磷酸加王水复溶-电感耦合等离子体质谱（ICP-MS）法测定土壤样品中的20种金属元素

先用磷酸溶解样品,后加入王水复溶,可同时测定锂、铍、钪、钒、铬、钴、镍、铜、锌、锗、钼、镉、钡、镧、铈、钨、铊、铅、钍和铀元素。研究了消解体系、ICP-MS的最佳测量模式和最佳工作状态,并以铑为内标校正仪器的漂移。通过选择高、中、低几个国家一级水系沉积物和土壤标准物质随同样品一起溶解建立标准曲线,消除消解、分取和定容时带来的不确定误差和基体干扰,选择8个土壤标准物质为实验样本。最终结果表明,方法准确度(Δlgc)小于0.1,精密度(RSD)小于8%,方法满足测定要求,适用于地质普通样品的多金属检测。     

封闭压力酸溶-盐酸提取-电感耦合等离子体原子发射光谱法(ICP-AES)测定页岩中的多种微量金属元素

采用高温、高压消解罐法前处理页岩矿石样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定了页岩标准物质中的多种微量元素的含量。实验过程中确定了最佳工作条件,选择了最佳分析谱线。实验结果表明,该方法线性相关系数良好r0.999 8,方法检出限低,精密度高,RSD小于3.0%,可同时测定页岩矿石中的多种金属元素,方法完全能满足岩石、土壤、沉积物中多种元素的检测需求。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定锰结壳中的多种金属元素

采用硝酸-盐酸-氢氟酸高压封闭消解样品,电感耦合等离子体光谱法测定锰结核GBW07296和富钴结壳GSMC-1标准物质中的18种常、微量元素。实验过程中确定了最佳工作条件,选择了最佳分析谱线。实验结果表明,该方法线性相关系数良好r>0.999 8,方法检出限低,精密度高,RSD小于2.0%(n=6),可同时测定锰结壳中的多种金属元素,方法完全能满足岩石、土壤、海洋沉积物中多个元素的检测需求。     

灵芝、枸杞等样品中微量锗的胶束增溶分光光度法测定

研究用离子缔合物胶束增溶分光光度法测定灵芝、枸杞、蘑菇、茶叶和大蒜中锗的含量,采用标准加入法考查了不同的消解方法对样品中锗的溶解情况,用高压罐密闭消解处理样品,锗的测定结果的相对标准偏差(n=4)小于4.3%,回收率为90%～105%.     

电感耦合等离子体质谱法同时测定地质样品中镉、锗、钴

建立电感耦合等离子体质谱法同时测定地质样品中镉、锗、钴含量的分析方法。样品用氢氟酸-硝酸混合溶液加热溶解,然后加热浓缩驱酸,再用硝酸溶液(1+1)复溶提取,在选定的仪器工作条件下进行测定。镉、锗、钴的含量分别在0.00~0.10,0.00~5.00,0.00~50.00 μg/g范围内与质谱峰强度呈良好的线性关系,相关系数均大于0.999,方法检出限分别为0.01,0.02,0.02 μg/g。用该方法对国家一级标准物质进行测定,测定值的相对误差均小于10%,测定结果的相对标准偏差为0.79%~8.45%(n=12)。该方法样品处理过程简便,检测效率高,适用于批量地质样品中镉、锗、钴的测定。     

高分辨电感耦合等离子体质谱法测定地质样品中的微量锗

应用高分辨电感耦合等离子体质谱法测定地质样品中的微量锗。研究了地质样品中不同酸消解方法、提取方法对测定锗的影响,以及在高分辨电感耦合等离子体质谱仪高、中、低分辨率模式下测定地质样品中锗的质谱行为。用氢氟酸-硝酸体系分解样品,硝酸提取,在中分辨率模式下进行测定。方法的检出限(3s)为10ng·g-1。方法用于10个国家标准物质中锗含量的测定,测定值与认定值相符,测定值的相对标准偏差(n=10)小于4.5%。     

