is related to measurand's refractive index. This amplitude modulated signal offers a higher signal to noise ratio and eliminates additive noise in the sensor system. A preliminary investigation using saline buffers with different NaCl concentrations shows a resolution of 2.3 × 10^?6 refractive index unit by our approach. Resolution can be controlled by the amplitude of the applied modulation voltage and can be further enhanced by optimizing the device structure or improving the electro-optical (E-O) coefficient of the E-O material. This approach is simple, stable, and promising for low-cost or multi-channel SPR biosensor applications.     

Improved forest biomass estimates using ALOS AVNIR-2 texture indices

Optical remote sensing is still one of the most attractive choices for obtaining biomass information, as new sensors are available with fine spatial and spectral resolutions. Better biomass estimates may be possible if suitable processing techniques for these sensors can be demonstrated. This research investigates the potential of high resolution optical data from the ALOS AVNIR-2 sensor for biomass estimation in a mountainous, subtropical forested region using four different types of image processing techniques including i) spectral reflectance and simple spectral band ratio, ii) commonly used vegetation indices, iii) texture parameters and iv) ratio of texture parameters. Simple linear and stepwise multiple regression models were developed between biomass data from 50 field plots, and image parameters derived from these techniques.Results indicate that spectral reflectance, the simple band ratio, and commonly used vegetation indices have relatively low potential for biomass estimation, as only about 58% of the variability in the field data was explained by the model (adjusted r² = 0.58 and RMSE = 64 t/ha). However, the texture parameters of spectral bands were found to be effective for biomass estimation with an explained variability of ca. 76% (adjusted r² = 0.76 and RMSE = 46 t/ha). The result was further improved to adjusted r² = 0.88 (RMSE = 32 t/ha) using the simple ratio of texture parameters. The results suggest that the performance of biomass estimation can be improved significantly using the texture parameters of high resolution optical data, and further improvement can be obtained using the ratio of texture parameters, as this combines the advantages of both texture and ratio.     

The infrared spectral signature of volcanic ash determined from high-spectral resolution satellite measurements

High-spectral resolution infrared spectra of the earth's atmosphere and surface are routinely available from satellite sensors, such as the Atmospheric Infrared Sounder (AIRS) and the Infrared Atmospheric Sounding Interferometer (IASI). We exploit the spectral content of AIRS data to demonstrate that airborne volcanic ash has a unique signature in the infrared (8-12 μm) that can be used to infer particle size, infrared opacity and composition. The spectral signature is interpreted with the aid of a radiative transfer model utilizing the optical properties of andesite, rhyolite and quartz. Based on the infrared spectral signature, a new volcanic ash detection algorithm is proposed that can discriminate volcanic ash from other airborne substances and we show that the algorithm depends on particle size, optical depth and composition. The new algorithm has an improved sensitivity to optically thin ash clouds, and hence can detect them for longer (~ 4 days) and at greater distances from the source(~ 5000 km).     

Leaf chlorophyll content retrieval from airborne hyperspectral remote sensing imagery

Hyperspectral remote sensing has great potential for accurate retrieval of forest biochemical parameters. In this paper, a hyperspectral remote sensing algorithm is developed to retrieve total leaf chlorophyll content for both open spruce and closed forests, and tested for open forest canopies. Ten black spruce (Picea mariana (Mill.)) stands near Sudbury, Ontario, Canada, were selected as study sites, where extensive field and laboratory measurements were carried out to collect forest structural parameters, needle and forest background optical properties, and needle biophysical parameters and biochemical contents chlorophyll a and b. Airborne hyperspectral remote sensing imagery was acquired, within one week of ground measurements, by the Compact Airborne Spectrographic Imager (CASI) in a hyperspectral mode, with 72 bands and half bandwidth 4.25-4.36 nm in the visible and near-infrared region and a 2 m spatial resolution. The geometrical-optical model 4-Scale and the modified leaf optical model PROSPECT were combined to estimate leaf chlorophyll content from the CASI imagery. Forest canopy reflectance was first estimated with the measured leaf reflectance and transmittance spectra, forest background reflectance, CASI acquisition parameters, and a set of stand parameters as inputs to 4-Scale. The estimated canopy reflectance agrees well with the CASI measured reflectance in the chlorophyll absorption sensitive regions, with discrepancies of 0.06%-1.07% and 0.36%-1.63%, respectively, in the average reflectances of the red and red-edge region. A look-up-table approach was developed to provide the probabilities of viewing the sunlit foliage and background, and to determine a spectral multiple scattering factor as functions of leaf area index, view zenith angle, and solar zenith angle. With the look-up tables, the 4-Scale model was inverted to estimate leaf reflectance spectra from hyperspectral remote sensing imagery. Good agreements were obtained between the inverted and measured leaf reflectance spectra across the visible and near-infrared region, with R² = 0.89 to R² = 0.97 and discrepancies of 0.02%-3.63% and 0.24%-7.88% in the average red and red-edge reflectances, respectively. Leaf chlorophyll content was estimated from the retrieved leaf reflectance spectra using the modified PROSPECT inversion model, with R² = 0.47, RMSE = 4.34 μg/cm², and jackknifed RMSE of 5.69 μg/cm² for needle chlorophyll content ranging from 24.9 μg/cm² to 37.6 μg/cm². The estimates were also assessed at leaf and canopy scales using chlorophyll spectral indices TCARI/OSAVI and MTCI. An empirical relationship of simple ratio derived from the CASI imagery to the ground-measured leaf area index was developed (R² = 0.88) to map leaf area index. Canopy chlorophyll content per unit ground surface area was then estimated, based on the spatial distributions of leaf chlorophyll content per unit leaf area and the leaf area index.     

