Speciation of antimony in polyethylene terephthalate bottles

Antimony contamination has been reported in drinking water from polyethylene terephthalate (PET) bottles. Micro‐X‐ray fluorescence (XRF) analysis has been used to identify the distribution and chemical form of residual antimony used as a catalyst in the manufacture of PET bottles. The results are consistent with clusters of Sb(III) having dimensions of the order of tens of micrometers, clearly showing the ability of synchrotron radiation analyses to both map elemental distribution and determine oxidation state. Copyright © 2010 John Wiley & Sons, Ltd.     

Evaluating radon loss from water during storage in standard PET,bio-based PET,and PLA bottles

Polyethylene terephthalate (PET) and polylactic acid (PLA) bottles were tested to evaluate radon loss from water during 15 days of storage. PET bottles (lower surface/volume-ratio vials) lost 0.4–7.1% of initial radon, whereas PLA bottles lost 3.7% of it. PET bottles with volume of 0.5 L, lower surface/weight ratio, and hence higher thickness display proportionally reduced radon loss. Corrections for dissolved radium are needed during analyses. Formulas for calculating degassing efficiency and water interference on electrostatic collections are developed.     

Carbonized waste for the cut-down of environmental pollution with heavy metals

Nowadays, an increasing concern about the treatment and disposal of waters contaminated by toxic heavy metals is noticed. The toxic pollutants must be removed from the sewage water which then is fed back into the materials cycle. Any candidate technology should result in reusable by-products. With this in mind, the aim of the present study is to test a low cost procedure for utilization of the carbonized waste, a product of PET (polyethylene terephthalate) bottles pyrolysis on sand bedding, for this purpose. Both the water present in PET bottles waste and combustion exhaust probably contribute to the conversion of carbon char to activated carbon directly within the pyrolysis oven. Preliminary results, obtained for several heavy metal ions under laboratory conditions are presented and discussed. Adsorption of heavy metals on the carbonized PET waste is tested by both the electrochemical methods and X-ray fluorescence spectrometry. A simple desorption procedure for the regeneration of prepared active carbon is proposed.     

石墨炉原子吸收光谱法快速测定塑料饮水管浸出液中的痕量锑

采用铜作基体改进剂、横向塞曼扣背景石墨炉原子吸收光谱法快速测定塑料饮水管浸出液中痕量锑。对石墨炉加热程序中的灰化温度和原子化温度进行了优化 ,同时也研究了介质酸度的影响。选定了最佳测量条件 ,提高了方法的灵敏度和精密度。本方法的线性范围为 0 2 7～ 2 0 0 μg·L-1 ,工作曲线回归方程为Y=0 0 0 6 8X - 0 0 0 0 2 ,相关系数r=0 9996 ,特征质量为 6 7pg ,最低检测量为 5 4pg ,回收率在 92 2 %～1 0 2 5 %。对 5 0 ,1 0 0 ,2 0 0 μg·L-1 锑的标准溶液连续测定 6次 ,相对标准偏差分别为 6 4 7% ,4 97% ,2 4 5 %。结果表明 ,该方法简便、快速、灵敏、重现性好、准确度高 ,用于实际样品分析结果满意     

ICP-AES结合SVDV技术应用于饮用水品质检测性能诊断

采用电感耦合等离子体原子发射光谱(ICP-AES)技术,通过轴向、径向、同步垂直双向(SVDV)三个视角配置,快速检测生活饮用水样本中的As,Ba,Mg和Ni等微量元素。ICP-AES光谱仪在三个检测视角均能实现快速预热,预热时间仅需2 min,而且,ICP-AES光谱的短期稳定性和长期稳定性表现良好,其相对标准偏差(RSD)均低于2%。以3份商业瓶装饮用水和2份添加标准物的饮用水为检测的对象,利用ICP-AES技术结合SVDV视角,分别从轴向和SVDV两个视角检测As,Ba,Cr,Cu,Mn,Mo,Ni,V和Zn等元素,利用水微量元素含量的国家标准来验证结果的准确性,这两个视角的检测具有较高的准确度和灵敏度。检测所得结果符合国家环境保护总局发布的饮用水微量元素限制标准,并符合国际卫生组织的标准,满足人类所需饮用水标准要求。     

