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Non-destructive colorimetric analysis of drugs for fluoroquinolones using a smartphone 使用智能手机对氟喹诺酮类药物进行无损比色分析
Pub Date : 2024-01-22 DOI: 10.26896/1028-6861-2024-90-1-17-25
V. G. Amelin, O. E. Emelyanov
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引用次数: 0
Chromatographic determination of iodoacetate in lipid nanostructures 用色谱法测定脂质纳米结构中的碘乙酸酯
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-5-12
D. Korshunov, I. A. Kondakova, E. Sidenko, E. Sereda, N. Y. Zolotukhina
A liposomal form of anticancer drugs is often used to improve pharmacokinetics and reduce systemic toxicity of the drugs. The goal of the study is to develop a method for quantitative analysis of a liposomal form of sodium iodoacetate (IA), glycolysis inhibitor, which exhibits a pronounced antitumor activity. Liposomes were prepared by extrusion at a temperature of 25 – 55°C under argon pressure ranged from 2 to 10 MPa. The obtained liposomes were purified from the non-incorporated component using dialysis. The method of HPLC was used to analyze the inhibitor solution in liposomes. The method of hydrophilic interaction chromatography revealed a high selectivity of iodoacetate with aminopropyl silica gel as a stationary phase. The best option for analysis was to use a spectrophotometric detector. The results of analysis showed that the dose of the inhibitor in 1 ml of liposomes was 0.20 – 0.23 mg regardless of the liposome size. In terms of the weight of an animal, the amount of iodoacetate was 8 – 9 mg/kg. The analysis of liposomes by the developed method showed that the highest yield and a high degree of purification is attained at low temperature (no more than 40°C) and duration of dialysis for about 3 h. For these purposes, the use of liposomes with a diameter of 400 nm turned out to be the best option.
抗癌药物的脂质体形式通常用于改善药物的药代动力学,降低药物的全身毒性。本研究的目的是开发一种方法,用于定量分析具有明显抗肿瘤活性的糖酵解抑制剂碘乙酸钠(IA)的脂质体形式。脂质体是在氩气压力为 2 至 10 兆帕斯卡、温度为 25 至 55 摄氏度的条件下挤压制备的。获得的脂质体通过透析从非结合成分中纯化出来。采用高效液相色谱法分析脂质体中的抑制剂溶液。亲水相互作用色谱法显示,以氨基丙基硅胶为固定相,碘乙酸酯的选择性很高。分析的最佳选择是使用分光光度检测器。分析结果表明,无论脂质体大小如何,1 毫升脂质体中的抑制剂剂量为 0.20 - 0.23 毫克。按动物体重计算,碘乙酸盐的用量为 8 - 9 毫克/千克。用所开发的方法对脂质体进行的分析表明,在低温(不超过 40°C)和透析时间约为 3 小时的情况下,脂质体的产量和纯度最高。
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引用次数: 0
Studying the effect of the argon flow introduced into the arc discharge in the atomic-emission spectrometry of powdered samples using the spillage-injection method 利用溢出注入法研究电弧放电中引入的氩流对粉末样品原子发射光谱分析的影响
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-13-21
S. Dodonov, A. A. Dzyuba, V. А. Labusov
Atomic emission spectral analysis of a powder sample by the method of spillage-injection into the plasma of an arc discharge burning in air is accompanied by the formation of cyanide, nitride and oxide compounds which form molecular bands in the spectrum thus impeding measuring the intensity of the analytical lines of the elements to be determined. Feeding an argon flow into the arc discharge can reduce the amount of spectral interference and increase the plasma temperature, which promotes more a complete evaporation of the analyzed sample injected into the arc discharge and, accordingly, increases the degree of ionization of the elements and the intensity of ion spectral lines. The aim of the study was to develop a device for argon introduction into the arc discharge zone and simultaneous sample delivery by a spillage-injection method, as well as to study the effect of argon consumption on arc discharge parameters and emission spectra of powder samples. The argon input device (up to 2.25 L/min) is developed on the basis on glass funnels, the geometric dimensions of which are selected with the goal of gaining the maximum intensity of spectral lines and reduced intensity of molecular bands at the minimal argon consumption. The study carried out on a «Grand Potok» spectrometer demonstrated that with an increase in argon consumption, the intensity of SiO molecular bands decreases, the plasma temperature increases by 350 – 540 K, and the intensity of ion and atomic lines with the ionization energy above 8 eV increases by more than 4.7 and 2.9 times, respectively. The developed device can be used in analysis of geological materials to improve the metrological characteristics of the results of atomic emission spectral analysis.
