用国产GDX-103色谱柱测定脂肪醇聚氧乙烯醚类产品中的1,4 -二(噁)烷

用顶空气相色谱法,选择了色谱固定相和实验条件,用国产高分子多孔小球GDX-103色谱柱测定脂肪醇聚氧乙烯醚(AEO)及其硫酸盐(AES)和含有AES的餐具洗涤剂中的1,4-二噁烷。结果表明:所测7个AEO样品中1,4-二噁烷的质量浓度小于2μg.mL-1;所测9个AES样品中1,4-二噁烷质量浓度为6.0μg.mL-1-928.3μg.mL-1;所测8个餐具洗涤剂样品中1,4-二噁烷质量浓度为2.9μg.mL-1-59.7μg.mL-1。该方法测定1,4-二噁烷的标准曲线的相关系数为0.999 9,检出限为0.3μg.mL-1。     

饮用水中全氟辛酸和全氟辛烷磺酸的固相萃取-高效液相色谱-串联质谱测定法

目的:建立了饮用水中全氟辛酸和全氟辛烷磺酸的固相萃取-高效液相色谱-串联质谱测定法.方法:水样经C18固相萃取柱富集,甲醇和氨水甲醇溶液依次洗脱目标物,洗脱液氮吹浓缩定容至1 mL.采用ZORBAX Eclipse Plus C18色谱柱,多重反应监测负离子模式进行检测,内标法定量.结果:全氟辛酸和全氟辛烷磺酸在0.2～5μg/L浓度范围内呈良好的线性关系,相关系数(r2)均大于0.995,方法检出限分别为1.69和2.08 ng/L,在3个加标水平下的平均回收率为84.1％～107.0％,相对标准偏差(RSD,n=6)为2.0％～9.2％.结论:本方法快速,简便,灵敏度高,精密度、回收率理想,适用于饮用水中全氟辛酸和全氟辛烷磺酸的分析测定.     

1,4-二正烷氨基蒽醌系聚丙烯用蓝色染料的合成及应用

本文以正烷基胺和1,4-二羟基蒽醌为原料,在氯化锌和硼酸作用下制备了1,4-二正丁氨基蒽醌、1,4-二正辛氨基蒽醌、1,4-二正十二氨基蒽醌和1,4-二正十八氨基蒽醌4只蓝色染料。在反应条件下,正烷基胺和1,4-二羟基蒽醌配比为2.2:1时,4只染料收率分别为54.3％、76. 6％、74.9％、69.4％;它们的熔点分别为105.℃、76 8℃、80. 5℃和98.5℃;热分解温度分别为327.0℃、342.2℃、314.0℃和324.5℃,最大吸收波长分别为649.2nm、649.4nm、649.6nm和649.6nm;在染色条件下,经过120分钟染色,47,染料在聚丙烯纤维上的上染率分别为51.2％、56.3％、71.5％和67.4％。     

1,4-二氨基-2,3-二氯蒽醌合成的新工艺

将1,4-二氨基蒽醌隐色体在溶剂中直接通入氯气进行氯化,可以得到色谱含量98％以上的1,4-二氨基-2,3-二氯蒽醌,收率93％左右.     

顶空-气相色谱法对水中甲醇和丙酮的测定

目的:本研究采用带有氢火焰离子检测器(FID)的顶空-气相色谱仪测定水中甲醇和丙酮的含量,以色谱保留时间定性,外标法定量.结果:甲醇检出限为0.072mg/L,丙酮检出限为0.009mg/L.甲醇和丙酮的精密度分别为1.9％～4.4％和2.4％～3.7％,其加标回收率平均值范围分别为93.0％～100％和97.9％～9...     

船舶防污底漆中Cybutryne测试方法研究

建立了船舶海洋防污涂料中Cybutryne的气相色谱-质谱(GC-MS)和液相色谱-串联质谱(LC-MSMS)的分析方法.样品可以用乙酸乙酯进行快速萃取.在该实验条件下,Cybutryne标准溶液在0.05～5 mg/L的体积浓度范围内线性关系良好,相关系数分别为0.999和0.998.对Cybutryne阴性样品进行加标回收实验.结果表明本方法的平均回收率为89％～111％,相对标准偏差≤10％.气相色谱-质谱法检出限为5μg/g,液相色谱-串联质谱法检出限为0.8μg/g.本方法简单、快速、重复性好,能够满足检测工作的实际要求.     

