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On the requirements for statistical methods of data analysis (generalizing article) 关于数据分析统计方法的要求(概括性文章)
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-98-106
A. I. Orlov
Half a century activity in consulting researchers of various specialties, reviewing articles and books, opposing dissertations provided the possibility of getting acquainted with hundreds of specific studies on the development and application of statistical methods. A variety of shortcomings in conducting research and publishing the results of studies have been revealed, which hinder the perception of the data obtained, and in some cases cast doubt on the adequacy of the conclusions. Therefore, it appeared advisable to develop natural requirements for methods of data processing and presentation of the results of statistical data analysis. This study is devoted to an initial consideration of a number of formulations of such requirements. We proceed from the modern paradigm of applied statistics, based on non-parametric and non-numerical statistics which replace the primitive paradigm of the 19th century and the paradigm of the middle of the 20th century using parametric distribution systems. When describing and discussing the procedures for analyzing statistical data, it is necessary to start with probabilistic-statistical models for generating the data under study. It is necessary to proceed from the theory of measurements, according to which the first step in the data analysis is identification of the scales in which they are measured. Statistical inference must be invariant under the allowable transformations of data measurement scales. Since almost all distributions of real data are non-normal, a preference should be given to non-parametric formulations. The possibility of using parametric families of distributions must be carefully justified. In accordance with the theory of testing statistical hypothesis, both the null and alternative hypotheses must be specified. It is necessary to study the stability of the conclusions drawn from the model with respect to acceptable changes in the initial data and assumptions of the model. A number of further publications of the author will be devoted to the problems of developing a system of requirements for statistical models and methods.
半个世纪以来,在向不同专业的研究人员提供咨询、审阅文章和书籍、反对学位论文等活动中,我们了解了数以百计的关于统计方法的发展和应用的具体研究。在进行研究和发表研究成果时发现了各种不足之处,这些不足之处妨碍了对所获数据的理解,在某些情况下还使人对结论的充分性产生怀疑。因此,对数据处理方法和统计数据分析结果的呈现方式提出自然要求似乎是可取的。本研究旨在对此类要求的若干表述方式进行初步探讨。我们从现代应用统计范式出发,以非参数和非数字统计为基础,取代 19 世纪的原始范式和 20 世纪中叶使用参数分布系统的范式。在描述和讨论统计数据的分析程序时,有必要从生成所研究数据的概率统计模型入手。必须从测量理论出发,根据测量理论,数据分析的第一步是确定测量的尺度。统计推论必须在数据测量尺度的允许变换下保持不变。由于几乎所有真实数据的分布都是非正态分布,因此应优先考虑非参数公式。使用参数系列分布的可能性必须经过仔细论证。根据统计假设检验理论,必须明确零假设和备择假设。有必要研究从模型中得出的结论在初始数据和模型假设发生可接受的变化时的稳定性。作者的其他一些著作将专门讨论统计模型和方法要求系统的开发问题。
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引用次数: 0
Study of the effect of the morphology of initial powders on the structural and dimensional characteristics of SiC-based porous ceramic materials 研究初始粉末形态对 SiC 基多孔陶瓷材料结构和尺寸特征的影响
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-44-51
R. Kapustin, A. O. Kirillov, V. I. Uvarov, V. V. Zakorzhevsky
The realization of the necessary energy-efficient technological solutions for the production of highly porous SiC-ceramic materials requires appropriate research. The results of developing energy-efficient one-step methods for the synthesis of porous SiC-based ceramics and studying the characteristics of the obtained ceramics are presented. The effect of the morphology of initial powders on the synthesized product is considered. Ultrafine silicon carbide powders of two types, identical in characteristic particle size, but quite different in the surface morphology, were used as fillers in the synthesis of experimental samples of porous ceramics. The first one was obtained by the traditional furnace method (SiCf), the second one was synthesized by the technology of self-propagating high-temperature synthesis (SiCshs). It is shown that the particle morphology of initial powder components determines the structural parameters and characteristics of synthesized porous ceramics. The pore space parameters (average pore size, specific surface area, equivalent hydraulic diameter, permeability, etc.) can vary significantly. Porous ceramic materials synthesized on the basis of SiCf have an open porosity of 47%, high liquid permeability (up to 2 mDarcy), overwhelming dominance of α-SiC phase, and a narrow pore distribution with an average pore size of about 1 μm. High open porosity (more than 58 %), highly developed nanostructured pore space surface with an area of more than 12 m2/g, and wider pore size distribution (average pore size — 140 nm) are observed in porous ceramic materials based on SiCshs. The obtained results can be used to improve energy-efficient synthesis technologies and methods for predicting the properties of highly porous SiC-based ceramic materials. This will make it possible to create highly porous SiC ceramics within a priory predicted limits of effective applicability for the processes of ultrafiltration or catalysis.