用溢出注入在空气中燃烧的电弧放电等离子体的方法对粉末样品进行原子发射光谱分析时,会形成氰化物、氮化物和氧化物化合物,这些化合物在光谱中形成分子带,从而妨碍测量待测元素分析线的强度。向电弧放电中注入氩气流可以减少光谱干扰,提高等离子体温度,从而促进注入电弧放电的分析样品的完全蒸发,相应地提高元素的电离程度和离子光谱线的强度。这项研究的目的是开发一种将氩气引入电弧放电区的装置,并通过溢出注入法同时输送样品,同时研究氩气消耗对电弧放电参数和粉末样品发射光谱的影响。氩气输入装置(最高 2.25 L/min)是在玻璃漏斗的基础上开发的,其几何尺寸的选择目标是以最小的氩气消耗量获得最大的光谱线强度并降低分子带的强度。在 "Grand Potok "光谱仪上进行的研究表明,随着氩气消耗量的增加,氧化硅分子带的强度会降低,等离子体温度会升高 350 - 540 K,电离能高于 8 eV 的离子线和原子线的强度会分别增加 4.7 倍和 2.9 倍以上。开发的装置可用于地质材料分析,以提高原子发射光谱分析结果的计量特性。
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引用次数: 0
Determination of iron in water by flame atomic absorption spectrometry with sorption preconcentration 利用吸附预浓缩火焰原子吸收光谱法测定水中的铁含量
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-22-30
U. U. Ruzmetov, E. S. Jumaeva, B. T. Orziqulov, Z. A. Smanova
Determination and monitoring of pollutants in the natural environment is an urgent task because of their impact on living organisms as a result of numerous anthropogenic impacts. For this reason, a large number of publications are devoted to the development, modification or optimization of analytical methods that can solve these problems. When determining trace elements present in various samples, such as natural and waste water, biological samples and alloy samples, direct determination by various instrumental methods is often impossible due to the matrix effect and rather low concentration of metal ions in the sample. The atomic absorption method is one of the methods widely used for the determination of iron ions, which has such advantages as simplified sample preparation, low probability of contamination and loss of elements, increased analytical productivity, the detection limit of components in the analyzed mixture reduced by several orders of magnitude, and the ability to determine trace amounts of elements in small samples. The aim of the study was to develop a technique for the preliminary concentration of Fe (III) ions in waters of various origins using a sorbent immobilized with sulfosalicylic acid and their further determination by flame atomic absorption spectrometry. Sorbents obtained on the basis of polyacrylonitrile modified with polyethylene polyamine (PPF-1 and PPA-1) with sulfosalicylic acid immobilized on their surface were used for selective sorption of Fe (III) ions. Optimal conditions for the immobilization of sulfosalicylic acid on sorbents and the formation of complexes with Fe (III) ions were studied. The developed sorption-atomic absorption technique provided determination of low concentrations of Fe (III) ions in various waters. The use of PPF-1 as a sorbent with immobilized sulfosalicylic acid for pre-concentration of iron has a number of advantages compared to traditional atomic absorption procedure, i.e., the simplicity, high degree of iron extraction, high sensitivity and selectivity of iron determination, as well as a low cost. The detection limit of iron ions is 0.01 μg/L, Sr does not exceed 0.033.
