Separation and Quantitation of Urinary Phthalates by HPLC

Abstract

A method was developed for the separation and quantitation of plasticizers and their metabolites from human urine using HPLC, Urine was diluted with an equal volume of water and extracted at pH 2.0 with diethyl ether, The extract was dried, the solvent vacuum stripped, and the residue dissolved in methanol for injection into the chromatograph. A C₁₈ reverse phase column containing 10 μ particles was used for the analysis. Ionic suppression, 0.5% acetic acid in water, at pH 3.0 was used to resolve the acidic components. A step gradient of acetonitri1e:water (containing acetic acid) was used to elute the polar metabolites as well as the non-polar plasticizers. Mass spectrometry was used t o identify the compounds in the HPLC fractions. From the HPLC fractions of the urine extract collected, phthalic acid, MEHP, DEHP and normal urinary constituents (e.g., hippuric and benzoic acid derivatives) were identified     

石墨炉原子吸收光谱法测定硬聚氯乙烯饮水管中痕量锡

本文按标准GB／T10002．1－1996方法前处理样品,硝酸钙作基体改进剂,使锡的灰化温度提高并消除干扰。方法简便,快速,准确,灵敏度和精密度高,相对标准偏差为4．55％,回收率在90％－104％范围内。     

STUDY ON THE MORPHOLOGY OF POLYVINYL CHLORIDE/POLYSTYRENE BLENDS BY ELECTRON MICROPROBE ANALYSIS*

The morphology of polyvinyl chloride/polystyrene (PVC/PS) blend samples with different mass ratios, preparedby means of solution casting and melt mixing, have been successfully examined by electron microprobe analysis (EMP). Thisexperiment was performed in a scanning electron microscope attached to an energy dispersive X-ray analyzer. Differentialscanning calorimetry was also used to investigate the phase separation of the blends. The results show that PVC and PS areincompatible and the blends have sea-islands phase structures. Blends prepared via melt mixing have finer phase-dispersionthan those prepared via solution casting.     

One-pot polyvinyl chloride preparation utilizing polyacrylate latex with tertiary amine groups for improved thermal stability,toughness, and reduced reactor scaling

In this paper, crosslinked polyacrylate latex with tertiary amine groups (ACLN) and base latex without tertiary amine groups (ACL) were prepared by emulsion polymerization using butyl acrylate as the monomer and 1,4-butanediol dimethacrylate as the crosslinker. Composite resins of polyvinyl chloride (PVC), ACL/PVC and ACLN/PVC, were prepared by suspension polymerization of vinyl chloride in a 20 L high-pressure reactor by adding ACL and ACLN as modifiers. The inner pressure of the reactor and initiator concentration as a function of reaction time during suspension polymerization were studied. Morphology of resin particles, processing properties, thermal stability and mechanical properties of ACL/PVC and ACLN/PVC products were investigated. A commercial PVC product named PVC-SG5 was used as the control sample for comparison. It was found that compared with typical PVC-SG5 preparation, ACL/PVC fabrication took less time while initiator concentrations needed to be increased to 2400 ppm in ACLN/PVC preparation in order to complete the polymerization within the same time. Reactor scaling occurred during ACL/PVC preparation, but could be avoided in ACLN/PVC preparation owing to the hydrophilicity of ACLN. The morphology of ACL/PVC and ACLN/PVC particles was smooth microspheres and mosaic particle shapes, respectively, the diameter of which were all smaller than PVC-SG5 particles. The covalent-bonding existing in ACL/PVC and ACLN/PVC, and ionic-bond formation of quaternary ammonium in ACLN/PVC composite resins, between tertiary amine groups in ACLN and chlorine atoms in PVC, contributed to the dramatic increase in thermal stability. ACLN/PVC exhibited the shortest plasticizing time and the longest elongation at break, followed by ACL/PVC. The toughness of both ACL/PVC and ACLN/PVC were greatly enhanced without affecting the tensile strength and softening temperature of the resin. Thus, three issues, namely, low thermal stability, low toughness and reactor scaling during polymerization of PVC have been comprehensively solved by introducing ACLN to PVC through a one-pot method.     

Electrical conduction mechanism of polyvinyl chloride (PVC)-polymethyl methacrylate (PMMA) blend film

The electrical conduction mechanism in polyvinyl chloride (PVC)-polymethyl methacrylate (PMMA) blend film has been studied at various temperatures in the range 313 K to 353 K. The results are presented in the form of I-V characteristics. Analysis has been made in the light of Poole-Frenkel, Fowler-Nordheim, Schottky, log(J) vs. T plots and Arrhenius plots. It is observed that, Schottky-Richardson mechanism is primarily responsible for the observed conduction.      

Studies on the Diisocyanate-Modified Polyvinyl Alcohol Reverse Osmosis Membranes

The hydroxyl group in polyvinyl alcohol (PVA) membranes had been partially reacted with diisocyanates such as 4,4′-diphenylmethane diisocyanate (MDI) or the prepolymers containing different functional groups. The transport properties toward water and salt and the stress-strain properties of these modified membranes were investigated. The results showed an improvement in salt rejection and a considerable increase in the wet strength of the modified membrane. The water absorption and permeabilities of these modified membranes depended largely upon the functional groups introduced into them.     

Thermally stable and flame-retardant poly(vinyl alcohol)/montmorillonite aerogel via a facile heat treatment

The PVA/MMT aerogels prepared by a simple freeze-drying and heat treatment process exhibited a significant improvement of thermal stability and flame retardant property.     

Highly sensitive potentiometric immunosensor for hepatitis B surface antigen diagnosis

Immunosenors are of great interest because oftheir potential utility as specific, simple, label-free anddirect detection techniques and reductions in size, costand time of analysis compared with conventional im-munoassay techniques. The immunoassays with …     

含有稠环侧链的聚硅氧烷的合成及其对加成型高温硫化硅橡胶性能的影响

将含有多乙烯基的聚硅氧烷与菲式环戊二烯酮和苊式环戊二烯酮分别在α-氯萘中进行Diels-Alder反应,生成含有稠环侧链的聚硅氧烷.该聚硅氧烷具有较好的耐热性.将其作为组分制成高温加成型硅橡胶,综合性能达到较高水平(高模量).随着其用量的增加,可使其耐热性能得到较大改善。     

聚乙烯醇用于碳纳米管的开口及修饰研究

在低温(250 ℃)下,用聚乙烯醇(polyvinyl alcohol, PVA)和提纯后的碳纳米管(carbon nanotubes, CNTs)的混合物在空气中加热,以研究聚乙烯醇对碳纳米管的修饰作用,并采用TEM对不同条件下所得的产物进行了形态分析.结果发现,碳纳米管的顶端被打开,随着时间的增加,弯曲的碳纳米管断裂成较短的碳纳米管.聚乙烯醇对碳纳米管的氧化及修饰在实验中得到证实.讨论分析了氧化和修饰机理,认为可能是聚乙烯醇在空气中分解所得的产物的一种或几种在氧化和修饰过程中起主要作用.