Sample Preparation for the Determination of Metals in Food Samples Using Spectroanalytical Methods—A Review

Abstract

The present article gives an overview of recent publications and modern techniques of sample preparation for food analysis employing atomic and inorganic mass spectrometric techniques, such as flame atomic absorption spectrometry, chemical vapor generation atomic absorption and atomic fluorescence spectrometry, graphite furnace atomic absorption spectrometry, inductively coupled plasma optical emission spectrometry, and inductively coupled plasma mass spectrometry. Among the most frequently applied sample preparation techniques for food analysis are dry ashing, usually with the addition of an ashing aid, and acid digestion, preferably with the assistance of microwave energy. Slurry preparation, particularly with the assistance of ultrasound, is increasingly used to reduce acid consumption and sample preparation time. Direct analysis of solid samples is gaining importance in the field of food analysis as it offers the highest sensitivity, avoids the use of acids and other aggressive reagents, makes possible the analysis of micro‐samples, and can be applied for fast screening analysis, e.g., of fresh meat.     

事后分层方法及其在交通运输抽样调查中的应用

本文介绍事后分层技术，说明了它不仅可用于简单随机抽样，而且可以用于放回ＰＰＳ抽样。给出了事后分层估计量的形式，证明了它的无编性，并给出了它在交通运输抽样调查中的应用。     

高盐样品中锂的电感耦合等离子体发射光谱法(ICP-OES)测定研究

锂是重要的战略金属和新能源材料,其开发利用受到全球的高度关注。在高盐卤水特别是盐湖卤水和地下卤水中富含巨量的锂资源,在对这些资源进行锂的开发利用过程中,需对锂的含量进行准确测定,然而卤水中共存的高浓度Na+, K+, Ca2+和Mg2+会对微量锂的准确测定产生严重的干扰。电感耦合等离子体发射光谱法(ICP-OES)具有线性范围宽和多元素同步分析能力,针对卤水中锂的快速准确测定,详细开展了高盐样品中锂的ICP-OES分析方法研究。结果表明,锂在610.364 nm处具有较高的信噪比,且Na+, K+, Ca2+, Mg2+和Ar不会对锂的测定产生显著的谱线干扰。然而,样品中大量共存的Na+, K+和Mg2+会对锂的测定产生严重的基体正干扰,而Ca2+产生负干扰。尽管内标法在消除基体干扰方面具有广泛的应用,但传统的以钇和钪为内标元素的内标法不能有效解决该问题。此外,针对标准加入法操作繁琐、不适合批量样品分析问题,以及基体匹配法需多离子匹配,且不适合样品基体组成变化的批量样品分析等问题,考察了采用单一组分进行复杂基体匹配的可行性。由于NaCl广泛存在于卤水中,且对锂的测定具有显著的增敏效应,通过系列研究发现,通过同时向样品和标准溶液中加入10 g·L-1的NaCl,成功解决了总量不超过40 g·L-1的NaCl, KCl和MgCl2所产生的干扰。尽管采用该法或沉淀预分离方式均不能消除Ca2+产生的负干扰,但当样品中Ca2+含量不高于1.8 g·L-1时,对测定不产生显著的影响。通过采用该方法对三种不同基体组成的卤水样品进行加标回收测定,其回收率在96.60%~104.20%范围内。此外,通过与电感耦合等离子体质谱法(ICP-MS)测定结果进行对比,充分论证了该法的准确性和可靠性(相对误差±3.66%)。该法仅以单一的NaCl进行复杂基体匹配,不仅简化了操作,还实现了基体组成变化的批量样品分析,因而在卤水中锂的快速准确测定及锂资源开发利用方面具有重要意义。     

基于邻域贡献权值细化的圆心亚像素定位算法

针对传统的圆心算法过程复杂、定位精度受初始边缘提取效果影响较大等问题,提出了一种基于邻域贡献权值细化的圆心亚像素定位算法。首先引入邻域贡献权值系数,改进传统非极大值抑制法,细化边缘;然后在边缘点的梯度方向对灰度值进行高斯拟合,确定亚像素边缘位置;最后针对边缘突变点提出了基于随机抽样一致的最小二乘法来拟合圆心。实验结果表明,该算法具有较好的精度和稳定性,圆心的提取精度可以达到0.1个像素。     

