Method for determining remoteness of a shot and device for realization of method

FIELD: technical expertise of firearms, possible use in forensic evaluations and investigations, and also during field operations.

SUBSTANCE: method for determining remoteness of shot from a firearm includes taking samples of diphenylamine from internal surface of barrel of firearm being examined, absorption of diphenylamine by sorbent, following desorption of diphenylamine and measurement of its amount in samples, on basis of which remoteness of shot is determined. Prior to taking samples barrel of firearm is heated, two samples of diphenylamine are taken by suction. Second sample is taken after experimental shot from current firearm, performed directly after taking first sample in the moment of firearm receipt. Then ratio of amount of diphenylamine in second sample to its amount in first sample is calculated, and remoteness of shot is determined as a result of comparison of received ratio to analogical ratio for firearm with known shot remoteness value. Device for taking samples when determining firearm shot remoteness contains heating element, positioned on the barrel of weapon, aspirator, concentration shell, having a layer of sorbent inside, and an adapter for hermetic connection of barrel channel outlet to concentration shell, output of which is connected to aspirator.

EFFECT: increased precision when determining remoteness of a shot.

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The invention relates to the technical methods of the examination of firearms - ballistic examination and can be used in the investigative, forensic, criminalistic and forensic practice, as well as when conducting operational-search activities.

A known way to determine the presence of traces of products of the shot and the fact of its production on the clothing and arms firing by the determination of trace sediment trace metals (antimony, barium, etc.) and diphenylamine (DFA) is an organic compound that is included with almost all smokeless powders to firearms, as a stabilizer chemical resistance (see Methodological recommendations Mvelopes, Lowbury, OOO and others - M.: state forensic science center of the Russian interior Ministry, 2001, p.24-32 (copy attached).

The method uses the evaporation of structural materials (metals) firearms and ammunition, the process is incomplete decomposition and sublimation (sublimation) of organic compounds included in the composition of smokeless powders (DFA), due to the large amount of heat released during explosive transformation throwing explosives gunpowder, and their subsequent deposition in the "cooling" on surfaces directly exposed to the powder gases (surface firearms,clothing and hands of the shooter and so on). The method of determining a shot in this method consists in the following:

- produce sample preparation by using solvent extraction of organic and inorganic (acid) solvents with subsequent detection of traces of products of shot - metals and diphenylamine;

- produced a study swabs by atomic absorption spectrophotometry or by emission spectral analysis for detection of trace metals;

- produced a study swabs gas chromatography-mass spectrometry for trace detection DFA;

- by the presence or absence of traces of products of the shot (metals, DFA) concludes the fact of its production.

The disadvantage of this method is the use of sophisticated equipment and the complexity of sample preparation, the ability to change or destruction of items of media during the liquid extraction from their surfaces, provide only qualitative results about the shot and the inability to determine its limitations.

The closest technical solution to the claimed method is a method that allows to determine the duration of discharge of a firearm by using the method of thin-layer (TLC) or gas (gas-liquid chromatography - mass spectrum of the industry - see the Definition of limitation shot: guidelines VNIISI, Vaishnav - M.: state forensic science center of the Russian interior Ministry, 2001.

The method uses the existing correlation between the age of organic products shot (diphenylamine), otlichayuschihsya on the inner surface of the bore of the firearm, and their chemical composition changes over time (diphenylamine =2-nitrodiphenylamine): the longer the duration of the shot, the more detectable products of nitration DFA oxides of nitrogen (2-nitrodiphenylamine), adsorbed on the inner surface of the bore of the firearm, and Vice versa. This method uses the change in the concentration of 2-nitrodiphenylamine through processes of chemical interaction with nitrogen oxides in the course of time and does not take into account the fact that education nitration products of diphenylamine already at the moment of the shot, due to its interaction with nitrogen oxides present in the powder gases (products of explosive transformation of the powders). The method of determination of the fact and duration of the production shot from firearms used in this method consists in the following:

- detection of diphenylamine and 2-nitrodiphenylamine in flushing organic solvent (methylene chloride) with the inner surface of the barrel of the firearm with the use that is coloinal chromatography or gas-liquid chromatography-mass spectrometry;

- a qualitative comparison of the concentration of diphenylamine and 2-nitrodiphenylamine in the sample, which varies in the direction of 2-nitrodiphenylamine with age products shot (his older). The concentration ratio of diphenylamine and 2-nitrodiphenylamine gives the original criterion for determining the limitation shot from the study of firearms.

The disadvantages of this method include low accuracy and the time interval of determining the limitation of production shots (up to year and over one year), the need to determine the chemical composition (identification of diphenylamine and 2-nitrodiphenylamine) compared to other substances, extragenomic with them with this method of sample preparation and preventing their identification, the use of expensive equipment - a gas-liquid chromatograph with a mass selective detector.

In this regard, the technical problem solved by this method and device is to improve the accuracy of establishing the limitations of the shot.

In the method of determining the limitation of the shot, which consists in the fact that you get samples of diphenylamine by removing it from the inner surface of the barrel studied firearms and adsorption by the sorbent, and then diphenylamine is desorbed and measure its amount, and duration of the shot is determined proceeding from the ratio of the quantities of given lamina in these samples depending on the time thus, before obtaining samples of the firearm's barrel is heated, remove diphenylamine produce extractor, the first sample receive a receipt of firearms, and the second immediately after the first one after experimental shot from the weapon, then calculate the ratio of the number of diphenylamine from the second sample to the number of the first sample and compare it with the same respect of amounts received for weapons with a predictable timing of the shots from it are presented in graphical or tabular form.

Device for determining the limitation of shots produced from the study of a firearm's barrel, includes a heating element placed on the trunk, the hood, the concentration of the cartridge with the sorbent, while the adapter is made with the possibility tight connection channel output shaft with a concentration cartridge, and the output concentration of the cartridge is connected to the aspirator.

