GC-MS法测定焦化厂气溶胶中多环芳烃

利用气相色谱-质谱(GC-MS),电子轰击离子化(EI)法测定焦化厂气溶胶中多环芳烃的含量。超声波抽提气溶胶样品,用GC-MS的选择离子监测(SIM)方式测定EPA提出的优先监测的16种多环芳烃的含量。该法的检出限为0.167pg·m~(-3),PAHs的回收率为85.1％～110.5％,相对标准偏差为4.62％～19.4％。应用该法测定气溶胶中PAHs获得满意的结果。     

High yield synthesis and reactivity of a phosphinidene bridged dimolybdenum complex

Protonation of [Mo2Cp2(mu-H)(mu-PHR*)(CO)4] (Cp = eta5-C5H5, R* = 2,4,6-C6H2tBu3) with HBF4.OEt2 gives the hydridophosphinidene complex [Mo2Cp2(mu-H)(mu-PR*)(CO)4]BF4, which is easily deprotonated with H2O to give the known phosphinidene complex [Mo2Cp2(mu-PR*)(CO)4] in 95% yield. Reaction of the latter with I2 gives the unsaturated phosphinidene complex [Mo2Cp2I2(mu-PR*)(CO)2], which exhibits an intermetallic distance of 2.960(2) A. Irradiation of solutions of [Mo2Cp2(mu-PR*)(CO)4] with UV light gives a mixture of the triply bonded [Mo2Cp2(mu-PR*)(mu-CO)2] and the hydridophosphido derivative [Mo2Cp2(mu-H){mu-P(CH2CMe2)C6H2tBu2}(CO)4] as major species. The latter complex results from an intramolecular C-H bond cleavage from a tBu group and has been characterized by spectroscopy and an X-ray study. Irradiation in the presence of HCC(p-tol) results in the insertion of the alkyne into the Mo-P bond to give [Mo2Cp2{mu-eta1:eta2,kappa-C(p-tol)CHPR*}(CO)4] structurally characterized through an X-ray study.     

Setting up of recovery profiles: A tool to perform the compliance with recovery requirements for residue analysis

The use of the recovery term has presented some confusion in Analytical Chemistry. Recent IUPAC recommendations propose to distinguish between two terms: recovery or recovery factor, ℜ, and apparent recovery, ℜ*. Apparent recovery includes recovery factor and a new recovery term proposed in this paper, named calibration recovery, ℜ^C, which depends of the type of systematic error due to the matrix effect (constant and/or proportional) and is related to the applied calibration methodology. This paper highlights the dependence of the calibration recovery on the sample analyte concentration and, for extension, of the apparent recovery, defines the recovery profile, and makes evident the need to determine a “fit for purpose” analyte concentration interval to comply with a regulated recovery requirements. An approach to estimate the calibration recovery and its associated uncertainty in relation to the above-mentioned dependence is presented. The usefulness of the proposed methodology has been shown in the quantification of a pesticide by GC-ECD for assessing dermal exposure.     

新型光学活性α-氨基磷酸及其酯合成进展

α-氨基膦酸酯是一类很重要的天然氨基酸类似物，具有新颖的化学结构和多 种生理活性。综述了近年来光学活性α-氨基膦酸及酯的合成进展。     

Structure of Low Temperature Phase b-Ba_3Y(BO_3)_3 Crystal

1 INTRODUCTION Recently the series of compounds M3Ln(BO3)3 (M = Sr, Ba and Ln = LaLu, Sc, Y) with space group P63cm or -3R have been reported[1～5], and some of them exhibit interesting optical properties when doped with the active Cr3+ or Yb3+ ions as laser materials. For example, Yb3+-doped Sr3Y- (BO3)3 crystal is a promising laser material for both tunable and femtosecond laser applications[6～8]. The Ba3Y(BO3)3 crystal melts congruently at 1256 ℃ and has a phase transitio…     

Synthesis of 4″-benzyloxyimino-4″-deoxyavermectin Bla derivatives

Six new 4″-benzyloxyimino-4″-deoxyavermectin Bla derivatives were synthesized from avermectin Bla by the selective protection of C-5-hydroxy group,oxidation of C-4″-hydroxy group,and deprotection followed by reaction with O-substituted hydroxylamine hydrochlorides.Their structures were confirmed by IR,~1H NMR,~(13)C NMR and MS.Insecticidal activities of the derivatives against Phopalosiphum pseudobrassicae,Spodoptera exigua and Pluteua xylosteua were evaluated.     

Ω型分子筛脱铝的核磁共振研究

在不同投料比（ＳｉＯ２／Ａｌ２Ｏ３＝１３．８，１９及２１）条件下，合成了三种Ω型分子筛原粉．对投料比为１３．８的原粉样品进行了四种不同方式的脱铝处理，即水热、ＳｉＣｌ４、ＥＤＴＡ和（ＮＨ４）２ＳｉＦ６处理，而形成了系列脱铝Ω型分子筛样品．对原粉及其脱铝样品进行了２９Ｓｉ和２７ＡｌＭＡＳＮＭＲ测试，确定出样品骨架硅铝比和铝在两种晶体学不等价Ｔ位上的占据比率，以探索四种脱铝方法的效果．实验结果与分析表明：在所有样品中，铝原子的占据具有择优Ｂ位的倾向；且铝在ＴＡ与ＴＢ位上的占据比率与合成条件有关；四种处理方式对Ω型分子筛的脱铝效果不尽相同．     

烯土—铌（钽）复合溴氧化物的结构与光谱特性

用高温固相法合成了系列化合物ＲＥ０．０６Ｌａ０．９４Ｍ２Ｏ６Ｂｒ（Ｍ＝Ｎｂ，Ｔａ；ＲＥ＝Ｅｕ，Ｔｂ，Ｐｒ，Ｓｍ），并测定了其激发和发射光谱。室温下Ｅｕ＾３＋，Ｔｂ＾３＋，Ｐｒ＾３＋，Ｓｍ＾３＋在稀土－铌（钽）复合溴氧化物中呈现特征激发谱线，但Ｎｂ和Ｔａ的光谱特性稍有不同。     

High performance liquid chromatography post-column chemiluminescence determination of sulfonamide residues in milk at low concentration levels using bis[4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl] oxalate as chemiluminescent reagent

The determination of seven sulfonamides by means of HPLC with chemiluminescence detection is proposed for the first time. The analytes are derivatized with fluorescamine, separated and subsequently they participate in the post-column chemiluminescence (CL) peroxyoxalate system using imidazole as a catalyst. Among the different peroxyoxalates tested, bis[4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl] oxalate provides higher sensitivities and stabilities, avoiding precipitation problems. A rigorous optimization of the significant variables by means of experimental designs has been developed in order to reconcile the chromatographic conditions with the CL reaction. The method provides detection limits in the low microgl(-1) range and has been satisfactorily applied to the analysis of spiked raw milk samples.     

倾斜交叉差分式激光热透镜光谱法特性研究

本文描述了一个倾斜交叉、差分式激光热透镜光谱法。采用本方法可消除较高的溶剂空白的影响。文章讨论了调制频率和泵浦光功率对热透镜信号的影响,给出了检测Cu~(2+)的工作曲线,讨论了影响方法灵敏度的诸因素,提出了可能的改进方案。