要实现生产高多孔碳化硅陶瓷材料所需的高能效技术解决方案,需要进行适当的研究。本文介绍了开发高能效一步法合成多孔碳化硅基陶瓷的成果,以及对所获陶瓷特性的研究。研究考虑了初始粉末形态对合成产物的影响。在合成多孔陶瓷实验样品时,使用了两种类型的超细碳化硅粉末作为填料,它们的特征粒度相同,但表面形态却截然不同。第一种是通过传统炉法获得的(SiCf),第二种是通过自蔓延高温合成技术合成的(SiCshs)。研究表明,初始粉末成分的颗粒形态决定了合成多孔陶瓷的结构参数和特性。孔隙空间参数(平均孔径、比表面积、等效水力直径、渗透率等)会有很大变化。以 SiCf 为基础合成的多孔陶瓷材料的开放孔隙率为 47%,液体渗透率高(达 2 mDarcy),α-SiC 相占优势,孔隙分布窄,平均孔径约为 1 μm。基于 SiCshs 的多孔陶瓷材料具有较高的开放孔隙率(超过 58%)、高度发达的纳米结构孔隙表面(面积超过 12 m2/g)和较宽的孔径分布(平均孔径为 140 nm)。所获得的结果可用于改进高能效合成技术和预测高多孔碳化硅基陶瓷材料性能的方法。这将使在超滤或催化过程的有效适用范围内制造高孔隙碳化硅陶瓷成为可能。
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引用次数: 0
Modes of wear of babbitt-based composite materials produced by hot pressing 热压法生产的巴比妥基复合材料的磨损模式
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-89-97
P. Bykov, I. Kalashnikov, L. Kobeleva, I. Katin, R. Mikheev
The effect of additives of Ti2NbAl intermetallic compound on the friction of B83 babbitt samples obtained by hot pressing was studied using optical, electron microscopy and EDS analysis. The structure, friction surface and wear products were studied. Tribological tests were carried out on a universal test system under conditions of dry sliding friction according to the scheme of axial loading: a steel bush against a disk of the material under study. The temperature values near the friction zone were recorded. The limits of application of the material depend on the mode and mechanism of wear occurring in the tribocontact. Changes in the mode and mechanism of wear were assessed by differences in the behavior of the friction coefficient, temperature, difference in the state of friction surfaces, wear intensity and wear products. The results obtained indicate the prospects of using the method of hot pressing of powder from the B83 alloy and discrete particles of the high-strength Ti2NbAl intermetallic phase to get composite materials with improved tribological properties compared to a babbitt alloy. The introduction of reinforcing high-modulus particles of intermetallic compounds changed the structure of the material and affected the friction processes in babbitt, pushing aside the onset of change in the mode of wear towards more severe friction conditions. A significant decrease in the wear intensity of babbitt-based composite materials compared to the original alloy makes it possible to predict an increase in the service life of tribo-units. The data obtained enable us to determine and recommend modes that improve the performance of tribo-nodes in the manufacture of both volumetric inserts and plain bearings made of B83 alloy and, moreover, to create new functionally organized layered compositions with enhanced tribotechnical properties with a base of structural steels and working surface layers not only using B83 babbitt, but also of composite materials based on B83 babbitt.
