Sensor for obtaining giant raman scattering spectra and method of making said sensor
SUBSTANCE: invention relates to a method of making a sensor for obtaining giant Raman scattering spectra, which is a glass capillary whose inner wall is coated with silver nanoparticles. The silver nanoparticles are obtained and attached to the glass surface via reduction of silver ions with alkylamines. The glass capillaries are washed with a detergent solution for optical devices, distilled water while mixing with ultrasound, absolute ethanol and dried in air, placed in a teflon vessel with a reaction mixture of 1 mmol/l AgNO3 and 1 mmol/l alkylamine in ethanol; the reaction mixture is heated at 45-50°C for 40 min with intense agitation along the axis of the capillaries. After the reduction reaction, the capillaries are washed with ethanol and cleaned on the outside.
EFFECT: invention enables to obtain a high-resolution giant Raman scattering sensor.
2 cl, 4 ex
The invention relates to nanotechnology. In particular, to obtain sensors for identifying and determining the concentrations of various substances using the spectra of giant Raman scattering.
- Enhanced Raman scattering (GOR) is an effect, the essence of which is to substantially increase the intensity of the Raman signal of adsorbed molecules when adsorbed on metal surfaces, when the adsorbed molecules may have an abnormally high value of the cross section of Raman scattering of light due to electron transfer from the surface of metal nanoparticles on the molecule.
Existing sensors receive a coating of metal (silver, gold) on the basis of, for example, made of silicon probe. Article: Nanoscale chemical analysis by tip-enhanced Raman spectroscopy, Raoul M. Stockle, Yung Doug Suh, Volker Deckert 1, Renato Zenobi, Chemical Physics Letters 318, 2000, 131-136, a probe for an atomic force microscope, made of silicon, deposited silver. In the article "a Simple Chemical Method for Forming Silver Surfaces with Controlled Grain Sizes for Surface Plasmon Experiments" Y. Saito, J. J. Wang, D. N. Batchelder, and D. A. Smith, - Langmuir 2003, 19, 6857-6861 is disclosed a method of manufacturing a sensor by chemical deposition of silver (the silver mirror reaction) on a flat basis. The coating on the base has the disadvantage of creating a nonuniform layer of silver nanoparticles. Chemical osuzhdeni is through reaction of the silver mirror is complicated by the influence of carbon dioxide of the atmosphere at the complex of silver ion with ammonia. Note that even the breath of the experimenter can affect the reaction of the silver mirror.
Closest to the proposed sensor is a known sensor for obtaining spectra of GOR, which is a glass capillary tube, on the inner side of which is coated with silver nanoparticles (see WO 2008116093 A2, 25.09. 2008, prototype)
In the known sensor silver nanoparticles on the substrate surface are in the composition and therefore the dimensional effect GOR to identify and determine the concentration of substances weakened.
The task of the invention to provide using the proposed sensors spectra GOR with high resolution.
The problem is solved by a method of manufacturing a sensor for obtaining spectra of GOR, which is a glass capillary tube, on the inner side of which is coated with silver nanoparticles produced according to the invention, the attachment to the glass surface of silver nanoparticles through reduction reaction of silver ions bonds alkylamines. The method according to the invention, is carried out in the following sequence.
Take a glass capillary, preferably with capillary effect of raising solution for convenient analysis. With an inner diameter slightly larger diameter of the needle of the syringe to be placed in the capillary researched solution. The capillary was washed with detergent is redstem for optics, distilled water, ethanol. Dried in air at 70°C for 30-40 minutes and Then the capillary is placed in a Teflon beaker with a reaction mixture of 1 mmol/l AgNO3and 1 mmol/l of the alkylamine in ethanol. The reaction mixture is heated at 70°C for 30-40 minutes, Preferably under stirring along the axis of the capillary. After the reduction reaction of the capillary is washed with ethanol and purified from the outside.
