WO2017076907A1 - Système d'analyse qualitative de matériaux énergétiques - Google Patents

Système d'analyse qualitative de matériaux énergétiques Download PDF

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Publication number
WO2017076907A1
WO2017076907A1 PCT/EP2016/076431 EP2016076431W WO2017076907A1 WO 2017076907 A1 WO2017076907 A1 WO 2017076907A1 EP 2016076431 W EP2016076431 W EP 2016076431W WO 2017076907 A1 WO2017076907 A1 WO 2017076907A1
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WO
WIPO (PCT)
Prior art keywords
sample
heating
heater
space
housing
Prior art date
Application number
PCT/EP2016/076431
Other languages
German (de)
English (en)
Inventor
Gerald Njio
Florian Börner
Gerhard Holl
Kostyantin Konstantynovski
Original Assignee
Hochschule Bonn-Rhein-Sieg
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by Hochschule Bonn-Rhein-Sieg filed Critical Hochschule Bonn-Rhein-Sieg
Publication of WO2017076907A1 publication Critical patent/WO2017076907A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22—Fuels, explosives
    • G01N33/227—Explosives, e.g. combustive properties thereof
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00—Furnaces of a kind not covered by any preceding group
    • F27B17/02—Furnaces of a kind not covered by any preceding group specially designed for laboratory use
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—Specially adapted to detect a particular component
    • G01N33/0057—Specially adapted to detect a particular component for warfare agents or explosives

Definitions

  • the present invention relates to an analysis system and a library-independent analysis method for the qualitative detection and classification of energetic materials, in particular for the detection of explosives and explosives as well as for complex compositions which find use in IEDS (Improvised Explosive Devices).
  • IEDS Improvised Explosive Devices
  • the detection of explosive / hazardous substances by means of spectroscopic (eg IR, Raman, MS) methods.
  • the devices used have a spectral library of known substances and substance mixtures. If the spectrum of the sample corresponds to a known spectrum from the library, this information and the degree of agreement of the spectra are communicated to the user. Variations in the sample preparation However, as well as minor changes in the chemical formulation, the spectral characteristics can be changed in such a way that reliable identification of the sample is no longer possible.
  • additional detection methods for energetic materials not only use the static, spectroscopic properties of the substances, but also carry out dynamic measurements in which the sample properties are detected as a function of changing environmental conditions for identification purposes.
  • 6,406,918 B1 discloses a device which evaluates energetic substances (explosives) on the basis of a measured heat flow (comparable to DSC measurements).
  • substance-specific data sets are compared with thermoanalytical parameters such as the melting and decomposition point of a database.
  • thermoanalytical parameters such as the melting and decomposition point of a database.
  • these physical / chemical parameters are influenced by the sample morphology and composition and are only conditionally characteristic of energetic materials.
  • a device described in US 2010/0240140 AI works library-free and detects contactless the radiation energy and intensity of particles that arise during heating by decomposition (thermal fingerprint).
  • This device is primarily designed for trace detection and can only process solid samples. In addition, only substances can be detected by means of this device, which react strongly exothermic. Explosive liquid systems with volatile constituents such as nitroglycerin or hydrogen peroxide or substances which show an entropy-dominated reaction (eg TATP) can not be detected reliably due to the method.
  • Another structure for the qualitative analysis of energetic materials is described, for example, in the publication by Maurer et al.
  • the object of the present invention to provide a system and method which is capable of safely identifying energetic materials and which, moreover, can be operated inexpensively and without the use of skilled personnel.
  • the object is achieved by a system and a method having the features of the independent claims. Preferred embodiments of the invention are given in the subclaims.
  • the system according to the invention for the qualitative analysis of energetic materials comprises at least
  • the sample heater forms a sample space which at least partially encloses a sample and heats the sample from at least two different sides.