使用光学、电子显微镜和 EDS 分析方法研究了 Ti2NbAl 金属间化合物添加剂对热压获得的 B83 巴比特样品摩擦的影响。研究了样品的结构、摩擦表面和磨损产物。根据轴向加载方案,在干滑动摩擦条件下,在通用测试系统上进行了摩擦学测试:钢衬套与所研究材料的圆盘相对。记录了摩擦区附近的温度值。材料的应用范围取决于摩擦接触中发生磨损的方式和机理。磨损模式和机理的变化是通过摩擦系数、温度、摩擦表面状态差异、磨损强度和磨损产物的行为差异来评估的。研究结果表明,与巴比特合金相比,使用 B83 合金粉末和高强度 Ti2NbAl 金属间相离散颗粒的热压方法可以获得摩擦学性能更好的复合材料。高模量金属间化合物增强颗粒的引入改变了材料的结构,影响了巴比特合金的摩擦过程,使磨损模式开始向更严重的摩擦条件转变。与原始合金相比,巴氏合金基复合材料的磨损强度明显降低,这使我们有可能预测三元组使用寿命的延长。所获得的数据使我们能够确定并推荐在制造 B83 合金的体积插入件和滑动轴承时提高三节点性能的模式,此外,还能以结构钢和工作表面层为基础,不仅使用 B83 巴比特,还使用基于 B83 巴比特的复合材料,创建具有增强摩擦技术性能的新功能组织分层组合。
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引用次数: 0
Analysis of cerium-substituted yttrium iron garnets by inductively coupled plasma atomic emission spectrometry with preliminary microwave decomposition 利用电感耦合等离子体原子发射光谱法和初步微波分解分析铈代钇铁石榴石
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-24-33
N. A. Korotkova, K. V. Petrova, V. B. Baranovskaya
An analytical procedure for inductively coupled plasma atomic emission (ICP-AES) analysis of iron garnets of the composition Y3 – xCexFe5 – yGayO12, where x = 0.4 – 0.5 and y = 2.4 – 2.6 with preliminary microwave decomposition of the sample is described. The compositions of acid mixtures (HCl/HNO3), as well as modes of microwave heating (holding time and temperature), providing complete dissolution of the samples are proposed. In addition to optimized sample preparation, conditions for ICP-AES analysis of cerium-doped yttrium iron garnets were studied. The effect of matrix components (Y, Ce, Fe, Ga) on the determination of doping elements was revealed and studied. The operating parameters of the spectrometer (ICP power and nebulizer flow rate) have been substantiated, which make it possible to reduce the matrix effect of Fe, Ga, Y, Ce on the elements Na, Mg, Al, Si, P, K, Ca, Sc, Cr, Mn, Co, Ni, Cu, Zn, Se, Cd, Sn, Te, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Pb in iron yttrium garnets by the ICP-AES. ICP-AES measurements were performed in the axial and radial mode for trace elements and in the radial mode for matrix elements. The limits of quantification (LOQs) of most elements ranged within n × 10–5 – n × 10–4 wt.%. The accuracy is confirmed by the spike recovery test. The relative standard deviation is in the range of 1 – 5% depending on the selected plasma view mode and the analyzed analytes. The developed method makes it possible to determine macro- and microcomponents in yttrium iron garnets in a wide range of concentrations with a high accuracy.