The inside glass capillaries as the basis convenient for several reasons. First, the reaction occurring therein, is separated from the atmosphere. Secondly, after applying a layer of silver nanoparticles and receiving sensor analyzed the solution can be entered by dipping the tip of the capillary in the analyzed solution, which will spontaneously enter into the capillary by capillary forces. If this method does not allow you to enter an analyte in the capillary, it is injected with a syringe. Thirdly, the capillaries can be stored for long periods, covering them from the atmosphere plastic and inert to silver substance, such as paraffin. The reaction must be carried out in a Teflon beaker from wasting reagents in the case of reaction in a glass vessel, which is covered with a layer of silver nanoparticles. During the reaction layer of the nanoparticles, not only covered the inside of the capillary, but also external. Therefore, is and must be cleaned from the layer of silver nanoparticles. In the reaction used primary amines: butylamine, ethanolamine. The invention is illustrated in the examples.
The method of producing the sensor. Example 1. To obtain the sensor take a glass capillary with an inner diameter of 0.9 mm, a wall thickness of 0.3 mm and length 10 mm Capillary together with other capillaries are washed with 0.5% detergent solution for optics Helmanex II at pH=9.5 for 3 hours, and then distilled water (resistivity greater than 18 Mω·cm) under stirring ultrasound. Then washed with absolute ethanol and dried in air at 70°C for 30-40 minutes and Then the capillary is placed in a Teflon beaker with a reaction mixture of 1 mmol/l AgNO3and 1 mmol/l of butylamine in ethanol. The reaction mixture was heated at 45-50°C for 40 min under vigorous stirring along the axis of the capillary. After the reduction reaction of the capillary is washed with ethanol and purified wool on the outside. Air-dried. Get the sensor in the form of a glass capillary on the inner side of which is attached silver nanoparticles of size 92±35 nm.
The method of producing the sensor. Example 2. Sensor gain as in example 1, except that instead of butylamine take ethanolamine. Get the sensor size of the nanoparticles 102±35 nm.
Obtaining the spectrum of GOR. Example 1. Prepare a 2.5·10-5M solution bestiola in methanol. To the surface of the solution touch the end of the Senso is and. The solution will rise to 3 mm in inner channel of the sensor. The methanol from the sensor is removed by drying in air. Then get range on GOR combined system OmegaScope™, combining scanning probe microscope with confocal Raman and fluorescence spectrometer company Aist NT. Use a blue laser with a wavelength of 473 nm, an average power of 25 mW and a laser spot with a diameter of 500 nm. The exposure time 30 s Receive a range of GOR, in which analysis to choose the band 1573 cm-1. Determine its intensity and pre-constructed calibration curve to determine the concentration bestiola 2.4 x 10-5M
Obtaining the spectrum of GOR. Example 2. Cook 5·10-6M solution of adenine in distilled water. Prepare the sample to obtain a spectrum GOR, as in example 1. Shooting range during exposure to 2 C. For analysis, you can select the band with the maximum scattering at 734 cm-1. Determine its intensity and pre-constructed calibration curve the concentration of adenine 5.2 x 10-6M
Thus, the proposed sensor suitable for storage, allows to obtain spectra of GOR with a small content of substances in solutions and therefore can be applied in practice.
1. A method of manufacturing a sensor for obtaining spectra of GOR, which is a glass capillary, vnutrenniy the side of which is coated with silver nanoparticles, characterized in that the silver nanoparticles are obtained and attached to a glass surface using a reduction reaction of silver ions bonds alkylamines, namely the glass capillary is washed with wash solution for optics, distilled water with stirring, ultrasound, absolute ethanol and air-dried, placed in a Teflon beaker with a reaction mixture of 1 mmol/l AgNO3and 1 mmol/l of the alkylamine in ethanol, the reaction mixture is heated at 45-50°C for 40 min under vigorous stirring along the axis of the capillary, after the reduction reaction of the capillary is washed with ethanol and purified from the outside.
2. The method according to p. 1, characterized in that the recovery of silver ions using butylamine and ethanolamine.
FIELD: oil and gas industry.
SUBSTANCE: invention is related to research of composition and properties of multicomponent hydrocarbon systems in process of oil and gas condensate deposits, and namely to photometric methods for determination of diethylene glycol concentration in saturated (upon moisture absorption from gas) diethylene glycol (sDEG) and recovered diethylene glycol (rDEG). DEG concentration in field diethylene glycol solutions is measured by IR-spectrometric method that includes determination of their optical density and determination of DEG content against pre-plotted calibration dependence of optical density on DEG concentration in the solvent such as diethylene glycol of SOP brand (99.9%), which is also used as a blank sample during calibration and measurements. At that, before measurement of optical density of calibration solvents and the tested sample, preliminary scanning of their spectra is done and wave length corresponding to the maximum signal in the measured spectrum is fixed, while measurement of optical density for the blank, calibration and tested samples are made at wave lengths corresponding to the maximum value of the signal for each sample.
