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Converting the Instrumented Indentation Diagrams of a Ball Indenter into the Stress–Strain Curves for Metallic Structural Materials 将球形压头的仪器压痕图转换为金属结构材料的应力-应变曲线
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523150116
V. M. Matyunin, A. Yu. Marchenkov, P. V. Volkov, M. A. Karimbekov, D. A. Zhgut, M. P. Petrova, N. O. Veremeeva

Abstract

The available approaches to converting indentation diagrams into stress–strain curves are reviewed. It is noted that most studies on converting the instrumented indentation diagrams of a ball indenter into the stress–strain curves have been carried out within the uniform deformation limits using various computational and experimental approaches, including the finite element method and neural networks. In the authors’ opinion, however, it is reasonable to perform the conversion of one diagram to another using the established relationship between indentation and tension deformations. This makes it possible not only to perform the conversion with a higher accuracy but also to evaluate the mechanical properties under tension from the indentation characteristics. The formulas most frequently used to determine plastic deformation contain a relative indentation diameter as the main parameter. Meanwhile, at the same relative indentation diameter and a constant ratio between the average contact pressure (Meyer hardness) and the true tensile stress, the indentation and tensile strain values can be significantly different owing to different strain hardening abilities of materials. The authors have established a relationship between the true elastoplastic deformation in the tensile tests and the relative depth of an unrecovered indentation obtained with a ball indenter with allowance for the strain hardening parameter determined from the instrumented indentation diagram. On the basis of the established relationship, a technique for converting the instrumented indentation diagram into a stress–strain curve in the uniform deformation region with the determination of the yield strength, tensile strength, and ultimate uniform tension has been developed. The technique has been verified by testing steels and aluminum, magnesium, and titanium alloys with strongly different Young’s moduli, strength characteristics, plasticity, and strain hardening.

摘要 综述了将压痕图转换为应力应变曲线的现有方法。研究指出,将球压头的仪器压痕图转换为应力应变曲线的大多数研究都是在均匀变形极限范围内使用各种计算和实验方法进行的,包括有限元法和神经网络。但作者认为,利用压痕和拉伸变形之间的既定关系将一种图表转换为另一种图表是合理的。这样不仅能以更高的精度进行转换,还能根据压痕特征评估拉伸下的机械性能。最常用于确定塑性变形的公式包含一个作为主要参数的相对压痕直径。同时,在相同的相对压痕直径和平均接触压力(梅耶尔硬度)与真实拉伸应力的恒定比值下,由于材料的应变硬化能力不同,压痕值和拉伸应变值可能会有很大差异。作者建立了拉伸试验中的真实弹塑性变形与球形压头获得的未恢复压痕相对深度之间的关系,并考虑了从仪器压痕图中确定的应变硬化参数。根据已建立的关系,开发了一种技术,可将仪器压痕图转换为均匀变形区域的应力-应变曲线,并确定屈服强度、抗拉强度和极限均匀拉力。该技术已通过测试具有强烈不同杨氏模量、强度特性、塑性和应变硬化的钢、铝、镁和钛合金得到验证。
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引用次数: 0
Chemical Analysis of CsPbBr2X (X = Cl, I) Nanocomposites by Total Reflection X-Ray Fluorescence Spectroscopy (TXRF) 利用全反射 X 射线荧光光谱 (TXRF) 分析 CsPbBr2X(X = Cl,I)纳米复合材料的化学性质
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523140054
D. G. Filatova, A. S. Chizhov, M. N. Rumyantseva

Abstract

An approach to TXRF determination of the composition of perovskite nanocomposites of the putative compositions CsPbBr2Cl and CsPbBr2I is proposed. Sample preparation consists in the treatment of hydrophobic samples with dimethylformamide (DMFA) and the subsequent dilution of the obtained solutions with water. When using a copper solution as an internal standard, the reproducibility of the results of TXRF determination of the elements is attained with Sr no more than 0.05. The validity of the determination of Cs, Pb, Br, and I is confirmed by the results of their determination by ICP-MS in solutions after processing samples in DMFA followed by dilution with 2% HNO3 for Cs, Pb, and Br or tetramethylammonium hydroxide (TMAH) for Cs, Pb, Br, and I, whereas the determination of chlorides is confirmed by the method of direct potentiometry in diluted solutions. It is shown that lead does not form insoluble chlorides in the TMAH solution and does not interfere with the determination. The effect of bromides on the determination of chlorides is characterized by a potentiometric coefficient of 10–3. The results obtained provide the determination of the stoichiometry of the synthesized compounds CsPbBr2Cl and CsPbBr2.7I0.3.