The invention is illustrated by figures 1-6, where figure 1 shows the calibration dependence for determining the number of DFA in the sample; figure 2 - illustration of the completeness of adsorption of DFA in the absorption tube; figure 3 shows a device for implementing this method; figure 4 - a typical chromatogram of the extract from the absorption tube; figure 5 - mass spectrum of D Is A, detectable absorption in the cartridge after desorption; figure 6 - the ratio of the number of DFA in the barrel of the firearm immediately after the shot to the number of DFA in the barrel after the shot, produced after a certain period of time.

The essence of the invention lies in the fact that in determining the limitation of a shot from a firearm with ammunition loaded with gunpowder, containing in its composition diphenylamine as a stabilizer chemical resistance, used the ability of diphenylamine as compounds with high vapour pressure at normal conditions, evaporation under natural conditions, leakage and channel messages the barrel with the environment-air, resulting by the difference in concentrations is the diffusion of vapour in air and, thus, reduce over time its concentration on the inner surface of the bore of the investigated firearms.

To test the possibility of quantitative adsorption of vapors of diphenylamine (DFA) from the gas phase bore firearms were manufactured adsorption (concentration) tube inner diameter of 4 mm and a thickness of the absorbent layer 20 and 30 mm as the adsorbent used was the standard bearer for gas-liquid chromatography the raffia (GC) mark "Selipar 600" (silica-based). Next on the walls of a glass tube with a length of 150 mm and a diameter of 9 mm, imitating the barrel of a firearm, was applied a well-known trademark of the DFA, which it has placed an aliquot of the solution DFA in acetonitrile and the solvent was ususually at room temperature. The tube was heated, and through it within a certain time using the aspirator standard semi-automatic device chemical reconnaissance type PPR was pumped current of air that went in the absorption tube. Then DFA, it was decarbonators washing 2 ml of acetonitrile, and its quantity was determined using the method of high performance liquid chromatography (HPLC) on a standard chromatograph "milikhrom-4" (produced in Russia). Detection was carried out spectrophotometrically at a wavelength of 284 nm. To determine the number of DFA in the sample obtained calibration dependence presented in figure 1.

To monitor the completeness of adsorption desorption tubes were washed again with 2 ml of acetonitrile, the analysis showed the absence of DFA in the resulting solution, indicating full recovery of DFA with the inner surface of the tube, imitating the firearm's barrel.

As can be seen, for quantitative transfer of the DFA from the walls of the heated tube - barrel firearms in the absorption tube enough temperaturescale 90° With and purging for 15 minutes. Additionally controlled by the fullness of the acquisitions, which were installed in series two absorption tubes. The analysis showed the absence of DFA in the second of them, which further confirms the quantitative adsorption and efficiency of the method.

Figure 3 shows a concrete implementation of this method in the form of the device.

Device for determining the limitation of the shot contains the analyzed barrel 1 of the weapon to host the heating element, which, in particular, can be an electric heating tape 2. The adapter 3 provides a tight connection channel output shaft 1 with the concentration of the cartridge 4. The cartridge 4, which is a glass tube that has an inside layer of the sorbent 5, for example, selipar 600. The exit concentration of the cartridge 4 is connected to the suction pump 6.

The operation of the device in accordance with the claimed method is as follows.

The analyzed sample of small arms - trunk 1, with traces of carbon powder, wrapped with electric heating tape 2 and is heated to a temperature of 80±10°C. Temperature is monitored by thermocouple 7. In the chamber is inserted into the adapter 3, which provides a tight connection with the concentration of the cartridge 4. Within 10 minutes is bleeding the air from the barrel through the concentration of the cartridge 4. Diphenylamine contained in the powder Nagar, under the influence of high temperature evaporates from the barrel 1 and adsorbed on silica gel - sorbent 5 - concentration cartridge 4.

Order desorption DFA concentration cartridge was rinsed with 2 ml of acetonitrile. The solution DFA was analyzed quantitatively by gas-liquid chromatograph production company Agilent Technologies model 6890N (USA) with mass-selective detector model "5893" from the same company. Diphenylamine was determined by the time of its release and mass spectrum. Figure 4 shows a typical chromatogram, figure 5 - mass spectrum of diphenylamine detected after desorption in the solution of the adsorption Chuck.

Figure 6 shows a plot of the ratio of the number of diphenylamine, desorbed from the inner surface of the bore of the investigated firearms immediately after pilot shot in relation to its quantity, obtained through different periods of time after its production. Directly from Fig.6 clearly the dependence of this value on the old shot.

The proposed method significantly reduces the time and effort in the production of complex physico-chemical studies of traces of products of a shot from a firearm and has high accuracy when Oprah is the bookmark of his prescription.

1. The method of determining the limitation of the discharge of a firearm, including a sampling of diphenylamine with the inner surface of the investigated barrel of the firearm, the adsorption of diphenylamine sorbent, subsequent desorption of diphenylamine and measurement in samples of its quantity, which determines the duration of the shot, characterized in that before sampling, the firearm's barrel is heated, produce a selection of two samples of diphenylamine hood, while the second sample is taken after an experimental shot from the weapon produced immediately after collection of the first sample at the time of receipt of the weapons, and then calculate the ratio of the number of diphenylamine in the second sample to the number in the first sample, and the remoteness the shot is determined by comparing the obtained relations with the same respect for weapons with a known amount of limitation of the shot.

2. Device for sampling in determining the limitation of the discharge of a firearm containing the heating element is placed on the barrel of the gun, extraction, concentration Chuck with inside layer of the sorbent, and adapters for sealed connection of the output of the barrel with a concentration cartridge, the output of which is connected to the aspirator.



 

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