2,4,6—三（N,N—甲基,羧甲基氨基）—1,3,5—三嗪的合成

近代研究结果表明,不少含氮的杂环化合物对铜或其它金属有较好的缓蚀效果,同时也发现苯骈三唑(BTA)、巯基苯骈噻唑(MBT)虽然对铜有很好的缓蚀性,但在含氯或高浓度     

Tb^3＋,Eu^3＋r N,N‘,N“—1,3,5—三嗪—2,4,6—三—（N—羧甲基）—氨基…

合成了Ｔｂ＾３＋和Ｅｕ＾３＋的Ｎ，Ｎ’，Ｎ”－１，３，５－三嗪－２，４，５－三－（Ｎ－羧甲基）－氨基乙酸配合物，并用元素分析、热重－差热分析、紫外吸收光谱、红外光谱、荧光光谱、磷光光谱等进行了表征。结果表明，该配体能够敏化Ｔｂ＾３＋的荧光，而不能敏化Ｅｕ＾３＋的荧光，根据配体磷光光谱对发光机理进行了讨论。     

α（1,2,4—三唑—1—基）—α—苯甲酰基烯酮N,S;N,N;N,O和O,S…

以α（１，２，４三唑－１－基）－α－苯甲酰基烯酮二甲硫缩醛为反应中间体，与取代苯胺、邻苯二胺、乙二胺、乙醇胺和巯基乙醇反应，合成了２７个标题化合物，初步的生物活性测定表明，所合成的部分化合物具有抑菌及植物生长调节活性。     

N,N-Di-isopropyl-O,O-Di-p-methoxybenzylphosphoramidite——A New Phosphorylating Reagent

Thedibenzyldiisopropylphosphoramidite"',whichcouldbecleavedbyreduction(hydrogenolysis),isaveryusefulreagentforthephosphorylationofhydroxygroupespeciallyvicinalhydroxygroup.Itisusedveryoftenforthesynthesisofnucleotideandmyo-inositolpolyphosphates.However,itcannotbeusedforthephosphorylationofthecompoundshavinganolefinicgroupwhichwouldalsobereducedtoparaffininthereductioncleavingofthebenZylgroup.Now,WereportthesynthesisofanewphosphorylatingreagentN,N-di-isopropyl-O,O-di-P-methox1.Sincep-methox…     

偏振—导数—同步荧光法同时测定痕量芴,苊,蒽,北

本文采取偏振－导数－同步扫描联用技术同时测定痕量的芴、苊、恩和北多环芳烃。实验结果表明，多种荧光分析技术联用可以弥补单独应用其中一种或两种技术的不足，扬长避短，大大改善此类化合物的检测限。该方法同时测定上述四种组份，检测限依次为０．０８９、２．４、０．０４５、０．００９６ｎｇ／ｍＬ，相对标准偏差不大于５％。     

Fe—Ce—N—O,Fe—Y—N—S溶液的热力学研究

本文主要研究了在1570～1650℃范围内Fe-Ce-N-O、Fe-Y-N-S溶液的热力学性质,得到主要结果如下:(1)铈、钇增加氮的溶解度,氧轻微地增加氮的溶解度,硫轻微地减少氮的溶解度;(2)铈、钇、氧、硫与氮的相互作用系数与温度的关系。e_N~(Ce)=(-6230/T) 2.670,e_N~Y=(-6640/T) 2.986,e_N~O=(-3497/T) 1.650,e_N~S=264/T-0.128;(3)铈、钇脱氮产物为CeN、YN;(4)铈、钇脱氮常数与温度的关系:1gK_(CeN)-(-20960/T) 7.972,1gK_(YN)=(-20440/T) 7.863。     

N,N,N‘,N’—四异丁基—3—氧—戊二酰胺萃取铀钍的研究

放射性废液中含有大量的钢系和铜系元素,众多学者作了大量研究工作。如焦荣洲等［’］用三烷基氧磷（ＴＲＰＯ）、赵沪根等［’］用ＤＨＤＥＣＭＰ从放射性废液中分离啊系和湖系元素进行了系统研究。但所用革取剂均为含磷化合物,使用后被放射性污染的革取剂最终处置困难。为此面临寻求革取效率高、价廉,又便于最终处置的新型革取剂的任务。文章ｐｌ合成了二酚胺类化合物（Ｒ‘ＲＺＮＣＯ）。Ｒ３系列车取剂,它能有效地从放射性废液中革取分离回收钢系与调系元素。本文探讨了其中的Ｎ,Ｎ,Ｍ,ＮＷ四异了基一３一氧一戊二酚胺（简写为Ｌ…     