摘要 提出了一种利用 TXRF 测定推定成分 CsPbBr2Cl 和 CsPbBr2I 的包晶纳米复合材料成分的方法。样品制备包括用二甲基甲酰胺 (DMFA) 处理疏水性样品,然后用水稀释得到的溶液。使用铜溶液作为内标时,TXRF 元素测定结果的重现性不超过 0.05。在 DMFA 中处理样品后,用 2% HNO3 稀释 Cs、Pb、Br 和 I,或用四甲基氢氧化铵(TMAH)稀释 Cs、Pb、Br 和 I,然后用 ICP-MS 测定溶液中的 Cs、Pb、Br 和 I,其结果证实了测定 Cs、Pb、Br 和 I 的有效性。结果表明,铅在 TMAH 溶液中不会形成不溶性的氯化物,也不会干扰测定。溴化物对氯化物测定的影响以 10-3 的电位系数为特征。所获得的结果有助于确定合成化合物 CsPbBr2Cl 和 CsPbBr2.7I0.3 的化学计量学。
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引用次数: 0
Development of ICP-AES Method for Analysis of Iron Ore Raw Materials 开发用于分析铁矿石原料的 ICP-AES 方法
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523140042
I. I. Chernikova, A. A. Potokina, O. V. Farafonova, T. N. Ermolaeva

Abstract

A method for the determination of Fetot, SiO2, P, V2O5, TiO2, Cr2O3, Ni, Cu, and Zn in iron ore raw materials (i.e., pellets, iron ore agglomerate, aspiration dust and slag component of scrap) by the method of atomic emission spectrometry with inductively coupled plasma (ICP-AES) has been developed using microwave sample preparation in analytical autoclaves. The composition of the acid mixture for the complete dissolution of the sample component was proposed, and the parameters of microwave decomposition, excluding the depressurization of the autoclave and the loss of sample elements which form volatile compounds, were selected. The developed method of microwave sample preparation in closed autoclaves made it possible to decompose iron ore samples using the minimum amount of acid (17 cm3) in 45 min. Conditions for the determination of normalized elements in iron ore samples by the ICP-AES method after microwave sample preparation were determined: the operating parameters of the spectrometer were optimized, the analytical lines of each determined element free from spectral overlaps were selected, and the efficiency of using cadmium as an internal standard was experimentally proved. The equations for calibration dependences and the ranges of determinable contents are presented. When using cadmium as an internal standard in the analysis of iron ore, a decrease in the value of the standard deviation from 0.17 to 0.04 is observed when determining Cr2O3; from 0.02 to 0.004 when determining Fe; from 0.03 to 0.002 when determining SiO2; from 0.015 to 0.008 when determining TiO2; and from 0.17 to 0.02 when determining V2O5. The correctness of the determination of the standardized elements by the developed method is evaluated using certified reference samples (CRS) similar in composition to the analyzed material. The results of determining the standardized elements according to the developed methodology were compared with the data obtained using GOST-approved methods of analysis and then checked in accordance with the recommendations of RMG 76-2014. The developed ICP-AES technique is characterized by a wider linear range of the determined concentrations than that in GOST-approved techniques, thus providing determination of the components in iron ore raw materials that could not be controlled before.