  • the invention according to at least two-sided heat transfer to the sample material in the sample chamber can be higher overall and reproducible heating rates of the sample, since the energy transport is proportional to the ratio contact surface heater to sample surface. Accordingly, higher reaction speeds can be generated in the inventive embodiment in the sample. For example, burn pyrotechnic sets with free ignition with flame, whereas under the heating conditions according to the invention comes to a violent deflagration. Therefore, for example, nitramines with the previous systems (prior art) using only small amounts of sample can not or insufficiently recognized by their heat of reaction or pressure development as explosive substances.
  • a qualitative analysis of energetic material implies that an unknown substance sample can be assigned to a known energetic material or class of energetic materials. One possible qualitative statement is therefore that the sample does not contain any energetic material. Possible substance classes of energetic materials may also be exothermic, explosive or thermal substances. In addition, it is also possible that the system provides data that allows a direct assignment of the unknown sample to a specific chemically defined substance class.
  • Energetic materials in the context of the invention are energetic or high-energy materials such as primary or secondary explosives, fuels and pyrotechnic products with military or civil application.
  • the energetic materials may have both a solid and a liquid consistency at room temperature.
  • the system according to the invention has a housing which can mechanically isolate the entire system towards the environment.
  • the housing may be connected to the environment at one or more locations via openings such as valves or flaps.
  • further compartments for mechanical or thermal insulation are arranged.
  • certain sensor groups or the sample heater may be mechanically isolated by additional walls within the housing.
  • the housing expediently has sensors for analyzing the sample before, during or after the heating up.
  • the housing may be designed to be mechanically stable in such a way that there is no risk of mechanical destruction of the system even when investigating large amounts of substance.
  • the housing may also contain means for safe storage. tentently hazardous combustion products and suitable filter systems, which protects the operating personnel against harmful effects of reaction products.
  • the sample heater forms a sample space which at least partially surrounds a sample.
  • the sample heater according to the invention has a three-dimensional, non-planar shape, which comprises the sample from more than one side.
  • the sample heating can form different three-dimensional structures, such as a cube, gutter, sink, cone, cuboid, cylinder, which are filled with the sample substance.
  • sample heaters with irregular, three-dimensional structures are conceivable. These may result, for example, in that the sample is placed on a flat metal foil and the film is formed by twisting or rolling into an (irregular) cylinder or other bodies.
  • a sample heater which forms only an area on which a sample is superficially charged is not in the sense of the invention.
  • the sample heater is at least enclosed by the housing. But it is also possible that the sample heater and thus the sample chamber are mechanically isolated by further shields to the housing.
  • the sample heater can be connected via suspensions to the housing.
  • the suspensions may include supplying the sample heater with power cables and / or control and measurement leads. In this way, the sample heater can be largely decoupled from the housing thermally and mechanically. This can lead to higher heating rates.
  • this arrangement allows for clean zero measurements without error sources just prior to heating, thus providing a clean background spectrum which can contribute to more accurate spectroscopic identification of the reaction products. Volatile substances escaping from the sample can not falsify background measurements with this setup.
  • sample quantities can be freely selected as a function of the sample chamber size and the amount is expediently in the range a few milligrams up to 1 g.
  • sample amounts 0.5 to 25 mg, preferably 1 mg to 10 mg can be used.
  • the detectors / sensors for detecting physical / chemical parameters may, for example, record the energy released by the introduced substance in the form of radiation intensities (as a function of wavelength), quasi-static pressure and pressure waves as a function of time and / or the sample or heating temperature.
  • analysis systems suitable for the person skilled in the art for example IR, Raman, UV, NIR, LLS, NMR systems can be used for the qualitative determination of the reaction products.
  • chemical sensors can be used to measure the chemical background and to characterize volatile reaction products. These sensors can, for example, have further chemical reactants and indicate the presence of certain substance classes by a color change.
  • the detectors can be arranged both within the sample space and / or within the housing.
  • both the sample space itself, the housing or both compartments can be equipped with sensors separately from each other.
  • the sensors can also be accommodated within the housing in further chambers, which are connected via controllable lines with the remaining volume of the housing and / or the environment.
  • the detectors arranged in the housing can be used in particular for the investigation of the reaction products after a potential ignition.
  • volatiles which have already evolved from the sample are explicitly analyzed via the detectors in the housing.
