Reagent Pretreatment of Polychlorobiphenyls prior to Breakdown

Russian Journal of Applied Chemistry - Reactions of commercial polychlorobiphenyl mixtures with alkali in polyalkanolamines were studied. The major reaction products are hydrophilic mixtures of...     

Preparation of Amino Derivatives from Industrial Mixtures of Polychlorobiphenyls

Chemical utilization (conversion) of polychlorobiphenyls by nitration of their industrial mixture was studied. Reduction of the nitro derivatives gave mixtures of aminopolychlorobiphenyls.     

染料中间体2,6-二氯-4-硝基苯胺中痕量多氯联苯的GC-MS分析

用气相色谱－质谱联用仪,采用选择离子的方法对染料中间体２,６－二氯－４－硝基苯胺中的多氯联苯进行分析。检出了五氯联苯、六氯联苯、七氯联苯。并对其中六氯联苯用内标法进行了定量。方法快速、准确。     

Polymers Based on Epoxy Resins and Functional Derivatives of Polychlorobiphenyls

A new way to utilize polychlorobiphenyls was suggested: transformation of Sovol base hydrolysis products into glycidyl ethers and titanates. The resulting products were tested as components of epoxy compounds which are subsequently cured to obtain three-dimensional polymer networks.     

生物样品中多氯联苯的微波皂化萃取气相色谱法测定

以KOH－甲醇－正己烷为皂化萃取溶剂,利用微波皂化萃取－气相色谱法测定了生物样品中的多氯联苯（PCBs）,实现了在皂化的同时对待测物的萃取。方法的检出限为质量分数6.25×10     

微波皂化萃取气相色谱法测定生物样品中的多氯联苯

１引言 多氯联苯（ＰＣＢｓ）的性质稳定、毒性大,贻贝等海洋生物能摄取和富集海水中的ＰＣＢｓ,因此研究其中ＰＣＢｓ的测定具有重要意义。生物样品中 ＰＣＢｓ的测定一般要进行预分离处理,索氏萃取分离 ＰＣＢｓ耗时至少８ｈ,加碱皂化生物组织再以液－液萃取提取ＰＣＢｓ需要在沸水浴中回流１～２ｈ,微波直接革取能有效地分离环境样品中的ＰＣＢｓ。本文利用微波皂化萃取（ＭＡＳＥ）气相色谱法（ＧＣ）测定生物样品中的多氯联苯,实验以未受ＰＣＢｓ污染的淡水鱼为空白,用正交试验系统优化了微波功率、微波加热时间、皂化及萃取溶…     

Polychlorobiphenyls differentiation and identification by gas chromatography/fourier transform infrared spectroscopy

Reference infrared vapour phase spectra of 20 polychlorobiphenyls (PCBs) have been obtained by gas chromatography/Fourier transform infrared spectroscopy (GC/FTIR). These spectra are consistent with those of PCB obtained by diffuse reflectance IR spectroscopy (DRIFT) and with those of more simple molecular structures (iodochlorobenzenes, 1-bromodichlorobenzenes). The IR frequencies of the GC/FTIR spectra of PCB are assigned in terms of substitution patterns. This work shows that GC/FTIR can be a good approach for differentiation and identification of PCB in complex mixtures.     

Reaction of Dinitropolychlorobiphenyls with O- and N-Nucleophiles as a New Route of Reprocessing Polychlorobiphenyls

The reactivity of a mixture of dinitropolychlorobiphenyls in nucleophilic substitution of aromatic chlorine by polyethyleneoxy and amino groups was studied. New polychlorobiphenyl derivatives were obtained.     

沉积物内多氯联苯测定中有机氯农药的排除及质量控制/质量保证研究

报道了沉积物样品中多氯联苯(PCBs)的分析方法及质量控制/质量保证(QA/QC)研究,结果表明多级复合硅胶柱对有机氯农药去除效果良好.采用25种PCBs同族体标样PCB25对分析方法进行了QA/QC研究,PCBs的平均回收率在97%～118%之间.用本方法测定25种多氯联苯同族体的检测限范围在0.5～1.4ng/g之间.     