摘要 利用电感耦合等离子体原子发射光谱法(ICP-AES),在分析高压釜中进行微波样品制备,开发了一种测定铁矿石原料(即球团矿、铁矿团块、吸尘和废渣中的矿渣成分)中Fetot、SiO2、P、V2O5、TiO2、Cr2O3、Ni、Cu和Zn的方法。提出了使样品成分完全溶解的酸混合物成分,并选择了微波分解参数,其中不包括高压釜减压和形成挥发性化合物的样品元素损失。所开发的在封闭高压釜中进行微波样品制备的方法可以在 45 分钟内用最少的酸(17 立方厘米)分解铁矿石样品。确定了微波样品制备后采用 ICP-AES 法测定铁矿石样品中归一化元素的条件:优化了光谱仪的运行参数,选择了每种测定元素的分析线,避免了光谱重叠,并通过实验证明了使用镉作为内标物的效率。文中给出了校准相关方程和可确定的含量范围。在分析铁矿石时使用镉作为内标,测定 Cr2O3 时,标准偏差值从 0.17 降至 0.04;测定 Fe 时,标准偏差值从 0.02 降至 0.004;测定 SiO2 时,标准偏差值从 0.03 降至 0.002;测定 TiO2 时,标准偏差值从 0.015 降至 0.008;测定 V2O5 时,标准偏差值从 0.17 降至 0.02。使用与被分析材料成分相似的有证标准样品 (CRS) 对所开发方法测定标准元素的正确性进行了评估。根据开发的方法测定标准元素的结果与使用 GOST 批准的分析方法获得的数据进行了比较,然后根据 RMG 76-2014 的建议进行了检查。与 GOST 批准的技术相比,所开发的 ICP-AES 技术的特点是测定浓度的线性范围更广,因此可以测定以前无法控制的铁矿石原料中的成分。
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引用次数: 0
Determination of Methylphosphonic Acid and Alkyl Methylphosphonic Acid Esters in Soils by Liquid Chromatography–High-Resolution Mass Spectrometry 利用液相色谱-高分辨质谱法测定土壤中的甲基膦酸和甲基膦酸烷基酯
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523140157
M. F. Vokuev, A. V. Braun, T. M. Baygildiev, I. V. Rybalchenko, I. A. Rodin

Abstract

A method has been optimized for simultaneous extraction of ethyl methylphosphonic acid ester (EMPA), isopropyl methylphosphonic acid ester (IPMPA), isobutyl methylphosphonic acid ester (IBMPA), pinacolyl methylphosphonic acid ester (PMPA), and methylphosphonic acid (MPA), which are highly polar products of nerve agent hydrolysis, from soil with their further determination by high-performance liquid chromatography–high-resolution tandem mass spectrometry (HPLC–HRMS/MS). The ions observed in the fragmentation mass spectra of deprotonated EMPA, IPMPA, IBMPA, PMPA, and MPA molecules and their deuterated analogs (d3-EMPA, d3-IPMPA, d3-IBMPA, d3-PMPA, and d3-MPA), as well as possible structural formulas of the fragment ions, are presented. Liquid extraction with deionized water followed by concentration by evaporation was used to prepare soil samples for analysis. The components were separated using reverse-phase chromatography. The time required for the sample preparation and analysis of the soil samples was no more than 1 h. The detection limits in soil were 0.05 ng/g for EMPA and IPMPA, 0.02 ng/g for IBMPA and PMPA, and 1 ng/g for MPA.

摘要 优化了一种同时萃取乙基甲基膦酸酯(EMPA)、异丙基甲基膦酸酯(IPMPA)、异丁基甲基膦酸酯(IBMPA)、频哪醇甲基膦酸酯(PMPA)和甲基膦酸(MPA)的方法、通过高效液相色谱-高分辨串联质谱法(HPLC-HRMS/MS)进一步测定土壤中神经毒剂水解的高极性产物--异丁基甲基膦酸酯(IMPA)、频哪醇甲基膦酸酯(PMPA)和甲基膦酸(MPA)。介绍了在去质子化的 EMPA、IPMPA、IBMPA、PMPA 和 MPA 分子及其氚代类似物(d3-EMPA、d3-IPMPA、d3-IBMPA、d3-PMPA 和 d3-MPA)的碎片质谱中观察到的离子,以及碎片离子的可能结构式。使用去离子水进行液体萃取,然后通过蒸发浓缩来制备用于分析的土壤样本。采用反相色谱法分离各成分。土壤样品的制备和分析时间不超过 1 小时。EMPA 和 IPMPA 的检测限为 0.05 纳克/克,IBMPA 和 PMPA 为 0.02 纳克/克,MPA 为 1 纳克/克。
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引用次数: 0
Determining the Total Content of Similar Substances Using Integrated Indices or Multivariate Calibrations at a High Intragroup Selectivity of Signals 利用综合指数或多元校准在高组内信号选择性条件下确定类似物质的总含量
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523140145
V. I. Vershinin, A. E. Abramova

