Device for chromatographic identification of components of complex mixtures
(57) Abstract:Usage: gas chromatography to determine the composition of multicomponent mixtures. The inventive device comprises at least three series-connected identical columns Packed with sorbents with different sorption ability towards identifiable substances, the registration unit and the detection unit. The output of each column is the node sampling is made in the form of a capillary, the geometrical dimensions of which are chosen from the condition of selection of the required number of samples. 3 C.p. f-crystals, 2 Il. The invention relates to gas chromatography and can be used to determine the qualitative and quantitative composition of multicomponent mixtures in various industries: chemical, oil, gas, petrochemical, metallurgy, medicine, biology, ecology, etc.A device for chromatographic identification of components of complex mixtures. As well as a device for chromatographic identification of components of complex mixtures, described in the work.Device for chromatographic identification shall contain the identification of components of complex mixtures by the method, based on chromatographic spectra.The disadvantage of these devices is unreliable identification of components of complex mixtures, as they contain one detector.Known devices for group and individual identification of components of complex mixtures closest to the proposed invention, the set of essential features for a device group for the identification of components of complex mixtures using chromatographic spectra.A device for implementing group identification contains five series-connected columns Packed with sorbents of different polarity, the buffer column, two detector and recorder. Each speaker has an output of the first detector.The device operates as follows: the flow of carrier gas, the sample is introduced into the system, consisting of five series-connected columns. After passing the first section of the flow is diverted into the first detector and the chromatogram is recorded first peak. A similar pattern is observed after passing the sample through sections 2, 3, 4 and 5. After elution through the whole system registers range of one substance with the first detector and the chromatogram is recorded one peak of the analyte, and its area represents the total amount of the substance minus the amount of the substance received by the detector 1. The device has the following disadvantages:
1. Because the ultimate goal is the identification of an unknown substance, in order to achieve this it is necessary to obtain a correct chromatographic spectrum of the substance. The correctness of the spectrum depends on the sorbent and the conditions of work. For optimal performance of sorbent required approximately the same flow of carrier gas in each section. In the prototype this condition is not met, and the range of substances is incorrect.2. The ratio of the signals of the two detectors, the ratio of peak areas (Q1/Q2) does not give reliable information about the substance, as it depends on the ratio of the flow of carrier gas (and hence the ratio of the share of the sample).3. Group identification by means of the described device is difficult, and the individual is simply impossible.The objective of the invention is the provision of the correct chromatographic spectrum of the substance due to the optimum working conditions of the sorbent without deterioration of its properties and transport in the detector after each column is necessary, strictly specified number in the for Chet, in a device for chromatographic identification of components of complex mixtures using chromatographic spectra containing at least three series-connected identical columns Packed with sorbents with different sorption ability towards identifiable substances registration unit and the detection unit, we have introduced five microcapillaries, the diameter and length of which are selected from the condition of selection of the required number of samples. In addition, the problem is solved due to the fact that the recording unit is connected to at least two detectors and one of the non-destructive detectors, and the detectors are connected in series and supply samples processed in the first detector, the second detector.When the task is achieved technical result, which is that 1-2% of the bulk sample after each column is given in the first detector, and the total number of samples that fall through the microcapillaries in the detector 1, is 5-10% of the total amount of a substance in accordance with the ratio of flow of carrier gas released in the detector 1 through the microcapillaries, to the total gas flow-notlocal well resolved spectrum of the substance. A new set of essential features, namely: after each of the speakers connected microcapillaries, the length and the diameter of each of which is selected so that the first detector was specified number of substances ensures the achievement of the technical result of obtaining well-resolved chromatographic spectrum of the substance and maintaining optimum operating conditions of each column, and increase the reliability of identification of components of complex mixtures.In Fig. 1 shows a device for identification of components of complex mixtures. In Fig. 2 spectrum of n-heptane, where (a) spectroheliogram n-heptane, obtained after passing through the substance of the first detector detector thermal conductivity, b) spectroheliogram n-heptane, obtained after passing through the substance of the second detector flame ionization.The device consists of columns K1K5, microcapillaries 6-10, detectors D11and D12, Registrar P13and P14.The device operates as follows. The sample is analyzed component by a flow of carrier gas is transferred to a system of series-connected columns 1-5, filled with various sorbents p is found in the detector D11. The chromatogram is recorded first range of substances Registrar P13. Range is a set of peaks, the number of which equals the number of columns used in the system. As initially used a heat conductivity detector, which is non-destructive, the probe after it completely misses the detector D12flame - ionization. After the detector D12Registrar P14registered second range of substances.On a specific device to identify components of complex mixtures obtained chromatographic spectrum of the substance n-heptane. Chromatographic spectrum was obtained on a system of series-connected columns Packed with sorbents of different polarity. As stationary phases were used Apiezon - triphosphopyridine oil (QF-1), pentagonally ether (PE), polyethylene glycol with molecular weight of 20M (PEG-20M), 1,2,3-Tris-( b-cyanoethoxy)propane, applied to chromaton N-AN, the grain size of 0.12 to 0.16 mm in an amount of 10 to 15 wt. The flow of carrier gas of nitrogen in the system set 12 to 15 ml/min Temperature thermostat columns 120oC. the Output of each column is connected to the first detector microcapillaries with a diameter of 20, 30, 40, 50, 60 MK is of the five peaks. Since the length and diameter of the capillaries is chosen appropriately, it is well resolved spectrum of the substance.The use of the invention allows comparison with the prototype to obtain well resolved correct range of substances and to improve the reliability and validity gas chromatographic identification of components of complex mixtures. 