本文介绍了对成分为 Y3 - xCexFe5 - yGayO12(其中 x = 0.4 - 0.5 和 y = 2.4 - 2.6)的铁榴石进行电感耦合等离子体原子发射(ICP-AES)分析的分析程序,并对样品进行了初步的微波分解。提出了可使样品完全溶解的酸混合物(HCl/HNO3)的成分以及微波加热模式(保温时间和温度)。除了优化样品制备,还研究了掺铈钇铁石榴石的 ICP-AES 分析条件。揭示并研究了基体成分(Y、Ce、Fe、Ga)对掺杂元素测定的影响。对光谱仪的操作参数(ICP 功率和雾化器流速)进行了论证,从而降低了 Fe、Ga、Y、Ce 对 Na、Mg、Na 元素的影响、铈对 Na、Mg、Al、Si、P、K、Ca、Sc、Cr、Mn、Co、Ni、Cu、Zn、Se、Cd、Sn、Te、La、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Pb 等元素的影响。痕量元素的 ICP-AES 测量采用轴向和径向模式,基体元素的 ICP-AES 测量采用径向模式。大多数元素的定量限(LOQ)在 n × 10-5 - n × 10-4 wt.%之间。通过尖峰回收测试确认了其准确性。相对标准偏差在 1 - 5% 之间,具体取决于所选的血浆观察模式和所分析的分析物。所开发的方法可以在较宽的浓度范围内准确测定钇铁石榴石中的宏观和微观成分。
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引用次数: 0
Study of the phase characteristics of vibration sensors and conditions of orthogonalization of their measuring basis for the systems of vibration control and vibration testing of materials 研究振动传感器的相位特征及其测量基础的正交化条件,用于振动控制和材料振动测试系统
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-34-43
A. Zhdanov
To identify the most vibration-sensitive structures of the materials during vibration tests, it is necessary to determine the vibration vector in an orthogonal basis The effectiveness of the tests depends on the accuracy of the vector measurement. The transverse sensitivity of tri-axial vibration transducers, which have found vast application in various vibration measuring and material testing systems, leads to increased measurement errors and limits the frequency range of measurements. The errors can be reduced to almost zero using the proposed method of electronic orthogonalization, which involves rotation of the sensitivity vectors until they coincide with the orthogonal basis, resulting in zero transverse sensitivity. This approach has been successfully developed and works rather well in the low frequency band of the vibration transducer frequency response, wherein the amplitude-characteristics are linear and there is no phase shift in the channels. An emphasis is made on the influence of the phase characteristics of vibration sensors on the formation of orthogonalizing matrices that determine the requirements for an orthogonalizer. The structure of the installation for automated recording amplitude-frequency and phase-frequency responses of the vibration transducer, methodology and results of experimental study of a tri-axial piezoelectric accelerometer (TPA) with one inertia element and oblique-angle measuring basis are presented. The results obtained under vibration activated in three mutually perpendicular directions along the measuring axes show that the transducer measuring system is properly designed to provide for effective broadband orthogonalization of the measuring basis. The results obtained can be used to develop orthogonalizing transducers that eliminate transverse sensitivity in a wide frequency range, as well as to improve the design of sensors and their metrological characteristics.
为了在振动测试中确定材料中对振动最敏感的结构,有必要在正交基础上确定振动矢量。在各种振动测量和材料测试系统中得到广泛应用的三轴振动传感器的横向灵敏度导致测量误差增大,并限制了测量的频率范围。使用所提出的电子正交化方法,可将误差降至几乎为零,该方法包括旋转灵敏度矢量,直到它们与正交基重合,从而使横向灵敏度为零。这种方法已经成功开发出来,在振动传感器频率响应的低频段效果相当好,其中的振幅特征是线性的,通道中没有相移。重点是振动传感器的相位特性对形成正交矩阵的影响,正交矩阵决定了对正交器的要求。文中介绍了自动记录振动传感器振幅-频率和相位-频率响应的装置结构,以及对带有一个惯性元件和斜角测量基础的三轴压电加速度计(TPA)进行实验研究的方法和结果。在沿测量轴三个相互垂直方向的振动激活下获得的结果表明,传感器测量系统设计得当,可以有效地对测量基础进行宽带正交化。所获得的结果可用于开发正交化传感器,以消除宽频率范围内的横向敏感性,并改进传感器的设计及其计量特性。
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引用次数: 0
Fields of residual stresses near open assemblage holes of aircraft wing panel 飞机机翼面板开放式装配孔附近的残余应力场
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-71-88
S. Eleonsky, M. D. Zaitsev, Y. G. Matvienko, V. Pisarev