Abstract

The total content cΣ of similar organic compounds is conventionally determined without their separation by measuring their generalized spectral signals at one or several analytical wavelengths. The possibility of the correct cΣ estimation with the strongly pronounced intragroup selectivity of signals has not been previously tested. To verify this group analysis option, model hexane solutions of the known composition containing mono-, bi-, and tricyclic arenes at cΣ ~ 10–4 mol/dm3 simultaneously have been analyzed. At a fixed wavelength, the molar absorptivities of arenes with different numbers of rings differ by two to three orders of magnitude. Two options of group analysis have been compared: (i) measuring the generalized signal of arenes at 260 nm with the subsequent calculation of the result using the univariate calibration in terms of naphthalene or anthracene and (ii) measuring the generalized signals at m wavelengths in the spectral range of 250–290 nm with the subsequent calculation of the result using the inverted multivariate calibration. The first method (the calculation of the total index) has led to large systematic errors, sometimes over 100% in the absolute value, which do not decrease upon variation in the wavelength and nature of a standard substance. The second method has ensured more correct results, and already at m = 11, the errors of group analysis have been no more than 10%. Thus, at the strongly pronounced intragroup selectivity of the signals, the group analysis can and should be carried out using inverted multivariate calibrations. It has been established that the errors of cΣ estimation sharply grow if a sample contains components of a desired group that were not taken into account when constructing the inverted calibration.

摘要 类似有机化合物的总含量 cΣ 通常是通过测量它们在一个或几个分析波长上的通用光谱信号,在不分离它们的情况下确定的。在组内信号选择性非常明显的情况下,正确估算 cΣ 的可能性尚未得到验证。为了验证这种组分析选择,我们同时分析了已知成分的正己烷模型溶液,其中含有 cΣ ~ 10-4 mol/dm3 的单环、双环和三环烷烃。在固定波长下,不同环数的烷烃的摩尔吸收率相差两到三个数量级。我们对两种分组分析方法进行了比较:(i) 在 260 纳米波长处测量烷烃的广义信号,然后使用萘或蒽的单变量校准法计算结果;(ii) 在 250-290 纳米波长的光谱范围内的 m 个波长处测量广义信号,然后使用倒置多变量校准法计算结果。第一种方法(计算总指数)会导致较大的系统误差,有时绝对值会超过 100%,而且这种误差不会随着波长和标准物质性质的变化而减小。第二种方法确保了更正确的结果,在 m = 11 时,分组分析的误差已经不超过 10%。因此,在信号的组内选择性非常明显的情况下,组分析可以而且应该使用倒置多元定标法进行。已经证实,如果样本中含有在构建反向定标时未考虑在内的所需组别成分,cΣ 估计的误差会急剧增大。
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引用次数: 0
Study of Carbon Dioxide Corrosion Products by X-Ray Diffraction 通过 X 射线衍射研究二氧化碳腐蚀产物
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s002016852315013x
R. K. Vagapov, O. G. Mikhalkina

