Comparison of microwave-assisted digestion procedures for total trace element content determination in calcareous soils

The aim of the study was to determine total trace (Cd, Co, Cr, Cu, Mn, Pb and Zn) and major (Al and Fe) element concentrations in calcareous soils using microwave-assisted digestion procedures. The literature showing lack of consensus regarding digestion procedures and unsatisfying recoveries for calcareous materials, four procedures using various acid combinations (HCl, HNO₃, H₂O₂, HF) and volumes were tested using a certified reference material (CRM 141R) and natural calcareous soil samples. Digests were analysed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Repeatability (R.S.D. <5%) and recoveries (82-116%) showed that the procedures were precise and accurate for most elements. Five calcareous soil samples from a Champagne vineyard plot were, then, subjected to these procedures. In calcareous materials, the presence of HF resulted in Al being severely underestimated (recovery <5%) and Co overestimated (recovery >124%) due to complex formation or spectrochemical interferences, respectively. As digestion was not significantly influenced by the addition of H₂O₂, the procedure corresponding to Aqua regia (HCl-HNO₃) appeared as the best compromise and was selected for further multielemental environmental studies on calcareous materials, even if the absence of HF could lead to incomplete digestion of accessory silicate minerals. Results for a vineyard plot showed that the soils were contaminated (3.65 mg kg⁻¹ Cd, 67 mg kg⁻¹ Cr, 278 mg kg⁻¹ Cu, 143 mg kg⁻¹ Pb and 400 mg kg⁻¹ Zn) as a consequence of urban waste and copper-treatment applications.     

Influencing parameters on measurement accuracy in dynamic mechanical analysis of thermoplastic polymers and their composites

Long-term predictions of material properties such as stiffness and creep resistance are important in many engineering applications and require high reliability and accuracy. This is especially true for polymer materials and their composites as their viscoelastic nature results in time-dependent material behaviour and any measurement uncertainties or errors amplify in long-term predictions. To measure this behaviour at smallest loadings, Dynamic Mechanical Analysis (DMA) is frequently declared as an ideal method. However, the measurement accuracy and repeatability of this method is strongly influenced by (i) the testing fixture and corresponding loading mode, (ii) the sample preparation and (iii) the plotting scale to interpret the test results. In this study, relevant experimental parameters were found for DMA and a proper procedure was designed, which was then applied to measure the viscoelastic behaviour of a highly temperature and creep resistant thermoplastic polymer (polyethersulfone) and of a highly graphite filled polypropylene composite. In combination with finite element simulations and in-situ strain measurements by digital image correlation (DIC), the main influences on measurement accuracy of three-point-bending DMA were identified and subsequently used to determine measurement guidelines. Using these guidelines, DMA measurements allow quantitative determination of the viscoelastic response for rigid polymer and composite materials.     

一种多元非线性模型在激光诱导击穿光谱定量分析中的应用

现有的激光诱导击穿光谱定量分析模型大多是基于激光诱导等离子体处于局部热平衡这一假设,而实际上等离子体只是在有限的时间、空间内近似处于热平衡状态。非热平衡状态下各个能级上的粒子布居数不服从玻尔兹曼分布,故用某一能级的单一谱线做定量分析会带来一定误差。考虑到等离子体的非热平衡状态,提出了一种多元非线性定量分析模型,该模型充分利用了待分析粒子的不同上能级对应的多条跃迁谱线信息,能够有效减小信号不稳定对定量分析结果的影响。利用此模型和建立在等离子体局部热平衡假设上的单谱线内标模型分别对30块钢铁样品中Mn元素的含量进行定量分析对比,对比结果表明,多元非线性模型的测量准确性和重复性均优于单谱线内标模型。     

两位置球面面形检测方法研究

三位置球面面形绝对检测方法在一定的条件下可以简化为两位置球面面形检测方法.本文在研究三位置绝对检测原理的基础上,提出了基于菲索干涉系统新的两位置球面面形检测方法.该方法的简化条件分为参考面面形误差偶对称或被检面面形误差偶对称两种不同的情况.实验结果表明,两位置检测方法可以有效实现PVr值λ/30的高准确度检测,且检测结...     

