气相色谱法同时测定日化工业废水中16种防腐剂

建立气相色谱法同时测定日化工业废水中16种防腐剂的含量。样品用甲醇溶解后,经0.22μm有机滤膜过滤,以DB-5毛细管柱（30 m×0.25 mm,0.25μm）为分离柱,柱温箱初始温度为110℃,载气流量为0.7 mL/min,采用氢火焰离子化检测器检测,利用色谱峰面积外标法定量。2-甲基-4-异噻唑啉-3-酮、苯氧乙醇、2,4-二氯苄醇、辛基异羟肟酸、对羟基苯乙酮、对羟基苯甲酸甲酯、乙基己基甘油、4-丁基间苯二酚、吡罗克酮乙醇胺盐的质量浓度在5～100μg/mL范围内,2.6-二叔丁基对甲酚、氯苯甘醚、苯乙基间苯二酚的质量浓度在1～100μg/mL范围内,对羟基苯甲酸正丙酯的质量浓度在2.0～100μg/mL范围内,3-碘-2-丙炔基-N-丁基氨基甲酸酯甲酸酯的质量浓度在10.0～100μg/mL范围内,单辛酸甘油酯、单癸酸甘油酯的质量浓度在15～100μg/mL范围内,与色谱峰面积具有良好的线性关系,相关系数均不小于0.998,检出限为1.12～15.12μg/mL。样品加标回收率为87.0%～109.6%,测定结果的相对标准偏差为0.3%～5.6%(n=6)。该方法操作简单,可...     

气相色谱法快速同时测定室内装饰装修材料胶黏剂中的苯、甲苯、二甲苯的含量

建立了快速、同时测定室内装饰装修材料胶黏剂中苯、甲苯、二甲苯含量的气相色谱检测法.样品用乙酸乙酯溶解处理后,用改性的聚乙二醇(FFAP)毛细管色谱柱分离,氢火焰离子化检测器检测,外标法定量.胶粘剂中苯、甲苯、二甲苯的浓度分别在8.58～171.40μg/mL、9.04～180.62μg/mL、8.80～175.92μg...     

气相色谱法测定乙酸阿比特龙中1,1,3,3-四甲基胍

建立气相色谱测定乙酸阿比特龙原料药中1,1,3,3-四甲基胍的方法。选择乙酸乙酯为溶剂溶解样品，以安捷伦CP-Volamine毛细管柱（30 m×0.32 mm,0.45μm）作为分离色谱柱，采用氢火焰离子化检测器（FID）进行检测，外标法定量分析。1,1,3,3-四甲基胍的质量浓度在10.22～204.38μg/mL范围内与色谱峰面积线性关系良好，相关系数为0.999 4，定量限为10.22μg/mL。样品加标回收率为97.9%～113.7%,9份样品测定结果的相对标准偏差为5.0%。该方法操作简单，可用于乙酸阿比特龙原料中1,1,3,3-四甲基胍的测定。     

铜掺杂钙铝水滑石催化氧化异丙苯制备异丙苯过氧化氢

采用共沉淀法制备了铜掺杂钙铝水滑石Ca₄Cu _x Al-LDHs（x=0,0.1,0.3,0.5,0.8,1.0）,并对其催化异丙苯液相氧化制备异丙苯过氧化氢的活性进行了研究。采用X射线衍射、傅里叶红外光谱、扫描电子显微镜和热分析等手段对Ca₄Cu _x Al-LDHs进行了表征,制备的Ca₄Cu _x Al-LDHs保留了水滑石的片层状结构,铜的掺杂使孔径变小,比表面积增大。当进料比（催化剂/异丙苯）为7.5 mg/mL,反应温度85 ℃,氧气流速为15 mL/min,反应时间7 h,异丙苯的转化率为34.5%,异丙苯过氧化氢的选择性为86.9%,催化剂循环使用5次后,异丙苯的转化率为31.2%,异丙苯过氧化氢的选择性为83.3%。研究为异丙苯过氧化氢开发了新的催化体系。     