Abstract

Internal carbon dioxide corrosion is one of the most common types of corrosion in gas field development. The results of studying the composition of carbon dioxide corrosion products by X-ray diffraction are presented. FeCO3 is the main product resulting from dissolution of steel upon carbon dioxide corrosion. Siderite is characterized by the phenomenon of isomorphism in the crystal structure (a change in the chemical composition of the phase at the same crystal structure). Here, some iron ions in FeCO3 can be replaced by manganese, calcium, and magnesium ions. It is found out that the phases of the formed precipitates with a nonstoichiometric composition (CaxMgyMnzFe)CO3 have poor crystallinity. This is associated with the presence of defects in the crystal structure. They will exhibit poorer protective properties when compared to stoichiometric FeCO3, the film of which is packed, uniformly distributed, and tightly adheres to the steel surface. An analysis of the diffraction patterns evidences good crystallinity of FeCO3, the shape of the particles of which tends to a regular hexagonal habitus. The results obtained can be used in studying the resistance of corrosion products formed on the internal surfaces of gas production equipment under aggressive conditions in the presence of CO2 in produced and transported hydrocarbons.

摘要内部二氧化碳腐蚀是气田开发中最常见的腐蚀类型之一。本文介绍了通过 X 射线衍射研究二氧化碳腐蚀产物组成的结果。FeCO3是二氧化碳腐蚀时钢铁溶解产生的主要产物。菱铁矿的特点是晶体结构的同构现象(同一晶体结构中相的化学成分发生变化)。在这里,FeCO3 中的一些铁离子可以被锰、钙和镁离子取代。研究发现,所形成的沉淀物中的非化学成分 (CaxMgyMnzFe)CO3 相结晶度较差。这与晶体结构中存在缺陷有关。与化学合成的 FeCO3 相比,它们的保护性能更差,因为后者的薄膜排列整齐、分布均匀并紧紧地附着在钢表面。对衍射图样的分析表明,FeCO3 具有良好的结晶性,其颗粒形状趋向于规则的六角形。所获得的结果可用于研究天然气生产设备内表面在生产和运输碳氢化合物中存在 CO2 的侵蚀条件下形成的腐蚀产物的抗腐蚀性。
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引用次数: 0
Electroanalytical Properties of Unmodified and Modified Solid-Contact Potentiometric β-Lactam Sensors in Aqueous and Biological Media 水介质和生物介质中未改性和改性固体接触式电位计 β-内酰胺传感器的电分析特性
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s002016852314008x
E. G. Kulapina, R. K. Mursalov, O. I. Kulapina, V. D. Ankina

Abstract

A comparative study of the electroanalytical properties of solid-contact sensors (tubular, planar) in solutions of cefuroxime (Cefur), cefotaxime (Ceftx), cefixime (Cefix), and amoxicillin (Amox) is performed. Associates of tetraalkylammonium—tetradecylammonium (TDA) and dimethyldistearylammonium (DMDSA)—with complex compounds of silver(I) and β-lactam antibiotics [Ag(β-lac)2]TAA and modifiers such as ZnO, polyaniline, and polyaniline nanotubes are used as electrode-active components (EACs). The sensors under study based on [Ag(Cefur)2]TDA and [Ag(Amox)2]DMDSA are characterized by a short response time in solutions of cefotaxime, cefuroxime, cefixime, and amoxicillin: 20–25 and 12–17 s for tubular unmodified and modified, respectively; 20–25 and 10–15 s for planar unmodified and modified, respectively. The linear range of electrode functions in solutions of antibiotics is 1 × 10–4–1 × 10–2 mol/L; the limit of detection is 2.5 × 10–5–8.9 × 10–5 mol/L for unmodified, 5.6 × 10–6–7.5 × 10–5 mol/L for modified, and 4.2 × 10–5–7.2 × 10–5 mol/L for planar sensors. The potential drift is 8–12 mV/day for unmodified and 5–7 mV/day for modified planar sensors; the service life is 1.5–2 months. An advantage of planar sensors is their use in microassay detection, which is relevant in the analysis of biological media. Application of solid-contact sensors for determination of the antibiotics under study in model aqueous solutions, medicinal products, and oral fluid in the case of various infectious diseases is demonstrated.

