修正制品中氯代烃多组分检测技术研究及应用

应用带有电子捕获检测器的毛细管气相色谱法分析了修正制品中氯代烃多组分,用对测定无干扰的溶剂萃取、离心过滤后,以溴丙烷为内标物测定了其中的8种对人体有害的氯代烃,即二氯甲烷、三氯甲烷、三氯乙烯、四氯化碳,1,1-二氯乙烷、1,2-二氯乙烷、1,1,1-三氯乙烷及1,1,2-三氯乙烷。方法的检出限(3S/N)在0.010~2.5mg/kg范围内,相对标准偏差(n=6)小于5%,标准加入回收率在90.2%~98.8%之间。     

离子色谱法分析防冻液和切削液中卤族元素

建立了等度离子色谱电导检测器分析防冻液和切削液中卤族元素的方法。采用CarboPacAS19分离柱对分离条件进行了优化,确定柱温为30℃、淋洗液为20mmol·L-1的KOH溶液。在0.10～20.0mg·L-1范围内氟、氯、溴呈良好线性,回收率分别为90.0%~100.4%、80.0%~100.3%、87.2%~97.0%,方法检出限分别为0.005、0.01、0.01mg·kg-1,精密度分别为1.64%~5.46%、0.83%~4.99%、1.07%~5.29%。检测了防冻液和切削液中的卤族元素,效果良好。     

气相色谱法测定木家具中五氯苯酚的含量

文章研究了气相色谱—电子捕获检测器定量测定木家具中五氯苯酚含量的方法。样品经甲醇超声波提取,乙酸酐衍生化,衍生物再用正己烷萃取,有机相针式过滤头过滤后采用气相色谱—电子捕获检测器进行检测。结果表明,在0.04~1μg/m L的范围内线性关系良好,相关系数为0.9996,平均回收率为92.7%~103.6%,相对标准偏差≤4.85%,方法检出限为0.05 mg/kg。方法操作简便,回收率好,适合于木家具中五氯苯酚含量的检测。     

毛细管气相色谱法同时测定三磷酸胞苷二钠中5种有机溶剂残留量

研究建立了同时测定三磷酸胞苷二钠中乙醇、丙酮、氯甲醚、甲苯、苯乙烯5种有机溶剂残留量的毛细管气相色谱法。样品以乙腈为溶剂,经DB-FFAP(30 m×0.32 mm×0.25μm)毛细管柱分离,氢火焰离子化检测器检测,这5种有机溶剂呈良好的线性响应,平均回收率在98.3%~99.5%,精密度RSD在0.21%~1.92%,最低检出限可达5.0~7.5 mg/kg。本方法简单、灵敏、准确,完全能满足药品中所述有机溶剂残留量的测定要求。     

柱前衍生-高效液相色谱质谱联用测定氯吡格雷中的甲醛残留

采用柱前衍生-液相色谱质谱联用法测定氯吡格雷原料药中甲醛溶剂残留。通过2,4-二硝基苯肼衍生,反相色谱柱分离,质谱检测器选择离子检测测定了氯吡格雷中甲醛残留。在方法考察浓度范围内具有良好线性,,回归方程为A=5367.3C(μg/m L)+319.3,相关系数r=0.999,回收率在92.0%~106.0%之间,精密度良好。该方法灵敏、准确,可以用于氯吡格雷原料药中甲醛残留量检测。     

化妆品中氯乙酰胺检测方法的研究

建立了气相色谱测定化妆品中氯乙酰胺含量的方法。样品用乙醇超声提取,经净化离心过滤后,采用HP-INNOWax色谱柱分离,氢火焰离子化检测器(FID)检测。结果表明,氯乙酰胺的质量浓度在10~1 000 g/mL范围内与响应值有良好的线性关系,相关系数r大于0.999,在0.05%、0.3%和0.6%3个水平上对液体类、膏霜乳类和固体类化妆品分别进行添加回收试验,回收率范围为94.4%~98.1%,相对标准偏差(RSD)为1.12%~2.59%,定量低限为0.05%,满足国际上通行的0.3%的限量要求。     

气相色谱法测定橡胶木材中五氯苯酚残留量

建立了气相色谱-电子捕获检测器法(GC-ECD)定量检测橡胶木材及制品中五氯苯酚(PCP)残留的方法。样品经甲醇提取、衍生化后GC-ECD进行定量分析,PCP浓度在20~400μg/L范围内线性关系良好(r=0.9968),检出限(LOD,S/N=3)为0.03 mg/kg,回收率范围为86.2%~108.1%,相对标准偏差小于2.6%。该方法简单、准确度高、分析时间短,可用于快速检测橡胶木材及制品中的五氯苯酚残留。     

气相色谱法检测淀粉微球中的氯丙醇残留量

采用FFAP毛细管柱(30 m×0.53 mm×1.0μm),载气为N2,柱温80℃,进样口温度230℃,FID检测器温度250℃,分流比10∶1。使用外标法进行了氯丙醇(1-氯-2-丙醇和2-氯-1-丙醇)含量测定的气相色谱方法学研究。对分析方法的专属性、精密度、准确度、检测限等进行了验证。结果表明,气相色谱检测氯丙醇具有良好的线性(氯丙醇的浓度在0.1~0.5 mg/m L呈线性,相关系数R2=0.999 2),重复测定相对标准偏差小于5.0%,加标回收率为94.3%~104.5%,结果表明外标气相色谱法可以用于氯丙醇的残留量定量分析。     

离子色谱法测定用水中痕量氟、氯、硫酸根和硝酸根

介绍了利用离子色谱法测定用水中痕量的硝酸根、硫酸根、氯、氟等离子;优化了检测器电流、淋洗液浓度和样品进样量等,使各阴离子的检出限降低,硝酸根、硫酸根、氯、氟等离子的检出限分别为0.016、0.074、0.014、0.012mg/L,加标回收率达到90%~110%;6次检测环境标准204715,相对标准偏差RSD低于2%。离子色谱法测定阴离子方法速度快、精准且灵敏度高,可在同一时间内透析水中不同的阴离子。     

三氯乙烯生产废水中氯代烃的脱除

以三氯乙烯生产工业废水为处理对象,采用0价铁催化还原、混凝沉淀法,对氯代烃进行脱除处理,探讨了脱氯处理效果及其反应机理。结果表明,三氯乙烯的脱氯效率大于99％,其他氯代烃脱氯效率大于90％。催化还原反应在常温、常压下进行,反应条件温和,对三氯乙烯生产废水中的氯代烃具有很好的脱除效果。     

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。