A new micro reaction calorimeter

Traditional reaction calorimeters require highly trained operators and the use of a large sample size (10 ml to 1000 ml) which is incompatible with highly reactive substances. A new calorimeter with a 2 ml or less sample size lends itself to the determination of reactivity of materials for process safety and to the determination of safety of materials shipped in compartment tank cars. The TC-100 Titration Calorimeter meets these requirements. A cost effective instrumentation of a differential cell design provides high sensitivity heat flow measurements. Automatic liquid injection and continuous mixing provides information on the heat of reaction and its rate. A portable instrument with small sample size allows for rapid temperature equilibration and safe handling of very reactive materials.     

Measurement of natural radioactivity in Jordanian sand

Sand samples were collected from Adasiah (near Amman), Jerash and Ghor As-Safi (near Karak). ²²⁶Ra, ²³²Th and ⁴⁰K activities, present in these samples, were measured using a gamma ray spectroscopy technique. The average values of the radium equivalent activities were calculated and were found to be 41.06 Bq kg⁻¹, 54.7 Bq kg⁻¹ and 85.53 Bq kg⁻¹ in samples collected from Adasiah, Jerash and Ghor As-Safi, respectively. These values are within the limit (i.e. less than 370 Bq kg⁻¹) recommended for the safe use of construction materials for dwellingsby OECD.     

Selection between proportional and stratified hazards models based on expected log-likelihood

The problem of selecting between semi-parametric and proportional hazards models is considered. We propose to make this choice based on the expectation of the log-likelihood (ELL) which can be estimated by the likelihood cross-validation (LCV) criterion. The criterion is used to choose an estimator in families of semi-parametric estimators defined by the penalized likelihood. A simulation study shows that the ELL criterion performs nearly as well in this problem as the optimal Kullback–Leibler criterion in term of Kullback–Leibler distance and that LCV performs reasonably well. The approach is applied to a model of age-specific risk of dementia as a function of sex and educational level from the data of a large cohort study.     

长江中下游现代河漫滩土层物理力学性质及工程地质评价

长江出三峡南津关口自宜昌而下, 由于河谷增宽, 水力梯度减小, 沉积物的颗粒由上游至下游逐渐变细、各类土层的工程地质性质也逐次变差。本文以长江中下游河谷两岸漫滩土层的物理力学性质和基本地质环境条件予以工程评价, 欲望能对长江中下游河谷两岸的各类土木工程建筑提供基础资料。     

采用天然标准是提高AES粉末法准确度的有效途径──同时测定地质样品中Ag等8个痕量元素

本文进一步研究ＡＥＳ法用天然标准代替合成标准，实验证明ＡＥＳ粉末法的最大误差来自合成标准。同时测定地质样品中Ａｇ等８个痕量元素。大批量的分析结果表明，只要严格控制操作条件，分析准确度可以提高到一个新的水平。     

Efficient Algorithm for Computing Maximum Likelihood Estimates in Linear Transformation Models

Linear transformation models, which have been extensively studied in survival analysis, include the two special cases: the proportional hazards model and the proportional odds model. Nonparametric maximum likelihood estimation is usually used to derive the efficient estimators. However, due to the large number of nuisance parameters, calculation of the nonparametric maximum likelihood estimator is difficult in practice, except for the proportional hazards model. We propose an efficient algorithm for computing the maximum likelihood estimates, where the dimensionality of the parameter space is dramatically reduced so that only a finite number of equations need to be solved. Moreover, the asymptotic variance is automatically estimated in the computing procedure. Extensive simulation studies indicate that the proposed algorithm works very well for linear transformation models. A real example is presented for an illustration of the new methodology.     