EFFECT: invention allows fast determination of DEG content with high accuracy and without sample treatment.
2 dwg, 1 tbl
FIELD: measurement equipment.
SUBSTANCE: invention relates to nano-, microelectronics and analytical instrument making industry and can be used for development of technologies and for production of products of micro- and nanoelectronics, as well as for production of pure materials and for diagnostics and control of liquid process media. A method for determining atomic composition of active impurities in liquid media consists in preparation of an analysed object and its arrangement in vacuum. Then, irradiation of surface with a beam of charged particles and recording of secondary particles, as per which composition of surface atoms is determined, is performed. Preparation of the analysed object is performed by preparation of surface of a semiconductor plate by chemical etching, treatment in a peroxide alkali solution and by washing in deionised water. A drop of analysed liquid with the size of at least one micron is applied to the prepared surface of a clean semiconductor plate, then, it is removed, and for the purpose of analysis, the removed drop trace is irradiated with a beam of charged particles.
EFFECT: improvement of analysis rapidness, as well as improvement of a detection limit, and namely at least by 10-100 times.
SUBSTANCE: invention may be used to determine paleotemperatures of catagenesis that characterises the degree of catagenetic maturity of organic matter (OM) of rocks. The sampling of sediments is carried out from the studied rocks, the insoluble organic matter microphytofossils is isolated from them and studied with optical method with the determining of paleotemperature. The study with the optical method is carried out in two stages. At the first stage in transmitted light the dominant group of microphytofossils is isolated from the morphological groups of microphytofossils, the groups of thick-walled and thin-walled microphytofossils is isolated in it. For each isolated group the index of colour is determined. At the second stage of the study the quantitative characteristics are clarified on the basis of spectral characteristics of selected groups of microphytofossils in infrared band of light. The resulting estimates of paleotemperatures of microphytofossils are determined on the basis of comparing the results of studies of the first and second stages.
EFFECT: improving reliability of determining paleotemperatures of catagenesis of vitrinite-free deposits.
2 cl, 1 dwg, 2 tbl
FIELD: radio engineering, communication.
SUBSTANCE: invention relates to a terahertz antenna, particularly a tunable terahertz antenna based on a semiconductor material. The antenna has a semiconductor film (3) on a piezoelectric material (10), having a surface capable of exhibiting surface plasmons in the terahertz frequency range. The surface of the semiconductor film (3) is structured by an antenna structure (4), capable of supporting local surface plasmon resonances in the terahertz frequency range.
EFFECT: invention increases sensitivity and selectivity.
15 cl, 6 dwg
SUBSTANCE: adaptive sensor for identifying and monitoring the position of three types of articles has a sensitive surface, a contactless sensor for identifying three types of articles, a NOR logic element, six AND logic elements, a resetting unit, an electric pulse binary counter, first, second and third display units, a clock generator with corresponding electrical connections thereof. The point of connection of outputs of the fourth, fifth and sixth AND logic elements and the second input of the NOR logic element is the first output of the adaptive sensor. Outputs of the third, second and first AND logic elements are the second, third and fourth outputs of the adaptive sensor, respectively. When one or another or a third type of article moves relative to the sensitive surface, potential information signals for monitoring the position of said articles with a logic 1 levels are output at the first output. A three-bit binary digital code, the values 100, 010 and 001 of which are identification codes of the one or other or third type of monitored article, respectively, is obtained at the second, third and fourth outputs. Information signals on identification of one or another or a third type of controlled articles in form of visual signals are output from the first, second and third display units, respectively. The adaptive sensor enables automatic monitoring of articles without mechanical contact with said articles and automatic adaptation thereof to a specific type of monitored article.
EFFECT: broader functional capabilities.
9 cl, 1 tbl, 1 dwg
FIELD: medicine, pharmaceutics.
