Sensor-containing microspheres of chitosan crosslinked with 8-hydroxyquinoline-5-sulphonic acid for determination of Cu(II) in instant coffee

A novel carbon paste electrode containing chitosan microspheres for the determination of Cu(II) in instant coffee by anodic stripping voltammetry was developed. Chitosan was crosslinked with the chelating agent 8-hydroxyquinoline-5-sulphonic acid and glutaraldehyde. The microspheres of the crosslinked chitosan biopolymer were obtained by the spray drying technique and employed in the construction of the sensor. In acetate buffer solution (0.1 mol L⁻¹, pH 6.0), the calibration curve obtained was linear for concentrations of 5.0 × 10⁻⁷ to 1.4 × 10⁻⁵ mol L⁻¹ (r = 0.9990); the detection limit was 5.5 × 10⁻⁸ mol L⁻¹. The relative standard deviation (n = 8) was lower than 3.0% for solutions containing 6.0 × 10⁻⁶, 5.0 × 10⁻⁵ and 1.5 × 10⁻⁴ mol L⁻¹ of Cu(II). The method was successfully employed for determination of Cu(II) in instant coffee and the results obtained showed good agreement when compared with those using electrothermal atomic absorption spectrometry.     

磁性壳聚糖微球固定化脂肪酶研究

以磁性壳聚糖微球为载体,通过戊二醛交联进行脂肪酶固定化,对影响脂肪酶固定化各种因素进行考察,确定最佳条件,并比较游离酶与固定化酶pH和热稳定性。结果表明,固定化适宜条件为:脂肪酶加入量5.0 mg/100 mg载体、温度40℃、时间5 h、pH 8.04、戊二醛浓度10%、最高固载率可达90.56%,酶活4034 U/g载体;与游离酶相比,固定化酶pH和热稳定性都有较宽适用范围。     

因子设计-效应面法优化交联淀粉微球的合成工艺

为了优化用反相悬浮法合成了新型交联淀粉微球(CSM) 的工艺,采用效应面法(RSM)分析交联荆质量分数、反应温度和引发剂浓度对于 CSM 品质(产率和溶胀度)的影响,并建立了相应的预测模型.方差分析的结果表明:交联剂质量分数、反应温度和引发剂浓度对于 CSM 产率和溶胀度这两项指标都有着极为显著的影响.优化所得的较优工艺参数为:交联剂质量分数为 0.5%、交联温度为 48℃、引发剂浓度为 3.7 mmol/L,对应的 CSM 产率和溶胀度的预测值分别为 77.5%和 246%.经试验证明:应用效应面法所得到的 CSM 合成工艺参数是可行的.     

磁性淀粉微球固定化脂肪酶的研究

磁性淀粉微球为载体,采用戊二醛交联法固定化脂肪酶。磁性淀粉微球的主要组成是淀粉和磁粉。结果得到,磁性固定化脂肪酶的总活力、蛋白载量、比活、活性回收率、最适温度和最适pH值分别为4897.15U/g、50.59mg/g、98.58U/mg、72.73%、45℃和8.0。Ca2+、Na+和Mg2+对固定化脂肪酶和自由酶有激活作用,作用大小顺序为Ca2+>Mg2+>Na+。Cu2+和Fe2+对固定化脂肪酶和自由酶有抑制作用,Cu2+的作用尤其明显。脂肪酶被固定化后其热稳定性(在水介质和正己烷中)、操作稳定性、pH稳定性均比自由酶明显提高。固定化脂肪酶和自由酶在4℃下,pH8的PBS和正己烷中保存34d后,其相对活力分别是78.3%和98.8%。     

Acetamide‐modified hyper‐cross‐linked resin: Synthesis,characterization, and adsorption performance to phenol from aqueous solution

Acetamide‐modified hyper‐cross‐linked resin, HCP‐HMTA‐AA, was prepared and its adsorption performance was evaluated using phenol as the adsorbate. The prepared HCP–HMTA–AA owned predominant micro/mesopores and medium polarity, making it possess a superior adsorption to phenol as compared with polystyrene (PS), chloromethylated polystyrene (CMPS), hyper‐cross‐linked polymer (HCP) and amino‐modified hyper‐cross‐linked resin (HCP–HMTA). The adsorption enthalpy was ?99.56 kJ/mol at zero fractional loading, multiple hydrogen bonding contributed to such a great adsorption enthalpy and an approximately planar hexahydric ring was formed between acetamide of HCP–HMTA–AA and phenol. The dynamic capacity of phenol on HCP–HMTA–AA was 291.3 mg/g at a feed concentration of 946.2 mg/L and a flow rate of 48 mL/h and the resin column was almost regenerated by a mixed solvent including 50% of ethanol (v/v) and 0.01 mol/L of sodium hydroxide (w/v). HCP–HMTA–AA was repeatedly used for five times and the equilibrium adsorption capacity for the five time reached 94.2% of the equilibrium adsorption capacity for the first time. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41597.     