The results of fatigue tests of two geometrically identical and similar in design models of the lower wing panel of a commercial aircraft are were analyzed. The panels differed in the way of installing mounting bolts, which connect the skin and stringers. Cold expansion of holes drilled both in the skin and stringer has been performed for the first panel before joining. The second panel includes no additional treatment after drilling pilot holes and final reaming. Bolts are mounted with an interference fit varying from 1.3 to 2.1% and from 2.9 to 3.2% for the first and the second panel, respectively. Changes in the interference fit are the consequence of a scatter attributed to the presence of a tolerance zone for the diameters of both bolts and mounting holes. A two-step comparison of both technologies is based on the experimental study of residual stress fields. The first stage, being a subject of the present study, includes the analysis of residual stress fields, which arise after removing bolts and separation of skin from stringers. Hole drilling and gradual crack growth were used to determine the components of residual stresses. Deformation response is measured by electronic speckle-pattern interferometry. High quality interferograms, which provide a reliable resolution of the interference fringes of ultimate density over the hole edge or directly along the notch borders, have been obtained for both ways of local removing the material. The first point-wise method based on drilling a probe hole, provides a quantitative determination of the residual stress components, starting from 1.4 mm distance from the assemblage hole edge. The second technique implements the crack compliance method of subsequent lengthening of the notch, starting directly from the mounting hole edge. This approach provides for a quantitative analysis of residual stress fields, related to different bolt mounting technologies, proceeding from the comparison of SIF values. A high level of compressive residual stresses near open holes is characteristic for both types of panels. Both experimental approaches showed the benefits of joints, where bolts are mounted into cold-expanded (reinforced) holes. For this case, the estimation of the relaxation parameters of the principal component of residual stresses in the direction of the external load is presented.
我们分析了两架几何形状相同、设计相似的商用飞机下翼面板的疲劳试验结果。这两种机翼面板在安装连接蒙皮和弦杆的螺栓的方式上有所不同。第一个面板在连接前对蒙皮和弦杆上的钻孔进行了冷膨胀处理。第二块面板在钻孔和最后铰孔之后没有进行额外的处理。第一块面板和第二块面板的螺栓安装过盈配合分别为 1.3%至 2.1%和 2.9%至 3.2%。过盈配合的变化是由于螺栓和安装孔直径存在公差带而产生的散差。通过对残余应力场的实验研究,对两种技术进行了两步比较。第一阶段是本研究的主题,包括对残余应力场的分析,残余应力场产生于螺栓拆除和蒙皮与弦杆分离之后。采用钻孔和裂纹逐渐增长的方法来确定残余应力的成分。变形响应是通过电子斑点模式干涉仪测量的。这两种局部去除材料的方法都获得了高质量的干涉图,对孔边缘或直接沿缺口边界的极限密度干涉条纹提供了可靠的分辨率。第一种方法以钻探孔为基础,从距装配孔边缘 1.4 毫米处开始,对残余应力成分进行定量测定。第二种技术采用裂纹顺应性方法,直接从安装孔边缘开始,随后延长缺口。这种方法通过比较 SIF 值,对与不同螺栓安装技术相关的残余应力场进行定量分析。两种类型的面板在开孔附近都存在较高的压缩残余应力。两种实验方法都显示了将螺栓安装到冷膨胀(加固)孔中的接头的优点。针对这种情况,介绍了外部载荷方向残余应力主分量松弛参数的估算。
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引用次数: 0
Study of the electrophysical and magnetic properties of a Dirac 3D semimetal Cd3As2 with nanogranules of MnAs 具有 MnAs 纳米颗粒的狄拉克三维半金属 Cd3As2 的电物理和磁特性研究
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-52-59
L. A. Saypulaeva, N. Melnikova, M. M. Gadzhialiev, A. Tebenkov, A. Babushkin, V. Zakhvalinskii, M. H. Al-Onaizan, A. Ril