  • the detectors monitor the housing and / or the sample space before, during and after the heating.
  • the control and evaluation unit are provided, in particular, to control and regulate the heating, the detectors, a possible mechanical closure of the sample space, possible valves in and on the housing and to ensure the processing of the measured data for identification of the sample.
  • this includes the definition of limit values above which a reliable assignment of the investigated sample to the class of explosive substances and substance mixtures is clearly possible (library-independent evaluation algorithm).
  • heating sources known to the person skilled in the art can be used as sample heaters. These heating sources may include, for example, surface heating or heating wires.
  • the area heaters can simultaneously represent the sample space, ie, that the sample is filled for example in a sample space, which is formed by one, two or more surface heating of metal foils. If wires are used to heat the sample, they can be brought into a suitable shape, for example, by winding or bending. It is possible that the sample is then placed directly on the heating coil or the metal foil, or that another material (eg metal sheet) separates the coil from the sample substance. In the case of non-planar heating elements (eg heating wires), it is sufficient if the heating wires cover at least 30% of the area considered.
  • the heating of the sample can be done by passing an electric current through the heating coil or the surface heating.
  • radiant heaters are installed.
  • Heating coil may be made of an alloy with a resistivity of between 1- 10 "Qm and 5 x 10 ⁇ are 6 Qm and a melting point of, for example> 600 ° C.
  • materials for example, constantan, manganin or chrome-nickel are suitable.
  • the wire may be formed by bending
  • the wire can be wound into a helical heating structure, which consists of circular windings with different inner diameters This results in a conical winding with an opening formed by the largest diameter winding, this opening facing upwards, and a conical hollow cone made of a metal foil can then be inserted into the conical winding .
  • the Sample is poured into this hollow cone.
  • the sample heating can also be designed as an electrical resistance heater with a foil as an electrical resistance heating element.
  • a sheet of an alloy can having a resistivity between lxlO "6 Qm and 5x10 -6 square meter and a melting point of> 600 ° C are used.
  • Possible materials include, for example, constantan, manganin or chrome nickel.
  • the film may favor of a
  • the foil may be folded or kinked in the middle, whereby the fold or the kink can take up the sample material, In this embodiment it is ensured that the sample material is present at the site
  • the sample is heated from at least three sides and, in addition, the fold ensures at least partial enclosure of the sample, which partially counteracts evaporation of volatile substances to the sides.
  • additional metal strips for example made of copper foil, can be used, which are wound around the ends of the sample heating and then pressed together.
  • a metal foil sample heater can also be connected to a power source by means of mechanical clamps or contact springs.
  • the contact springs make the electrical connection to the heater control / power supply and can also serve for mechanical fixation of the heating element.
  • two contact springs on each side of the sample heater can be electrically connected to one connection of the heating control / power supply.
  • the electrical connection can either via temperature resistant ring, Luster terminals or cable lugs (screwed with the mounting holes) are made.
  • the attachment via contact springs can allow a quick replacement of the sample heating.
  • the sample heater can either be pushed directly between the contact springs or the upper contact springs can be folded up. In the latter case, the sample heater is first placed on the lower contact springs. Then the upper contact springs are folded down and mechanically locked. By pushing together / turning the contact springs, the sample is enclosed in the sample heater.
  • the power of the heater is designed so that temperature gradients of several 1000 K / s can be generated in the sample.
  • the heating power of the sample heating can be in the range of 1000-5000 K / s, preferably 2000-4000 K / s.
  • a voltage-dependent constant-current source By an externally given control voltage, the current through the sample heater and thus its temperature can be controlled. This allows high heating rates without the fear of melting the sample heating.
  • capacitors can be used as temporary energy storage. This is advantageous because the charging current for the capacitors is significantly lower than the discharge current and thus the power can be made smaller (smaller batteries / rechargeable batteries for mobile use).
  • the sample is heated by at least two different sides.
  • the sample heater forms a three-dimensional space which accommodates the sample. In this way, the sample is at least partially enclosed by the sample heater. But it is also possible that the sample heater completely encloses the sample.