不稳定交联剂在微球合成中的应用及性能影响

通过Ⅰ型稳定交联剂(MBA)与Ⅱ型不稳定交联剂(PEGDA)复合使用,采用反相乳液聚合法制备一种不稳定交联微球。通过本体聚合法考察PEGDA的分解温度为60~65℃,并结合激光粒度仪研究Ⅱ型交联剂对微球粒径、膨胀性能的影响,SEM观察微球水化前后的形态。研究发现,适量的Ⅱ型交联剂与MBA复合使用能够减小微球的初始粒径;微球水化前后形态近似球形,初始粒径约为3μm,膨胀后颗粒间发生团聚作用;不稳定交联微球尺寸分布较宽,在常温下几乎不膨胀,60℃后Ⅱ型交联剂失效,微球膨胀速率加快,膨胀倍率优于单一交联微球,1.95×105mg/L矿化度地层水中,微球18 h内中值粒径(D0.5)从13.94μm增加到70.71μm。     

Anionic synthesis of aromatic carboxyl functionalized polymers. Chain-end functionalization of poly(styryl)lithium with 4,5-dihydro-4,4-dimethyl-2-[4-(1-phenylethenyl)phenyl] oxazole

The novel syntheses of 4-(4,5-dihydro-4,4-dimethyl-2-oxazolyl)benzophenone, 1-[4-(4,5-dihydro-4,4-dimethyl-2-oxazolyl)phenyl]-1-phenylethanol and 4,5-dihydro-4,4-dimethyl-2-[4-(1-phenylethenyl)phenyl]oxazole ( 1 ) are described. ω-Oxazolyl polystyrene ( 2 ) was synthesized in quantitative yields by the reaction of poly(styryl)lithium with stoichiometric amounts of 4,5-dihydro-4,4-dimethyl-2-[4-(1-phenylethenyl)phenyl]oxazole ( 1 ) in toluene/tetrahydrofuran (4 : 1 v/v) at −78°C. Deblocking of the oxazoline protecting group by acid hydrolysis followed by saponification quantitatively provides the corresponding aromatic carboxyl chain-end functionalized polystyrene ( 3 ). The functionalization agent and functionalized polymers were characterized by HPLC, thin layer chromatography, size exclusion chromatography, vapor phase osmometry, spectroscopy (¹H NMR, ¹³C NMR and FTIR), potentiometry and elemental analysis.     

Influence of free volume fraction,inter/intramolecular energy ratio,and chain segment density on the Gibbs-DiMarzio theory of the glass transition

Based upon computer analysis, the Gibbs-DiMarzio (G-DM) theory is evaluated for the case of (a) constant V₀ and (b) constant r where V₀ is the fractional free volume at T_g and r is the ratio of the hole (E₀) to the flex (ε) energy. For each respective case, results are presented in a reduced variables format that indicate the extent to which r and V₀ vary at the transition temperature as a function of the reciprocal degree of polymerization (P^?1). To further account for chemical differences that exist among polymers, an index (n) is introduced that ultimately incorporates the effective number average of chain atom segments (x?) per P?. Using these reduced variables plots, the effects of V₀, r, and n are compared with the T_g data for four well-documented polymers. Although the theory adequately describes the PMMA, PS, and PVC data, for PαMS the fit is doubtful. The analysis demonstrates that, in order to maintain V₀ within the range of 0.015–0.045, r must remain within approximately 1.0–1.1. Moreover, under conditions of either constant V₀ or r, other more flexible polymers require that $\text{n?10}$.     

壳聚糖磁性微球的制备及其对牛血清白蛋白的吸附性能研究

以Fe/C为磁性内核、液体石蜡为分散介质、Span-80为乳化剂、环氧氯丙烷为交联剂,采用反相悬浮包埋法制备了壳聚糖磁性微球.对微球表面的活性基团含量进行了测定.研究了用戊二醛活化、Cibacron Blue 3G-A修饰后的微球对牛血清白蛋白的吸附性能.结果表明,小粒径壳聚糖磁性微球经戊二醛活化后对牛血清白蛋白的饱和吸附量为46.3 mg·g-1,经Cibacron Blue 3G-A修饰后对牛血清白蛋白的饱和吸附量为66.2 mg·g-1.     

高透明抗冲聚苯乙烯中试研究

在连续本体聚苯乙烯中试装置上对高透明抗冲聚苯乙烯树脂进行了研究。结果表明,中试产品冲击性能与增韧剂相当,比小试产品稍差。小试产品、中试产品及增韧剂具有相似的互穿网络结构。