We report on the main results of studying the electrical and magnetoresistance (MR) of a composite material consisting of 70 % mol. Dirac semi-metal Cd3As2 and 30 % mol. ferromagnet MnAs at pressures up to 50 GPa in a diamond anvil cell with a «rounded cone-flat» type anvils, as well as magnetization at hydrostatic pressures up to 6 GPa in a toroid-shaped high-pressure cell, both at room temperature and in the temperature range of 180 – 350 K at atmospheric pressure. A mixture of methanol and ethanol in a ratio of 4:1 was used as a pressure transmitting medium. Elemental analysis of Cd3As2 + 30 % mol MnAs composites showed that much of the volume is occupied by the Cd3As2 phase. The proportion of MnAs phase inclusions is less than 5 %. The feature of Cd3As2 + MnAs is the presence of a significant region of non-mixing of the Cd3As2 and MnAs phase melts. A negative MR was revealed with increasing pressure in the entire studied baric zone. The maximum negative MR is observed in the baric zone of 22 – 26 GPa. Further increase in the pressure up to the maximum level result in the appearance of several extrema on the ΔR/R0(P) curve, with negative MR not exceeding 4 %. Upon pressure release from 50 GPa, the baric dependence of ΔR/R0(P) is characterized by an inversion of the MR sign: at pressures around 40 GPa, a negative MR is replaced by a positive MR, and at around 20 GPa, the maximum value of positive MR of ~5.3 % is observed. Signs of the instability of the monoclinic structure of Cd3As2 resulted from its partial decomposition upon decompression were revealed. The results obtained can be used in spintronics when using appropriate composite materials.
我们报告了由 70% mol.我们报告了在室温和大气压下 180 - 350 K 温度范围内,在带有 "圆锥扁平 "型砧的金刚石砧池中,在高达 50 GPa 的压力下,以及在环形高压池中,在高达 6 GPa 的静水压力下,对一种由 70 % mol.的狄拉克半金属 Cd3As2 和 30 % mol.的铁磁体 MnAs 组成的复合材料进行磁电阻(MR)研究的主要结果。使用甲醇和乙醇以 4:1 的比例混合作为压力传输介质。Cd3As2 + 30 % mol MnAs 复合材料的元素分析表明,Cd3As2 相占据了大部分体积。砷化锰相夹杂物的比例小于 5%。Cd3As2 + MnAs 的特点是 Cd3As2 和 MnAs 相熔体存在一个显著的非混合区域。在所研究的整个巴里克区,随着压力的增加,磁共振呈负值。在 22 - 26 GPa 的巴压区观察到最大的负磁阻。压力进一步增加到最大值时,ΔR/R0(P) 曲线上会出现几个极值,负磁阻不超过 4%。当压力从 50 GPa 释放时,ΔR/R0(P) 的巴氏相关性表现为 MR 符号的反转:在压力约为 40 GPa 时,负 MR 被正 MR 取代,而在约为 20 GPa 时,观察到正 MR 的最大值约为 5.3%。减压时部分分解导致 Cd3As2 的单斜结构出现不稳定迹象。当使用适当的复合材料时,所获得的结果可用于自旋电子学。
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引用次数: 0
Metrological assurance for the analytical control of flotation reagents based on aliphatic alkoxyamines in technological media and waste of iron ore enrichment processes 基于脂肪族烷氧基胺的浮选试剂在技术介质和铁矿石浓缩过程废物中的分析控制的计量保证
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-14-23
A. Y. Ivanova, I. B. Maksakova, V. A. Zirina, A. I. Krylov, N. A. Yurlova
Methodological developments related to the determination of the content of cationic flotation reagents (collectors) based on aliphatic alkoxyamines (Flotigam EDA, Tomamine M-4213, Feiying: TG-928) in technological media and waste of iron ore enrichment processes are considered to ensure the analytical control of technological processes in view of a danger character of generated waste. A spectrophotometric method for determination of cationic amino-containing surfactants can be used for express- and screening analysis. The method of gas chromatography was used to increase the reliability of alkoxyamine measurement and in arbitration cases. The ranges of determinable content for the photometric method in aqueous media were 0.04 – 100 mg/dm3 (extended uncertainty from 20 to 25%) and 3 – 1000 (extended uncertainty from 22 to 30%) in solid media; whereas for gas chromatographic procedure the content ranged within 0.02 – 100 mg/dm3 (extended uncertainty from 20 to 25%) in aqueous media and from 1.0 to 1000 mg/kg (extended uncertainty from 20 to 30%) in solid media, respectively. The methods for determination of the main components, alkoxyamines, in commercial compositions of amine-containing flotation reagents are also presented. The methods have been tested in modeling flotation procedures (to optimize relevant conditions and regimes of real production), certified and included in the Federal State Information System (FSIS) «Arshin».
