共振瑞利散射法测定药物及生物样品中的头孢硫脒

建立了测定痕量头孢硫脒的共振瑞利散射法。在NaOH介质中,甲基紫(MEV)与头孢硫脒(CEFA)反应生成的配合物使体系的共振瑞利散射(RRS)显著增强,并出现新的RRS光谱,最大共振瑞利散射峰位于338nm,CEFA的质量浓度在0.094~0.47mg/L范围内与共振瑞利散射强度(ΔIRRS)呈线性关系,检出限(3Sb/S)为0.068mg/L。该法用于人体血液、尿液及市售头孢硫脒药物中头孢硫脒含量的测定,回收率为98.9%~102%,测定值的相对标准偏差为1.2%~1.4%。     

钼(Ⅵ)-PV-CV体系共振瑞利散射法测定痕量钼

在p H为3.5的邻苯二甲酸氢钾-盐酸缓冲溶液中,在聚乙烯醇存在下,钼(Ⅵ)与邻苯二酚紫(PV)形成的配阴离子[Mo(PV)2]2-与结晶紫(CV)阳离子结合形成的离子缔合物具有较强的共振瑞利散射光谱。其最强共振瑞利散射峰位于647 nm处。基于共振瑞利散射峰的逐渐增强,建立了测定痕量钼(Ⅵ)的共振瑞利散射法。该方法钼(Ⅵ)质量浓度在0.1~0.6 mg/L范围内与共振瑞利散射光强度呈良好的线性关系,检测限为1.5×10-4 mg/L,可用于水样中钼的测定。     

吖黄素盐酸盐共振瑞利散射光谱法测银离子含量

提出了共振瑞利散射光谱技术(RRS)测定Ag~+含量的新方法。在p H为2. 87～8. 95的Britton-Robinson(B-R)缓冲溶液中,吖黄素盐酸盐(AH,Acriflavine hydrochlorde)与Ag~+结合生成配合物,使溶液的共振瑞利散射(RRS)增强,并且在321 nm、489 nm处的散射峰强度显著增加。以321 nm为测定波长,Ag~+的浓度在0. 05～10 mg/L范围内,与RRS强度变化有良好的线性关系,对Ag~+的检出限(3σ)达0. 019 mg/L。研究了反应的适宜条件和影响因素,并用于环境水样中Ag~+含量的测定,回收率为93. 5%～106%。     

灿烂绿共振瑞利散射法测定功能饮料中的牛磺酸

建立了快速、准确、灵敏地测定功能饮料中牛磺酸的共振瑞利散射法。在弱碱性Tris-盐酸缓冲介质中,灿烂绿能与牛磺酸结合使体系的共振瑞利散射(RRS)显著增强,并产生新的RRS光谱。最大共振瑞利散射峰位于367 nm,牛磺酸的质量浓度在0.005~0.13 mg/L范围内与RRS增强强度(|ΔIRRS|)呈线性关系,定量限为3.12 mg/100 m L。该方法简便、快速、灵敏,有较高的准确度和选择性,可用于市售功能饮料中牛磺酸的测定,加标回收率为98.39%~102.1%,测定值的相对标准偏差为2.0%~2.5%。     

共振瑞利散射法定量检测药物中的吡哌酸

建立了快速、准确检测药物中吡哌酸的高灵敏共振瑞利散射法。在pH为9. 64的碱性Tris-HCl介质中,吡哌酸与碱性艳蓝B相互作用生成二元离子缔合物,使共振瑞利散射(RRS)信号显著增强,并产生新的RRS光谱。最大共振瑞利散射峰位于365 nm,吡哌酸的质量浓度在0. 007～0. 55 mg/L范围内与体系的共振瑞利散射增强强度(ΔI_(RRS))呈线性关系,检出限为0. 006 5 mg/L。该方法用于药物中吡哌酸的测定,加标回收率为98. 2%～103%,相对标准偏差(n=5)为2. 0%～2. 5%。     