自动样品前处理在乳品中二恶英和共平面多氯联苯同时测定中的应用

采用索氏提取及自动净化处理系统对乳品进行提取和净化,在高分辨气相色谱-高分辨双聚焦质谱仪(HRGC/HRMS)上进行定性和定量检测。在3种不同残留水平的奶粉样品中,17种多氯代二苯并-对二恶英和多氯代二苯并呋喃（PCDD/Fs）的测定结果与给定值具有很好的一致性,且所有具有保证值的二恶英同系物测定结果的相对标准偏差（RSD）均小于20%;12种共平面多氯联苯（PCBs）测定结果的RSD均在15%以内,内标物的回收率为44%～133%,完全符合国际标准方法的要求。母乳样品的国际考核结果表明本方法在不同实验室间具有良好的准确度和精密度。本方法定量准确可靠,适用于乳品中二恶英及共平面PCBs的同时检测。     

Supercritical Fluid Extraction of Bivalve Samples for Simultaneous GC-MS Determination of Polychlorobiphenyls and Polycyclic Aromatic Hydrocarbons

Abstract

A method is presented for the simultaneous determination of polychlorobiphenyls and polycyclic aromatic hydrocarbons in bivalve samples. The method implies the fortification of the freeze-dried sample with isotopically labeled internal standards; followed by extraction with supercritical carbon dioxide modified with 3% methanol, then a simple clean-up step on a silicagel packed Pasteur pipette and, finally, determination by gaschomatography-mass spectrometry. The method requires little time and labor compared to traditional methods, uses negligible amounts of solvents and produces little wastes. Sixty different PCB congeners and seven selected PAHs are analyzed. Six replicate analyses were performed on the SRM 2974 certified material and the results are discussed.     

不同方法提取海岸带沉积物中多氯联苯及有机氯农药测定的比较

针对海岸带沉积物基质的复杂性,以美国国家标准技术研究院研制的海洋沉积物标准样品(SRM 1944)为研究对象,采用气相色谱-电子捕获检测器进行测定。比较了索氏提取、加速溶剂萃取、超声波辅助提取对其中多氯联苯(PCBs)和12种有机氯农药(OCPs)的提取效率。结果表明:索氏提取的回收率在87.9%~104%之间,加速溶剂萃取在80.1%~106%之间,超声波辅助提取在78.6%~93.8%之间,并用实际海岸带浅层沉积物样品进行验证。     

食品纸包装材料中指示性多氯联苯的固相萃取/气相色谱-质谱联用法测定

建立了一种简单、快速测定食品纸包装材料中指示性多氯联苯的分析方法.采用溶剂超声萃取样品,通过C18固相萃取柱、浓硫酸净化后,用气相色谱-质谱联用仪(GC-MS)进行测定.并对不同的萃取溶剂和萃取方法进行了系统地比较,优化了实验条件,方法的回收率为88%～102%,相对标准偏差为3%～7%,定量下限为1.0 μg/kg.     

UV Radiation Exposure of Outdoor Workers in Antarctica

The Antarctic region is a place of increasing interest. A growing number of personnel are working outdoors in extreme environmental conditions. They receive significant exposure to solar ultraviolet radiation (UVR) and are thereby at increased risk of adverse consequences. The aim of this study was to evaluate the UVR dose received by the outdoor workers at the Bulgarian Antarctic Base. Ten Caucasian healthy subjects, 8 males and 2 females with a mean age of 38 years (29–51) were enrolled. Of them, 5 were scientists and 5 were logistic workers. We measured the accumulated daily dose of UVR assessed by standard erythemal dose (SED) in the two groups. All subjects wore personal dosimeters located near the face—he only noncovered skin area. The dosimeters were factory calibrated for use in the Antarctic region. No statistical difference (P = 0.441) could be revealed between the SEDs in the two groups. The maximum UVR dose detected in a single day was 67.9 SEDs, and the highest cumulative dose was 548.03 SEDs. Study results are showing extreme measurements of UVR received by the members of the expeditions. We suggest meticulous UV protection for outdoor workers.     

Neutron activation analysis of snow and ice in Antarctica

In order minimize the possible contamination during storing and pre-treatment of such pure samples as ice and snow collected in Antarctica, trace elements in experimental tools such as bottles, beakers, tubings and filters were determined by neutron activation analysis. By using well certified tools, ice and snow samples from Antarctica and high mountains in China and in Japan were analyzed. Relative concentrations of volatile elements such as Zn, Cd, As, Sb or Ag to Al or Fe which are major components in the earth crust were found to be 10 to 1000 times higher than in the ordinary soil for the samples from Antarctica and Mt. Naimonanyi in China.     

