Comprehensive branching analysis of polyethylene by combined fractionation and thermal analysis

Linear low density polyethylene (LLDPE) and low density polyethylene (LDPE) differ significantly in their branching types and branching distributions. For a comprehensive analysis, preparative temperature rising elution fractionation and/or preparative molar mass fractionation are used to fractionate typical LLDPE and LDPE bulk resins into narrowly distributed fractions. The chain structures of the bulk resins and their fractions are further analysed using SEC, crystallization analysis fractionation, DSC and high‐temperature HPLC to provide detailed information on short chain branching in LLDPE and long chain branching in LDPE. For LDPE it is shown that the multiple fractionation approach is a powerful source of sample libraries that may have similar molar masses and different branching structures or alternatively similar branching but different molar masses. The analysis of these library samples by thermal analysis provides a much deeper insight into the molecular heterogeneity of the samples compared to bulk sample analysis. © 2018 Society of Chemical Industry     

硫脲浸出液活性炭负载洗脱研究

从硫脲浸出液中活性炭负载洗脱金是比较困难的,目前在这方面发表的文献并不很多。本文着重研究并讨论了从负载活性炭上洗脱金的不同方法,包括酸性硫脲有机溶液和非有机洗脱液。研究了丙酮、乙腈、丁醇、乙二醚和乙醇5种有机溶剂。研究了不同的硫脲、硫酸和有机溶剂的浓度和温度对洗脱的影响。试验表明了这5种有机溶剂对金的洗脱能力按如下顺序排列: 丁醇>乙腈>乙二醚>乙醇>丙酮当采用5%丁醇,50～100g/L硫脲和50～100g/L硫酸,温度40～60℃时,金的洗脱率可达98～99%,此时活性炭含金降至0.10mg/g以下。对于非有机洗脱液,像硫化钠和硫代硫酸钠,研究表明金的洗脱率主要取决于溶液的浓度和温度,在室温时,1～2mol的硫化钠溶液可以洗脱99%的金。如果溶液的浓度降低至0.5mol,则温度需升至80℃以上才可能获得相同的洗脱率。     

Concentration du virus de l'hepatite a sur des membranes de celluloseHepatitis a virus concentration on cellulose membranes

Viral hepatitis type A is the most prevalent waterborne disease in U.S.A. and the number of cases has been increasing in recent years (Melnick et al., 1978). Till now, few works were performed on Hepatitis A Virus (HAV) concentration in water (Hejkal et al., 1982, Elkana et al., 1983). In this paper the filter adsorption-elution method, widely used with other viruses (Wallis and Melnick, 1967; Fields et Metcalf, 1975; Smith and Gerba, 1982), was selected to concentrate HAV from experimentally-contaminated distilled water. Filtration was performed through two cellulose membranes (RAWP 04700 and HAWP 04700 Millipore). Eluate or filtrate viruses were precipitated by polyethylene glycol 6000. HAV is detected by solid phase radioimmunoassay according to a previously described method (Deloince et al., 1982). Figure 1 shows the results of adsorbing HAV at different pH levels. Analysis of variance pointed out that, for the pH levels between 3 and 4, the differences were not significant (P = 0.05). Table 1 shows the effects of pH and number of passages of 3% beef extract or 0.2 M glycin buffer on HAV elution. For both eluents the differences in function of pH levels and number of passages of eluent through the membrane were not significant (variance analysis P = 0.05). On the other hand, the comparison between the two eluents pointed out the higher efficiency of beef extract (t-test, P = 0.001). After this procedure, HAV replication occurred in human hepatocarcinoma cells PLC/PRF/5 (Fig. 2) inoculated according to a previously described method (Crance et al., 1983). As poliovirus (Sobsey et al., 1973), HAV adsorption is the most efficient at acid pH levels. Between pH 4.5 and 5, the remarkable adsorption decrease might be related to the inversion of the HAV electrostatic charges sign, i.e. to the occurrence of an isoelectric point. The HAV elution is different from the poliovirus one, the efficiency of which increased with pH (Wallis et al., 1972) and eluent passage numbers (Farrah et al., 1976). That might suggest that from pH 7.5, both the HAV particles and membranes have negative charges which give enough repulsive forces to allow a good elution efficiency. Improvement of HAV elution efficiency by beef extract is similar to a result obtained with poliovirus by Landry et al. (1978). This effect might be explained by the proteinous material presence in beef extract. HAV replication in cell cultures shows the biological properties preservation after this procedure.     

HPLC法同时测定化妆品中的12种防腐剂

建立了化妆品中12种常用防腐剂(甲基氯异噻唑啉酮、2-溴-2-硝基丙烷-1,3-二醇、甲基异噻唑啉酮、苯甲醇、苯氧乙醇、苯甲酸、4-羟基苯甲酸甲酯、4-羟基苯甲酸乙酯、4-羟基苯甲酸异丙酯、4-羟基苯甲酸丙酯、4-羟基苯甲酸异丁酯、4-羟基苯甲酸丁酯)的HPLC检测方法。采用Waters symmetry(250 mm×4.6 mm×5μm)色谱柱,流动相为乙腈-0.1%(体积分数)磷酸,梯度洗脱,柱温35℃,DAD检测器,以各物质的紫外光谱数据和保留时间定性。检测波长设定为:甲基氯异噻唑啉酮和甲基异噻唑啉酮在280 nm检测,其余成分在254 nm检测。结果发现,在所建立的方法下,12种防腐剂的分离度良好、线性范围广、准确度高。     

