近年来科普模式进入新的发展阶段,创新科普理念与工作方式,打造新时代社会化大科普生态,是大势所趋.以杭州市萧山区气象科普体验馆为例,介绍了萧山区气象局聚焦气象科普高质量发展,以展馆为核心,一核多跨,联合教育、宣传、科协等10多个部门通过"建机制、强基础、亮品牌",推进气象科普创新发展,广泛融入部门、镇村、社区、医院、景区、校园等,着力构建多元社会气象科普平台,阐述了杭州市萧山区气象局围绕社会公众气象科普需求,联合部门协作发展、创新科普形式的实践与探索.
A liquid chromatography method for the determination of diphenylmethane diisocyanate(MDI) in import and export medical devices by liquid chromatography was established. In this method, methanol was used as the extraction solvent and derivatization reagent, and MDI was derived into methylene diphenyl dicarbamate(MDC). The amount of MDC was determined by high performance liquid chromatography(HPLC) to deduce the amount of MDI dissolved. The calibration curve was linear over the concentration range of 0.5-100 μg/m L, and the correlation coefficient was 0.9999. The average recoveries of standard addition ranged from 83.5% to 98.7%, the RSDs of intra and inter day were 0.10%(n = 6) and 0.91%(n = 3), respectively. This method had a high accuracy with satisfactory results, which can be used for the determination of MDI dissolution in import and export medical devices.
A novel method for the preparation of poly(thioether)s by copolymerizing PC with COS is reported, which also expands the application of PC.
本文通过整理2015-2017年杭州萧山围垦养殖区大棚气温及水温监测数据, 旨在为杭州地区南美白对虾养殖提供参考.分析认为, 围垦区南美白对虾的放养时间以3月底4月初为宜, 捕捞以10月中旬前完成为好; 影响南美白对虾摄食的水温 (超过32 ℃或低于20 ℃) 年际差异大, 分别集中在7月中旬至8月下旬、10月中旬及以后; 影响南美白对虾生长的暴雨、高温、连阴雨、强冷空气等高影响天气的水温变化幅度小于气温, 对缓解应激反应有利.
The epoxy thermosets have a series of advantages,and are one of the most important electronic materials.However,the common epoxy materials are highly flammable.In this paper,two nitrogen-containing flame-retardant curing agents was synthesized by using phenolphthalein as the raw material.The bisphenol A epoxy resin E51 and the phosphorus-containing epoxy resin were cured with the diamine and diphenol halogen-free flame-retardant curing agents,which contain the phthalazinone moieties and have the twisty and unsymmetrical structural,and the cured exhibited excellent thermal and dynamic mechaincal properties,T of 157℃,and lower linear expansion coefficient.When curedg with the phosphorus-containing epoxy resin,it exhibited excellent flame retardant performance(UL 94 V-0).
Halogen-, phosphorous- and lead-free flame-retardant epoxy-based thermosets are environmental-friendly materials and expected to be applied to the electronic materials. Nitrogen heterocyclic ring is highly efficient flame-retardant with low toxicity and has been covalently introduced into the backbone of the epoxy polymers, but so far the structure of such nitrogen heterocyclic ring and its flame-retardant property for epoxy resin has not yet closely correlated. Based on our previous works in the field, this article summarizes recent research progress for synthesis and application of the flame retarded epoxy-based thermosets containing nitrogen heterocyclic ring, including triazine, isocyanurate, azo phthalazinone, imide, benzoxazine and hydantion rings, etc. The structure-property relationships of these systems are presented in detail. Generally, introducing nitrogen heterocyclic structures into epoxy resin systems by covalent bonding can maintain the overall performance while endow the flame retardancy to the final materials. Moreover, nitrogen heterocyclic structure can improve the thermal stability of the cured epoxy resins. As a result, epoxy resin containing nitrogen heterocyclic structures might be a good choice to obtain halogen-, phosphorous- and lead-free flame retardant epoxy-based electronic materials. However, it is still a big challenge to get flame-retardant epoxy-based thermosets just depending on nitrogen heterocyclic structure in these materials. Most of the reported systems had contained low content of phosphorous for bettering the flame retardancy. As a result, it is important to intensively understand the structure-property relationship of nitrogen heterocyclic ring-containing epoxy resin. Several methods are proposed for improving the flame retardancy of nitrogen heterocyclic ring-containing epoxy resin.