毛细管气相色谱法测定鞋和箱包用胶粘剂中正己烷的含量

采用丙酮作为溶剂,选用19091N-213型毛细管色谱柱(30 m×0.32 mm i.d.,0.5μm)和氢火焰离子化检测器,以毛细管气相色谱法测定鞋和箱包用胶粘剂中正己烷含量。正己烷的浓度在0~1 000μg/mL与色谱峰面积成线性关系,线性回归方程为A=127 107c 383.26,相关系数r=0.999 1,检出限为0.003μg/mL,用该方法对胶粘剂样品进行测定,测定结果的相对标准偏差为2.8%~4.5%(n=5),加标回收率为96.4%~107.8%。     

气相色谱法测定交联透明质酸钠凝胶的修饰度

建立一种气相色谱测定交联透明质酸钠凝胶中修饰度的分析方法。通过沸水酸解的方法提取凝胶中的丙三醇物质，以丙三醇为外标，采用气相色谱法进行定量分析。采用PEG-20M毛细管柱（30.0 m×0.32 mm,0.50μm），柱温为250℃，采用氢火焰离子化检测器（FID）检测，检测器温度为290℃，载气流量为30 mL/min，载气为高纯氮气，流量为3.0 mL/min。丙三醇质量浓度在8.16～122μg/mL范围内与色谱峰面积线性关系良好，线性方程为y=3 266.9x-8 404.7，相关系数r=0.999 7，方法检出限为0.037μg/mL，定量限为0.83μg/mL，样品加标回收率为99.17%～99.94%，测定结果的相对标准偏差为0.77%(n=6)。     

衍生化气相色谱法测定早强剂中三乙醇胺含量

建立了衍生化气相色谱法定量分析水泥早强剂中三乙醇胺含量的方法。以丙三醇作为内标,采用HP-5毛细管柱分离样品,氢火焰离子化检测器(FID)测定三乙醇胺含量。三乙醇胺在0.2～5.0mg/mL范围内与三乙醇胺/内标的乙酰化物色谱峰面积的比值呈线性关系,相关系数r=0.9996。方法检出限为42.6μg/mL,平均回收率为96.6%,相对标准偏差(RSD)为0.759%。该方法具有操作简便、快速、准确等优点,可用于测定水泥早强剂中三乙醇胺的含量。     

顶空-气相色谱法测定土壤和沉积物中丙烯酸酯类化合物

提出了顶空-气相色谱法测定土壤和沉积物中丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酸丙酯和丙烯酸丁酯等5种丙烯酸酯类化合物含量的方法。分别选择70℃及20 min作为样品在顶空瓶中的平衡温度和平衡时间。用HP-INNOWAX毛细管色谱柱（30 m×0.32 mm,0.32μm）分离,氢火焰离子化检测器测定。5种丙烯酸酯类化合物在9 min内能完全分离。5种丙烯酸酯类化合物的质量分数在20.0～2000μg·kg^-1范围内与其峰面积呈线性关系,检出限（3S/N）在2.0～10.0μg·kg^-1之间。方法用于土壤和沉积物样品分析,加标回收率在86.8%～104%之间,测定值的相对标准偏差（n=6）在3.5%～5.4%之间。     

气相色谱法同时测定环境空气中6种丙烯酸酯

建立气相色谱法同时测定环境空气中丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酸丙酯、丙烯酸丁酯和甲基丙烯酸丁酯6种丙烯酸酯化合物。采用活性炭吸附环境空气中的丙烯酸酯,然后用二氯甲烷解吸,选用DB-35色谱柱,采取程序升温方式,用带氢火焰离子化检测器的气相色谱仪检测。6种丙烯酸酯的质量浓度在2～80μg/mL范围内与色谱峰面积线性关系良好,相关系数均为0.999 9。当采样体积为20 L时,方法检出限为0.008～0.01 mg/m3。样品加标回收率为82.3%～104%,测定结果的相对标准偏差为1.1%～9.8%(n=6)。该方法样品处理简单,抗干扰,便于推广应用。     