HAP合成中交换树脂与羟胺离子交换的影响因素

为寻找适宜合成高氯酸羟胺(HAP)的离子交换树脂,对不同交联度、不同形态的强酸性阳离子交换树脂与羟胺交换过程进行了研究,发现了树脂与羟胺交换的主要影响因素,优选出适宜合成HAP的交换树脂为001×7型。根据流出曲线计算了不同条件下硫酸羟胺(HAS)加料系数的取值范围,并讨论了HAS浓度及流速对交换过程的影响,确定HAS的较佳加料系数为1.2。     

Selective elution of tea catechins and caffeine from polyvinylpolypyrrolidone

Desorption of catechins and caffeine from polyvinylpolypyrrolidone (PVPP) was comprehensively investigated. The result showed that caffeine could easily be desorbed from PVPP by the tested solvents except n‐hexane, while catechins could only be thoroughly done by dimethyl sulphoxide (DMSO) and N, N‐dimethylformamide (DMF). Excellent desorption efficiency of DMSO and DMF might be attributed to their high dipole moments and H‐bond potentials. Addition of ethanol was recommended considering the elution efficiency and fluidity, but ethanol volume should be <40% (v/v) for DMSO or 20% (v/v) for DMF. Desorption would get to equilibrium within 1 h and followed the pseudo‐second‐order model. Caffeine and catechins could be separately desorbed through two‐stage elution procedure, that is, water or 20% aqueous ethanol for desorbing caffeine and part of nongalloylated catechins and DMSO/ethanol (8/2, v/v) for eluting the remaining catechins. Highly purified catechins (~95%) with high level (~70%) galloylated catechins would be achieved when the desorption procedure was applied in column chromatograph.     

Evaluation of Elution Parameters for Cesium Ion Exchange Resins

Abstract

Cesium ion exchange is one of the planned processes for treating and disposing of waste at the U.S. Department of Energy Hanford Site. Radioactive supernatant liquids from the waste tanks will undergo ultrafiltration, followed by cesium ion exchange using a regenerable organic ion exchange resin. Two resins, SuperLig^®644 and a resorcinol‐formaldehyde resin, are being evaluated for cesium removal and cesium elution characteristics. The main purpose of this study is to optimize the cesium elution to provide a resin that, after undergoing elution, would meet the U.S. Department of Energy/Office of River Protection Project‐Waste Treatment Plant processing and resin disposal criteria. Columns of each resin type were loaded to greater or equal to 90% breakthrough with a Hanford waste stimulant and eluted with nitric acid. The temperature, flow rate, and nitric acid concentration were varied to determine the optimal elution conditions. Temperature and eluant flow rate were the most important elution parameters. As would be predicted based upon kinetic consideration alone, decreasing the eluant flow rate and increasing the temperature provided the optimal elution conditions. Varying the nitric acid concentration did not have a significant effect on the elution completion; however, elutions performed using both high acid concentration (1 M) and elevated temperature (45°C) resulted in resin degradation, causing gas generation and resin bed disruption.     

Interpolymer radical coupling: A toolbox complementary to controlled radical polymerization

The current review focuses on the relevance and practical benefit of interpolymer radical coupling methods. The latter are developing rapidly and constitute a perfectly complementary macromolecular engineering toolbox to the controlled radical polymerization techniques (CRP). Indeed, all structures formed by CRP are likely to be prone to radical coupling reactions, which multiply the available synthetic possibilities. Basically, the coupling systems can be divided in two main categories. The first one, including the atom transfer radical coupling (ATRC), silane radical atom abstraction (SRAA) and cobalt-mediated radical coupling (CMRC), relies on the recombination of macroradicals produced from a dormant species. The second one, including atom transfer nitroxide radical coupling (ATNRC), single electron transfer nitroxide radical coupling (SETNRC), enhanced spin capturing polymerization (ESCP) and nitrone/nitroso mediated radical coupling (NMRC), makes use of a radical scavenger in order to promote the conjugation of the polymer chains. More than a compilation of macromolecular engineering achievements, the present review additionally aims to emphasize the particularities, synthetic potential and present limitations of each system.     

阳离子树脂净化铂族金属溶液的研究

研究了阳离子交换树脂净化含大量贱金属的铂族金属溶液的工艺条件,结果表明,在p H=1~1.5时001×7阳离子交换树脂吸附贱金属的次序为:NiCuCoFe;Fe、Ni、Co、Cu的穿透容量分别为(g/kg):0.13,1.25,0.42,0.87;饱和容量分别为(g/kg):0.32,6.65,2.33,4.72,合计为14.02 g/kg;贱金属的分离效率主要取决于贵贱金属浓度及交换柱的数量;吸附在树脂上的贱金属极易被6 mol/L HCl洗脱,所有贱金属的最大洗脱均发生在洗脱液体积与床体积之比为1.0/1.7处,当洗脱液体积为床体积的2.0倍时贱金属被完全洗脱。实验结果为离子交换分离贱金属净化铂族金属溶液的工业化应用提供了强有力的理论依据。     

脉冲淋洗塔树脂移动自动控制系统中PLC的应用研究

介绍PLC在脉冲淋洗塔树脂移动自动控制系统中的应用，较系统地阐述了控制系统的设计原理及软硬件组成。