抑制型离子色谱快速测定I^—,SCN^—,S2O^2—3

本用抑制型离子色谱，薄壳强碱性阴离子交换树脂为分离柱，柱温为３０±１℃，在常规淋洗液ＮａＨＣＯ３－Ｎａ２ＣＯ３中加入对－硝基苯酚作为有机改进剂，测定了Ｉ＾－、ＳＣＮ＾－、Ｓ２Ｏ＾２－３离子。它们有良好的线性关系，三种离子浓度在５．０～３０．０ｍｇ／Ｌ范围内其相关系数分别为：ｒＩ＾－０．９９９４、ｒｓｃｎ＾－０．９９０６、ｒｓ２ｏ＾２－３０．９９８５，检测限分别为：Ｉ＾－０．１７ｍｇ／Ｌ、ＳＣＮ＾     

SYNTHESIS OF 1, 1-DIALKYLTHIO—1, 3, 5—HEXATRIENES WITH α—OXOKETENE DITHIOACETALS

α-Oxoketene dithioacetals 2 via, 1,2-nucleophilic addition by allyl magnesium bromide afforded corresponding alcohols (3).Treated with water and catalyzed by Lewis acid, the alcohols 3 were converted regiospecifically to the conjugated 1,1—dialkylthio—1,3,5 hexatrienes (4). Both the alcohol 8 and its methoxy methyl ether 9 were sensative to dilute sulfuric acid and cyclized under this condition to form the aryl methylthio ether (10).     

Direct determination of germanium in botanical samples by graphite furnace atomic absorption spectrometry with palladium-zirconium as chemical modifier

A method has been described for the direct determination of trace levels of germanium by graphite furnace atomic absorption spectrometry (GFAAS) using chemical matrix modification technique. The stabilization and the pyrolysis temperatures for germanium were investigated with various chemical modifiers including palladium, palladium–magnesium, palladium–strontium and palladium–zirconium. The highest pyrolysis temperature and highest integrated absorbance were obtained using palladium–zirconium modifier, and the severe matrix interference from sulfate can be eliminated. The characteristic mass and absolute detection limit (3σ) of germanium were found to be 16 and 12 pg, respectively. The proposed method was applied to the determination of trace levels of germanium in botanical samples with a recovery range of 92–106%. The hydride generation atomic fluorescence spectrometric (HGAFS) method was employed to analyze the samples and the results agree well with those obtained by GFAAS. The contents of germanium in standard reference materials were determined and the results were in good agreement with the reference values.     

微型氢化物发生-原子吸收光谱法测定纺织品中的痕量砷和锑

采用三毛细管微型在线氢化发生技术和装置, 建立了氢化物发生-电热石英管原子吸收法测定纺织品中痕量As、 Sb的分析方法. 研究了共存离子对As、 Sb检测的干扰及消除方法. 结果表明: 该方法除Co、 Sn对As和Ni对Sb有干扰外, 其它干扰元素允许量都较大. 采用酒石酸和KI混合掩蔽剂可抑制Co、 Sn对As和Ni对 Sb的干扰. As和Sb的检出限分别为0.7和0.4 ng/L, 已用于测定纺织品中痕量As和Sb的分析.     

原子荧光光谱法测定镉锭中锡的含量

采用氢化物发生-原子荧光光谱法测定镉锭中锡含量,研究了基体镉对锡的干扰及消除方法,优化了氢化物的发生条件,建立了镉锭中锡含量的快速分析方法。实验证明,原子荧光光谱法对锡的检出限为0.08mg/kg,回收率为99.0%～104.0%,方法准确、可靠,用于日常样品分析,取得了很好的效果。     

碱式模式氢化物发生原子荧光法测定食用菌中痕量锗

研究了碱式模式氢化物发生原子荧光法测定痕量锗。考察了HG－AFS仪器参数及氢化物发生条件对锗荧光强度的影响以及常见共存元素的干扰。在选定的最佳工作条件下,测定了真菌中的痕量锗。方法检出限（3σ）为0.76μg/L,相对标准偏差(RSD)为0.81％,回收率为94.6％－101.3％。     

Atomic absorption spectrometric screening and gas chromatographic-mass spectrometric determination of organotin compounds in marine mussels: an application in samples from the Venetian Lagoon

A new analytical approach for the determination of organotin compounds (OTC) in mussel samples has been developed and evaluated. A preliminary step, performed by graphite furnace atomic absorption spectrometry (GFAAS) for the total tin determination may be followed by gas chromatographic-mass spectrometric (GC/ MS) speciation only for the characterization of those samples exhibiting total tin concentration higher than 30 ng/g wet weight (GFAAS limit of detection). The GFAAS method was optimized using Pd nitrate under reducing conditions as matrix modifier to minimize NaCl interferences. Organotins were derivatized with a Grignard reagent for GC/MS analysis (TBT limit of detection = 80 ng/g). An application of this strategy was performed on mussel samples collected from the Venetian Lagoon.     