高效液相色谱法同时测定环境水中5种邻苯二甲酸酯

建立了萃取-高效液相色谱法对环境水样中的5种邻苯二甲酸酯类化合物(PAEs)[邻苯二甲酸二甲酯(DMP),邻苯二甲酸二乙酯(DEP),邻苯二甲酸二丁酯(DBP),邻苯二甲酸二辛酯(DOP),邻苯二甲酸二(2-乙基己基)酯(DEHP)]同时进行定量分析的方法。最佳色谱条件:色谱柱:Agilent-C18(250mm×4.6mm,5μm);流动相:甲醇:水(V/V)=80:20(0—10min)—90:10(10—35min);流速:1.0mL/min;紫外检测器,检测波长:280nm。该方法加标回收率在99.00%—100.43%之间,相对标准偏差小于5%。     

Surface modification of low cost carbons for their application in the environmental protection

In this work, the CO₂ capture capacity of a series of activated carbons derived from recycled polyethylene terephtalate (PET) was tested, facing two problems at the same time: minimising plastic waste and developing an adsorbent for CO₂ capture. The PET raw material, obtained from post-consumer soft-drink bottles, was chemically activated with KOH. In addition, a series of nitrogen-enriched activated carbons was obtained by mixing the raw material with different nitrogen compounds (i.e., acridine, carbazole and urea). The influence of temperature on the CO₂ capture capacity of the adsorbents was evaluated in a thermogravimetric system. The CO₂ uptake was also related to the chemical and textural characteristics of the samples.     

Argon ion beam interaction on polyethylene terephthalate surface by a 4 kJ plasma focus device

Polyethylene terephthalate (PET) has a wide variety of applications ranging from making regular bottles to biosensors. However, for many of these applications, surface treatment is needed to improve its surface characteristics such as adhesion to other materials. In this study, we focussed on treating PET foils by dense Ar pulsed plasma produced by a 4.5 kJ Mather-type plasma focus device (20 kV, 40 µf, 115 nH) to examine its ability to make the PET surface hydrophilic. The most common method to examine this characteristic is measuring the water contact angle on a polymer surface. The results show that while the energy and density of plasma in our device are higher compared to other devices, as the exposure time is very low, the device can enhance the wettability of PET film surfaces.     

An Indirect Competitive Fluorescence Immunoassay for Determination of Dicyclohexyl Phthalate in Water Samples

A sensitive and specific indirect competitive fluorescence immunoassays (FIA) has been developed for the quantitative determination of dicyclohexyl phthalate (DCHP) using an antigen-coated plate format. The polyclonal antibodies raised against dicyclohexyl 4-amino phthalate conjugated to bovine serum albumin (BSA) by the amino diazotization linkage method. Antiserum with a sufficiently high titer was generated in rabbits and fluorescein isothiocyanate (FITC) was used as sensitive labels to construct the fluorescence immunoassay (FIA) for measurement of targeted compounds. Under optimized FIA condition, the quantitative working range was from 0.1 to 200 μg L⁻¹ with a limit of detection of 0.05 μg L⁻¹. Other similar phthalate compounds do not interfere significantly in the analysis using this immunoassay technique, and the cross-reactivity rates were less than 10%. Four kinds of water samples (tap water, lake water, river water and leachate) had been detected in this assay, the recovery was 91.3–107.8%. The proposed fluorescence immunoassay turned out to be a powerful tool for monitoring of dicyclohexyl phthalate in water samples at trace level.     

A method for the determination of residual beta activity in drinking water samples

The determination of residual beta activity in drinking water is usually needed in most monitoring programs. In this work a procedure for its determination is described and expressions for the calculations of detection limits and uncertainties are proposed.     

基于苯溶剂化效应的多种邻苯二甲酸酯(PAEs)拉曼特征振动光谱辨识

利用密度泛函与自洽反应场理论在B3LYP/6-311G(d)水平下对16种邻苯二甲酸酯(PAEs)进行结构优化,并计算气态环境及溶剂中PAEs的拉曼光谱振动频率和去偏振度。研究显示,16种PAEs拉曼振动归属为苯环变形、酯基振动、C—C伸缩、C—H摇摆、C—H伸缩与耦合振动。其中酯基官能团出峰位置在1 700~1 780cm-1之间,拉曼峰较强,去偏振度较低(振动的对称性较强),可将酯基振动作为特征振动;但气态环境下仅12种PAEs拉曼峰之间的最小波数差大于显微拉曼光谱仪的检出限(0.2 cm-1),即利用酯基频区的去偏振度和拉曼峰不能完全辨识16种PAEs。溶剂化效应分析显示,溶剂苯对16种PAEs具有明显的溶剂化增强效应,16种PAEs拉曼峰之间最小波数差均增大到0.2 cm-1以上,且峰强增加了23%~183%,说明溶剂化效应下可利用酯基频区的去偏振度和拉曼峰辨识16种PAEs。本文的研究结果为PAEs拉曼光谱检测提供了理论依据。     