顶空气相色谱法测定羧甲基壳聚糖中氯乙酸残留量

采用顶空气相色谱法间接测定了羧甲基壳聚糖中氯乙酸的残留量。样品(0.2g)于顶空瓶中超声溶解在水3mL中,加入甲醇2.5mL,硫酸1.5mL,在70℃水浴反应40min使之酯化。按顶空条件进样,用HP-INNOWAX毛细管色谱柱分离,氢火焰离子化检测器测定。分别选择15min和85℃作为样品在顶空瓶中的平衡时间和平衡温度。氯乙酸的质量在0.2～20mg范围内与其峰面积呈线性关系,方法的检出限(3S/N)为5.6mg·L-1。方法用于实样中氯乙酸的测定,用标准加入法做回收试验,测得回收率在90.0%～92.0%之间,测定值的相对标准偏差(n=5)在0.7%～0.9%之间。     

纳米氧化铜用于温和条件下的异丙苯氧化研究

采用水热合成方法制备了具有片状结构的纳米CuO催化剂.该催化剂在温和的条件下对以分子氧为氧化剂的异丙苯氧化反应表现出高效的催化活性.在85℃、常压、催化剂用量为0.02g/mL异丙苯的条件下,反应9h,异丙苯的转化率、选择性和收率分别为55.1%、94.1%和51.8%.研究发现,该纳米CuO催化剂可以循环使用.同时对该纳米CuO催化剂催化其它含有α-H的芳烃化合物甲苯和乙苯的氧化反应进行了研究.实验结果表明,该催化剂的活性顺序为异丙苯>乙苯>>甲苯.     

Synthesis of Cumene from Lignin by Catalytic Transformation

Cumene is an important intermediate and chemical in chemical industry.In this work,directional preparation of cumene using lignin was achieved by a three-step cascade process.The mixture aromatics were first produced by the catalytic pyrolysis of lignin at 450℃ over 1% Zn/HZSM-5 catalyst,monocyclic aromatics with the selectivity of 85.7 wt% were obtained.Then,the catalytic dealkylation of heavier aromatics resulted in benzene-rich aromatics with 93.6 wt% benzene at 600℃ over Hβ catalyst.Finally,the cumene synthesis was performed by the aromatic alkylation,giving cumene selectivity of 91.6 C-mol% using the[bmim]Cl-2AlCl₁₃ ionic liquid at room temperature for 15 min.Besides,adding a small amount of methanol to the feed can efficiently suppress the coke yield and enhance the aromatics yield.The proposed transformation potentially provides a useful route for production of cumene using renewable lignin.     

Cumene Liquid Oxidation to Cumene Hydroperoxide over CuO Nanoparticle with Molecular Oxygen under Mild Condition

CuO nanoparticle was synthesized via wet chemical method and was characterized by X-ray diffraction(XRD),nitrogen adsorption-desorption,and scanning electron microscopy(SEM).Catalytic oxidation of cumene with molecular oxygen was studied over CuO nanoparticle.The catalysts showed markedly higher activities as compared to CuO prepared by conventional method,CuO/Al_2O_3,or ho- mogeneous copper catalyst under comparable reaction conditions.The cumene conversion,comene hy- droperoxide(CHP)yield,and selectivity using 0.25 g CuO nanoparticle catalyst and 0.1 mol cumene at 358 K for 7 h were 44.2%,41.2% and 93.2%,respectively.The catalyst can be recycled.After 6 recycled experiments,no loss of catalytic activity was observed.     