由于许多人为因素对生物体造成了影响,因此对自然环境中污染物的测定和监测是一项紧迫的任务。因此,大量出版物都致力于开发、修改或优化能够解决这些问题的分析方法。在测定各种样品(如天然水和废水、生物样品和合金样品)中的痕量元素时,由于基体效应和样品中金属离子浓度相当低,通常无法用各种仪器方法直接测定。原子吸收法是广泛应用于测定铁离子的方法之一,它具有样品制备简单、元素污染和损失概率低、分析效率高、分析混合物中成分的检测限可降低几个数量级以及能够测定小样品中的痕量元素等优点。本研究的目的是开发一种技术,利用固定了磺基水杨酸的吸附剂初步浓缩各种来源水体中的铁(III)离子,并进一步利用火焰原子吸收光谱法测定其含量。吸附剂是在聚丙烯腈的基础上用聚乙烯多胺(PPF-1 和 PPA-1)改性而成的,其表面固定有磺基水杨酸,用于选择性吸附铁(III)离子。研究了磺基水杨酸固定在吸附剂上以及与铁(III)离子形成络合物的最佳条件。所开发的吸附-原子吸收技术可测定各种水体中低浓度的铁(III)离子。与传统的原子吸收法相比,使用 PPF-1 作为固定化磺基水杨酸的吸附剂进行铁的预浓缩具有许多优点,即操作简单、铁提取率高、铁测定的灵敏度和选择性高以及成本低。铁离子的检测限为 0.01 μg/L,Sr 不超过 0.033。
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引用次数: 0
Study of the structure of yttrium-based nanoporous ceramic materials 钇基纳米多孔陶瓷材料的结构研究
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-53-59
R. Kapustin, V. I. Uvarov, A. O. Kirillov, V. O. Koputsky
Porous ceramic materials with high filtration performance are widely used in conditions of high chemical, thermal and radiation loads. The results of studying the structure and morphology of the pore space of ceramic membranes are presented. Ultradispersed refractory powder Y2O3 was used as a main component-filler. The synthesis was carried out using compaction, technological combustion and self-propagating high-temperature synthesis. The use of ultradisperse sintering additives with highly developed surface (MgO — 5 μm, SiC — 3, SiO2 — 5 μm) allowed us to ensure the energy efficiency of synthesis of high- porous ceramic materials at low temperatures. Analysis of the structure and pore space using mercury porometry and alternative methods showed that the average pore size in the synthesized 3D matrix composite material based on yttrium orthosilicate matrix with yttrium oxide filler is 1.1 μm, the equivalent hydraulic pore diameter being about 100 nm. The difference is attributed to the variability of cross sections and high tortuosity of pore channels. Since the density of the material is 2.3 g/cm3 and the compressive strength is about 2 MPa, it can be easily machined with carbide tools being a promising material for manufacturing products with complex shapes. The obtained results can be used in developing energy-efficient technologies of one-stage production of yttrium oxide-based filters with high porosity to be used under conditions of exposure to radiation, aggressive media and high temperatures.
具有高过滤性能的多孔陶瓷材料被广泛应用于高化学、热和辐射负荷条件下。本文介绍了对陶瓷膜孔隙结构和形态的研究结果。超分散耐火粉末 Y2O3 被用作主要成分-填料。合成采用了压制、技术燃烧和自蔓延高温合成法。通过使用表面高度发达的超分散烧结添加剂(MgO - 5 μm、SiC - 3、SiO2 - 5 μm),我们确保了在低温下合成高多孔陶瓷材料的能效。利用水银孔隙测量法和其他方法对结构和孔隙空间进行的分析表明,基于正硅酸钇基体和氧化钇填料合成的三维基复合材料的平均孔径为 1.1 μm,等效水力孔直径约为 100 nm。造成这种差异的原因是横截面的变化和孔道的高迂回度。由于这种材料的密度为 2.3 g/cm3,抗压强度约为 2 MPa,因此很容易用硬质合金工具进行加工,是一种制造复杂形状产品的理想材料。所获得的结果可用于开发高能效技术,用于在辐射、侵蚀性介质和高温条件下单步生产高孔隙率的氧化钇基过滤器。
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引用次数: 0
On the features of inhomogeneous residual stress identification using the digital speckle interferometry and the hole-drilling method 利用数字斑点干涉仪和钻孔法识别不均匀残余应力的特征
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-60-73
A. S. Plotnikov, E. Zavoychinskaya
A phenomenological approach to the actual problem of determining the inhomogeneous residual stress-strain state in the components of high-tech engineering systems at the stages of their design and operation is presented. The approach is based on physical and mechanical methods of measuring displacements. Current physical models describe the physical regularities of the residual states attributed to changes in the structure by the interaction of defects and dislocations in the field of micro- and meso-stresses. At the same time, there are the problems of the transition to the macrolevel, the construction of multilevel models, and the conversion of these models in engineering practice. In the framework of phenomenological approaches, in the general case, the solution of this problem requires the solution of three-dimensional inverse problems of thermoelasticity. A