DNA Damage Induced by Late Spring Sunlight in Antarctica

Sunlight ultraviolet (UV) radiation constitutes an important environmental genotoxic agent that organisms are exposed to, as it can damage DNA directly, generating pyrimidine dimers, and indirectly, generating oxidized bases and single-strand breaks (SSBs). These lesions can lead to mutations, triggering skin and eye disorders, including carcinogenesis and photoaging. Stratospheric ozone layer depletion, particularly in the Antarctic continent, predicts an uncertain scenario of UV incidence on the Earth in the next decades. This research evaluates the DNA damage caused by environmental exposure to late spring sunlight in the Antarctic Peninsula, where the ozone layer hole is more pronounced. These experiments were performed at the Brazilian Comandante Ferraz Antarctic Station, at King’s George Island, South Shetlands Islands. For comparison, tropical regions were also analyzed. Samples of plasmid DNA were exposed to sunlight. Cyclobutane pyrimidine dimers (CPDs), oxidized base damage and SSBs were detected using specific enzymes. In addition, an immunological approach was used to detect CPDs. The results reveal high levels of DNA damage induced by exposure under the Antarctic sunlight, inversely correlated with ozone layer thickness, confirming the high impact of ozone layer depletion on the DNA damaging action of sunlight in Antarctica.     

Chlorofluorocarbons Measurement in the Lower Atmosphere of the Antarctica

Abstract

Data concerning chlorofluorocarbons and other halogenated hydrocarbons concentrations in ground-level atmosphere at Antarctica are reported. Measurements were carried out during two campaigns: Austral summer 1989/90 and 1990/91. Samples collected were analyzed in the laboratory by gas chromatography-mass spectrometry and “in situ” by gas chromatography-electron capture detection. Substantial improvements in the instrumentation are also reported where for what trapping and injection of both air samples and calibration mixtures are concerned.     

Trends of volatile chlorinated hydrocarbons and trihalomethanes in Antarctica

In order to understand behaviour and environmental fate of manmade chemicals in remote and cold areas, during the XXVII Italian Expedition carried out in Antarctica throughout the austral summer 2011/2012, superficial snow and lake water were sampled along the Ross Sea's South coast and their content of some low-molecular weight volatile halogenated hydrocarbons was evaluated. In consideration of their important role in stratospheric ozone chemistry, some volatile chlorinated hydrocarbons (VCHCs) and trihalomethanes (THMs) were investigated. The analyses were realised with a dedicated system composed by a purge-and-trap injector coupled to a gas chromatograph with a mass spectrometer (PTI-GC-MS) operating in SIM mode. The investigated VCHCs (chloroform; 1,1,1-trichloroethane; tetrachloromethane; trichloroethylene and tetrachloroethylene) were present in all analysed samples, and concentration levels ranged from units to hundreds of ng L^?1 according to considered matrix. For the first time, THMs (bromoform; dibromochloromethane; bromodichloromethane), were measured in Antarctic lake waters and freshly deposited snow; their concentration levels ranged from units to tens of ng L^?1. In order to assess eventual temporal variations, VCHC content in aqueous Antarctic matrices was compared with levels occurring in the past Italian Antarctic expeditions: for some banned substances, a decrease in concentration was observed, probably due to worldwide use restrictions. Finally, current Antarctic and Italian VCHC and THM levels in snow and lake water samples were compared and were found to be quite similar, differing at most by one order of magnitude, corroborating the hypothesis of an accumulation of halogenated compounds in Antarctic aqueous matrices.     

A Rapid Method for the Determination of Organochlorine, Pyrethroid Pesticides and Polychlorobiphenyls in Fatty Foods Using GC with Electron Capture Detection

A new, single-step extraction and purification method was developed for the separation of 26 organochlorine pesticides (OCPs), three pyrethroid pesticides (PPs) and six polychlorinated biphenyls (PCBs) from fatty foods of either animal or vegetable origin. The method includes homogenisation of extracted fat and diatomaceous earth. Separation was achieved using a mini Pasteur pipette where a matrix solid-phase dispersion extraction was carried out with only 5 mL of dimethyl sulphoxide as an eluting solvent. A Pasteur pipette was joined to a prepacked slurry filled Florisil column, water deactivated to 15% where a liquid–liquid extraction and adsorption chromatography successively took place. The elution of OCPs, PPs and PCBs was performed with n-hexane/diethyl ether. Recoveries for PCBs were from 81 to 86% and for OCPs 68 to 94%, except for β-HCH, which gave lower, more variable recoveries. Excellent recoveries were obtained for pyrethroid pesticides, mostly more than 80%. The method was applied to 509 fatty samples for monitoring of these compounds. GC, with two columns connected to two electron capture detectors (ECD), was used.