  • the present sample space geometry can be approximated as a cube with the side pairs bottom-up, front-rear, right-left side. By definition, the upper side is the side from which the sample is filled. The heating energy must therefore act on the sample from at least two different sides.
  • the radiator or radiators whose radiation vectors include at least an angle of 90 ° to the center of the sample.
  • the heating from different sides can be done both by only one (eg bent) or by several separated heating surfaces.
  • the sample heater may heat the sample from at least five different sides.
  • This heating geometry can contribute to a much more uniform heating of the sample substance, which means that even volatile substances have a lower tendency to directional evaporation. They remain trapped inside the sample substance and this results in an ignition behavior which corresponds more clearly to the real situation. Heating five different sides also results in a significantly lower temperature gradient within the sample. This can help to determine ignition or explosion temperatures more accurately.
  • the heating of five different sides means that only one of the spatial directions of the sample is not heated by a sample heating. Lies For example, a cubic sample space geometry, so for example, the sample remains unheated from above, while from the other spatial directions each heating energy acts on the sample.
  • the sample heater may comprise a shaped heating wire or a shaped metal foil.
  • these heating elements have proven to be so flexible and durable that both forms of materials through, for example, bending, spiraling, notching, buckling, rolling is easily possible and high heat outputs can be generated. This can contribute to a more uniform heating of the samples under high heating rates.
  • the sample heater may comprise a metal sheet and the sample space may be formed by notching, folding or bending the metal sheet.
  • the sample is in direct contact with the heating plate.
  • a three-dimensional depression or space can be formed, which can be filled with a sample.
  • the mechanical processing thus creates a sample space which is surrounded by the sample heating through several sides.
  • a groove is formed in the film, which is particularly suitable for the examination of solid samples.
  • a conical shape can be formed, which is suitable for the investigation of liquid substances.
  • the sample heater can comprise a metal sheet and a closed sample space can be formed by folding or bending the metal sheet.
  • a closed sample space can be formed by folding or bending the metal sheet.
  • the sample heater can completely enclose the sample.
  • This embodiment can be realized, for example, by filling the sample into a sample space which is designed to be heatable from at least five sides. After filling the sample, the opening is then closed mechanically with another heating element.
  • the sample can be heated evenly from all sides and there is no risk that volatile substances are driven out of the sample by a temperature gradient before the actual reaction. Closed means in particular that the sample is surrounded on all sides by the sample heating, wherein the sample heater mechanically shields the sample from the housing.
  • a sample is placed on a heating plate and the heating plate is then placed around the sample by kinking, folding, rolling or combinations thereof.
  • the interior of the sample space may include at least one pressure or force sensor.
  • the sensors either in the housing or else directly on the sample heater, for example in the sample space.
  • the increase in reproducibility can be attributed to the fact that values are obtained from a significantly smaller volume, whereas in an arrangement on or in the housing, the housing volume must also be taken into account. In this way, smaller sample quantities can be investigated.
  • the dead volume of the sample space after filling and after closure may be ⁇ 50, preferably ⁇ 40% and more preferably ⁇ 25% of the sample chamber volume.
  • the detectors may comprise at least one pressure sensor and one optical sensor (preferably a photodiode).
  • the equipment of the sample space or the housing with pressure and / or optical sensors have led to good results in the context of assignment of energetic materials to certain explosive classes. This could be attributed to the fact that more stable pressure profiles are obtained through more uniform heating of the sample. Hence, more reproducible explosion products, which can then be clearly assigned via optical sensors arise. To the optical sensors can be counted photodiodes and among these particular IR sensors. Especially these sensor types are able to detect significant chemical properties of the reaction products. This refinement results in an improved evaluation with a library-independent evaluation algorithm.
  • the sample heating can be designed conically.
  • a conical configuration of the sample heating can be advantageous, in particular when investigating liquid samples. Due to the weight distribution as a function of the sample height, a more uniform inclusion of volatile substances in this geometry can be achieved be ensured within the sample. This can contribute to a higher detection rate.
