硫代乙酰胺-聚苯乙烯树脂吸附剂制备及其对铅、镉、铜、镍、铁的萃取

以大孔聚苯乙烯苄胺树脂为载体通过Mannich反应制备了一种新型固相萃取吸附剂TAA-PS(硫代乙酰胺改性聚苯乙烯树脂)。利用FTIR和元素分析对其进行表征。研究了其对痕量金属离子的萃取性能,确定了对Pb2 、Cd2 、Cu2 、Ni2 和Fe3 等金属离子的最佳吸附条件。与其它吸附剂相比,本研究合成的固相萃取吸附剂具有高吸附容量和相当快的吸附速率。应用于自来水和湖水中痕量Pb2 、Cd2 、Cu2 、Ni2 和Fe3 的萃取富集,取得较好结果。     

固相萃取-高效液相色谱法同时测定苹果中残留的克菌丹和灭菌丹

采用硅镁吸附剂和硅胶作吸附剂,建立了固相萃取-高效液相色谱法同时测定苹果中残留的克菌丹和灭菌丹的分析方法。研究了甲醇-乙腈-水(含0.1 mmol/L乙酸-乙酸钠缓冲溶液（pH 3.80）)三元体系下克菌丹和灭菌丹的最佳分离条件,在波长210 nm下检测,克菌丹和灭菌丹的线性范围为0.40～8.00 mg/kg,线性相关系数均大于0.9999;最低检出限克菌丹为0.27 mg/kg、灭菌丹为0.20 mg/kg;保留时间的相对标准偏差（RSD）≤0.60%。苹果样品中3个添加水平的平均加标回收率为克菌丹69.3%～106%,RSD为3.7%～4.7%;灭菌丹101%～108%,RSD为1.3%～5.4%。     

Sorption Studies of Acid Dye by Mixed Sorbents

The sorption of Acid Blue 9 onto the mixture of activated clay and activated carbon has been studied in terms of pseudo-first order and pseudo-second order chemical sorption processes. The batch sorption model, based on the assumption of a pseudo-second order mechanism, has been developed to predict the rate constant of sorption and the equilibrium capacity with the effect of initial dye concentration, mass of mixed sorbent, temperature and initial solution pH. The rates of sorption were found to conform to pseudo-second order kinetics with good correlation. Batch isotherm studies showed that the sorption of Acid Blue 9 by the mixed sorbent from aqueous solution was described by the Langmuir isotherm equation. A comparison of the evaluated equilibrium capacity of sorption has been made by the pseudo-second order rate equation as well as by the Langmuir isotherm and operating line method. In addition, an activation energy of sorption has also been determined based on the pseudo-second order rate constants.     

热重分析法研究贝壳固硫反应动力学

采用热分析法研究了贝壳和石灰石固硫反应过程, 用等效粒子模型对固硫反应过程进行了表征, 计算分析了其固硫反应动力学参数. 结果表明, 贝壳比石灰石含有较多的碱金属盐, 其作用是提高了贝壳固硫反应速率常数和有效扩散系数. 贝壳固硫反应中存在补偿效应. 根据等动力学温度判别固硫剂活性适用于不同反应控制区的活性判断. 碱金属成分对钙基固硫剂活性有正负两个方面的影响, 含量过大或过小都会削弱固硫剂活性, 因而存在最适含量. 在1 073～1 273 K温区固硫时, 钙基固硫剂中碱金属离子与钙离子摩尔比为1∶50左右时固硫活性较高.     

Determination of Ciprofloxacin,Enrofloxacin, and Marbofloxacin in Bovine Urine,Serum, and Milk by Microextraction by a Packed Sorbent Coupled to Ultra-High Performance Liquid Chromatography

