北京城市污泥中铅砷镉形态浓度的ICP-MS分析

城市污泥中重金属的难降解和高毒性限制了污泥的资源化利用。以北京G和Q污水处理厂的压滤出厂污泥为实验材料,采用BCR三步浸提法对污泥中铅砷镉Pb,As,Cd的三种形态进行提取,以HNO₃-HClO₄进行全量消解,利用ICP-MS检测Pb,As,Cd的全量和各形态的含量,从而为北京城市污泥的资源开发研究提供基础数据。实验结果表明,北京城市污泥中Pb和Cd含量比上世纪末明显降低：其中,G污泥中Pb,As,Cd的全量(干重)分别为19.60,37.96和1.34 mg·kg-1,而Q污泥中分别为19.58,23.46和2.30 mg·kg-1;两种污泥中Pb含量相差甚微,G污泥中As明显高于Q污泥,而Cd则显著低于后者;两种污泥中相应金属的三种形态的变化趋势基本一致：Pb与As以HAc酸溶态为主,H₂O₂可氧化态最少;而Cd主要以NH₂OH-HCl可还原态存在,HAc酸溶态最少。三种重金属中生物毒性大的形态均占70％以上。     

Relative position determination of a lunar rover using high-accuracy multi-frequency same-beam VLBI

Multi-frequency same-beam VLBI means that two explorers with a small separation angle are simultaneously observed with the main beam of receiving antennas. In the same-beam VLBI, the differential phase delay between two explorers and two receiving telescopes can be obtained with a small error of several picoseconds. The differential phase delay, as the observable of the same-beam VLBI, gives the separation angular information of the two explorers in the celestial sphere. The two-dimensional relative position on the plane-of-sky can thus be precisely determined with an error of less than 1 m for a distance of 3.8×105 km far away from the earth, by using the differential phase delay obtained with the four Chinese VLBI stations. The relative position of a lunar rover on the lunar surface can be determined with an error of 10 m by using the differential phase delay data and the range data for the lander when the lunar topography near the rover and the lander can be determined with an error of 10 m.     

中药提取过程在线紫外动态趋势回归分析及终点判定

随着中药生产行业的转变,中药生产过程现代化成为了必然趋势。而目前由于缺乏有效的在线检测手段,中药生产检测滞后性大,产品质量参差不齐。针对中药提取过程在线监控及终点判定的问题,基于朗伯比尔定律及中药提取动力学方程建立提取液紫外吸光度随时间变化模型,并提出动态分析及终点判断方法, 该方法包括紫外吸光度序列拟合、稳健性分析以及终点计算。以千年健提取过程为例,使用本实验室自主研发的中药提取液在线采样系统进行光谱收集,并对离线样本求取其有效固体物质含量作为参考。分析过程中,首先对实时检测的光谱进行插值及滤波处理,计算230.2～400 nm紫外谱区的吸光度均值并结合前期数据组成吸光度均值序列;随后,进行了该吸光度序列与提取液固体含量之间的相关分析,得到线性相关系数r2=0.9828,证明二者存在较强的线性关系;最终对吸光度均值序列进行动态模型稳健回归及提取终点判定。结果表明：回归过程通过稳健性分析能够充分识别出测量异常点,提高了拟合曲线与原始吸光度的复相关系数,使其达到0.99,并通过终点判定将千年健提取时间由最初人工设定的180 min缩短至122 min。实验证明,紫外在线监控方法实现了提取过程的在线监控及终点判定,对稳定产品质量、提高经济效益具有重要意义。     

Precise orbit determination of a maneuvered GEO satellite using CAPS ranging data

Wheel-off-loadings and orbital maneuvers of the GEO satellite result in additional accelerations to the satellite itself. Complex and difficult to model, these time varying accelerations are an important error source of precise orbit determination (POD). In most POD practices, only non-maneuver orbital arcs are treated. However, for some applications such as satellite navigation RDSS services, uninterrupted orbital ephemeris is demanded, requiring the development of POD strategies to be processed both during and after an orbital maneuver. We in this paper study the POD for a maneuvered GEO satellite, using high precision and high sampling rate ranging data obtained with Chinese Area Positioning System (CAPS). The strategy of long arc POD including maneuver arcs is studied by using telemetry data to model the maneuver thrust process. Combining the thrust and other orbital perturbations, a long arc of 6 days’ CAPS ranging data is analyzed. If the telemetry data are not available or contain significant errors, attempts are made to estimate thrusting parameters using CAPS ranging data in the POD as an alternative to properly account for the maneuver. Two strategies achieve reasonably good data fitting level in the tested arc with the maximal position difference being about 20 m. Supported by the National Natural Science Foundation of China (Grant No. 10703011) and the Science & Technology Commission of Shanghai Municipality of China (Grant No. 06DZ22101)     

