X射线反散射法测量塑料薄膜厚度

为实现快速、无损、精确的塑料薄膜厚度分析,讨论了XRF方法在塑料薄膜厚度测量中的应用,采用源初级射线散射法对塑料薄膜厚度进行相对测量。结果表明,厚度在10～800μm时,反散射X射线荧光强度与塑料薄膜厚度线性关系良好。对仪器标定后进行200 s快速测量,测量的厚度绝对误差<3μm(10～135μm),相对误差<4%(36～576μm),有较高的测量精度。XRF方法可用于塑料薄膜厚度的测量,该法对塑料工业的生产有现场指导的意义。     

能量色散X射线荧光光谱法现场测定钾盐钻井泥浆中的钾、溴、锶

建立了适用于野外钾盐钻探现场快速分析泥浆清液K,Br,Sr元素的能量色散X射线荧光光谱(EDXRF)方法,并实际应用于江陵凹陷野外钾盐科探井钻探过程现场。方法的精密度RSD(n=10)优于1.28%,校准曲线相关系数均大于0.9982,加标回收率为90.4%~101.0%,基本符合允许限的要求。对深度200~800 m区间内以设定间隔采集的15个泥浆样品的测量结果与实验室ICP-AES结果基本一致。方法可用于钾盐钻探现场泥浆中K,Br,Sr等指示元素的快速监测,为钻井决策提供数据支持。     

XRF在稀土分析中的应用与进展

X射线荧光光谱分析技术（XRF）是元素分析的有效工具,其快速、无损、多元素同时测定的特性能满足稀土元素的分析需求,在地质、冶金等多个领域中发挥着十分重要的作用。21世纪以来,稀土产业以及二次资源再利用的发展使得XRF分析方法的同步研发得到重视。本文对近年X射线荧光光谱技术的发展,样品制备方法的完善,稀土分析方法的优化及其在组分、微区与形态的分析中的应用现状进行概述,旨在为XRF技术在稀土分析方面的发展及推广提供参考思路。     

XRF方法在铜镍尾矿分析中的应用

介绍了XRF方法在铜镍尾矿分析中的基本原理,讨论了湿度、压样力度、基体效应对测量结果的影响,建立了基体效应校正模型。对某矿区的铜镍尾矿样品进行了分析。结果表明,该法精密度好,测定Cu的相对标准偏差为1.215%,N i为1.768%,可实现铜镍尾矿中Cu、N i元素含量的准确、无损、快速分析。     

铀矿样FPXRF分析中Th、Sr的影响与校正

探讨了Th、Sr元素与U伴生的地质学依据以及伴生元素的存在对U含量的FPXRF分析的干扰机理:铀样品中Th、Sr元素的影响主要表现为FPXRF仪器谱上ThLα和SrKα特征X射线对ULα特征X射线的干扰。结果表明,采用U、Th、Sr多元回归模型能有效地校正谱线重叠干扰,应用FPXRF分析铀矿样品中铀含量与推荐值相对误差控制在一定范围内,基本满足野外生产要求。     

应用手持式XRF分析仪快速测定白铜中的Cu、Ni、Co含量

采用国产手持式XRF分析仪快速分析了白铜合金主元素的含量,探讨了白铜合金基体效应对测量结果的影响,采用经验系数法中多元回归分析建立数学模型,较好地校正基体效应,分析白铜合金中铜、镍、钴的平均相对误差分别为0.39%、1.83%、1.59%。     

X射线荧光光谱熔融法测定锶永磁铁氧体中各组分含量

本文使用自制标准样品,采用混合熔剂熔融样品,用X射线荧光光谱法(XRF)测定锶永磁铁氧体半成品中Fe,Sr,Si等元素的含量.熔融制样有效地消除了矿物效应,并降低了基体效应的影响.实验结果表明,本法准确度高,重现性好,平行测定11次相对标准偏差(RSD)可达到0.1%.该方法用于实际样品分析,其结果与传统化学分析方法结...     

古人类骨骼中微量元素的分析及其与古代食谱的关联

采用等离子体质谱(ICP-Ms)法对三峡地区及长江下游地区出土的古墓中的人体骨骼中的微量元素Zn、Sr、Ba、Ca进行了分析，并与原子吸收光谱(AAS)对照，结果表明：ICP-MS是骨化学微量元素分析很好的方法，它相对FAAS，具有灵敏度高，检出限低，可快速进行多元素检测等优点，对溶液中元素的检出限可达到ng/L数量级，对元素的高含量和低含量都能进行准确测量。本实验以Zn、Sr、Ba、Ca为指示剂，根据其测量结果，还对上述两地区的古人类食谱进行了初步探讨。     

烟煤的拉曼光谱分析

为了分析煤的化学结构及性质,本文对大同塔山矿的煤样进行拉曼光谱测试。结果表明:在拉曼光谱一级模内存在两个明显的振动峰,分别为1 367cm~(-1)的D峰与1 593cm~(-1)的G峰,通过峰强度比(I_D/I_G=0.72)和半峰宽等信息可以确定出样品中芳香层排列有序化程度较高,侧链及杂原子含量较低。除此之外,在拉曼光谱中还发现方解石、白云石、金红石、锐钛矿、磁铁矿等无机矿物质的特征峰。对煤样进行X-射线衍射(XRD)和X-射线荧光光谱(XRF)测试,在XRD光谱中发现了金红石、锐钛矿及磁铁矿的衍射峰,在XRF测试中发现Al、Si、P、S、Ca、Ti、Fe、Sr等元素类型,证实了上述矿物质的存在。     

X射线荧光光谱法结合多元统计学对热敏纸的检验研究

为建立一种快速且无损检验热敏纸的科学有效的方法,利用能量色散型X射线荧光光谱(XRF)对38个不同商家,不同规格的热敏纸样品进行检验,首先根据每个样品所测量得到的元素的不同,将38个样品分成四大类,同时采用SPSS25.0软件中的系统聚类法对38个样品的元素数据进行聚类分析处理,结果分成了12小组,再结合SPSS25.0软件中的判别分析法对上述结果进行验证,实现了基于X射线荧光光谱结合聚类分析建立数学模型用于区分热敏纸种类的目的,该方法简单易行,可以为案件侦破提供线索、指明方向。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.