1. Device for chromatographic identification of components of complex mixtures containing at least three series-connected identical columns Packed with sorbents with different sorption abilities in relation to the identifiable substances, the registration unit and the detection unit, wherein the output of each column is the node sampling is made in the form of a capillary, the geometrical dimensions of which are chosen from the condition of selection of the required number of samples.2. The device under item 1, characterized in that the recording unit is connected to at least two detectors.3. The device according to p. 2, characterized in that one of the detectors is non-destructive.4. The device according to PP. 1 and 2, characterized in that the detectors are connected in serial is
SUBSTANCE: device has an outer case (1) with a first end part (1a) and a second end part (1b), as well as an intermediate section (1c) and an inner cavity in which there is a first inner chamber (2a) and a second inner chamber (2b). The device also has one first (3) passage from the first chamber (2a) to a waste removal pipe (8) and one second passage (4) from the second chamber (2b) to the outside of the injector. The device also has an inner pipe (5) lying in the inner cavity, a separation element (9, 11a) which grips the inner pipe (5) and separates the first inner chamber (2a) from the second inner chamber (2b). The inner chamber (5) has a first section (5a) lying in the first inner chamber (2a) and a second section (5b) lying in the second inner chamber (2b). The first section (5a) ends in at the first end (5c) with a first hole (5d) and the second section (5b) ends at the second end (5e) with a second hole (5g). The device also has an inner channel (5f) which passes between the first and second holes (5d, 5g). In the channel (5f) there is one absorbing material (6) and one inorganic wool material (7) lying in the first section (5a) of the inner pipe. The first end (5c) of the inner pipe (5) has holding apparatus (10a, 10b) for holding inorganic wool material (7), and the first hole (5d) of the inner pipe (5) is connected to the first passage (3) in the waste removal pipe (8) exclusively through the first inner chamber (2a).
EFFECT: possibility of designing interfaces having a simple structure which meet requirements for reliability, universality and automation possibility, more sensitive analysis using the interface injector for direct interfacing a liquid chromatograph with a gas chromatograph.
12 cl, 7 dwg
FIELD: process engineering.
SUBSTANCE: invention relates to chromatography. It covers continuous or quasi-continuous cleaning of multicomponent mix (Fd). Hear used are at least four separate chromatographic columns where through forced is initial mix using at least one solvent. Multicomponent initial mix (Fd) is to be divided in integer number (n) of fractions (Fi), where n equals at least 5. Said columns are grouped to least six (α1, …, αn-3, β1, …, βn-3, γ, δ). Note here that every section (α1, …, αn-3, β1, …, βn-3, γ, δ) includes at least one column proved that functions of said sections can be performed sequentially and by separate columns. There are at least two collection sections, at least two circulation sections (β1, …, βn-3), collection section (γ) for collection of strong adsorbate section and feed section (δ). Functions of sections (α1, …, αn-3, β1, …, βn-3, γ, δ) are performed either in synchronism or serially. On elapse or during time (t*) said columns are displaced in direction opposite the main direction of displacement of the solvent. First column of every collection section (α1, …, αn-3) displaces to the last position of appropriate circulation section (β1, …, βn-3). First section of upstream circulation section (β1) displace to first position of collection section (γ) to collect said strong adsorbate. First columns of the next circulation channels (β1, …, βn-3) displace to the last positions of the next upstream connection sections (α1, …, αn-4). First column of collection section (γ) for strong sorbate collection displaces to the last position of feed section (δ), while first column of said feed section (δ) displaces so that its renders the last column of downstream collection section (αn-3).
EFFECT: separation of true multicomponent mixes into.
15 cl, 14 dwg, 4 tbl
SUBSTANCE: determination of the chemical resistance is carried out by a content of an effective stabiliser, which represents the sum of DPA and its mononitro- and nitroso-derivatives taking into account their efficiency coefficient, in extracts of gunpowder with acetonitrile by a method of highly efficient liquid chromatography by dissolution of gunpowder in acetonitrile for 1 hour with an intensity of mixing 600±100 min-1. Chromatography is performed in an acetonitrile-water medium with a ratio 70:30, at a rate of the mobile phase consumption 0.5 ml/min at a temperature of 50°C. Determination of guaranteed storage terms for gunpowders is performed by formula:
EFFECT: elaboration of a quantitative method of determining the content of effective SCS.
SUBSTANCE: system for gas-chromatographic analysis of air samples has two chromatographs 1 with plasma ionisation detectors 2, a chromatograph 4 with a heat conductivity detector 5, chromatographic packed columns 12 filled with an adsorbent, concentrators 13 installed in chromatographs 1 and 4. The system also includes an information conversion device 14 connected to a computer 15, having special software. The system also includes a device 8 for obtaining deionised water, a hydrogen generator 9, three gas preparation units 10 with three control panels 11, two electrometer amplifiers 3 and detector power supply 6. The device 8 for obtaining water is connected to the hydrogen generator 9 which is connected to each gas preparation unit 10 of chromatographs 1 with plasma ionisation detectors 2 through the control panel for feeding hydrogen 16, and to the detector power supply 6, connected to the chromatograph 4 with the heat-conductivity detector 5, and the two electrometer amplifiers 3, connected to two chromatographs 1 with plasma ionisation detectors 2, are connected to connecting cables from control panels 11 and the information conversion device 14.
EFFECT: providing quality and accurate estimation of content of hazardous impurities and concentration thereof in air samples, improved operational qualities of the system.