well-known mechanical method for determining a uniform field of residual elastic stresses recommended by ASTM E837 is described. The method proposed earlier by one of the authors for determining an inhomogeneous (in the plane) field of residual elastic stresses is discussed. A method of the three-dimensional inhomogeneous residual elastic stress-strain state determination based on the experimental determination of the displacement vector components by the method of step-by-step point hole-drilling and data of digital speckle interferometry and digital image correlation is developed. The constitutive relations for the components of the displacement vector are written in the form of Volterra integral operators. The basic operator functions are the functions of four variables, i.e., the coordinates of the cylindrical system (r, θ, z) associated with the hole, and the hole depth h. A method for verification of the basic functions is presented. The problem is reduced to the determination of three displacement functions of three variables: hole radius r, h, and z. Numerical simulation of basic functions is carried out. The obtained results are consistent with the known experimental data and calculated values of the deformation on the surface depending on the depth of the hole according to the ASTM E837 Standard.
针对高科技工程系统部件在设计和运行阶段的非均质残余应力-应变状态的实际问题,提出了一种现象学方法。该方法基于测量位移的物理和机械方法。当前的物理模型描述了残余状态的物理规律性,这些残余状态归因于微应力和介应力场中缺陷和位错相互作用导致的结构变化。同时,还存在向宏观层面过渡、构建多层次模型以及在工程实践中转换这些模型的问题。在现象学方法的框架内,在一般情况下,该问题的解决需要解决热弹性的三维逆问题。本文介绍了 ASTM E837 推荐的确定残余弹性应力均匀场的著名力学方法。还讨论了其中一位作者早先提出的确定不均匀(平面内)残余弹性应力场的方法。根据逐步点钻孔法对位移矢量分量的实验测定以及数字斑点干涉测量和数字图像相关数据,开发了一种三维非均质残余弹性应力-应变状态测定方法。位移矢量分量的构成关系以 Volterra 积分算子的形式书写。基本算子函数是四个变量的函数,即与孔相关的圆柱系统坐标 (r, θ, z) 和孔深度 h。问题简化为确定孔半径 r、h 和 z 这三个变量的三个位移函数。获得的结果与已知的实验数据和根据 ASTM E837 标准计算的孔深度表面变形值一致。
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引用次数: 0
Determination of the shear characteristics of polymer composite materials 测定聚合物复合材料的剪切特性
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-74-80
O. V. Abashev, E. I. Smagin, A. G. Yashutin
Layered polymer composite materials (LPCM) based on carbon fiber and epoxy are widely used in the construction of commercial aircraft both in manufacturing lightly loaded and main power elements of aircraft airframes. The level of mechanical characteristics for all the composite constructions must be confirmed by experimental data of coupon testing. One of the most important characteristics of a layered composite material is the ability to perceive shear loads. Standard test methods ASTM D5379 and ASTM D7078 are used to determine the shear characteristics. These test methods enable determination of the shear properties of composite materials based on a polymer matrix reinforced with a high-modulus fiber. Comparative tests were carried out according to both methods. The samples were made from the wall and the tehnological zones of the spar to determine the values of destructive stresses and shear modulus. The results showed that the shear stresses in the material obtained by ASTMD7078 significantly (1.8 times) exceed those determined by ASTM D5379. At the same time, the modulus of elasticity differs slightly (by 1.1 times). This is due to the sensitivity of the test results to the method of loading and the quality of the specimens. When stretched according to ASTMD7078, the load is transmitted through the front surfaces of the coupons, which are obtained with sufficiently high quality from the tooling or vacuum bag. When compressed by ASTM D5379, the parallelism of the faces through which the load is distributed becomes critical. Moreover, the thickness of the sample also affected the test results obtained according to ASTM D5379, the greater the thickness, the greater the shear modulus. Proceeding from the results obtained, the recommendations on the choice of the method to be used for determining the shear characteristics of LPCM are formulated.