Trace elemental determination by portable total reflection X‐ray fluorescence spectrometer with low wattage X‐ray tube

A specimen containing nanograms of Sb, rare earth elements, Pb, and Bi and a specimen containing a few nanograms each of As and Pb were measured using a portable total reflection X‐ray fluorescence spectrometer. Nanograms of Sb, rare earth elements, Pb, and Bi were detected. Although the As Kα line (10.54 keV) overlapped with the Pb Lα line (10.55 keV) in a spectrum of the specimen containing nanograms of As and Pb, the Pb Lβ line was detected. Therefore, the net intensity of the As Kα line was calculated using the Pb Lα/Lβ intensity ratio in a spectrum of a Pb standard solution and the net intensity of the Pb Lβ line in the spectrum of the specimen containing As and Pb. This result indicates that these two elements can be quantified by using the portable spectrometer. Commercially available bottled drinking water was also measured. The portable spectrometer detected several tens of ppb of V in the drinking water sample. Copyright © 2013 John Wiley & Sons, Ltd.     

气动雾化进样-微波等离子体炬全谱仪测定矿泉水中的Na,Mg, Ca,Li, Sr

采用微波等离子体炬(MPT)作为激发光源,通过气动雾化系统进样,循环水冷凝-浓硫酸吸水装置作为去溶系统,以Ar为等离子体工作气体,建立了氩微波等离子体炬全谱仪检测矿泉水中Na, Mg, Ca, Li和Sr等五种元素的方法。详细探究了微波功率源功率、工作气流量及载气流量等实验参数对待测元素发射信号的影响,并且对这些参数进行了优化。在优化的实验条件下,对11种瓶装饮用矿泉水进行了检测,方法对Na, Mg, Ca, Li和Sr的检出限分别为4.4,21,56,11和84 μg·mL-1,相对标准偏差范围为1.30%～5.45%(n=6),加标回收率在84.6%～98.5% 之间。实验结果表明,此装置简单便捷、分析成本低;此方法分析速度快、精确度与准确度高、能够同时测定多种元素,适用于矿泉水中元素检测,为打击非法商家提供了手段,同时也为人们的饮用水质量提供了安全保障,有望用于食品安全、药品安全、临床诊断及更多领域的分析检测。     

ICP-MS在土壤元素污染评价中的应用

以云浮黄铁矿矿石作原料的某硫酸厂堆渣场土壤剖面为研究对象, 应用ICP-MS同时测定了污染元素和部分参考元素的含量,快速找出各元素的相关性,用富集因子评价了土壤的污染状态,并指出了污染元素的背景选择问题。结果表明：V已呈显著及高度污染,Co呈中度污染,并有显著污染的倾向,Cr, Mo和Cd在轻度和中度污染之间,Zn和Sb呈轻度污染,并有中度污染的潜在危险,Cu呈轻度污染。富集的高位点V和Cr在土壤剖面的上部(4.0～10. 5 cm)和深部(44.0～75. 5 cm),Co和Mo集中在土壤剖面表面(0～5.0 cm)、中上部(9.5～10.5 cm)和中部(29.5～46.0 cm),Cd和Cu集中在土壤剖面中部(29.5～46.0 cm)。高富集点的污染来自于以花岗岩为母质的亚热带强风化红壤的残余金属离子的淋溶淀积和堆渣场废渣中释放的金属元素在土壤中的迁移累积相互叠加的结果。其中V污染主要为土壤母质贡献,其次是硫酸生产过程失活催化剂挥发引入废渣的V淋溶淀积。     

Establishment of a method for measurement of gross alpha/beta activities in water from Vojvodina region

Very important part of environmental studies is the determination of the quality of drinking water, which often requires measuring of alpha and beta activity in analyzed water samples. The usual method for monitoring of low-level α and β radioactivity is to use gas-proportional detectors where ionization and proportional regions are used for α and β counting, respectively Simultaneous measurement of gross alpha and gross beta activities by liquid scintillation counting technique using Quantulus 1220 liquid scintillation counter (LSC) equipped with Pulse Shape Analyzer (PSA) is described. Water samples were prepared for measurements according to the ASTM D 7283-06 Standard Test Method. More than 50 samples of drinking water from Vojvodina region were measured. The data obtained can provide important information for the consumer regarding the preliminary dose exposure risk due to water intake.     