液相色谱-四极杆/飞行时间高分辨质谱组合化学计量学方法快速筛查婴幼儿配方乳粉中化学危害物

采用液相色谱-四极杆/飞行时间(LC-Triple TOF^®)高分辨质谱组合化学计量学方法建立了婴幼儿配方乳粉中化学危害物的快速筛查模型。实验采用人工添加外源化学物质(沙丁胺醇、林可霉素、磺胺嘧啶、螺旋霉素、双氯西林和醋酸甲地孕酮)模拟婴幼儿配方乳粉中未知化学危害物污染,15种不同的乳粉等量混合后用水复溶,配制代表性乳粉溶液样品。依据添加与否将样品分为参照组(不含添加的化合物)和添加组。乳粉溶液试样加入乙腈进行提取,经Captiva ND^Lipids固相萃取柱净化,CORTECS^TM UPLC C₁₈₊柱液相色谱分离,以0.3%(v/v)甲酸-5%(v/v)水-乙腈溶液和0.3%(v/v)甲酸-5%(v/v)乙腈-水溶液为流动相梯度洗脱;飞行时间质谱全扫描(TOF MS)-信息依赖性采集(IDA)-子离子扫描(product ion scan)正离子模式采集样品数据。数据经MarkerView^TM软件预处理后导入SIMCA-P软件,对比分析参照组和添加组样品数据,拟合构建正交偏最小二乘法-判别分析(OPLS-DA)模型,并利用此模型进行样品组别区分和添加化合物识别。结果表明,实验构建的筛查模型拟合度和预测能力良好(R²X(cum)=0.742, R²Y(cum)=0.997, Q²Y(cum)=0.905),参照组和添加组样品被显著区分,6种添加的化合物(最低添加水平为50 μg/kg,以乳粉计)全部被可靠地识别。该研究建立的方法为婴幼儿配方乳粉质量安全主动分析监控体系提供了有益技术参考。     

激光剥蚀电感耦合等离子体质谱法测定地质玻璃中铅同位素组成

将193nm准分子纳秒激光与四级杆电感耦合等离子体质谱联用,测量了国际参照物玻璃中Pb同位素丰度比。通过剥蚀NIST612,USGS和MPI-DING玻璃,探讨了利用激光剥蚀电感耦合等离子体质谱直接测定固体样品铅同位素比值的精密度及其适用范围。通过扣除Ar载气中204Hg对204Pb的同量异位素干扰,采用内标法和外标法校正LA-ICP-MS仪器的质量歧视效应,获得的206Pb/204Pb、207Pb/204Pb、208Pb/204Pb同位素比值测量的相对误差小于±1.2%,207Pb/206Pb、208Pb/206Pb同位素比值测定的相对误差小于±0.8%。对比结果表明,采用内标法校正的结果更接近真实值。测定的Pb同位素比值的精密度与样品中Pb含量密切相关,对Pb含量大于40μg/g的样品,同位素比值206Pb/204Pb、207Pb/204Pb、208Pb/204Pb的RSD在1.0%以内,207Pb/206Pb、208Pb/206Pb的RSD在0.5%以内。大气颗粒物样品中Pb含量很高,采用LA-ICP-MS测定Pb同位素比值,能够鉴别污染来源,满足示踪的要求。     

Hierarchical MoS2/polyaniline binary hybrids with high performance for improving fire safety of epoxy resin

Here we report a facile strategy to fabricate phosphoric acid doped polyaniline/molybdenum disulfide (PANI/MoS₂) hybrids as high-performance nanofillers in epoxy (EP) resin for the first time. In situ growth of PANI on the surface of two-dimensional MoS₂ template resulted in the uniform dispersion and strong interfacial adhesion of PANI/MoS₂ hybrids within EP matrix, which can be confirmed by the obvious increase (13.5°C) in glass transition temperature (T_g) of EP composites. The MoS₂ nanosheets also acted as a critical component to generate synergistic effect with PANI on reducing the fire hazards of EP resin. It resulted in a remarkable removal of flammable decomposed products and a considerable reduction of toxic CO yield. The dramatical decreases in real-time smoke density and total smoke production, and high-graphitized char layer in condensed phase were obtained for EP composite with 5 wt% PANI/MoS₂ hybrids. The multiple synergistic effects (synergistic dispersion and synergistic char formation) are believed to be the primary source for these obvious enhancements of properties of EP composites. This facile strategy may achieve the potential application of functionalized MoS₂ in polymeric nanocomposites.     

四川华蓥山地重力灾害类型及成因分析

从华蓥山所处的地理位置出发,全面的介绍了华蓥山地区近些年来的重力灾害发生的情况,可以看到重力灾害在本地区的影响之大,已经成为了本地区主要的灾害类型。通过各方面的调查研究,采用科学分析和经验指导相结合的方法,分析了引起重力灾害发生的各种因素,并重点从地质因素、水体因素、人为因素等3方面分析了华蓥山地重力灾害发生的成因,总结了可以引起重力灾害发生的外因和内因,可以看到重力灾害不单是某一个因素导致,而是由于众多的因素相互的影响所导致的。采取各种措施来预防灾害的发生,减少灾害给人类的生产和生活带来的危害。