A novel route to prepare pH- and temperature-sensitive nanogels via a semibatch process

A novel method via a semibatch process in the absence of surfactant has been adopted to prepare pH- and temperature-sensitive nanogels. The shape, charge distribution, temperature, and pH-induced volume phase transition behavior of the latexes were investigated by scanning electronic microscopy, zeta potentials, dynamic laser light scattering, and UV/vis spectroscopy. It was found that, in the absence of surfactant, with increasing the amount of AAc from 5 to 20 mol% of N-isopropylacrylamide (NIPAM), the hydrodynamic diameters (D_H) decrease from 230 to 60 nm. With increasing pH value from 3 to 11, the D_H values increase slightly, which is different than the dramatic increase seen when using a conventional batch method with a range from 680 to 1700 nm. However, at pH 3, the turbidity curves of these kinds of particles increase dramatically at temperatures between 33 and 37 °C, while remaining constant at first and then increasing directly at pH 11. Furthermore, the distribution of carboxylic groups located not only on the interior but also on the exterior of colloidal particles as a result of adoption of the semibatch method, other than simple surface distribution of poly(NIPAM-co-AAc) latexes via the batch method.     

直流辉光放电质谱法测定多晶硅中关键杂质元素的相对灵敏度因子

采用直流辉光放电质谱(dc-GD-MS)测定多晶硅中关键杂质元素的相对灵敏度因子(RSF).标样制作过程中主要是在连续通入氩气条件下将固定量的非标准多晶硅样品熔化,向硅熔体中均匀掺入浓度范围为1～30 μg/g的关键杂质元素(如B和P),采用快速固化法制成标样;再将制成的标准样品加工成一系列适合GD-MS扁平池(Flat Cell)的片状样品(20 mm×20 mm×2mm).采用二次离子质谱法(SI-MS)对标准样品中关键掺杂元素进行多次定量测定,取平均值作为关键杂质元素的精确含量.优化一系列质谱条件后,运用GD-MS对标样中关键掺杂元素的离子强度进行多次测定,计算平均结果,得到未校正的表观浓度,利用标准曲线法计算出关键杂质元素的相对灵敏度因子.     

Direct analysis of anabolic steroids in urine using Leidenfrost phenomenon assisted thermal desorption-dielectric barrier discharge ionization mass spectrometry

Rapid detection of trace level anabolic steroids in urine is highly desirable to monitor the consumption of performance enhancing anabolic steroids by athletes. The present article describes a novel strategy for identifying the trace anabolic steroids in urine using Leidenfrost phenomenon assisted thermal desorption (LPTD) coupled to dielectric barrier discharge (DBD) ionization mass spectrometry. Using this method the steroid molecules are enriched within a liquid droplet during the thermal desorption process and desorbed all-together at the last moment of droplet evaporation in a short time domain. The desorbed molecules were ionized using a dielectric barrier discharge ion-source in front of the mass spectrometer inlet at open atmosphere. This process facilitates the sensitivity enhancement with several orders of magnitude compared to the thermal desorption at a lower temperature. The limits of detection (LODs) of various steroid molecules were found to be in the range of 0.05–0.1 ng mL⁻¹ for standard solutions and around two orders of magnitude higher for synthetic urine samples. The detection limits of urinary anabolic steroids could be lowered by using a simple and rapid dichloromethane extraction technique. The analytical figures of merit of this technique were evaluated at open atmosphere using suitable internal standards. The technique is simple and rapid for high sensitivity and high throughput screening of anabolic steroids in urine.