氢化物发生–原子荧光光谱法同时测定锌锭中砷和锑

建立用氢化物发生–原子荧光光度计同时测定锌锭样品中砷和锑含量的方法。采用硝酸一次溶样,加入酒石酸防止锑水解。加入硫脲–抗坏血酸混合溶液作为还原剂和掩蔽剂,消除干扰元素的影响,对实验条件进行了优化。砷和锑的负高压分别为220,200 V,灯电流分别为80,60 mA,还原剂为1%硼氢化钾溶液(含0.5%KOH),载流为10%盐酸溶液,还原时间为30 min。测定砷的线性范围为0~80 ng/mL,相关系数r=0.999 8,检出限为0.35μg/L,测定结果的相对标准偏差为3.18%(n=11);测定锑的线性范围为0~80 ng/mL,相关系数r=0.999 6,检出限为0.42μg/L,测定结果的相对标准偏差为4.32%(n=11),砷和锑的加标回收率在97.46%~100.30%之间。用该方法对标准样品进行测定,测定结果与标准值相符。该方法基体干扰少,灵敏度高,适合于锌锭中砷和锑的日常测定。     

Electrochemical Hydride Generation:A Novel Sample Introduction Method for the Non-dispersive Atomic Fluorescence Spectrometry

Production of volatile covalent hydrides of environmentally important elements (As、Se、Bi、Ge、Sn、Sb and Pb) by reaction with sodium (potassium) tetrahydroborate (NaBH₄) in acidic media for determination by atomic absorption has been widely used in routine analysis. However, this technique has several disadvantages. NaBH₄ is a potential source of contamination, its aqueous solution is unstable. As an alternative to chemical hydride generation, hydride generation by electrochemical reduction (EcHG) has been reported in recent years by many authors^[1-3]. Compared with NaBH₄ hydride generation system, the EcHG with subsequent detection by atomic absorption spectrometry offers the high sensitivity, low detection limits, and the absence of interference from the transition metals. However, the hydrogen produced by EcHG reduced greatly, this led to the interference caused by hydride forming elements was serious due to the lack of free hydrogen (H·) radical in the quartz tube during the atomization. EcHG coupled with atomic fluorescence spectrometry system uses Ar-H2 mini-flame as an atomizer, in which the gaseous phase interference can be expected eliminated. In addition, non-dispersive atomic fluorescence spectrometry (NDAFS) system with a quite single structure, is a very sensitive and feasible method for the measurement of elements that form volatile hydrides. By combining with electrochemical hydride generation as a sample introduction technique, it is possible to develop a potential interface for chromatography or capillary electrophoresis in speciation analysis.     

Continuous flow hydride generation for the preconcentration and determination of arsenic and antimony by GFAAS

A method has been developed for the determination of arsenic and antimony at sub-ppb level using hydride preconcentration inside the graphite furnace. The influence of the quality of the graphite surface, of its modification with palladium coating and of the ways of introducing hydride into the furnace on the analytical signal is discussed. After optimization of system parameters, detection limits of 25 and 36 pg were obtained for arsenic and antimony. Characteristic masses (for arsenic and antimony, respectively) were 31 and 33 pg/0.0044 A·s for direct injection GFAAS and 69 and 57 pg/0.0044 A·s for hydride in situ preconcentration and atomization in the palladium coated graphite tube. Therefore the overall efficiency of the hydride generation and trapping was estimated to be 45 and 58% for arsenic and antimony, respectively.     

碱性体系氢化物发生-原子荧光光谱法测定矿物中的痕量硒

对碱性氢化物发生－原子荧光光谱法测定痕量硒的方法进行了探讨,研究了体系的最佳实验参数。与常规酸性 体系氢化物发生－原子荧光光谱法比较,本法能有效地消除大量铜、铁、钴、镍等过渡族元素的干扰,样品可不经分离直接进行测定。经过国家标样的分析验证,其测定值与推荐值吻合。方法的检出限为0.55ug/L,相对标准偏差为4.12％;原子加入回收率为99.8%.     

Non-dispersive atomic-fluorescence spectrometry of trace amounts of bismuth by introduction of its gaseous hydride into a premixed argon (entrained air)-hydrogen flame

A method has been developed for the determination of bismuth by generation of its gaseous hydride and introduction of the hydride into a premixed argon (entrained air)-hydrogen flame, the atomic-fluorescence lines from which are all detected by use of a non-dispersive system. The detection limit is 5 pg/ml, or 0.1 ng of bismuth, but the reagent blank found in a 20-ml sample volume was approximately 2 ng of bismuth. Analytical working curves obtained by measuring peak-heights and integrated peak-areas of the signals are linear over a range of about four orders of magnitude from the detection limit. Perchloric, phosphoric and sulphuric acids up to 2.0M concentration give no interference, but nitric acid gives slight depression of the signal. The presence of silver, gold, nickel, palladium, platinum, selenium and tellurium in 1000-fold ratio to bismuth causes pronounced depression of the signal, whereas mercury and tin slightly enhance the atomic-fluorescence signal. The method has been applied to the determination of bismuth in aluminium-base alloys and sulphide ores with use of the standard additions method. The results are in good agreement with those obtained by flame atomic-absorption spectrometry and optical emission spectrometry with an inductively coupled plasma.