考虑到铁矿石富集过程中产生的废物具有危险性,为确保对技术过程进行分析控制,我们考虑了与测定技术介质和废物中基于脂肪族烷氧基胺(Flotigam EDA、Tomamine M-4213、Feiying: TG-928)的阳离子浮选试剂(捕集剂)含量有关的方法学发展。测定含阳离子氨基表面活性剂的分光光度法可用于明示和筛选分析。气相色谱法用于提高烷氧基胺测量的可靠性和仲裁情况。光度法在水介质中的可测定含量范围为 0.04 - 100 mg/dm3(扩展不确定度为 20%至 25%),在固体介质中的可测定含量范围为 3 - 1000 mg/dm3(扩展不确定度为 22%至 30%);而气相色谱法在水介质中的可测定含量范围为 0.02 - 100 mg/dm3(扩展不确定度为 20%至 25%),在固体介质中的可测定含量范围为 1.0 - 1000 mg/kg(扩展不确定度为 20%至 30%)。此外,还介绍了测定含胺浮选试剂商业成分中主要成分烷氧基胺的方法。这些方法已在浮选程序模型中进行了测试(以优化实际生产中的相关条件和制度),并通过了认证,被纳入联邦国家信息系统(FSIS)"Arshin"。
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引用次数: 0
Non-target analysis of livestock products and feed for residues of drugs, pesticides, mycotoxins and their metabolites by high-resolution mass spectrometry (a review) 利用高分辨质谱法对畜产品和饲料中的药物、杀虫剂、霉菌毒素及其代谢物残留进行非目标分析(综述)
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-5-13
L. Kish, O. Lavrukhina, V. G. Amelin, A. Tretyakov, T. D. Pen’kov, D. Y. Nekrasov
A review of techniques of non-target analysis for simultaneous identification and determination of veterinary drugs, pesticides, mycotoxins, their metabolites, and substances of chemical transformation in livestock products using liquid chromatography and high-resolution mass spectrometry is presented. Some limitations of the approach are noted, such as the necessity of using common extraction conditions, the possibility of analyte transformations during the sample preparation, false positive results for isobaric and isomeric compounds, and the lack of spectral data for previously unexplored substances. However, the method is the most promising tool for the determination of pollutants not identified in the targeted analysis, as in the case of multicomponent screening of food and raw materials, and in the study of the parent compounds transformation.