A pulsed EPR method to determine distances between paramagnetic centers with strong spectral anisotropy and radicals: The dead-time free RIDME sequence

Methods to determine distances between paramagnetic metal centers and radicals are scarce. This is unfortunate because paramagnetic metal centers are frequent in biological systems and so far have not been employed much as distance markers. Successful pulse sequences that directly target the dipolar interactions cannot be applied to paramagnetic metal centers with fast relaxation rates and large g-anisotropy, if no echos can be detected and the excitation bandwidth is not sufficient to cover a sufficiently large part of the spectrum. The RIDME method Kulik et al. (2002) [20] circumvents this problem by making use of the T₁-induced spin-flip of the transition-metal ion. Designed to measure distance between such a fast relaxing metal center and a radical, it suffers from a dead time problem. We show that this is severe because the anisotropy of the metal center broadens the dipolar curves, which therefore, only can be analyzed if the full curve is known. Here, we introduce five-pulse RIDME (5p-RIDME) that is intrinsically dead-time free. Proper functioning of the sequence is demonstrated on a nitroxide biradical. The distance between a low-spin Fe(III) center and a spin label in spin-labeled cytochrome f shows the complete dipolar trace of a transition-metal ion center and a spin label, yielding the distance expected from the structure.     

基于四组分同时测定的PARAFAC和SWATLD算法及比较

邻苯二酚和对苯二酚是有毒物质,酪氨酸和色氨酸是天然氨基酸中仅有的会发光的组分,由于四组分光谱重叠,很难用常规方法直接定量检测。实验中采用三维荧光光谱结合平行因子和自加权交替三线性分解算法,邻苯二酚、对苯二酚、酪氨酸和色氨酸进行直接定量测定;同时,比较两种算法在定性测定和定量测定上的差别。当测量体系的成分数预估计值为4时,两种方法分辨后的回收率分别为(101.2±2.7)%,(99.3±3.0)%,(98.7±4.5)%,(101.6±4.7)%和(109.0±8.0)%,(91.3±11)%,(99.7±13)%,(98.1±11)%。试验结果表明,两种方法可用于四组分直接快速定量测定;通过对两种算法的比较,PARAFAC算法更具优势。     

Determination of Organic Chlorine by Aluminium Monochloride Molecular Absorption Spectrometry Using Lead Atomic Line

The present study was conducted to investigate the molecular absorption by AlCl in a carbon rod furnace for determination of chlorine in organic compounds, by using the lead atomic line at 261.418 nm emitted from a Pb-hollow cathode lamp. A deuterium lamp was used for the simultaneous background correction. The method enables rapid and accurate determination of trace chlorine in varying organic samples with good precision. The method was tested on different organic chloro-coumpounds and α-pinene products.     

双波长分光光度法测定痕量锌

本文研究了在稀硫酸介质中并有亚铁氰化钾存在时,锌与亚甲蓝所形成的配合物的双波长分光光度法。经摩尔比法测定,此配合物组成比为1∶2（锌∶亚甲蓝）,摩尔吸光系数为1.01L·mol-1·cm-1。桑德尔灵敏度为6.45×10-4μg/cm2。在25ml容积中,0—10μgZn遵守比尔定律,配合物可稳定2     

活血逐瘀颗粒剂中芍药甙的含量测定

本文采用了薄层色谱法将复方制剂活血逐瘀颗粒中的芍药甙与其他成分分离，用紫外分光光度法测定芍药甙的含量，其平均回收率为９８．７４％，变异系数为１．４３％，本文方法抗干扰能力强，适合于中药复方制剂中芍药甙的定量分析。     

激光剥蚀-电感耦合等离子体质谱测定植物样品中的元素

采用193 nm准分子激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)对标准植物粉末样品(GBW07602-GBW07603灌木枝叶、GBW07604杨树叶、GBW07605茶叶、GBW08514烟草)中13种元素(Li,B,Na,Mg,Al,K,Ca,Cr,Mn,Fe,Ni,Cu,Ba)进行定量测试.向植物粉末样...