皂石的合成、表征及其催化性能

用水热法合成了皂石,并用羟基铝低聚物与其交联制得AICLS。用XRD、~(27)Al和~(29)Si MASNMR及吡啶吸附量表征其晶相、结构和表面酸性。合成产物的结晶度很高。皂石中T—O—T片内四面体层上铝量可由合成条件控制,表明交联密度的柱间距与铝量有关。在异丙苯裂解反应中,AICLS的活性高于皂石,但活性衰减较慢;样品的催化裂化活性与探针分子可抵达的强酸中心数有关。     

Vanadia impregnated iron-pillared montmorillonite for aniline methylation

Vanadia impregnated iron-pillared montmorillonites with different weight percentages of vanadia have been prepared. Subsequent characterization by XRD, FT-IR, surface area and pore volume measurements was carried out. Acidity was determined by three independent techniques namely thermogravimetric desorption of 2,6-dimethylpyridine, spectrophotometric monitoring of adsorption of perylene and temperature-programmed desorption of ammonia. Conversion of cumene in the vapor phase has been performed as a test reaction of acidity. Aniline methylation was carried out to check the catalytic efficiency of the solids. This revised version was published online in August 2006 with corrections to the Cover Date.     

Excess Molar Volumes of n-Pentanol + Cumene,n-Pentanol + 1,4-Dioxane and Cumene + 1,4-Dioxane at Different Temperatures

Abstract

Molar excess volumes (V^E ) and partial molar excess volumes ( ^VE ) are reported for non-electrolyte binary mixtures of n-pentanol + cumene, n-pentanol + 1,4-dioxane and cumene + 1,4-dioxane at four temperatures and over the whole concentration range. In these systems, the n-pentanol is a highly polar molecule with association in its pure state, while the others two show little polarity without association in their pure states. The results of V^E are discussed in terms of the interactions between components. The Prigogine–Flory–Patterson model of solution thermodynamics has been used to predict V^E . This work shows the importance of the three contributions δV _int, δV _p? and δV_F to V^E .     

Polymer supported catalyst for the effective autoxidation of cumene to cumene hydroperoxide

The autoxidation of cumene to cumene hydroperoxide (CHP) in the presence of catalyst which was prepared by adsorbing copper(II) acetate onto polymer support, was investigated. When a styrene-divinylbenzene copolymer with sulfonic acid functional groups was used as a support, the resulting catalyst had no catalytic activity. When a macroreticular acrylic polymer containing carboxylic acid exchange groups was used as a support, an effective catalyst was obtained. In the presence of this catalyst (0.2 g Cu(OAc)₂-BR-0.6 per 10 mL of cumene) at 353 K, the steady autoxidation rate is 84% faster than that initiated with CHP; the selectivity is 99% at 6.8% conversion. The catalyst is stable at 383 K. Furthermore, the catalyzed cumene autoxidation rate increases linearly with copper acetate loading as well as the amount of catalyst. But when the steady autoxidation rate increases, the selectivity to cumene hydroperoxide reduces, but is still satisfactory. Hence, it is possible to speed up the cumene autoxidation rate by raising the reaction temperature, using catalysts with high metal loading and using more catalyst.     

3-Substituted Thietanes as Effective Inhibitors of Cumene Oxidation

3-Substituted thietanes were prepared by reaction of 1,2-epithio-3-chloropropane with various nucleophiles in aqueous solutions and were characterized. The inhibiting power of these compounds in cumene oxidation was studied.     

过氧化氢异丙苯催化氧化丙烯制环氧丙烷

研究了以钼－醇配合物为催化剂,过氧化氢异丙苯为环氧化剂,乙醇为溶剂的丙烯一步氧化制环氧丙烷的反应,结果表明,用不同的二醇和不同醇／钼比制备的钼醇催化剂具有不同的催化性能和配性,用乙二醇和丙二醇制备的催化剂,催化性能优于丁二醇制备的催化剂,考察了反应条件（温度、压力和时间）对环氧化反应活性的影响,在１００℃,０．５ＭＰａ的条件下反应２ｈ,过氧化氢异丙苯的转化率为６５．０％,环氧丙烷的选择性为７０．４