SUBSTANCE: invention refers to the chemical-pharmaceutical industry, particularly to a method for quantitation of anthracene derivatives in horse sorrel roots. The raw material is extracted in 70% ethanol; an aliquote of the prepared extract is diluted in an alkaline-ammonia solution; an optical density of the solution is measured at a wave length of 520 nm; the total anthracene derivates are re-counted at 8-O-β-D-glucoside emodin that is used as a reference substance.
EFFECT: method enables reducing labour input, reducing time and stages of the process, and decreasing the analyte loss.
1 dwg, 1 ex
SUBSTANCE: adaptive sensor for identification and control of articles position contains a sensitive plate, an inspection sensor for two types of articles, the first, second and third output terminals, a NEITHER-NOR gate, two AND gates, a trigger flip-flop, the first and second display units, an electric oscillation generator with respective electric couplings. When the sensitive plate is moved in regards to one article (e.g., heated metal article) or the other one (e.g., unheated non-metal article) potential signals for position control of these articles are generated at the first output terminal with logic level "1". At that at the second and third outputs two-digit binary code is generated which values of 10 and 01 are the identification codes for one or another inspected article. Data signals about identification of one or another type of the inspected articles in the form of visual signals are picked up from the first and second display units respectively. The adaptive sensor ensures automatic control for one or the other type of articles without mechanical contact with them and automatic adaption to the specific type of the inspected article.
EFFECT: expanding functionalities and improving operational performance.
12 cl, 2 dwg, 1 tbl
FIELD: machine building.
SUBSTANCE: proposed transducer comprises sensitive surface, contactless sensor for identification of four types of articles (heated metal, heated non-metal, unheated metal, unheated non-metal), OR-NO logical element, eight AND logical elements, reset unit, electric pulse binary counter, 1st, 2nd and 3rd indication units and clock oscillator with appropriate electric connections. Point of connection of outputs of 7th, 6th, and 5th logical elements AND and 2nd input of OR-NO logical element makes the 1st output of adaptive transducer. Outputs of 3rd, 2nd, 1st AND logical element and 3rd output ob binary pulse counter make 2nd, 3rd, 4th and 5th output of adaptive transducer, respectively. At displacement of whatever article along sensitive surface, 1st output processes potential data signals of article position with the level of logical "1". Note here that 2nd, 3rd, 4th and 5th outputs generate four-digit binary digital code, its values 1000, 0100, 0010 and 0001 are identification codes of the article appropriate type. Article type identification data signals are picked up at appropriate indication units. Adaptive transducer allows the automatic control over article with no mechanical contact therewith and automatic adaptation to its particular type.
EFFECT: expanded operating performances.
FIELD: machine building.
SUBSTANCE: proposed transducer comprises sensitive element composed by inductive sensor, capacitive sensor arranged inside central through bore of aforesaid inductive sensor and two IR photoreceiver, all being in straight line. Besides, it comprises logic OR-NO element, first and second indication units, first and second diodes. The point of connection between diode cathodes and second input of said logic element makes the first input of adaptive transducer. It includes counter trigger true and inverting outputs make the transducer second and third outputs. At displacement of hot or cold metal articles relative to adaptive transducer sensor in whatever direction its first output processes voltage potential data signals with logical "1" level that contain data on control over position of said articles. Second and third outputs process two-digit binary codes 10 and 01 of article identification. Visual control signals are picked up at appropriate indication units. Proposed adaptive transducer allows automatic contactless control and automatic adaptation to particular type of controlled article.
EFFECT: expanded operating performances, higher reliability and performances.
SUBSTANCE: invention relates to field of medicine and can be applied in control-analytic laboratories for standardisation and control over medication quality. Method deals with determination of drotaverine hydrochloride by spectrophotometry of determined substance and standard sample of comparison, as solvent for preparation solution to be determined applied is 0.1 M solution of hydrochloric acid, concentration of analysed solution constitutes 0.000017 g/ml, as comparison, sample potassium dichromate is applied, value of conversion rate 0.434 is introduced into formula for calculation of results and calculation is performed by formula.
EFFECT: method makes it possible to increase reproducibility of determination results, reduce cost, labour consumption, analysis error, to unify analysis methodology.
FIELD: physics, optics.