基于碳纤维和环氧树脂的层状聚合物复合材料(LPCM)在商用飞机的制造中得到了广泛应用,既可用于制造飞机机身的轻载部件,也可用于制造飞机的主动力部件。所有复合材料结构的机械特性水平都必须通过试样测试的实验数据来确认。层状复合材料最重要的特性之一是承受剪切载荷的能力。标准测试方法 ASTM D5379 和 ASTM D7078 用于确定剪切特性。通过这些测试方法,可以确定基于高模量纤维增强聚合物基体的复合材料的剪切特性。根据这两种方法进行了比较试验。样品取自撑杆的壁和技术区,以确定破坏应力和剪切模量的值。结果表明,用 ASTMD7078 方法获得的材料剪应力大大超过 ASTM D5379 方法确定的值(1.8 倍)。同时,弹性模量也略有不同(1.1 倍)。这是由于测试结果对加载方法和试样质量的敏感性造成的。当按照 ASTMD7078 拉伸时,载荷通过试样的前表面传递,试样从工具或真空袋中获得,质量足够高。当按照 ASTM D5379 标准进行压缩时,负载通过的面的平行度变得至关重要。此外,试样的厚度也会影响 ASTM D5379 的测试结果,厚度越大,剪切模量越大。根据获得的结果,提出了选择用于确定 LPCM 剪切特性的方法的建议。
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引用次数: 0
Analysis of the electromagnetic properties of 2000NN/2000NM composites with ferroelectric and polymer matrices 带有铁电和聚合物基质的 2000NN/2000NM 复合材料的电磁特性分析
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-44-52
V. Kostishin, R. Shakirzyanov, I. Isaev, E. S. Savchenko, B. M. Skibo
The results of studying the electrical properties of ferrite-dielectric composites containing inclusions of Mn-Zn and Ni-Zn spinel ferrites with the same initial magnetic permeability (grades 2000NM and 2000NN, respectively) and different electrical resistance are presented. Four matrix materials, polymer and ceramic dielectrics with a different dielectric permittivity were used in the experiments: polystyrene (PS525), polyvinylidene fluoride (grade F2MB), lead zirconate titanate (ZTS-21), and barium titanate (TBK-3). Experimental samples of composites were obtained by hot (for a polymer matrix) or cold pressing with a binder (in case of ferroelectric ceramic matrix). It has been shown that the microwave-absorbing properties of the resulting composites significantly depend on the electrical properties of the dielectric matrix and the electrical resistivity of the filler. The highest attenuation of electromagnetic waves of 25 – 27 dB in the frequency range 4 – 5 GHz is observed for ferrite-polymer composites with a semiconductor filler of 2000NM with a thickness of microwave-absorbing material of 6 mm. For composites with Mn-Zn ferrite filler, a pronounced shift in the dispersion region of magnetic permeability is also observed, which in turn changes the frequency position of peak radio absorption. For the composites with a ferroelectric matrix, the operating frequency range for both fillers shifted to the low-frequency region 1 – 4 GHz with a maximum attenuation of up to 22 dB at the same thickness. It was experimentally confirmed that at a concentration of ferrite Cm = 40 % wt., the value of the frequency of absorption peal center fc and the minimum value of the reflection loss Kref for a filler with high electrical resistance of 2000NN decrease with an increase in the dielectric constant of the matrix. As for the composites with a 2000NM filler, the (ε’ of the matrix) dependence passes through a minimum. The obtained composites can be considered as effective microwave-absorbing materials for the frequency range 1 – 6 GHz with peak attenuation of the electromagnetic wave in the range 14 – 27 dB and frequency band (less than 10 dB) in the range 1.1 – 2.5 GHz.