1-(1,4-苯并二(口恶)烷-2-羰基)哌嗪对映体的分离研究

1-(1,4-苯并二(口恶)烷-2-羰基)哌嗪是制备抗高血压药物多沙唑嗪的重要中间体,手性多沙唑嗪可以通过中间体的手性分离来制备.用柱前衍生化-反相高效液相色谱法对1-(1,4-苯并二(口恶)烷-2-羰基)哌嗪对映体进行了分离.结果表明,用乙酰葡萄糖异硫氰酸酯(GITC)为柱前手性衍生化试剂,C18柱(4.6 mm×250 mm)为色谱柱,可以将1-(1,4-苯并二(口恶)烷-2-羰基)哌嗪对映体分离,其他色谱条件为流动相组成为V(甲醇)V(0.02 mol/L磷酸二氢钾水溶液)= 5347,流速为0.5 mL/min,检测波长为250 nm.在选择的测定条件下,非对映异构体分离度约等于1.3(R=1.3).     

1,4-二羟基丁烷-2-磺酸钠的合成及其在聚氨酯离子聚合物合成中的应用

采用1,4 -丁烯二醇和亚硫酸氢钠反应合成了1,4-二羟基丁烷-2-磺酸钠,经甲醇/水混合溶剂提纯,产率90％以上.红外光谱(FT- IR)、核磁氢谱(1H- NMR)和碳谱(13C- NMR)证实了产物的结构,并对其物理性质(如熔点)和其在水、丙酮、甲醇等中的溶解性进行了测试.研究了反应温度、反应时间、反应物物质的量比对产率的影响,结果表明:反应温度为40℃,反应时间为3h,亚硫酸氢钠与1,4-丁烯二醇的物质的量比为1.2:1是合成1,4-二羟基丁烷-2-磺酸钠的最佳反应条件.以1,4-二羟基丁烷-2-磺酸钠为含离子的单体,聚己二酸己二醇新戊二醇酯(PHNA)、异佛尔酮二异氰酸酯(IPDI)、乙二胺(EDA)、1,4-丁二醇(BDO)为原料,采用丙酮法合成了聚氨酯离子聚合物,红外光谱证实了其结构.拉伸测试表明聚氨酯离子聚合物拉伸强度达41.3 MPa,断裂伸长率为1700％;聚氨酯离子聚合物分散后对分散体的基本性能进行测试,结果显示ξ电位为- 53.85 mV,说明分散体具有良好的稳定性;固含量为50.6％,黏度320 mPa·s,说明聚氨酯分散体具有高固含量、低黏度的特征.     

固相微萃取-气相色谱法测定氨苄青霉素中丙酮和异丙醇残留量

本文采用顶空-固相微萃取-气相色谱联用技术测定了氨苄青霉素中丙酮和异丙醇残留量。使用自制萃取头(苯-丙共聚物与SE-30复合),萃取时间为50min,温度为60℃,2m×3mm i.d.不锈钢色谱柱、内填充10%聚丁二酸乙二醇酯/202酸洗红色担体。丙酮测定结果的相对标准偏差(RSD)为0.38%,在0.11~20μg.g-1范围时,色谱峰面积与质量浓度之间相关系数(r2)为0.9897,回收率为98.5%~101%;异丙醇测定结果相对标准偏差(RSD)为0.56%,在0.17~20μg.g-1范围时,色谱峰面积与质量浓度之间的相关系数(r2)为0.9902,回收率为97.9%~102%。     