SUBSTANCE: invention relates to optical analysis of the composition of a substance based on Raman and luminescence spectra and a spectral-selective portable Raman-luminescent analyser. The spectral-selective portable Raman-luminescent analyser further includes a microscope lens or a microscope and a one- or two-dimensional sample translator connected to a computer. The analyser is adapted to control a sample movement device and synchronise step-by-step sample scanning and identification of a substance at each step while focusing a laser beam by the microscope lens into a spot of micrometre or submicrometer dimensions.
EFFECT: high sensitivity and resolution and avoiding the need to decode complex spectra multi-component mixtures.
SUBSTANCE: invention relates to optically active sensory technologies intended for detection of gas or fluid molecules, including those of toxic and explosive matters. Proposed method is implemented with the help of sensitive element based on slotted silicon microstructures with nano-structured porous ply of the surface of silicon walls. It consists in combination light dissipation in characteristic oscillatory modes of molecules amplified by partial light localisation in medium with periodically modulated reflective index (slotted silicon).
EFFECT: additional increase in probability of light interaction with molecules of detected gases or fluids results from availability of developed surface of porous ply which adds to sensitivity of gas sensor.
9 cl, 4 dwg, 1 tbl
FIELD: physics, optics.
SUBSTANCE: system can be used in investigating properties of gaseous media, including with chemical reactions, in small volumes by scattering spectroscopy or light absorption. The system includes assemblies of optical elements capable of moving towards a focal point, each having two flat swivel mirrors in an adjustment head which provides independent inclination of each mirror in two directions, or a lens in between, which is mounted at double the focal distance on the beam path from the measuring volume. The assemblies enable to focus a reflected beam at the same point. One assembly, having a lens and a flat mirror or only a concave mirror, directs the laser beam such that it travels its entire path in the reverse direction, wherein the number of passages is equal to or greater than 4 depending on the number of installed assemblies of optical elements.
EFFECT: high strength of the useful signal and reduced optical distortion of the laser beam due to multiple passage of the laser beam through the measuring volume.
2 cl, 2 dwg
SUBSTANCE: proposed method comprises measurement of intensities of the steel chemical elements by emission-spectral process on initial and heat-processed specimens.
EFFECT: high-precision comprehensive control.
3 cl, 2 tbl
SUBSTANCE: method comprises the following steps: moving a coated steel band on an arched path on the outer surface (813) of a drum (8) revolving about an axis (51), having a cylindrical wall guiding the band, directing an ablation laser beam inside the cylindrical wall such that its optical incidence occurs on the axis of the normal (41) to the outer surface of the drum at a target point (11) of contact of the band and the drum, passing the beam through the wall through an opening (811) on the wall which is transparent for the beam. Plasma spectral radiation from the laser ablation at the point of contact is collected through optical reflection towards the axis of the normal (41) to the outer surface of the drum and through the opening, after which it is directed into a spectral measurement unit. The axis of the normal (41) to the outer surface which corresponds to optical incidence and reflection is rotated synchronously with the drum.
EFFECT: enabling measurement during spectral analysis of a layer of metal coating deposited on the surface of a steel band which is in motion and has different formats and different speeds.
15 cl, 8 dwg
FIELD: instrument making.
SUBSTANCE: analysed gas medium is radiated with laser linearly polarised monochrome radiation, and two spectra of combination light scattering are recorded, J||(2) and J⊥(λ). For the first one the electric vector of scattered light is parallel to the electric vector of the exciting laser radiation, and for the second one - it is orthogonal. According to the isotrope spectrum of scattering produced from the condition J(λ)=J||(λ)-4/3·f(λ)·J⊥(λ), where f(λ) is the ratio of the spectral ratio of radiation transmission by equipment, the electric vector of which is parallel to the electric vector of the exciting laser radiation, to the identical coefficient of transmission for orthogonal polarisation, the composition of the analysed medium is defined.
EFFECT: possibility to identify larger quantity of components of analysed gas medium and increased validity of analysis.
