水样中邻苯二甲酸酯类增塑剂检测的综合实验设计

建立固相萃取-气相色谱法同时测定水中6种邻苯二甲酸酯类增塑剂含量方法。选取C18固相萃取小柱对水样进行富集净化,在0.2~1000 mg/L范围,有良好的线性关系,相关系数均大于0.999,检测限0.15~0.3μg/L,回收率90.2%~101.3%,相对标准偏差1.4%~8.8%。该方法不仅适用各种水样邻苯二甲酸酯类增塑剂的分析检测,而且有利于培养学生综合运用知识进行科学研究的能力。     

固相萃取-气相色谱/质谱法检测纺织品中的邻苯二甲酸酯

针对纺织品中邻苯二甲酸酯类(PAEs)环境激素富集困难的问题,建立了固相萃取-气相色谱/质谱法测定纺织品中PAEs的方法。通过比较3种性质不同固相萃取剂的萃取效果,筛选最优固相萃取柱,再探讨影响萃取效果的主要因素。结果表明,最优萃取条件为:选取C18为固相萃取柱,5 m L甲醇活化,上样流速1 m L/min,5 m L的乙酸乙酯洗脱,洗脱速率3 m L/min。该方法线性关系良好,相关系数为0.997 8~0.999 7,样品的加标回收率为86.3%~101.9%,含量检测的相对标准偏差小于4%,方法的检出限为1~3μg/L。对实际样品检测结果表明,该方法能够有效、便捷地检测出纺织品中痕量的邻苯二甲酸酯类物质。     

固相萃取-高效液相色谱法测定绿茶中微量邻苯二甲酸酯

以C18-H为固相萃取柱,V(甲醇):V(水)=77:23为流动相,建立了绿茶中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯和邻苯二甲酸二丁酯等3种邻苯二甲酸酯的固相萃取-高效液相色谱分离方法。在最佳条件下3种邻苯二甲酸酯在0.02~100μg/m L范围内线性良好,相关系数r≥0.9992。平均加标回收率为85.79%~95.31%,相对标准偏差(RSD)≤6.0%。该方法可有效消除绿茶中的基体干扰,定量准确可靠,适用于饮料中微量塑化剂的测定和监控。     

儿童用品中邻苯二甲酸盐的检测

文章采用超声震荡萃取—气相色谱法建立测定儿童用品中邻苯二甲酸酯的方法;以正己烷为萃取溶剂,然后采用气相色谱法—氢火焰离子检测器,进行检测分析,该方法的平均回收率为69.0%~103.2%,相对平均偏差为1.8%~5.9%。该方法用于儿童用品样品中14种邻苯二甲酸酯的测定,具有较好的准确性。     

固相萃取—气相色谱—质谱联用法检测羟丙基变性淀粉中氯丙醇含量

建立了固相萃取—气相色谱—质谱联用法(SPE-GC-MS)检测羟丙基变性淀粉中氯丙醇(1-氯-2-丙醇和2-氯-1-丙醇总量)的快速定量和确证方法。样品经水提取,固相萃取净化,衍生化后经气相色谱—质谱联用仪分析,内标法定量。该方法回收率在91.5%~99.8%之间,相对标准偏差(RSD,n=6)为3.28%~3.57%。检出限优于国标方法,结果准确、操作简便,可用于羟丙基变性淀粉中氯丙醇的检测。     

固相萃取-气相色谱法测定茶叶中多氯联苯和有机氯农药残留

建立了茶叶中15种多氯联苯（PCBs）和有机氯农药残留固相萃取（SPE）-气相色谱分析方法。用正己烷-丙酮（体积比2∶1）提取,经Envi-Carb/NH2复合固相萃取柱净化,以环氧七氯为内标,采用RTX-5毛细管柱分离,气相色谱-电子捕获检测器（GC-ECD）检测。当加标质量分数为0.03、0.07、0.2 mg/kg时,平均加标回收率为82.99%~127.10%,相对标准偏差（RSD）为1.07%~8.66%%,该方法的检测限（LOD）在0.0007~0.0110 mg/kg之间。     

中药材农药残留分析中的前处理方法比较

[目的]比较中药萝芙木中17种农药残留的2种前处理技术。[方法]样品经有机溶剂提取后,采用磺化法和固相萃取法进行净化,并采用GC-ECD进行检测,对前处理的提取条件和净化条件进行优化。[结果]石墨炭黑/氨基(CARBON/NH2)复合固相萃取小柱能够较好地去除杂质,磺化法不适用硫丹(含硫丹Ⅰ和硫丹Ⅱ)、狄氏剂和拟除虫菊酯类农药。[结论]采用CARBON/NH2复合固相萃取技术的方法平均回收率为75.11%~113.53%,相对标准偏差为0.34%~4.84%,适合中药萝芙木中17种农药残留的分析。     

GC/ECD测定白酒中的邻苯二甲酸酯类化合物

建立了液液萃取-气相色谱法测定白酒样品中16种邻苯二甲酸酯的方法。方法表明16种邻苯二甲酸酯化合物能得到有效分离;在0.4~5 mg·L-1范围内,16种邻苯二甲酸酯的线性相关系数R2均大于0.996;加标回收实验表明,回收率在86.3%~99.0%之间,相对标准偏差2.4%~7.1%;检出限低于0.10 mg·kg-1。该方法具有分离度好,较宽的线性范围,简单快速等优点,能够满足白酒中邻苯二甲酸酯类化合物的日常检测。     

ASE-GC/MS法测定EVA塑料消费品中的7种PAEs

建立了乙烯-醋酸乙烯(EVA)塑料消费品中7种邻苯二甲酸酯(DBP、Di BP、BBP、DEHP、DNOP、DINP、DIDP)残留量的加速溶剂萃取-气相色谱/质谱(ASE-GC/MS)测定方法。采用含有DBP、Di BP、DEHP等3种邻苯二甲酸酯(PAEs)的EVA洞洞鞋阳性样品优化确定了PAEs的加速溶剂萃取最佳条件是以二氯甲烷为提取溶剂,在120℃下循环萃取2次,每次9 min,萃取液经固相萃取净化后采用GC/MS法进行定性和定量分析。本方法对EVA塑料消费品中Di BP、DBP、BBP、DEHP和DNOP的检出限均为0.05 mg/kg,DINP和DIDP的检出限均为0.2 mg/kg。样品的加标回收率和相对标准偏差分别为76%~101%和2.3%~13%。     

固相萃取-气相色谱/质谱法检测纺织品中的邻苯二甲酸酯

针对纺织品中邻苯二甲酸酯类(PAEs)环境激素富集困难的问题,建立了固相萃取-气相色谱/质谱法测定纺织品中PAEs的方法。通过比较3种性质不同固相萃取剂的萃取效果,筛选最优固相萃取柱,再探讨影响萃取效果的主要因素。结果表明,最优萃取条件为:选取C18为固相萃取柱,5 m L甲醇活化,上样流速1 m L/min,5 m L的乙酸乙酯洗脱,洗脱速率3 m L/min。该方法线性关系良好,相关系数为0.997 8⁰.999 7,样品的加标回收率为86.3%0.999 7,样品的加标回收率为86.3%¹01.9%,含量检测的相对标准偏差小于4%,方法的检出限为1101.9%,含量检测的相对标准偏差小于4%,方法的检出限为1³μg/L。对实际样品检测结果表明,该方法能够有效、便捷地检测出纺织品中痕量的邻苯二甲酸酯类物质。     

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。