摘要 对固体接触传感器(管状、平面)在头孢呋辛(Cefur)、头孢他啶(Ceftx)、头孢克肟(Cefix)和阿莫西林(Amox)溶液中的电分析特性进行了比较研究。四烷基铵--十四烷基铵(TDA)和二甲基双十八烷基铵(DMDSA)--与银(I)和β-内酰胺类抗生素[Ag(β-lac)2]TAA的复合物以及改性剂(如氧化锌、聚苯胺和聚苯胺纳米管)的结合体被用作电极活性成分(EAC)。所研究的基于[Ag(Cefur)2]TDA 和[Ag(Amox)2]DMDSA 的传感器在头孢他啶、头孢呋辛、头孢克肟和阿莫西林溶液中的响应时间很短:管状未修饰和修饰的响应时间分别为 20-25 秒和 12-17 秒;平面未修饰和修饰的响应时间分别为 20-25 秒和 10-15 秒。在抗生素溶液中,电极功能的线性范围为 1 × 10-4-1 × 10-2 mol/L;非改性传感器的检测限为 2.5 × 10-5-8.9 × 10-5 mol/L,改性传感器的检测限为 5.6 × 10-6-7.5 × 10-5 mol/L,平面传感器的检测限为 4.2 × 10-5-7.2 × 10-5 mol/L。未改良平面传感器的电位漂移为 8-12 mV/天,改良平面传感器的电位漂移为 5-7 mV/天;使用寿命为 1.5-2 个月。平面传感器的一个优点是可用于微量检测,这与生物介质分析有关。我们展示了固体接触式传感器在各种传染病的模型水溶液、医药产品和口服液中用于测定抗生素的应用。
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引用次数: 0
Electroplastic Effect in Titanium Alloys Under Tension 钛合金在拉伸状态下的电塑性效应
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523150050
O. E. Korolkov, M. A. Pakhomov, V. V. Stolyarov

Abstract

The electroplastic effect (EPE) is a phenomenon which consists in a decrease in the strain resistance and enhancement of the plasticity of metals under the effect of the electric current of a sufficiently high density [1]. This study aims to compare the deformation behavior of single-phase commercially pure titanium Grade 4 and two-phase VT6 alloy under tension and external heating with the introduction of a pulsed current. Current of various pulse ratios and densities is supplied to the grips of the tensile testing machine from a pulse generator. To estimate the relative contribution of the electroplastic effect during passage of current to the reduction of flow stresses, the materials are also exposed to external heating. The microstructure of the samples in the sample head and in the vicinity of the fracture region in the longitudinal section is studied using optical microscopy. The electroplastic effect in the studied materials is manifested on the tensile curve through individual jumps in the downward flow stress at a high pulse ratio, whereas at a low current pulse ratio a decrease in the flow stress and strain hardening and increase in the plasticity are observed. It is shown that the tension of the sample under the effect of current results in a greater decrease in the flow stresses than that observed under external heating at the same temperature for both materials. This confirms the athermal nature of the pulsed current effect. The critical density of the high pulse ratio current (q = 5000) capable of providing manifestation of the electroplastic effect is two times lower for the VT6 alloy than for the pure titanium Grade 4. Under the same pulsed current modes, the flow stresses for VT6 decrease more than for Grade 4. The pulsed current of high pulse ratio caused an anomalous hardening effect in the VT6 alloy, but the physical nature of this effect requires an additional study. The pulsed current modes used in the study did not lead to any structural changes noticeable under optical magnification in the samples under tension, except for the disappearance of twins and separation of the impurity particles in Grade 4 and spheroidization of grains in VT6.