本文综述了利用液相色谱法和高分辨率质谱法同时鉴定和测定畜产品中兽药、农药、霉菌毒素及其代谢物和化学转化物质的非目标分析技术。报告指出了该方法的一些局限性,如必须使用普通的提取条件、样品制备过程中分析物可能发生转化、对异构体和同分异构体化合物的检测结果为假阳性,以及缺乏以前未开发物质的光谱数据。不过,该方法是测定目标分析中未发现的污染物的最有前途的工具,例如在食品和原材料的多组分筛选以及母体化合物转化研究中。
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引用次数: 0
The use of acoustic emission in assessing the ductility loss in steel products under the effect of impact 利用声发射评估钢制品在冲击作用下的延展性损失
Pub Date : 2023-11-21 DOI: 10.26896/1028-6861-2023-89-11-60-70
N. Makhutov, I. E. Vasil’ev, D. Chernov, A. Marchenkov
Acoustic emission (AE) diagnostics was carried out during tensile testing of 20KhN2MA steel samples to study the loss of ductility after the impact. We used V-notched samples (3.3 mm in depth) with overall dimensions of 300 × 20 × 6 mm. The impact in the concentrator zone caused the depletion of the plasticity of the material, which was accompanied by a decrease in the partial fraction of ductile fracture and an increase in brittle fracture. The test samples were divided into six batches. The samples of the first batch were not subjected to the impact. In the second batch, the impact energy was 50 J, in the third — 75 J, in the fourth — 100 J, in the fifth — 125 J and in the sixth — 150 J. The rupture tests were carried out at room temperature and at a speed of the movable traverse of 1 mm/min. The kinetics of damage in the notch zone during loading was monitored using the acoustic emission (AE) method and video recording. Processes of brittle and ductile (caused by cleavage and shear, respectively) destruction of the crystal lattice of a metal differ primarily in the speed and duration of stress waves. To separate AE pulses generated by these processes, spectrograms of time-frequency transformations and waveforms were analyzed. Pulse selection was carried out using a complex parameter reflecting the steepness of the amplitude drop at the phase of signal attenuation. Boundary values were determined that allow separation of the recorded pulses into flows caused by ductile and brittle structural damage to structural steels. It is shown that manifestation of the effect of impact on the exhaustion of the plastic properties of steel 20KhN2MA becomes noticeable when the level of specific work exceeds 50 J/cm2. Moreover, with an increase in the specific work up to 150 J/cm2, the weight content of location pulses characterizing the kinetics of brittle destruction of structural bonds increased by 3 – 4 times, relative to that recorded for the samples without impact. This result correlates with the duration of the rupture test of the samples, which was reduced by three times when the level of the specific work increased to 150 J/cm2
在对 20KhN2MA 钢样品进行拉伸测试时,我们进行了声发射 (AE) 诊断,以研究冲击后延展性的损失。我们使用了整体尺寸为 300 × 20 × 6 毫米的 V 型缺口样品(深度为 3.3 毫米)。集中器区域的冲击造成了材料塑性的损耗,并伴随着韧性断裂部分分数的减少和脆性断裂的增加。试验样品分为六批。第一批样品未受到冲击。第二批的冲击能量为 50 焦耳,第三批为 75 焦耳,第四批为 100 焦耳,第五批为 125 焦耳,第六批为 150 焦耳。断裂试验在室温下进行,移动横梁的速度为 1 毫米/分钟。利用声发射(AE)方法和视频记录对加载过程中缺口区的损伤动力学进行了监测。金属晶格的脆性和韧性(分别由劈裂和剪切引起)破坏过程主要在应力波的速度和持续时间上有所不同。为了将这些过程产生的 AE 脉冲区分开来,我们分析了时频变换的频谱图和波形。脉冲选择是通过一个反映信号衰减阶段振幅下降陡度的复杂参数进行的。确定的边界值可将记录的脉冲分为由结构钢的韧性和脆性结构损伤引起的流动。结果表明,当比功水平超过 50 J/cm2 时,冲击对 20KhN2MA 钢塑性耗尽的影响变得明显。此外,随着比功增加到 150 J/cm2,表征结构键脆性破坏动力学的位置脉冲重量含量比无冲击样品增加了 3 - 4 倍。这一结果与样品断裂测试的持续时间相关,当比功增加到 150 焦耳/平方厘米时,样品断裂测试的持续时间缩短了三倍。
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引用次数: 0
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Industrial laboratory. Diagnostics of materials
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