The infrared spectrum of isooctane, gasoline and methylal was analyzed with the result that the absorption peak of 1 145 cm–1 was appropriate for quantitative analysis of methylal in gasoline. The calibration curves were established respectively on Lamber–Beer equation law by 1 145 cm–1 peak absorbency of standard methylal solution with 0.1, 0.2 and 0.5 mm pathlength cells. The linear equation were Y=0.070X+0.001, Y=0.136X+0.001, Y=0.322X+0.002 with the correlation coefficents of 0.999 5,0.999 8,0.999 7, respectively. It was preferential to use 0.2 mm pathlength cell to quantitatively analyze methylal solution with the concentration between 0.1 g/L and 2.2 g/L, and the relative error of test results was less than 5%, and the relative standard deviation of repeatability was less than 2.0%(n=6).
The non-isocyanate route for synthesizing polyurethanes is a hot topic in the field of polyurethanes due to without using the isocyanates to be toxic and difficult to transport and store in the green synthesis process.This work reported the preparation of polyurethane with massive pendent hydroxyl groups based on the polyaddition of biscyclic carbonate and hexamethylenediamine. Herein, the biscyclic carbonate was obtained from the cycloaddition of bisphenol A diglycidyl ether and CO 2, using a binary catalyst system composed of Zn-Co(III) double metal cyanide complex [Zn-Co(III) DMCC] and cetyltrimethyl-ammonium bromide(CTBA). The polyhydroxy-urethanes were obtained by addition polymerization of the biscyclic carbonate and diamine in the presence of the guaternary ammonium salt catalyst.Therefore,a new route for synthesizing polyhydroxy-urethanes from the epoxy resin,carbon dioxide and diamine was provided.
通过对异辛烷、汽油和N-甲基苯胺的红外谱图进行分析,确定了3440cm-1处吸收峰作为N-甲基苯胺的红外定量谱带.基于朗伯-比耳定律,采用0.5mm光程池,对系列浓度标准溶液进行3440cm-1处吸光度的测定,并建立校准曲线.该曲线合适的溶液定量浓度范围在0.5-14g/L之间,并可定量测定含量不低于2.0g/L的汽油中N-甲基苯胺.方法准确性相对偏差小于5%,重复性(n=6)相对标准偏差小于2.0%.
Optimal ashing temperature for three primary forms of plastics' were studied by microwave ashing and differential scanning calorimetry.The residues were dissolved by tartaric acid and hydrochloric acid and were then determined by inductively coupled plasma-optical emission spectrometry.The microwave ashing results showed that the samples of polyethylene,polypropylene and polyethylene terephthalate could be absolutely ashed at 850 ℃ for 30 minutes with a gradient heating.The detection limits of Al,Ca,Co,Cr,Mg,Si,Ti and Zr were 0.24,0.12,0.08,0.03,0.03,0.35,0.01,0.02 mg/kg,respectively.The recovery results were in the range of 92.5%-116.3% and the relative standard deviation were 1.4%-9.7%.
建立了一种适用于内燃机油指纹信息采集的傅里叶变换衰减全反射(ATR)中红外光谱法,并考察了方法的精密度、重复性和稳定性等因数;对98个不同品牌、不同产地、不同质量等级的内燃机油样品进行扫描,建立了内燃机油的中红外指纹谱库;以欧式距离法、相关命中率指数法、相关系数法等3种算法对未知内燃机油进行鉴别,效果良好.
A reliable method for determination of water content in PTA by Oven samplechanger/Karl Fisher was established.The sample was heated at 230 ℃ for 20 min in the Oven samplechanger,the water in the sample was evaporated and transferred to the titration cell by dry gas,and the water make a quantitative reaction with the Karl Fisher reagent.Comparing with the SH/T 1612.4 standard,the method was convenient and no pyridine was used.
GC-MS was applied to the determination of tetrabromobisphenol A in plastics.The sample was extracted with ethyl acetate for 20 min,and concentrated to dryness by N2-blowing.The residue was dissolved with 5.0 mL of methylbenzene,and derivatized with acetic anhydride.The derivatized products were separated on DB-5MS column and EI source was used in MS.Linear relationship between values of peak area and mass concentration of tetrabromobisphenol A was kept in the range of 0.1-100 mg·L-1.Tests for recovery were made by standard addition method with 2 samples of plastics(ABS and PS) as matrixes;values of recovery found were 97.0% for ABS and 94.2% for PS with RSD′s(n=5) less than 6.5%.