本文介绍了研究铁氧体-介电复合材料电气特性的结果,这些复合材料含有具有相同初始磁导率(等级分别为 2000NM 和 2000NN)和不同电阻率的锰锌和镍锌尖晶石铁氧体夹杂物。实验中使用了四种具有不同介电常数的基体材料、聚合物和陶瓷电介质:聚苯乙烯(PS525)、聚偏氟乙烯(F2MB 级)、锆酸钛酸铅(ZTS-21)和钛酸钡(TBK-3)。复合材料的实验样品是通过热压(聚合物基体)或冷压(铁电陶瓷基体)获得的。实验结果表明,复合材料的微波吸收特性在很大程度上取决于介电基体的电特性和填料的电阻率。在频率范围为 4 - 5 GHz、微波吸收材料厚度为 6 mm、半导体填充物为 2000NM 的铁氧体-聚合物复合材料中,电磁波的最高衰减为 25 - 27 dB。对于含有 Mn-Zn 铁氧体填料的复合材料,还观察到磁导率色散区域的明显偏移,这反过来又改变了无线电吸收峰值的频率位置。对于含有铁电基体的复合材料,两种填料的工作频率范围都转移到了 1 - 4 GHz 的低频区域,在相同厚度下的最大衰减可达 22 dB。实验证实,在铁氧体浓度 Cm = 40% wt.时,具有 2000NN 高电阻的填料的吸收峰中心频率值 fc 和反射损耗最小值 Kref 会随着基体介电常数的增加而降低。至于含有 2000NM 填料的复合材料,其(基体的ε')相关性通过了一个最小值。所获得的复合材料可视为频率范围为 1 - 6 GHz 的有效微波吸收材料,其电磁波峰值衰减范围为 14 - 27 dB,频带(小于 10 dB)为 1.1 - 2.5 GHz。
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引用次数: 0
Experimental determination of the interlayer fracture toughness of a composite material 复合材料层间断裂韧性的实验测定
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-81-87
I. S. Belousov, V. A. Bespalov
Modeling the propagation of interlaminar defects in multilayer composite materials requires knowledge of the characteristics of the material under study associated with the fracture processes. The goal of the study is determination of the interlaminar fracture toughness in the case of normal traction (GIc). Finite element modeling of testing was carried out proceeding from the data obtained. The delamination process was modeled using the most common approaches within the finite element method: VCCT (virtual crack closure technique) and CZM (cohesive zone model), wherein the fracture toughness is used as the main parameter for the occurrence of delamination. The obtained data are compared with the experiment. To confirm the correctness of the obtained experimental data on the fracture toughness GIc, modeling of the process of compression testing of a strut-type specimen with a defect in the form of a through-the-width delamination was carried out. This problem includes a nonlinear static solution with buckling and subsequent post-buckling behavior, and, as a result, the spread of the delamination zone. The data obtained using finite element modeling are consistent with the available experimental data.
建立多层复合材料层间缺陷传播模型需要了解所研究材料与断裂过程相关的特性。本研究的目标是确定正常牵引(GIc)情况下的层间断裂韧性。根据获得的数据,对测试进行了有限元建模。分层过程使用有限元方法中最常见的方法进行建模:VCCT(虚拟裂缝闭合技术)和 CZM(内聚区模型),其中断裂韧性被用作分层发生的主要参数。获得的数据与实验结果进行了比较。为了证实所获得的断裂韧性 GIc 实验数据的正确性,对带有通宽分层缺陷的支柱型试样的压缩试验过程进行了建模。该问题包括一个非线性静态解决方案,包括屈曲和随后的屈曲后行为,以及分层区域的扩散。通过有限元建模获得的数据与现有的实验数据一致。
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引用次数: 0
Assessing the reliability of the forensic technique for the identification study of motor gasoline using gas-liquid chromatography 利用气液相色谱法评估鉴定车用汽油的法医技术的可靠性
Pub Date : 2023-12-18 DOI: 10.26896/1028-6861-2023-89-12-31-43
G. Bebeshko, G. G. Omel’yanyuk, O. V. Samoilova, A. I. Usov
A new approach to solving the problems of forensic examination of petroleum products, fuels and lubricants associated with establishing whether motor gasoline belongs to a common/different identification set is proposed. A methodology for the identification of gasoline using quantitative results of chromatographic determination of controlled parameters and subsequent evaluation of the results in pairwise compared samples according to the established criteria. The following parameters were selected as controlled indicators: values of research octane number (RON), concentrations of hydrocarbon groups (paraffins, isoparaffins, arenes, naphthenes, olefins) and oxygenates. Their determination was carried out using standardized methods. We used the hardware and software complex of a Chromatek-Crystal 5000 series, including the Chromatek-DHA data processing program. Estimated criteria or decision- making rules regarding the issues posed to an expert were determined to classify gasoline under one product name (generic set), one production technology (group set) or a common source of origin (one production batch, storage tank, etc.). The reliability of the method was assessed using a validation procedure consisted of three stages. We used a collection of AI-92 motor gasoline, selected at gas stations of four oil companies during six months of 2022 in various districts of Moscow. At the first stage, the performer analyzed 12 aliquots of each of four gasoline samples (samples that previously belonged to the common volume) at different times. It was established that the quality indicators of the proposed methodology (standard deviation of the repeatability and reproducibility, expanded uncertainty, limits of the repeatability and reproducibility) for each of the determined controlled indicators did not exceed the permissible errors established by standardized methods. At the second stage of the experiment, the performer combined 12 test samples into four groups from each manufacturer (one production technology) with three samples of different production times (different batches). By comparing the discrepancies in the measured values of the same controlled indicators between pairs of samples within groups and the discrepancy in average indicators between pairs of groups, the contractor identified gasolines manufactured using the same technology; gasolines produced by the same technology, but at different times (different batches) and, with a probability of 95%, gasolines having a common source of origin (previously belonging to a common volume). The conclusions of the validation study matched the original data on the samples, which confirmed the correctness of the developed comparison criteria. At the third stage (blind test), the performer examined seven gasoline samples of, information about the composition and properties of which was not provided to him. The results of the blind test were considered satisfactory. Thus, the validation results indicate the s
提出了一种新方法来解决石油产品、燃料和润滑剂的法医检验问题,即确定车用汽油是否属于共同/不同的鉴定组合。利用色谱法确定受控参数的定量结果以及随后根据既定标准对成对比较样品的结果进行评估的方法来鉴定汽油。选定以下参数作为控制指标:研究辛烷值 (RON)、碳氢化合物组(石蜡、异构烷烃、炔烃、环烷烃、烯烃)和含氧化合物的浓度。它们的测定采用标准化方法进行。我们使用了 Chromatek-Crystal 5000 系列的硬件和软件组合,包括 Chromatek-DHA 数据处理程序。就专家提出的问题确定了估计标准或决策规则,以便将汽油归类为一个产品名称(通用集)、一种生产技术(组集)或一个共同的原产地(一个生产批次、储罐等)。该方法的可靠性通过由三个阶段组成的验证程序进行评估。我们使用了 2022 年 6 个月期间在莫斯科各区四家石油公司加油站收集的 AI-92 车用汽油。在第一阶段,执行人员在不同时间分别分析了四个汽油样品(之前属于同一体积的样品)中的 12 个等分样品。结果表明,所建议方法的质量指标(重复性和再现性的标准偏差、扩大的不确定性、重复性和再现性的极限)中的每一个确定的控制指标都没有超过标准方法所规定的允许误差。在实验的第二阶段,执行人员将每个生产商(一种生产技术)的 12 个测试样品分成四组,每组有三个不同生产时间(不同批次)的样品。通过比较组内各组样品之间相同受控指标测量值的差异和各组之间平均指标的差异,承包商确定了使用相同技术生产的汽油、使用相同技术生产但生产时间不同(不同批次)的汽油,以及具有共同来源(以前属于同一批次)的汽油,概率为 95%。验证研究的结论与样品的原始数据相吻合,这证实了所制定的比较标准的正确性。在第三阶段(盲测),表演者检查了 7 个汽油样品,但没有向他提供这些样品的成分 和特性信息。盲测结果令人满意。因此,验证结果表明,该方法适用于解决与车用汽油有关的法医鉴定问题,执行人员的能力足以实施该方法。
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Industrial laboratory. Diagnostics of materials
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