ICP-AES法测定锌阳极中的铝、镉、铁、铜、铅

通过分析高频功率、雾化压力、辅助气流量和泵速等试验条件，建立了ICP-AES法测定锌阳极中铝、镉、铁、铜、铅的方法。用该方法测定锌阳极中的铝、镉、铁、铜、铅，其RSD分别为0.17%、0.63%、2.7%、5.2%、2.5%，回收率分别为99.3%-101.2%，99.3%-100.3%、97.1%-102.2%、97.8%-102.9%。对锌阳极试样进行测定，该方法的测定结果与GB4951-85方法的测定结果基本一致。     

络合滴定法快速测定重晶石中的钡

采用沉淀、给 合滴定法，间接快速地测定了重晶石中钡的含量。对重晶石熔样方式、络合反应条件及共存干扰离子的消除方法进行了研究。该方法快速、准确，加收率为98.5%-100.7%，RSD小于2.48%。     

高效液相色谱串联质谱法测定血清中内美通

研究了高效液相色谱串联质谱联用测定人血清中内美通的方法。用乙醚提取血清中的内美通,米非斯酮做内标,电喷雾离子化,选择内美勇母、子离子对m/z309-m/z241;内标的母、子离对对m/z430-m/z372;串联质谱采用多反应扫描监测方法,定量测定人血清的内美通。该方法测定速度快,灵敏度高,选择性好。方法的标准曲线线性范围3.5-177μg/L（r^2=-0.999);检出限0.8μg/L;进行6次平行测定,日间RSD=2.3%-13.7%,RD=4.8%-3.0%;日内RSD=5.5%-14.8%,RE=3.1%-6.7%;回收率内美通是91.0%,内标米非斯酮是90.6%。4min完成一个样品测定。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定蒙药壮西六味散中15种元素

用微波消解和灰化法对蒙成药壮西六味散进行预处理,并用电感耦合等离子体原子发射光谱（ICP-AES）法同时测定了15种常量、微量及重金属元素的含量,进行了加标回收实验。结果显示,壮西六味散中Ca、P和K的含量较高,富含Mg、Na等营养元素,Pb、Cd等重金属含量均低于国家标准;灰化法和微波消解法两种预处理方法对测定结果基本一致。相对标准偏差（RSD）在1.6%-3.5%,加标回收率为95.5%-103%。方法简便准确、选择范围广、可高效快速准确测定壮西六味散中各元素含量。     

顶空气相色谱法测定秦龙苦素中的残留溶剂

采用顶空气相色谱法对秦龙苦素中残留的苯、甲苯、对二甲苯、正己烷等有害物质进行分析,并讨论了流速、柱温、平衡温度、平衡时间、抽样次数等因素对测定的影响。分析结果表明,该方法对上述4种有害物质的检测限范围为3-98 μg/L,测定结果的相对标准偏差为0.59%-2.64%,样品的回收率为97.2%-120.0%。方法简便、快速、灵敏、重现性好。     

高频燃烧红外吸收法测定氧化钴粉中的硫

采用高频红外吸收法测定了氧化钴粉中硫的含量,并对样品作测定前的预处理（物理处理）,在测定上选用复合型助熔剂,解决了高频感应炉中因顶吹氧气流的作用而导致的样品喷溅问题,并将镍作为辅助助熔剂应用于碳硫测定。该方法可准确测定硫含量为0.001%-0.1%的氧化钴粉中的硫,回收率为95.6%-104.8%。RSD为2.2%-4.9％。     

快速溶剂萃取-凝胶渗透色谱净化-气相色谱-质谱法测定土壤中11种半挥发性有机物

建立了快速溶剂萃取–凝胶渗透色谱净化–气相色谱–质谱法测定土壤中11种半挥发性有机物的分析方法。取样量为10.0 g,萃取溶剂为丙酮–二氯甲烷(体积比为3∶7),使用凝胶渗透色谱净化,气相色谱–质谱仪进行测定。11种半挥发性有机物的质量分数在0.1-5 mg/kg的范围内,相对响应因子的相对标准偏差小于15%,方法的检出限为0.04-0.06 mg/kg,当加标量为0.25、0.5、1 mg/kg时,测定结果的相对标准偏差分别为4.8%-13.7%、3.8%-9.5%、3.4%-10.8%(n=6),加标回收率为55%-110%。该方法适用于土壤中11种半挥发性有机物的检测。     

尿酸-铁氰化钾-鲁米诺化学发光测定亚硝酸盐

在酸性介质中，亚硝酸盐氧化亚铁氰化钾为铁氰化钾，利用尿酸-铁氰化钾-鲁米诺化学发光体系，建立了一种间接测定亚硝酸盐的新方法。讨论了酸度、反应物浓度、干扰离子等因素的影响。方法的检出限为0.05μg/L，对样品进行了平行测定（n=11），其相对标准偏差为1.8%-3.2%，线性范围为0.001-10ng/L。方法简便，易于操作，并具有较高的灵敏度和选择性。用于环境水样及食品中亚硝酸盐的测定，回收率为95.7%-105.8%，结果令人满意。     

原子荧光光谱法测定多金属矿标准样品中的砷、汞、铋

采取减少试样反应量及必要的分离手段，以原子荧光光谱法测定基体成分复杂、待测元素含量差异较大的多金属矿标标准样品中的砷、汞、铋，砷、汞、铋的检出限分别为0.2、0.01、1.3ng/mL，测定结果的相对标准偏差分别为1.88%-4.04%、2.1%-5.8%、1.1%-8.9%，线性相关系数均大于0.9970。标准样品的测定结果与推荐值基本吻合。该方法具有简单、快速、准确、精密度好等优点。     

离子色谱法测定电厂炉管垢样中的Cl-、SO42-

介绍离子色谱法测定电厂炉管垢样中腐蚀介质Cl^-和SO4^2-的方法，并对使用在线淋洗液发生器与以前配制淋洗液的方法进行了对比，提出了其在应用中的特性。垢样中Cl^-和SO4^2-的相对标准偏差分别为2.7%和2.3%，回收率分别为89.0%-97.8%和91.0%-98.9%。     

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%.     

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.     

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.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

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.