摘要电塑性效应(EPE)是指在足够高密度的电流作用下,金属的抗应变性降低,塑性增强的现象[1]。本研究旨在比较单相 4 级商业纯钛和双相 VT6 合金在引入脉冲电流的拉伸和外部加热条件下的变形行为。脉冲发生器向拉伸试验机的夹具提供不同脉冲比率和密度的电流。为了估算电流通过时的电塑性效应对流动应力降低的相对贡献,还将材料置于外部加热条件下。使用光学显微镜研究了样品头部和纵切面断裂区域附近样品的微观结构。所研究材料的电塑性效应在拉伸曲线上表现为高脉冲比时向下流动应力的单独跳跃,而在低电流脉冲比时,流动应力和应变硬化下降,塑性增加。结果表明,对于两种材料,在相同温度下,样品在电流作用下的拉伸导致的流动应力下降幅度大于外部加热下的流动应力下降幅度。这证实了脉冲电流效应的非热性质。对 VT6 合金而言,能够产生电塑性效应的高脉冲比电流临界密度(q = 5000)比纯钛 4 级低两倍。在相同的脉冲电流模式下,VT6 的流动应力比 4 级合金的流动应力降低得更多。高脉冲比的脉冲电流在 VT6 合金中产生了异常硬化效应,但这种效应的物理本质还需要进一步研究。除了 4 级合金中孪晶消失、杂质颗粒分离以及 VT6 中晶粒球化之外,研究中使用的脉冲电流模式并未导致拉伸下的样品在光学放大镜下发生任何明显的结构变化。
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引用次数: 0
Ionometric Determination of Chlorine and Fluorine in Oil- and Gas-Bearing Wastewater 含油气废水中氯和氟的离子测定法
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523140108
I. V. Muravyeva, G. I. Bebeshko

Abstract—

Production and processing of oil and gas are associated with the formation of a huge volume of wastewater of complex composition disposed in different ways after thorough treatment. Environmental control of the composition and degree of purification of oil- and gas-bearing wastewater requires using effective methods for determining various pollutants, including chloride and fluoride. The object of the study was a sample of wastewater from the largest gas field Mustakillikning 25 yilligi in the Surkhandarya region of the Republic of Uzbekistan. It was shown that the sample was salty (dry residue was 34.1–31.7 g/dm3) and had a neutral reaction. The method of atomic emission analysis of water revealed high concentrations of potassium, sodium, and sulfur, a significant amount of calcium and magnesium, and a significantly smaller amount of a number of other elements contained in water. Study of various methods of sample preparation for ionometric measurements of chloride ion shows that a significant proportion of chlorine is bound with organic components of water. It is shown that boiling (~100°C) or fusing at 800–850°C with NaOH eliminates the interfering effect of accompanying components (sulfur, iodine, and organic matter) on the chloride determination. The results obtained provide quantitative determination of the total content of chlorine in water both in the form of a free chloride ion and in a bound state, probably in the composition of organochlorine compounds. The presence of fluorine in the organic part of the sample has not been revealed. The possibility of using a single sample preparation (boiling or fusing) for the determination of both chloride and fluoride ions has been shown. The interfering effect of the accompanying elements upon fluorine determination is masked by a buffer solution regulating the total ionic strength. The developed procedures are easy to use, selective, and cost-effective. The trueness and precision of the developed techniques have been evaluated and proved using a method of varying the sample volume.

摘要--石油和天然气的生产和加工过程中会产生大量成分复杂的废水,这些废水经过彻底处理后会以不同的方式排放。要对含油和含气废水的成分和净化程度进行环境控制,就必须采用有效的方法来测定各种污染物,包括氯化物和氟化物。研究对象是乌兹别克斯坦共和国苏尔汉河州最大的天然气田 Mustakillikning 25 yilligi 的废水样本。结果表明,样品含盐(干残渣为 34.1-31.7 克/立方米),呈中性反应。水的原子发射分析方法显示,水中含有高浓度的钾、钠和硫,大量的钙和镁,以及明显较少的其他一些元素。对离子测量氯离子的各种样品制备方法的研究表明,相当一部分氯与水中的有机成分结合在一起。研究表明,用 NaOH 煮沸(约 100°C)或在 800-850°C 温度下熔融,可消除伴随成分(硫、碘和有机物)对氯测定的干扰作用。所获得的结果可以定量测定水中氯的总含量,既可以自由氯离子的形式,也可以结合态的形式,很可能是有机氯化合物的成分。样品的有机部分中是否含有氟尚未揭示。已经证明了使用单一样品制备方法(煮沸或熔融)测定氯离子和氟离子的可能性。通过调节总离子强度的缓冲溶液,可以掩盖伴随元素对氟测定的干扰作用。所开发的程序易于使用,选择性强,成本效益高。使用改变样品量的方法对所开发技术的真实性和精确性进行了评估和证明。
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引用次数: 0
Flow-Injection Amperometric Determination of Adrenalin, Melatonin, and Cortisol on an Electrode Modified with a Gold–Palladium Binary System and a Nafion Film 用金钯二元体系和纳菲离子膜修饰的电极上的肾上腺素、褪黑素和皮质醇的流动注射安培测定法
IF 0.8 4区 材料科学 Q3 Materials Science Pub Date : 2024-03-20 DOI: 10.1134/s0020168523140121
L. G. Shaidarova, I. A. Chelnokova, Yu. A. Leksina, D. Yu. Khairullina, H. C. Budnikov