离子色谱法测定脑膜炎球菌多糖蛋白结合疫苗中的1,4-丁二胺含量

目的采用离子色谱法测定脑膜炎球菌多糖蛋白结合疫苗中的1,4-丁二胺含量,并对方法进行验证。方法采用Ion Pac CS17(4 mm×250 mm)分析柱,上样量25μl,以10 mmol/L甲基磺酸淋洗液进行等度洗脱,流速1.0 ml/min,电导检测器检测,Chromeleon色谱工作站记录并分析数据。对该方法进行专属性、线性、准确性、重复性验证,并确定该方法的最低检出限和最小定量限。结果该方法检测1,4-丁二胺专属性较强;在40μg/L~1 mg/L范围内,1,4-丁二胺浓度与色谱峰面积呈良好的线性关系,r2均大于0.999;向A、C、W135、Y群脑膜炎球菌多糖蛋白结合物原液中分别添加低、中、高浓度的1,4-丁二胺,重复测定5次的回收率在97.23%~104.94%之间,重复测定10次的相对标准偏差(RSD)在0.8%~1.8%之间;该方法的最低检出限为5μg/L(信噪比3∶1),最小定量限为40μg/L(信噪比10∶1)。结论离子色谱法简便、快速,灵敏度高,可用于检测脑膜炎球菌多糖蛋白结合疫苗中1,4-丁二胺的含量。     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

Methyl 2,4,6-decatrienoates Attract Stink Bugs and Tachinid Parasitoids

Halyomorpha halys (Stål) (Pentatomidae), called the brown marmorated stink bug (BMSB), is a newly invasive species in the eastern USA that is rapidly spreading from the original point of establishment in Allentown, PA. In its native range, the BMSB is reportedly attracted to methyl (E,E,Z)-2,4,6-decatrienoate, the male-produced pheromone of another pentatomid common in eastern Asia, Plautia stali Scott. In North America, Thyanta spp. are the only pentatomids known to produce methyl 2,4,6-decatrienoate [the (E,Z,Z)-isomer] as part of their pheromones. Methyl 2,4,6-decatrienoates were field-tested in Maryland to monitor the spread of the BMSB and to explore the possibility that Thyanta spp. are an alternate host for parasitic tachinid flies that use stink bug pheromones as host-finding kairomones. Here we report the first captures of adult and nymph BMSBs in traps baited with methyl (E,E,Z)-2,4,6-decatrienoate in central Maryland and present data verifying that the tachinid, Euclytia flava (Townsend), exploits methyl (E,Z,Z)-2,4,6-decatrienoate as a kairomone. We also report the unexpected finding that various isomers of methyl 2,4,6-decatrienoate attract Acrosternum hilare (Say), although this bug apparently does not produce methyl decatrienoates. Other stink bugs and tachinids native to North America were also attracted to methyl 2,4,6-decatrienoates. These data indicate there are Heteroptera in North America in addition to Thyanta spp. that probably use methyl 2,4,6-decatrienoates as pheromones. The evidence that some pentatomids exploit the pheromones of other true bugs as kairomones to find food or to congregate as a passive defense against tachinid parasitism is discussed.     

2007～2008年世界塑料工业进展

收集了2007年7月～2008年6月世界塑料工业的相关资料,介绍了2007～2008年国外塑料工业的发展情况,提供了世界塑料产量、消费量及全球各类树脂的需求量及产能情况.按通用热塑性树脂(聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂)、工程塑料(尼龙、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚)、特种工程塑料(聚苯·硫醚、液晶聚合物、聚醚醚酮)、通用热固性树脂(酚醛、聚氨酯、不饱和聚酯树脂、环氧树脂)不同品种的顺序,对树脂的产量、消费量、供需状况及合成工艺、产品应用开发、树脂品种的延伸及应用的进一步扩展等技术作了详细介绍.     

2005～2006年国外塑料工业进展

收集了2005年7月～2006年6月国外塑料工业的相关资料,介绍了2005—2006年国外塑料工业的发展情况。提供了世界塑料产量、消费量及全球各类树脂生产量以及各国塑料制品的进出口情况。作为对比,介绍了中国塑料的生产情况。按通用热塑性树脂（聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂）、工程塑料（聚酰胺、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚）、通用热固性树脂（酚醛、聚氨酯、不饱和树脂、环氧树脂）、特种工程塑料（聚苯硫醚、液晶聚合物、聚醚醚酮）的品种顺序,对树脂的产量、消费量、供需状况及合成工艺、产品开发、树脂品种的延伸及应用的扩展作了详细的介绍。