  • a method for the qualitative analysis of energetic materials is at least comprising the steps:
  • step ii) the heating of the sample takes place from at least two different sides.
  • the same provisos and definitions which were used within the scope of the description of the system according to the invention can be used.
  • this method even those energetic materials can be clearly assigned to a specific substance class; which were not reproducibly accessible with the previous analysis methods. In this way, unknown substances can be safely, quickly and inexpensively analyzed for their potential danger and qualitatively analyzed. This procedure can also be carried out by untrained persons.
  • step iii) physical / chemical parameters in the sample space and / or in the housing can be raised as a function of the heating.
  • the collection of data during the heating period does not preclude the collection of data before and after heating and the qualitative determination of the substances. In particular, this can be related to blank / zero measurements before heating to determine an experimental background.
  • data after heating for example by analyzing cooled combustion products / gases, can also be used to ven classification of the unknown sample are used.
  • the sensors can be arranged both in the immediate vicinity of the sample, for example on the sample heater, in the sample chamber or even within the housing.
  • a further preferred embodiment of the method may additionally include that after step i) and before step ii), the sample space (1) is mechanically insulated from the housing.
  • the implementation of the sample by the heating takes place in this embodiment, so in the quasi-inclusion. This can be done for example by pressing the sample into a helical structure with subsequent closure of the opening in the film heater.
  • the mechanical closure or the mechanical insulation can be effected by the task of different, preferably inert materials, such as metal, rubber, adhesive, etc. This additionally ensures that constituents of the sample do not escape excessively by, for example, evaporation, but that the entire sample is reacted.
  • RDX as a representative of the nitramines, for example, with this construction in the implementation of a clear pressure signal, which can not be achieved with the previously known heating systems without closure. Explosive mixtures are also implemented as the problem of premature escape of individual components is avoided thanks to the heating system.
  • the final temperature to be reached and the heating speed can be set within a wide range.
  • the sample quantity is automatically limited by the heater geometries, which means that too large or too small sample quantities are excluded.
  • the results of the analysis are quantity-independent, which facilitates the subsequent class assignment by means of PCA and significantly increases their reliability.
  • the system is suitable for both solids and liquids.
  • the sample space may, for example, also have a mechanical flap which mechanically isolates the sample space after filling the sample with a defined contact pressure. In this case, the same advantages arise as with a manual closure of the sample space.
  • the flap it is possible for the flap to be controlled via the control system.
  • the Flap also be equipped with a heating element. This can help to heat the sample from all sides.
  • the evaluation in step iv) can comprise at least one time-dependent comparison of the energy quantity delivered by the system to the system.
  • the optimized heater geometry that only taking into account the difference between the energy input and the energy emitted a clear assignment of energetic materials to certain classes of substances is possible.
  • This method can thus dispense with the use of expensive and sensitive chemical detectors. This can help keep the process low cost.
  • the registered energy is essentially the heating energy.
  • the energy emitted by the system is the radiant energy and the mechanical work. The latter energies can be detected easily and reproducibly via pressure and IR sensors.
  • the evaluation in step iv) can take place at least taking into account the position and the height of temperature and / or pressure maxima during the heating.
  • the evaluation of the temperature and pressure data in relation to the position of maxima and the ratio of the height of these maxima to the baseline provide simple and reproducible parameters for the assignment of unknown substances to defined hazard classes in accordance with the law on explosives.
  • This method can operate independently of the library and provides data that is independent of the amount of sample used.
  • the substances can be assigned by means of a principal component analysis (PCA - prinicpal component analysis) of the above parameters.
  • Fig. 1 shows a possible sample space geometry in section.
  • the hatched areas indicate the heatable areas.
  • the right and left surfaces of the sample chamber are heated;
  • Fig. 2 shows a possible sample space geometry in section.
  • the hatched areas indicate the heatable areas.
  • the right and bottom surfaces of the sample chamber are heated;
  • Fig. 3 shows a possible sample space geometry in the supervision.
  • the hatched areas indicate the heatable areas.
