Rapid determination of vitellogenin in fish plasma by anion exchange high performance liquid chromatography using postcolumn fluorescence derivatization with o-phthalaldehyde.

An analytical method involving anion exchange high performance liquid chromatographic determination of vitellogenin (Vtg) in fish plasma after postcolumn fluorescence derivatization with o-phthalaldehyde (OPA) was developed. The retention time of Vtg was about 11 min. The reagent variables for derivatization were optimized. The fluorophore was excited at 335 nm and detected at 435 nm. A calibration curve was established ranging from 0.13 to 11.28 microg. The determination limit of Vtg was found to be as low as 0.13 microg. The spiked recovery was 93.6% and interassay variability was less than 4%. The method developed was used to determine Vtg in fish plasma obtained from red sea bream (Pagrosomus major), black porgy (Sparus macrocephalus) and skew band grunt (Hapalogenys nitens), without complicated sample pretreatment. The results confirmed that the method showed advantages of being simple, rapid, reproducible and sensitive.     

Asymptotic robustness of standard errors in multilevel structural equation models

Data in social and behavioral sciences are often hierarchically organized. Multilevel statistical methodology was developed to analyze such data. Most of the procedures for analyzing multilevel data are derived from maximum likelihood based on the normal distribution assumption. Standard errors for parameter estimates in these procedures are obtained from the corresponding information matrix. Because practical data typically contain heterogeneous marginal skewnesses and kurtoses, this paper studies how nonnormally distributed data affect the standard errors of parameter estimates in a two-level structural equation model. Specifically, we study how skewness and kurtosis in one level affect standard errors of parameter estimates within its level and outside its level. We also show that, parallel to asymptotic robustness theory in conventional factor analysis, conditions exist for asymptotic robustness of standard errors in a multilevel factor analysis model.     

高纯金属镨中痕量稀土杂质的电感耦合等离子体原子发射光谱分析及光谱干扰的校正

本文提出了PGS-2型平面光栅光谱仪(色散率0.18纳米,二级光谱)与PlasmaTherm ICP-5000D射频发生器联用,乙醇预去溶方式进样,同时直接测定高纯金属镨中5个痕量稀土杂质元素的方法。并讨论了基体浓度对检出限的影响以及光谱干扰及其校正方法。当样品溶液中镨的浓度为5毫克/毫升时,测定下限分别为镧、钕和钐0.002%,铈0.003%和钇0.0005%。获得了良好的实验结果,其相对标准偏差为1.2-6.2%。     

3520ICP发射光谱仪维修二例

３５２０ＩＣＰ发射光谱仪维修二例房毅卓，原力（中国科学院青海盐湖研究所西宁８１０００８）３５２０型电感耦合等离子顺序扫描发射光谱仪，是由瑞士应用研究实验室（ＡＲＬ）生产的高速自动分析装置，主要应用于冶金、地质、石油、卫生和科研等部门的元素分析。以下介...     

等滴光度法测定钼铁中的钼

根据ΔAp=KΔ（bc)p原理，采用“等滴光度法”测定钼铁中的钼，通过试验确定了最佳测定条件。该方法简便、快速，用于钼铁标准样品中钼的测定，测定结果的精密度为0.196%，与标准值之间的相对误差为0.064%（n=4)。     

聚乙烯单晶的退火效应

用混合晶红外光谱法和ＳＡＸＳ、ＤＳＣ和ＬＡＭ等方法研究了聚乙烯单晶在７５℃、９０℃和１０５℃退火前后的结构变化，发现在９０℃以下和１０５℃以上退火，遵循不同的退火机制     

(4S)-4-羧基杂氮硅三环的合成

利用L-N,N-双(β-羟乙基)丝氨酸及L-N,N-双(β-羟乙基)苏氨酸与三乙氧基硅烷或氯烷基三乙氧基硅烷反应合成了具有手性的(4S)-4-羧基杂氮硅三环(1～5),并运用IR、~1HNMR、EI-MS等手段表征了结构。证据显示存在着贯穿笼状结构的N→Si配键。     

（±）—Salvinolone的全合成研究

以２－（３，４－环己基类二氧－５－异丙基）苯基乙醇（２）和３－异丙氧基－５，５－二甲基－１，３－环己烯酮（４）为原料，利用羰基α－位的烷基化反应和分子内的Ｆｒｉｅｄｅｌ－Ｃａｒｆｔｓ反应为关键步骤，经９步反应，合成了多氧芳香型三环二萜类天然产物Ｓａｌｖｉｎｏｌｏｎｅ。     

付里叶变换红外光谱仪的操作参数对光谱的影响

本文以二苯基甲酮的ＫＢｒ压片为标样，在Ｂｒｕｋｅｒ ＩＦＳ １２０ＨＲ付里叶变换红外光谱仪上系统考察了该仪器折一些重要操作参数（光源光栏、切趾函数、扫描速度）对光谱质量（信噪比，分辨率）的影响。从而获得了测样时的优化操作条件。