This article reports new, easy, and rapid microextraction by packed sorbent (MEPS)–ultra high performance liquid chromatography with photodiode array detection for the simultaneous determination in bovine urine, serum, and milk of three antibiotics belonging to the class of the fluoroquinolones, namely ciprofloxacin, enrofloxacin, and marbofloxacin, approved for veterinary and human use (ciprofloxacin). The chromatographic separation of the analytes and all aspects influencing the MEPS performance were optimized for the extraction from the considered biological samples. The optimized procedure required simple sample pretreatment, a short (<8?min) isocratic elution, and provided sufficient sensitivity for the determination of the analytes at trace levels in compliance with current legislation. Limits of quantitation were in the range from 0.002 (ciprofloxacin, urine) to 0.048?μg/mL (enrofloxacin, milk). Recoveries from 79% (enrofloxacin, milk) to 88% (ciprofloxacin, urine/serum) were obtained on spiked samples. The within-day (n?=?6) and between-day (n?=?6 over 3?days) relative standard deviation percentages in bovine urine, serum, and milk samples ranged from 2.2 (ciprofloxacin, urine) to 2.5 (enrofloxacin, serum) and from 3.1 (ciprofloxacin, urine) to 3.7 (enrofloxacin, milk), respectively, and were not concentration dependent. To the best of our knowledge, this is the first study describing a fast and simple method for the determination of fluoroquinolones in bovine biological samples.     

新型Mn-Fe/Al_2O_3高温脱除H_2S的实验研究(Ⅱ)

本文首先研究了粒度dp=07mm脱硫剂的脱硫反应和再生反应性能。研究表明当Mn∶Fe=2∶1(w)、载体在1000℃焙烧后,脱硫剂有较好的脱硫反应性能,其最佳的脱硫反应温度为550℃,且在710℃、O2浓度低于1083%(v)、空速2000～3000h-1再生条件下,可完全对脱硫剂进行再生;H2S浓度影响脱硫剂的初始脱硫反应速率和穿透反应时间,但对脱硫剂的脱除率和穿透硫容影响不大。并研究了粒度dp=3mm脱硫剂的脱硫情况。实验结果表明,小颗粒脱硫剂的脱硫反应主要为化学反应控制,大颗粒脱硫剂主要为扩散控制。为此对大颗粒脱硫剂进行了工程设计,即采用活性组分非均布脱硫剂。研究表明,非均布脱硫剂明显提高了脱硫剂的平均脱硫反应速率和硫容,同均布脱硫剂相比,非均布脱硫剂再生后具有较好的脱硫稳定性能。     

Modification of Crosslinked Poly(styrene) Based Polymers for Boron-Specific Extraction

A new polymeric resin with glucose sulfonamide functions has been prepared for the extraction of boric acid. This poly (styryl sulfonamide) based resin has been demonstrated to be an efficient sorbent for the removal of boron. The resin had a boron loading capacity of 2.365 mmol.g⁻¹ and showed reasonably rapid sorption ability. Splitting of sorbed boron can be achieved by simple acid leaching (2M H₂SO₄).     

Affinity sorbent from abscisic acid — Agarose A-6

Optimal conditions are found for synthesizing an affinity sorbent from abscisic acid (ABA) and aminopropylagarose A-6. A protein with high specific affinity for ABA is isolated from the microsomal fraction of four-day cotton sprouts using the synthesized sorbent.A. S. Sadykov Institute of Bioorganic Chemistry, Academy of Sciences of the Republic of Uzbekistan, Tashkent, fax (99871) 162 70 71. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 157–159, March–April, 2000.     

Removal of Zinc Ions by Sol-Gel Silica Doped with Cibacron Blue

Chemically doped sol-gel silica has been developed by entrapping organic dye cibacron blue as a complexing reagent in porous silica prepared by the sol-gel method for removal of metal ions from water samples. In the doped sol-gel silica, the large reagent molecules are entrapped inside the pores while small metal ions can diffuse into the pores where they are complexed by the reagent and retained inside the pores. This new solid sorbent was tested for removal of Zn(II) from aqueous solutions. The kinetics, isotherm, and pH effect of the removal were investigated. With a loading of 0.10 mmol cibacron blue/g, the sol-gel silica sorbent had a capacity of 0.09 mmol Zn/g. It was demonstrated that the sol-gel silica sorbent could be regenerated and reused repeatedly.     

O2/CO2方式下钙基吸收剂在脱硫过程中微观结构变化的研究

本文研究了O2/CO2方式下钙基吸收剂在脱硫过程中微观结构的变化。研究结果表明,不同浓度的CO2对孔隙结构的影响完全不同;且提高温度有利于改善高浓度CO2气氛下钙基吸收剂煅烧后的孔隙结构,较之空气气氛,高浓度CO2气氛更有利于高温下炉内喷钙脱硫。