SUBSTANCE: optical system for collecting scattered radiation for a Raman spectrometer has optically-connected laser and elliptical mirror, lens and spectrometer arranged in series along the principal optical axis. The device includes a spherical mirror with a radius which is equal to twice the focal radius of the elliptical mirror, and a focusing lens, wherein the spherical mirror has a hole at the centre and is placed on the principal optical axis such that its centre of curvature coincides with the first focus of the elliptical mirror, their mirror surfaces are turned towards each other, and its centre coincides with the second focus of the elliptical mirror. The focusing lens is placed outside the elliptical mirror on the optical axis of the laser, orthogonal to the principal optical axis, and its focus coincides with the first focus of the elliptical mirror. The elliptical mirror has two holes lying at points of intersection of the surface of the mirror with the optical axis of the laser, wherein their diameter matches the diameter of the laser beam.
EFFECT: enabling increase in intensity of a Raman signal and enabling increase in sensitivity of a Raman spectrometer.
SUBSTANCE: device has a radiation source capable of emitting light with initial polarisation, first and second light guides, the first light guide being optically connected to the radiation source for emitting light to the sample. The light guides have corresponding end parts essentially flush with each other, said end parts also being intended to detect radiation reflected from the sample. The device also has a detector which is optically connected to the first and second light guides, the detector being intended for measuring, within the optical subband, indication of the first polarisation of the reflected radiation, second polarisation of the reflected radiation, the second polarisation being different from the first polarisation, and the first and second intensities of the reflected radiation in the first and second light guides, respectively. The detector is operably connected to a processing device which is configured to calculate first and second spectral functions within the optical subband, both spectral functions essentially indicating instances of single scattering in the sample. The first spectral function is a measure of the difference in polarisation between the first polarisation of the reflected radiation and the second polarisation of the reflected radiation, and the second spectral function is a measure of the difference in intensity between the first and second intensities of the reflected radiation. The processing device is additionally meant for calculating the degree of correlation between spectral functions in order to estimate whether there are instances of single scattering from essentially the same optical depth inside the sample. The group of inventions also includes a catheter intended to operate with a connected optical device, and a computer data medium. The latter is meant to enable a computer system, comprising at least one computer, having a connected data storage means, to monitor the optical device disclosed in the present group of inventions.
EFFECT: obtaining a reliable signal from an optically thin layer.
15 cl, 8 dwg
SUBSTANCE: multipass optical system consists of two identical spherical mirrors whose centres lie at diametrically opposite points of the surface one imaginary sphere, having radius equal to the radius of curvature of the mirrors, as well as a laser and a focusing lens, lying on one optical axis which passes inside that sphere at a certain distance from its centre and cross the surface of the first mirror. The focus of the lens lies at about the distance of the radius of curvature of the mirror from that point of intersection. In the plane formed by the optical axis of the lens and the centre of the sphere, the optical axis of the second mirror makes an angle of γ=α2/[2(β-2α)] with the radius of the sphere extending to the centre of the second mirror, where α=arcsin(r/2R), β=arcsin(R0/R), wherein r is the radius of the laser beam, R0 is the size of the mirrors, R is the radius of curvature of the mirrors.
EFFECT: high intensity of the Raman scattering signal.
SUBSTANCE: proposed spectrometre to generate reference radiation, wideband laser and optical system to focus and intercross light beams in measured volume. Radiation from measured volume is registered by monochromator with multichannel photo detector. Proposed spectrometre comprises extra monochromator with photo detector to simultaneously register wideband laser radiation.
EFFECT: higher accuracy thanks to allowance for spectrum shape fluctuation.
SUBSTANCE: coherent light flux and movable periodic structure are produced in transparent medium located in displacement plane. Light flux is directed to transparent medium with movable periodic structure at preset angle selected subject to diffraction with the help of nonzero diffraction order formed by moving periodic structure. Measuring flux is formed. Reference flux is formed so that algebraic difference between reference and measuring fluxes aligned in the plane of periodic structure motion is proportional to periodic structure frequency. Said two fluxes are aligned in space. Then, interfering fluxes are converted into electric signal while periodic structure being looped with delayed feedback. Note here that light flux and moving periodic structure in transparent medium are formed in synchronous pulse medium. Parameters of pulse mode synchronisation are varied owing to control over time delay in feedback. Electric signal phase variations caused by displacements are compensated. Shifts in axis associated with periodic structure motion is defined by time delay.
EFFECT: higher precision of measurements, enhanced performances and higher resolution.