Surface plasmon resonance sensor based on a single-mode polarization-maintaining optical fiber

A novel wavelength modulation-based fiber-optic surface plasmon resonance (SPR) sensor is reported which utilizes both polarization separation and broad band radiation depolarization in polarization-maintaining fibers to enhance sensor stability. Theoretical analysis of the sensing structure with ideally separated polarizations based on the mode of expansion and propagation method is presented. The effect of polarization cross-coupling was also analyzed in the approximation of an equivalent bulk optic structure. A laboratory prototype of the fiber-optic SPR sensor was characterized in terms of sensitivity and resolution. Experimental results indicate that this fiber-optic SPR sensor is able to resolve refractive index changes as low as 4×10⁻⁶ under moderate fiber deformations.     

Multi-resolution spectral analysis of wildfire potassium emission signatures using laboratory, airborne and spaceborne remote sensing

Thermal remote sensing studies of actively burning wildfires are usually based on the detection of Planckian energy emissions in the MIR (3-5 μm), LWIR (8-14 μm) and/or SWIR (1.0-2.5 μm) spectral regions. However, vegetation also contains a series of trace elements which present unique narrowband spectral emission lines in the visible and near infrared wavelength range when the biomass is heated to high temperatures during the process of flaming combustion. These spectral lines can be discriminated by detector systems that are less costly than the longer wavelength, actively cooled instruments more typically used in EO-based active fire studies. The main trace element resulting in the appearance of spectral emission lines appears to be potassium (K), with features at 766.5 nm and 769.9 nm. Here we study K-emission line spectral signature in laboratory scale fires using a field spectrometer, at a series of moderately-sized woodland and shrubland fires using airborne imagery from a new compact hyperspectral imager (HYPER-SIM.GA) operating at a relatively fine spectral sampling interval (1.2 nm), and at large open wildfires using the EO-1 satellite's Hyperion sensor. We derive a metric based on band differencing of the spectral signal both close to and outside of the K-line region in order to quantify the magnitude of the K-emission signature, and find that variations in this metric appear to track quite well with the commonly used measures of fire radiometric temperature and fire radiative power (FRP). We find that substantial flaming activity is required to generate a potassium emission signature, but that once present this can be detected using airborne remote sensing even through a substantial smoke layer that apparently obscures fire across the remainder of the VIS spectral range. Being specific to flaming combustion, detection of the K-emission line signature could prove useful in refining estimates of the gases released in open wildfires, since trace gas emission factors can vary substantially between flaming and smouldering stages. Finally, we demonstrate the first identification of the K-emission line signature from space using the EO-1 Hyperion instrument, but find it detectable only in certain instances. We conclude that a finer spectral and spatial resolution than that offered by Hyperion is required for improved detection performance. Nevertheless, our results point to the potential effectiveness of airborne and spaceborne K-emission signature detection as a complement to the more common thermal remote sensing approaches to wildfire detection and analysis. Sensors targeting this application should consider careful placement of the measurement wavelengths around the location of the K-line wavelengths, in part to minimise influences from the nearby oxygen A-band features.     

Terbium doped strontium cerate enabled long period fiber gratings for high temperature sensing of hydrogen

This paper reports on a novel optical fiber based sensor for hydrogen detection at high temperatures (>600 °C). The optical sensor consists of a perovskite-type ceramic, SrCe_0.95Tb_0.05O_3−δ, as the sensing material, which is coated on the cladding layer of long period fiber gratings. Upon exposure to hydrogen, the reduction of Ce⁴⁺ to Ce³⁺ on the surface of SrCe_0.95Tb_0.05O_3−δ particle causes decrease in its refractive index. As a result, the resonance wavelength of long period fiber gratings shifts to a higher value. The rate of the shift is dependent on the hydrogen partial pressure and can be used as the sensing signal. The high temperature optical H₂ sensor exhibits high sensitivity for H₂ detection at a partial pressure of 0.005 atm, and a short response time. The sensor is reversible as exposing the sensor to air oxidizes Ce³⁺ to Ce⁴⁺.     

Highly accurate and sensitive surface plasmon resonance sensor based on channel photonic crystal waveguides

A highly sensitive surface plasmon resonance (SPR) sensor based on channel photonic crystal waveguide (PCW) is proposed. The PCW is based on widely used lithographic and nano-fabrication compatible materials like TiO₂ and SiO₂. Gold has been used as a SPR active metal. By rigorously optimizing the different waveguide parameters, we have shown that there is significant transfer of modal power around phase-matching or resonance wavelength which has been utilized to design a compact and highly sensitive sensor for lab on chip. The ultra narrow width (∼765 pm for an interaction length of 10 mm) of surface plasmon resonance curve and sensitivity as high as 7500 nm-RIU⁻¹ will open a new window for bio-chemical sensing applications.     

Determination of 3-nitrotyrosine in human urine samples by surface plasmon resonance immunoassay

This paper describes the detection of a low-molecular weight molecule, 3-nitrotyrosine (3-NT) (∼226 Da), in human urine by coupling indirect inhibition assay with a surface plasmon resonance (SPR) sensor. 3-NT antibody (anti-3-NT Ab, mouse IgG) was used in this assay. An optimal antibody concentration has been measured at 27.9 μg/mL in order to obtain the best performance of the sensor surface. The lowest detection limit for 3-NT with this method is 4.7 ng/mL (S/N = 3). Sensor reliability was demonstrated by good specificity, intra-assay and inter-assay relative standard deviations <8%, average recovery of 107.68 ± 19.4% and sensor surface (self-assembled monolayer) stability through more than 200 regeneration cycles and 15 days of repeated measurement. This is the first SPR biosensor assay of 3-NT in human urine. The high stability of the SPR sensor surface underlies the potential of the SPR method as a low cost diagnostic tool for clinical detection of 3-NT.