  • the right, left, front and back surfaces of the sample chamber are heated;
  • FIG. 4 shows a possible sample space geometry in section.
  • the hatched areas indicate the heatable areas.
  • the lower, right and left surfaces of the sample chamber are heated;
  • Fig. 5 is a cylindrical sample space geometry in the plan.
  • the hatched areas indicate the heatable areas. In the event that the bottom and the top are designed not heated, 4 surfaces are heated;
  • FIG. 6 shows a conical sample space geometry in the plan view.
  • the hatched areas indicate the heatable areas. There are 5 surfaces heated;
  • Fig. 7 shows a possible sample space geometry in section.
  • the hatched areas indicate the heatable areas.
  • 6 sides of the sample chamber are provided with a heater.
  • the top of the sample chamber is designed to be closed;
  • FIG. 8 shows a schematic representation of a construction of a system according to the invention for the qualitative analysis of energetic materials
  • FIG. 9a-c a schematic representation of a sample heater according to the invention in the form of a surface heating.
  • steps a) -c) a closure of the surface heating via an exemplary folding technique is shown.
  • FIG. 1 shows a possible heating geometry for a rectangular sample space.
  • the sample space (1) for receiving the sample is enclosed by unheated (2) and heatable surfaces (3).
  • the sample may be heated by the right and left surfaces.
  • FIG. 2 shows a possible heating geometry for a rectangular sample space.
  • the sample space (1) for receiving the sample is enclosed by unheated (2) and heatable surfaces (3).
  • the sample may be heated by the lower and left surfaces.
  • FIG. 3 shows a possible heating geometry for a square sample space in the top view.
  • the sample chamber (1) for receiving the sample is enclosed by the heatable surfaces (3).
  • the sample may be heated by the right, left, front and back surfaces (3).
  • FIG. 4 shows a possible heating geometry for a rectangular sample space.
  • the sample space (1) for receiving the sample is enclosed by the heatable surfaces (3) below, right and left.
  • FIG. 5 shows a possible heating geometry for a cylindrical sample space.
  • the sample chamber (1) for receiving the sample is enclosed by the heatable surfaces (3).
  • the sample may be heated by the front, back, right and left surfaces (3).
  • FIG. 6 shows a possible heating geometry for a conical sample space.
  • the sample chamber (1) for receiving the sample is enclosed by the heatable surfaces (3).
  • the sample may be heated by the front, back, bottom, right and left surfaces (3).
  • the conical shape of heating can be obtained by inverting a heating wire in circles of increasing diameters or by folding a heating plate into a conical shape.
  • FIG. 7 shows a sample heater in which the sample chamber (1) is enclosed on all sides by heatable surfaces (3).
  • This embodiment can be achieved for example by a mechanically controllable and closable lid, which closes this after filling the sample space.
  • FIG. 8 schematically shows an embodiment of a detector system (4) according to the invention.
  • the system (4) is connected to a supply (5) and an exhaust port (5) with the environment, wherein the air in the detector inside by means of gas lines (10), which may be provided with valves, is passed.
  • the sample heater (7) according to the invention is accommodated in a separate explosion chamber (13).
  • a sample heater is shown schematically heating the sample for analysis from each side.
  • a thin heating plate (14) are used, which has external contact points (16).
  • the sheet metal can be preconditioned in the middle region (15) by kinks (17) so that this region can take up a sample and then results in folding over the sheet along the creases (FIG. 9b) and pushing together into a shape (FIG. 9c) which enclosing the sample on all sides and mechanically isolated.
  • this situation can also be realized via other convolution patterns.

Abstract

La présente invention concerne un système d'analyse et un procédé d'analyse indépendant de la bibliothèque permettant l'identification qualitative et la classification des matériaux énergétiques, notamment l'identification de matières explosives et d'explosifs ainsi que des compositions complexes de matériaux qui trouvent une application dans les EEI (engins explosifs improvisés).
PCT/EP2016/076431 2015-11-02 2016-11-02 Système d'analyse qualitative de matériaux énergétiques WO2017076907A1 (fr)

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