Hydrothermal decomposition of esters under high pressure

Abstract

The hydrothermal decomposition of two esters (methyl formate and ethyl formate) was studied in the absence of oxygen over the temperature range of 373 – 673 K at pressures from 15 to 35MPa for residence times between 72 and 600s. At hydrothermal conditions, the esters were hydrolyzed to formic acid and the corresponding alcohols in equilibrium yields of more than 90%, and the disappearance rate of ester was more promoted with increasing temperature than with increasing pressure. In supercritical water, the conversion of the esters reached 100% at short times. From reaction experiments with various catalysts, it was found that the hydrolysis of alkyl formates was accelerated by acid, while retarded by base in a manner different from that in usual water. In addition, a delayed reaction start observed in ester disappearance. profiles suggested strongly a catalytic action of formic acid produced by hydrolysis.     

ICP-AES同时测定水中的痕量钼、钴、硼、锑、钒和钛

采用ICP-AES同时测定水中的痕量钼、钴、硼、锑、钒、钛等6种元素。结果表明,各元素检出限为1.5—13μg.L^-1,满足饮用水及其水源水分析要求;空白加标回收率为94.2%—105%,样品加标回收率为90.6%—98.8%,相对标准偏差（n=9）〈2.40%。该方法简便、高效、快速、线性范围宽,适于饮用水及其水源水质分析。     

分光光度法研究Sb(Ⅲ)的三元缔合物与Ce(Ⅲ)、Zr(Ⅳ)和U(Ⅵ)的浮选分离

在水溶液中,Sb(Ⅲ)与四丁基溴化铵和碘化钾形成不溶于水的三元缔合物[SbI4][TBAB],此三元缔合物沉淀浮于盐水相上层形成界面清晰的液-固两相。当四丁基溴化铵和碘化钾的浓度分别为4.0×10-4mol/L和6.0×10-3mol/L时,在pH1.6的克拉克-鲁布斯缓冲溶液中,Sb()的浮选率达到100%。而Ce(Ⅲ)、Zr(Ⅳ)和U(Ⅵ)离子在该体系中不被浮选,实现了Sb(Ⅲ)与这些金属离子的定量分离。对合成水样中Sb(Ⅲ)的分离和测定,结果满意。该方法具有简便、快速等特点,在微量锑的分离和富集分析中有一定的实用价值。     

轻质萃取剂的分散液液微萃取-石墨炉原子吸收光谱法测定生活用水中痕量Pb与Cd

以轻质溶剂辛醇为萃取剂,建立了分散液液微萃取-石墨炉原子吸收光谱分析法(LDS-DLLME-GFAAS),并应用于生活用水中痕量Pb及Cd的测定。在分散液液微萃取(DLLME)中,以二乙基二硫代氨基甲酸盐(DDTC)为螯合剂,用微量注射器将辛醇和甲醇的混合溶液快速注入到样品溶液中发生雾化分散现象,Pb2+和Cd2+与DDTC的络合物被萃取到辛醇微滴中。离心分离后,以GFAAS测定萃取至上层辛醇相中的分析物。实验考察了萃取剂种类和体积、分散剂种类和体积、pH、DDTC浓度、萃取时间等影响萃取效率的实验参数。在最优实验条件下,Pb和Cd的检出限分别为0.15和0.03 μg·L-1,富集倍数分别为87和48,具有良好的线性和精密度。该分析方法优势在于操作简便,快速,低成本,高富集倍数,萃取剂用量少,已成功应用于自来水、饮用水和南湖水中痕量Pb和Cd的检测。     

Lipase-ultrasound assisted synthesis of polyesters

Poly (ethylene glutarate), poly (ethylene malonate) and poly (ethylene phthalate), were enzymatically synthesized by immobilized Candida antarctica lipase B in solvent free conditions. The synthesis of these polyesters was based on the ester-ester exchange reaction between ethylene glycol diacetate and di-ethyl glutarate, di-benzyl malonate, di-n-octyl phthalate to produce poly (ethylene glutarate), poly (ethylene malonate) and poly (ethylene phthalate), respectively. The effect of ultrasound and PET polymeric beads was evaluated and showed to improve the synthesis of all polyesters. Ultrasound, as a green solvent-free technology, showed high potentiality for the polyester synthesis intensification.