碱熔-电感耦合等离子体原子发射光谱（ICP-AES）法测定锗精矿中锗的含量

针对锗精矿分析过程中样品难溶解、锗易损失以及滴定法测定流程复杂等难点,本文建立了碱熔-电感耦合等离子体原子发射光谱（ICP-AES）法测定锗精矿中锗含量的分析方法。考察了仪器的工作条件、不同的溶样方式、熔样温度和时间、介质酸度、共存元素对测定结果的影响,确定了最佳的实验条件：采用过氧化钠在700℃熔融10min,用硝酸浸取进行前处理;在电感耦合等离子体原子发射光谱仪上选择209.426nm作为分析谱线,仪器在200 nm处光谱的实际分辨率小于0.01 nm;在10%的硝酸介质中采用钠基体匹配的方式进行测定。在该实验条件下,实验结果表明方法中仪器的短期稳定性小于1.5%,工作曲线具有良好的线性相关性,相关系数为0.99993,方法的检出限是0.023μg/mL。同时,选择了两个锗精矿国家标准样品GSB 04-3358-2016（Ge 4.91%）和GSB 04-3361-2016（Ge23.57%）进行分析,分析结果与标值基本一致,无显著性差异;进行了精密度和回收率试验,相对标准偏差在0.42%~1.32%之间,回收率在98.1%~101.8%之间,该方法具有较好的精密度和稳定性,能够满足锗精矿中锗含量范围在1%~25%的快速准确测定。     

微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法同时测定土壤中主次元素

建立了微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法同时测定土壤中多种主次元素的分析方法。采用硝酸-氢氟酸-双氧水体系在微波消解仪中消解土壤样品,待消解完成后加入高氯酸驱赶氢氟酸,盐酸溶解盐类物质,将土壤中所有元素的矿物晶格破坏使待测溶液全部进入试液,采用ICP-AES法测定。通过筛选合适分析谱线和合理设置背景扣除位置提高样品分析中的精密度和准确度。选用国家土壤标准物质进行方法验证,绝大多数实验结果与标准值吻合,相对标准偏差(RSD)小于5%。方法具有同时测定土壤样品中多种元素、试剂用量少、操作简单等优点,表明方法适合大批量土壤中主次元素的快速检测。     

微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法同时测定土壤中主次元素

建立了微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法同时测定土壤中多种主次元素的分析方法。采用硝酸-氢氟酸-双氧水体系在微波消解仪中消解土壤样品,待消解完成后加入高氯酸驱赶氢氟酸,盐酸溶解盐类物质,将土壤中所有元素的矿物晶格破坏使待测溶液全部进入试液,采用ICP-AES法测定。通过筛选合适分析谱线和合理设置背景扣除位置提高样品分析中的精密度和准确度。选用国家土壤标准物质进行方法验证,绝大多数实验结果与标准值吻合,相对标准偏差(RSD)小于5%。方法具有同时测定土壤样品中多种元素、试剂用量少、操作简单等优点,表明方法适合大批量土壤中主次元素的快速检测。     

微波消解-电感耦合等离子体发射光谱法同时测定土壤中主次金属元素

建立微波消解-电感耦合等离子体发射光谱法同时测定土壤中多种主次元素的分析方法。采用硝酸-氢氟酸-双氧水体系在微波消解仪中消解土壤样品,待消解完成后加入高氯酸驱赶氢氟酸,盐酸溶解盐类物质,将土壤中所有元素的矿物晶格破坏使待测溶液全部进入试液,采用电感耦合等离子体发射光谱进行测定。通过筛选合适分析谱线和合理设置背景扣除位置提高样品分析中的精密度和准确度。选用国家土壤标准物质进行方法验证,绝大多数实验结果与标准值吻合,RSD小于5%。本方法具有同时测定土壤样品多种元素、试剂用量少、操作简单等优点,表明该方法适合大批量土壤中主次元素的快速检测。     

应用先进光谱技术研究无机离子的环境界面化学

发生在环境界面的吸附-解吸和氧化-还原等反应对于污染物在环境介质间传输、转化以及归趋起着重要的调控作用。传统的研究方法虽然可以在实验室模拟并进而描述污染物环境界面过程,但是不能揭示界面反应机制,限制了对污染物环境界面行为的认识。近二十年来,各种谱学技术(例如X射线吸收精细结构和傅里叶红外光谱等)应用于环境界面反应的研究,推动了这一领域研究的发展,特别是在分子水平研究污染物的环境界面过程。通过现代光/波谱技术原位分析,可以实时获取界面反应的定量与结构信息,从而更准确地判断反应机制,极大促进了对污染物在多介质环境界面迁移转化规律的认识。本文将在概述环境界面化学反应的基础上,针对无机离子在环境界面的反应过程,重点介绍几种关键光/波谱技术(X射线吸收精细结构光谱、傅里叶红外光谱、拉曼光谱、核磁共振谱和穆斯堡尔谱等)在环境界面化学研究中的应用,并展望其在环境界面过程研究中的应用前景。     