用方法精密度检验钛合金光谱分析标准物质的均匀性

采用方差分析方案使用重复性(r)检验钛合金光谱分析标准物质均匀性的方法.结果表明:这种方法能较好地反映出受检样品的不均匀性,较之其他方法简单,方便,但要求比较严格.     

A novel method for the determination of steady-state torque of polymer melts by HAAKE MiniLab

HAAKE MiniLab is an apparatus specially designed for compounding polymer material and on-line testing of rheological properties. For the first time, it was used to establish a dynamic speed test method for the rapid determination of steady-state torque of polymer melts. The choices of sample feed quantity and screw rotation speed, as well as calibration for real torque, were carefully studied before torque measurements. The repeatability and reliability of torque data were also evaluated. Results showed that the torque could be calibrated by subtracting the torque without samples. Also, a feed quantity of ca. 6 g with a dynamic speed test range of 10–105 r/min was suitable for the determination of steady-state torque of polyolefin samples. The new method was quick, effective and reliable to correlate the steady-state torque with rotation speed. Therefore, MiniLab would be a very useful tool in exploring and characterizing polymer flow behavior through its torque measurements.     

Approaches to optimisation of precision in capillary electrophoresis

Summary A study has been performed to obtain insight into the relative importance of critical factors affecting the repeatability of hydrodynamic injections in CE. Precision was measured for repeated analysis of a test mixture containing two acidic compounds.The use of an internal standard was clearly shown to improve precision especially when peak area precision was poor. It is suggested that precision is maximised by employing a combination of a constant temperature, an appropriate electrolyte system, an internal standard, long injection times, and high sample concentrations. Other factors are discussed, but are classified as having only a minor impact.     

Capillary electrophoresis of seed albumins fromVicia species using uncoated and surface-modified fused silica capillaries

Summary Capillary zone electrophoresis has been developed for the separation of seed albumins fromVicia faba using both uncoated and polyoxyethylene ether (Brij-35) coated octadecysilane derivatized capillaries. Optimal separation conditions were found by studying the effect of pH, buffer composition and applied voltage. The nonionic surfactant/C₁₈ coated capillary significantly reduced albumin adsorption and electroosmotic flow (EOF). A gradual washing out of the surfactant from the coated capillary during use altered not only the magnitude of the EOF, but also its reproducibility. The introduction of hydrophilic polymer solutions between analyses for dynamic modification of the Brij/C₁₈ coated capillary surface prevented desorption of coating material, allowed optimization of resolution and ensured stability of the EOF. CE with surface-modified capillaries was then used to compare seed albumin profiles of severalVicia species. This technique appears to provide a powerful tool for use in taxonomic investigations.     

Field measurement of airborne sound insulation between rooms with non-diffuse sound fields at low frequencies

Procedures for the field measurement of airborne sound insulation between rooms with diffuse fields are described in International Standard ISO 140-4. However, many dwellings contain rooms with volumes less than 50 m³, where low frequency measurements are less reliable; hence there is a need for a measurement procedure to improve the reliability of field measurements in rooms with non-diffuse fields. Procedures are proposed for sound pressure level and reverberation time measurements for the 50, 63 and 80 Hz third octave bands. The sound pressure level measurement combines corner microphone positions with positions in the central region of each room. This provides a good estimate of the room average sound pressure level with significantly improved repeatability.     

A study of repeated measures of softest and loudest phonations

One common way to describe one's voice in an objective way is to measure the sound levels of the softest (pianissimo) and loudest possible (fortissimo) phonations at given pitches (voice range profile measurement). However, the reliability of the measurement has not been thoroughly investigated. The aim of the present study was to describe the repeatability and reproducibility of the sound level measurement in statistical terms, focusing on five target frequencies within the estimated speaking pitch range. Ten healthy female university students volunteered as test subjects. The voice range profiles within the speaking pitch range were defined 10 times in succession and in five sample sessions between 45-minute-long oral readings. Our study followed the ideas of the Gage repeatability and reproducibility design. The results showed that the method used was reliable in fortissimo phonations at four of the measured frequencies. Better reliability can be achieved by measuring three successive phonations at each pitch prior to the next target tone.