Abstract

The control of the precise concentration of steroid hormones and their synthetic analogs in biomedical objects is a relevant analytical task. A method for selective and highly sensitive simultaneous amperometric determination of adrenaline, melatonin, and cortisol with the use of a two-detector flow-injection system is developed. Screen-printed carbon electrodes (SPE) with one or two working electrodes modified with a gold–palladium binary system that exhibits catalytic activity upon electrooxidation of the organic compounds under consideration are used as detectors. The high sensitivity of determination is attributed to the catalytic properties of the metal modifier: the transition from the metal to the binary system leads to an increase in the catalytic oxidation current of hormones. The selectivity of determination of adrenaline in the presence of melatonin and cortisol is provided by the difference in the oxidation potentials of the hormones on the proposed electrode. For selective determination of melatonin and cortisol, the surface of the modified working electrode is coated with a Nafion film. The difference of potentials of the peaks of oxidation of adrenaline, melatonin, and cortisol on such an electrode is 300 mV. The proposed method is tested in the analysis of urine samples. The flow-injection scheme is supplemented with a dialyzer and a chromatographic minicolumn to eliminate the interfering effect of electrophilic compounds. The linear bilogarithmic dependence of the analytical signal on the concentration of adrenaline, melatonin, and cortisol is observed in the ranges of 5.0 × 10–10–5.0 × 10–3, 5.0 × 10–11–5.0 × 10–3, and 5.0 × 10–12–5.0 × 10–3 mol/L, respectively. Amperometric determination of the hormones in the flow-injection system leads to an increase in the productivity of the analysis and a decrease in the consumption of the sample and makes it possible to automate the process.

摘要 控制生物医学对象中类固醇激素及其合成类似物的精确浓度是一项相关的分析任务。本研究开发了一种利用双检测器流动注射系统同时测定肾上腺素、褪黑素和皮质醇的选择性高灵敏度安培法。检测器采用丝网印刷碳电极(SPE),该电极带有一个或两个用金钯二元体系修饰的工作电极,金钯二元体系在有机化合物电氧化时具有催化活性。测定的高灵敏度归功于金属改性剂的催化特性:从金属过渡到二元体系会导致激素的催化氧化电流增加。在有褪黑激素和皮质醇存在的情况下测定肾上腺素的选择性是由激素在拟议电极上的氧化电位差决定的。为了选择性地测定褪黑激素和皮质醇,在改良工作电极的表面涂上了一层 Nafion 膜。在这种电极上,肾上腺素、褪黑激素和皮质醇氧化峰的电位差为 300 mV。所提议的方法在尿样分析中进行了测试。流动注射方案辅以透析器和色谱小柱,以消除亲电化合物的干扰作用。在 5.0 × 10-10-5.0 × 10-3、5.0 × 10-11-5.0 × 10-3 和 5.0 × 10-12-5.0 × 10-3 mol/L 的范围内,分析信号与肾上腺素、褪黑素和皮质醇的浓度呈线性双对数依赖关系。在流动注射系统中对激素进行安培测定可提高分析效率,减少样品消耗,并使分析过程自动化成为可能。
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引用次数: 0
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Inorganic Materials
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