Transition Metal–(μ-Cl)–Aluminum Bonding in α-Olefin and Diene Chemistry

Olefin and diene transformations, catalyzed by organoaluminum-activated metal complexes, are widely used in synthetic organic chemistry and form the basis of major petrochemical processes. However, the role of M–(μ-Cl)–Al bonding, being proven for certain >C=C< functionalization reactions, remains unclear and debated for essentially more important industrial processes such as oligomerization and polymerization of α-olefins and conjugated dienes. Numerous publications indirectly point at the significance of M–(μ-Cl)–Al bonding in Ziegler–Natta and related transformations, but only a few studies contain experimental or at least theoretical evidence of the involvement of M–(μ-Cl)–Al species into catalytic cycles. In the present review, we have compiled data on the formation of M–(μ-Cl)–Al complexes (M = Ti, Zr, V, Cr, Ni), their molecular structure, and reactivity towards olefins and dienes. The possible role of similar complexes in the functionalization, oligomerization and polymerization of α-olefins and dienes is discussed in the present review through the prism of the further development of Ziegler–Natta processes and beyond.     

中文化学名词醇醛酮醚酯之由来

1932年民国教育部颁布的《化学命名原则》为中文化学名词确立了统一的标准,并对于"元素及化合物定名取字"提出"取字应以谐声为主,会意次之,不重象形"的定名总则.它确立的中文化学名词醇、醛、酮、醚、酯是意译名,这似乎与其音译为主的命名原则相悖.本文讨论了醇、醛、酮、醚、酯的各种历史译名,并分析了它们被《原则》采纳的原因.     

Bestimmung von Fe, Co, Cu, Zn, Se, Rb und Cs in NBS-Ochsenleber, Blutplasma und Erythrocyten durch INAA und AAS

Zusammenfassung Der Gehalt von Fe, Co, Cu, Zn, Se, Rb und Cs wurde in Blutplasma und in Erythrocyten von sechs Normalpersonen mittels der instrumentellen Neutronenaktivierungsanalyse und der flammenlosen Absorptionsspektrometrie (Cu) bestimmt. Zur Überprüfung der Richtigkeit wurde der NBS-Standard 1577, Ochsenleber, verwendet. Die erhaltenen Resultate für Elemente mit höheren Gehalten (Fe, Cu, Zn) liegen weitgehend im Bereich der bisher veröffentlichten Daten. Bei Elementen mit kleineren Gehalten (Co, Se, Rb, Cs) liegen unsere Werte in dem unteren Bereich oder darunter. Für diese Elemente wurden in Blutplasma und in Erythrocyten (hier bezogen auf Trockenmasse) die folgenden Mittelwerte ermittelt: Für Co 0,22 ±0,14 ng/ml, 0,59±0,23 ng/g, für Se 103±18 ng/ml, 401±29 ng/g, für Rb 167±36 ng/ml, 12,1±2,5 g/g und für Cs 0,88±0,18 ng/ml, 13,0±5,7 ng/g.

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Determination of Fe, Co, Cu, Zn, Se, Rb and Cs in NBS Bovine Liver, blood plasma and erythrocytes by INAA and AAS

Summary The content of the above elements has been determined in blood plasma and in erythrocytes of six normal persons by instrumental neutron activation analysis and flameless atomic absorption spectrometry (Cu). The over-all accuracy of these techniques was checked by using the NBS standard 1577, Bovine Liver. The results obtained for elements of higher content (Fe, Cu, Zn) are essentially in the range of other published data. However, our results for elements occurring with lower contents (Co, Se, Rb, Cs) are in agreement with the lowest values of the published data and in some cases they are even significantly below these. For these elements, the following contents have been determined in blood plasma and in erythrocytes (here related to dry weight): for Co 0.22±0.14 ng/ml and 0.59±0.23 ng/g, for Se 103±18 ng/ml and 401±29 ng/g, for Rb 167 ±36 ng/ml and 12.1±2.5 g/g and for Cs 0.88 ±0.18 ng/ml and 13.0±5.7 ng/g, respectively.

Diese Arbeit wurde durch die Deutsche Forschungsgemeinschaft gefördert.Dem Kernforschungszentrum danken wir für den Erlaß der Bestrahlungskosten.Herrn Dr. med. K. Spenger sind wir für die Mitwirkung bei der Blutentnahme und für wertvolle Diskussion dankbar.     