A method for determination of calcium,iron,sodium,nickel,vanadium in asphalt by microwave ashing-inductively coupled plasma-optical emission spectrometry(ICP-OES) was developed.The asphalt samples were treated with sulfuric acid in order to solve the problem of low temperature ashing.The temperature of microwave ashing,amount of sulfuric acid,temperature program and weight of sample were studied in detail.Combined with differential scanning calorimetry,the optimum conditions of pre-treatment of microwave ashing were established.The detection limits of calcium,iron,sodium,nickel,vanadium were 0.04,0.10,0.64,0.28,0.22 mg·kg-1,respectively.The recoveries were in the range of 79.7%—97.8% and the relative standard deviations were between 3.4 % and 8.3 %.These results showed that the method met the elemental analysis in the asphalt.
Standard caprolactam was tested by differential scanning calorimetry(DSC) under various conditions.The method for determination of the purity of caprolactam was established by DSC,according to the Van't Hoff equation.Compared with the purity results of gas chromatography-karl fischer method,the obtained deviation was less than 0.1%.The relative standard deviation of repeatability was less than 0.02%(n=6) for the DSC method.The DSC method could rapidly and accurately determine the purity of caprolactam with good accuracy and repeatability.
Highly active calcium chloride (CaCl2) doped Zn-CoIII double metal-cyanide (Ca-DMC) catalysts were firstly reported. Ca-DMCs presented a very higher polymer yield (>54kg polymer/g catalyst) at relative low temperature (80–115°C) toward ring-opening polymerization (ROP) of propylene oxide (PO) than did DMC catalysts without modification.
A new method for the determination of loss on ignition in iron ores—thermogravimetry analysis(TGA) was developed.The measurement conditions were systematically studied and optimized.Samples were heated up to 1000℃ with heating rate of 20℃/min and held for 30 min under the protection with high pure argon flow rate of 50 mL/min throughout the experiments.The results of comparative test of TGA with traditional method(muffle furnace burning) for various kinds of imported iron ores showed that the TGV method provided the advantages of higher accuracy and reliability,more convenience,wide application range,smaller sample consumption and was especially suitable for the analysis of volatile components in iron ores.
Highly active CaCl2-modified Zn-Co(III) DMCs were prepared. XRD results showed that the modified catalyst Ca-DMC containing 0.14 wt.-% CaCl2 was amorphous. A higher polymer yield (>61 kg polymer/g catalyst) and a shorter induction period for ROP of PO were observed for Ca-DMC than for unmodified DMC catalysts. An initiator had an inhibitory effect on the initiation and polymerization rate of PO ROP. As the molar ratio of the initiator functionality to the catalyst was increased, the reaction rate and polymer yield decreased, whereas the induction period increased. An increase in reaction temperature tended to reduce the polymer yield and broaden the MWD. The C-13 NMR spectrum for an oligomer from a model polymerization without an initiator revealed that the main terminal unit of the polymer was -CH2CH(CH3)OH because H2O in the system participated in reaction initiation. Cl- and t-BuOH may also initiate the reaction according to the small amounts of terminal -CH2Cl and -OC(CH3)(3) units observed by C-13 NMR spectroscopy. On the basis of common characteristics and some new evidence for DMC catalysis, a mechanism similar to a classical coordination insertion process is proposed.
The content of each component in polyphenylene oxide (PPO)/Polystyrene (PS) blends was analyzed quantitatively by FT-IR. The absorption peak area ratio of the selected 1 305 cm-1 peak for PPO and 699 cm-1 peak for PS was used as the calibrating basis for quantitative analysis. The working curve which was used for calculating the composition of PPO/PS blends was established on the basis of Lamber-Beer equation law. This curve was available to quantitatively analyze PPO/PS blends of cPPO (or cPS)=5%-95%. The relative deviation was less than 5% compared with the results of FT-IR and 1H-NMR quantitative analysis. The relative standard deviation of detection results was less than 2.5%(n=6) for FT-IR quantitative method. FT-IR method is a simple, rapid and accurate method for quantitative analysis of PPO/PS blends.
采用气相色谱-质谱联用方法测定橡胶制品中的多环芳烃(PAHs)含量。确定试验条件为:萃取溶剂正己烷,超声波提取时间25min,正己烷/乙酸乙酯混合溶剂用量(样品量为1.0g)5mL;可对16种受控PAHs进行分离,定量分析回收率为88.6%~108.8%,检测限为0.38~3.56μg·kg-1,标准偏差为2.18%~8.20%。