用共振瑞利散射技术测定药物中的格列齐特

在pH 4.55 Tris-盐酸介质中,格列齐特与固绿FCF-溴化十六烷基吡啶反应生成绿色三元离子缔合物,使共振瑞利散射(RRS)信号明显增强,并产生两个较强的共振瑞利散射峰,在348 nm波长处,格列齐特的质量浓度在0.006～0.450 mg/L范围内与共振瑞利散射增强强度(ΔI_(RRS))呈线性关系,检出限为0.005 5 mg/L,由此建立了测定格列齐特的RRS新方法。还研究了RRS的光谱特征、适宜反应条件、方法的选择性及实际应用。实验表明,该法灵敏、简便、快速,用于市售格列齐特片剂中格列齐特的测定,结果满意。     

维多利亚蓝B共振光散射法测阿莫西林

建立了测定阿莫西林的共振瑞利散射法.在pH 9.98的Tris-HCI缓冲溶液中,阿莫西林和维多利亚蓝B相互作用后,共振瑞利散射显著增强,在337 nm处呈现最高散射强度.阿莫西林的质量浓度在0～0.4μg/mL范围内与△IRRS成正比,检出限(3Sb/S)为0.027μg/mL.该法简便、快速、灵敏,用于人体尿液、市...     

共振瑞利散射法测定硫酸卡那霉素

基于在pH值3.78~6.59的B-R缓冲溶液中,四碘荧光素钠(ST)与硫酸卡那霉素(KANA)结合生成离子缔合物使溶液共振瑞利散射(RRS)增强的原理,建立了共振瑞利散射法测定KANA的新方法。在其最大共振散射波长576nm处测定共振瑞利散射强度(IRRS),并研究了表面活性剂和共存物质对KANA测定的影响。结果表明:KANA浓度在0.04~1.60mg·L~(-1)范围内与ΔIRRS(样品与空白溶液的IRRS值之差)呈线性关系,方法的检出限为0.018 mg·L~(-1)。用于KANA注射液的测定,回收率为92.5%~96.5%。     

TPB增敏酸性品红共振瑞利散射测定皮蛋中的Cd

建立了检测皮蛋中Cd的共振瑞利散射法,研究了共振瑞利散射光谱特征、共存物质的影响及反应机理。在pH 4.81的Tris-盐酸缓冲介质中,溴代十六烷基吡啶(TPB)增敏酸性品红与Cd(Ⅱ)结合生成三元离子缔合物,使体系的共振瑞利散射(RRS)显著增强并产生新的RRS光谱,在最大共振瑞利散射峰372 nm处,Cd(Ⅱ)的质量浓度在0.004~0.39 mg/L范围内与体系的共振瑞利散射增强程度(ΔIRRS)呈线性关系,定量限为0.019 mg/kg。方法简便、准确、灵敏,加标回收率为97.1%~102%,相对标准偏差RSD(n=5)为2.3%~2.8%。方法适于皮蛋中Cd的测定。     

共振瑞利散射法测定尿中痕量砷

建立了一种测定尿中痕量砷的共振瑞利散射(RRS)新方法。在pH=5.6的HAc-NaAc缓冲溶液中,I3-与硫酸耐而蓝生成稳定的离子缔合物,体系共振瑞利散射增强。当加入微量As(Ⅲ)时,碘能定量氧化As(Ⅲ),导致共振瑞利散射减弱,在0.10~4.0μg/25 mL浓度范围内,共振瑞利散射强度的改变值ΔIRRS与As(Ⅲ)浓度呈线性关系,方法检出限为1.65μg/L。用于尿中痕量砷的测定,回收率为93.5%~106.7%。     

乙烯酮(双乙烯酮)下游产品废水的治理技术

乙烯酮(双乙烯酮)是十分重要的化工中间体,其下游产品较多。江苏某化工厂开发生产乙烯酮(双乙烯酮)下游产品三十多个,年生产规模三万多吨,是国内以乙烯酮(双乙烯酮)为中间体生产精细化学品的综合骨干企业。针对乙烯酮(双乙烯酮)下游产品废水特点,该厂结合企业实际,开展了产品优化,结构调整,清洁生产,资源循环利用,节水降耗等工作,从源头削减了污染物的生产。同时投资二千多万元新建预处理装置三套,6000m3/d废水生化处理装置一套,使全厂乙烯酮(双乙烯酮)下游产品的废水得到了有效的治理。     