Attenuation of Scopolamine-Induced Amnesia via Cholinergic Modulation in Mice by Synthetic Curcumin Analogs

Alzheimer’s disease is an emerging health disorder associated with cognitive decline and memory loss. In this study, six curcumin analogs (1a–1f) were synthesized and screened for in vitro cholinesterase inhibitory potential. On the basis of promising results, they were further investigated for in vivo analysis using elevated plus maze (EPM), Y-maze, and novel object recognition (NOR) behavioral models. The binding mode of the synthesized compounds with the active sites of cholinesterases, and the involvement of the cholinergic system in brain hippocampus was determined. The synthesized curcumin analog 1d (p < 0.001, n = 6), and 1c (p < 0.01, n = 6) showed promising results by decreasing retention time in EPM, significantly increasing % SAP in Y-maze, while significantly (p < 0.001) enhancing the % discrimination index (DI) and the time exploring the novel objects in NORT mice behavioral models. A molecular docking study using MOE software was used for validation of the inhibition of cholinesterase(s). It has been indicated from the current research work that the synthesized curcumin analogs enhanced memory functions in mice models and could be used as valuable therapeutic molecules against neurodegenerative disorders. To determine their exact mechanism of action, further studies are suggested.     

Phosphorescence of aromatic molecules in complexes with crystalline β-cyclodextrin at room temperature

The rate constants for the quenching by oxygen of triplet states of aromatic molecules (naphthalenes-d₈ and-h₈, phenanthrene) forming inclusion complexes with crystalline β-cyclodextrin in water at 290 K are equal to 900–1300 L mol⁻¹s⁻¹. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1450–1453, August, 1997.     

Direct benzylic functionalization of pyridines:Palladium-catalyzed mono-α-arylation of α-(2-pyridinyl)acetates with heteroaryl halides

Herein,we report a Pd-catalyzed mono-a-arylation reaction for pyridine benzylic functionalization.This approach serves as an efficient alternative to synthesize di-heteroaryl acetates in good yields and selectivities.Moreover,the method is applicable to heteroa ryl substrate combinations,and exhibits great functional group tolerance.A streamlined protocol also enables the rapid synthesis of diheteroaryl ketones.The synthetic value was also demonstrated by scale-up experiments.     

Unveiling Antimicrobial and Antioxidant Compositional Differences between Dukkah and Za’atar via SPME-GCMS and HPLC-DAD

Interest in plant-based diets has been on the rise in recent years owing to the potential health benefits of their individual components and the notion that plant-based diets might reduce the incidence of several diseases. Egyptian dukkah and Syrian za’atar are two of the most historic and famous Middle Eastern herbal blends used for their anti-inflammatory, hypolipidemic, and antidiabetic effects. Headspace SPME-GCMS and HPLC-DAD were adopted for characterizing the aroma profile and phenolic compounds of both herbal blends, respectively. Further, vapor-phase minimum inhibitory concentration was employed for assessing each blend’s antibacterial potential, while their antioxidant potential was estimated via in vitro antioxidant assays. SPME headspace analysis indicated the abundance of ethers and monoterpene hydrocarbons, while HPLC revealed the presence of several phenolics including rosmarinic acid, ferulic acid, and rutin. Biological investigations affirmed that vapor-phase of the tested blends exhibited antibacterial activities against Gram-positive and Gram-negative pathogens, while the antioxidant potential of the blends was investigated and expressed as Trolox (125.15 ± 5.92 to 337.26 ± 13.84 μM T eq/mg) and EDTA (18.08 ± 1.62 to 51.69 41 ± 5.33 μM EDTA eq/mg) equivalent. The presented study offers the first insight into the chemical profile and biological activities of both dukkah and za’atar.     

DC discharge in an alternating magnetic field as excitation source in emission spectroscopy

Summary The experimental study of the behaviour of a dc discharge in an alternating magnetic field is described. The lower electrode (anode) is a horizontally located chamber electrode. The alternating magnetic field causes oscillations along the lower electrode axis so that the oscillating arc can equably heat the anode. The axial distribution of the spectral line intensities for lead, bismuth, mercury, cadmium, tin and antimony is investigated. The intensity distributions are studied for near-to-cathode and near-to-anode regions of the discharge. The detection limits obtained for pure conditions show that the effects of chamber electrodes and of double arc could be achieved by means of a relatively simple technique.

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Ein Gleichstrombogen im Wechselmagnetfeld als Anregungsquelle in der Emissionsspektrographie

Zusammenfassung Untersuchungen über das Verhalten eines Gleichstrombogens in einem Wechselmagnetfeld werden beschrieben. Die untere Elektrode (Anode) ist eine horizontale Kammerelektrode. Das Wechselmagnetfeld verursacht Bogenschwingungen entlang der Achse der unteren Elektrode und ermöglicht dadurch deren gleichmäßige Heizung. Die axiale Verteilung der Linienintensitäten von Blei, Bismut, Quecksilber, Cadmium, Zinn und Antimon wurde für beide Elektroden untersucht. Die berechneten Nachweisgrenzen zeigen, daß die Wirkung der Kammerelektrode und des Doppelbogens mit einfachen Mitteln erreicht werden kann.