高温超导电缆导体层电流分布研究

通过建立高温超导电缆等效电路模型,并提出电流分布等效数学方程,求得高温超导电缆导体层电流分布。绕制一根0.2m长110kV/2kA高温超导电缆样缆,并进行载流能力实验,得到各层电流分布结果。分析发现,各层电流分布的实验结果与理论计算结果吻合,从而验证电流分布计算模型的正确性,以及调整绕制角度对均匀层间分流的有效性。研究结论对以后更长高温超导电缆的载流能力分析具有一定的指导意义。     

Observation of bulk like magnetic ordering below the blocking temperature in nanosized zinc ferrite

We investigated the magnetic behavior of nanosized zinc ferrite with the help of vibrating sample magnetometry and in-field Mössbauer spectroscopy. The nanoparticles of zinc ferrite with crystallite size ranging from 10 to 62 nm were synthesized by a nitrate method. The structure and phase were determined with the help of X-ray diffraction. Attributes of cation inversion were found with the calculated values of lattice parameter. The saturation magnetization decreases with the increase in crystallite size at room temperature, while these values are almost the same at 10 K for all the samples except the one with crystallite size of 10 nm. The thermal magnetization measurement shows a decrease in blocking temperature with increase in particle size for these samples. The synthesized samples exhibit the presence of antiferromagnetic ordering below the blocking temperature as investigated by in-field Mössbauer spectroscopy.     

六面顶压机高压腔体温度场的数值模拟

 以有限元法为分析手段,在模型和边界条件适当简化的条件下,对六面顶压机高压腔体的温度场进行了数值模拟计算,得出了腔体内的温度分布。在此基础上通过调整模型参数,定性讨论了样品组装设计中组装材料、加热器形状以及导电金属环厚度对温度场的影响。数值模拟结果表明：用氧化锆替代叶蜡石作为堵头和保温材料可以提高样品区的温度,降低功率的消耗并减小样品区的温度梯度;与圆筒形加热器组装相比,中间厚两端薄的变圆筒形加热器组装能提供更高的样品中心温度和较小的温度梯度;使用导电金属环的加热组装时,适当增加金属环的厚度有利于获得较理想的温度分布。研究结果对优化高压实验的样品组装设计、改善温度梯度及保护设备具有一定的参考价值。     

高能电子辐照绝缘厚样品的表面电位动态特性

采用数值计算和实验测量相结合的方法, 阐明了高能电子束照射下绝缘厚样品的表面电位和电子产额动态特性. 结果表明: 由于电子在样品内部的散射和输运, 沿着深度方向, 空间电位先缓慢下降到最小值, 然后逐渐升高并趋近于零; 随着电子束照射, 样品的表面电位逐渐下降, 可至负千伏量级, 电子总产额逐渐增大至一个接近于1的稳定值; 电子束停止照射后, 长时间放置下, 表面电位将逐渐升高, 但带电并不会消除; 表面电位随电子束能量的升高近似线性下降, 随入射角的增大而升高, 而随样品厚度的增大仅略有下降.     

How to measure energy dissipation in dynamic mode atomic force microscopy

When studying a mechanical system like an atomic force microscope (AFM) in dynamic mode it is intuitive and instructive to analyse the forces involved in tip–sample interaction. A different but complementary approach is based on analysing the energy that is dissipated when the tip periodically interacts with the sample surface. This method does not require solving the differential equation of motion for the oscillating cantilever, but is based entirely on the analysis of the energy flow in and out of the dynamic system. Therefore the problem of finding a realistic model to describe the tip–sample interaction in terms of non-linear force–distance dependencies and damping effects is omitted. Instead, it is possible to determine the energy dissipated by the tip–sample interaction directly by measuring such quantities as oscillation amplitude, frequency, phase shift and drive amplitude. The method proved to be important when interpreting phase data obtained in tapping mode, but is also applicable to a variety of scanning probe microscopes operating in different dynamic modes. Additional electronics were designed to allow a direct mapping of local energy dissipation while scanning a sample surface. By applying this technique to the cross-section of a polymer blend a material specific contrast was observed.     

电感耦合等离子体发射光谱测定植物精油中的重金属元素

植物精油是从芳香植物提取的天然复杂化合物,作为芳香植物的次生代谢产物具有挥发性和浓郁香味,其特有的多样化生物活性广泛应用于医药和化妆品行业.植物精油具有高渗透性,能以活跃的分子态渗透皮肤组织,经淋巴腺吸收后进入血液,其所含的重金属元素也极易随植物精油进入人体对健康构成潜在威胁.采用硝酸-双氧水对植物精油进行微波消解,在...