A study of miscibility of blends of polybutadienes of varying microstructure

The miscibility of various amorphous polybutadienes with mixed microstructures of 1,4 addition units (cis, 1,4 and trans 1,4) and 1,2 addition units have been investigated. The studies here involved optical transparency, differential scanning calorimetry, and small angle light scattering. It was found that a 90 percent (cis) 1, 4 addition polybutadiene was immiscible with high (91 percent) 1,2 addition polybutadiene. Reduction of the 1,2 content to 71 percent induced an upper critical solution temperature (UCST) with the cis 1,4 polymer. Polybutadienes with 50 percent and 10 percent 1,2 contents were miscible above the crystalline melting temperature of the cis 1,4 polybutadiene. Immiscibility of the 91 percent 1,2 addition polymer was also found with a 10 percent 1,2 polybutadiene. The latter polymer also exhibits an UCST with the 71 percent 1,2 polymer. The results are used to interpret the characteristics of blends of polybutadienes of varying microstructure.     

几种乙炔加压设备性能的比较

阐述并比较了几种加压设备在乙炔加压清净过程中的性能和特点。     

粉煤灰中烧失量检测的不确定度分析

以F类粉煤灰为例,详细介绍了测定粉煤灰中烧失量的步骤、计算数学模型、影响测量不确定度的因素以及各项测量不确定度分量评定,人员、设备、材料、方法、环境都是影响测量不确定的因素。     

生物油的成分分析及物性测定

以添加FeCl2的ZnCl2-KCl混合熔盐裂解纤维素和秸秆,制得生物油。采用傅立叶变换红外光谱法和气相色谱-质谱法分析生物油的成分。结果表明,生物油中成分复杂,含有氧元素、多种有机化合物,主要包括酮类、醛类、酚类及羧酸类等。测定了20～80℃生物油的密度和粘度,发现生物油的密度与温度呈较好线性关系,而生物油的粘度均大于水的粘度,且不同熔盐体系对秸秆生物油的粘度无较大影响。     

Effect of degree of deacetylation of chitosan on the kinetics of ultrasonic degradation of chitosan

The objective of the study was to explore the effect of the degree of deacetylation (DD) of the chitosan used on the degradation rate and rate constant during ultrasonic degradation. Chitin was extracted from red shrimp process waste. Four different DD chitosans were prepared from chitin by alkali deacetylation. Those chitosans were degraded by ultrasonic radiation to different molecular weights. Changes of the molecular weight were determined by light scattering, and data of molecular weight changes were used to calculate the degradation rate and rate constant. The results were as follows: The molecular weight of chitosans decreased with an increasing ultrasonication time. The curves of the molecular weight versus the ultrasonication time were broken at 1‐h treatment. The degradation rate and rate constant of sonolysis decreased with an increasing ultrasonication time. This may be because the chances of being attacked by the cavitation energy increased with an increasing molecular weight species and may be because smaller molecular weight species have shorter relaxation times and, thus, can alleviate the sonication stress easier. However, the degradation rate and rate constant of sonolysis increased with an increasing DD of the chitosan used. This may be because the flexibilitier molecules of higher DD chitosans are more susceptible to the shear force of elongation flow generated by the cavitation field or due to the bond energy difference of acetamido and β‐1,4‐glucoside linkage or hydrogen bonds. Breakage of the β‐1,4‐glucoside linkage will result in lower molecular weight and an increasing reaction rate and rate constant. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3526–3531, 2003     

分解炉扩径的技术改造

我厂3号回转窑(Φ4m×60m)生产线在1996年年底由SP窑(产量912t/d)改为NSP窑(产量1320t/d),预分解系统为四级旋风预热器带离线式分解炉     

水泥水化热测定方法综述

水泥水化热是中、低热水泥和核电工程用水泥的一项关键的技术指标。全球范围内测定水泥水化热的方法有溶解法、直接法/半绝热法、等温传导量热法三种。本文总结了中、美、欧相关方法标准,对其测试原理、仪器设备、试验过程等方面进行了比对,并对其在领域的应用做了简单的概括。