四元共聚高吸水树脂的合成及性能研究

以玉米淀粉为主要原料,聚乙二醇为交联剂制备四元共聚高吸水树脂。采用正交设计试验研究了各因素对吸水树脂吸液倍率的影响。结果表明丙烯酸用量为4.5mL、丙烯酰胺用量为2.5g、顺丁烯二酸酐用量为2.5g,引发剂浓度为1.4%、交联剂浓度为0.17%,反应时间为3.5h,吸水树脂的吸液性能最好。吸蒸馏水倍率为543g/g,吸0.9%NaCl倍率为96g/g,吸氨水倍率为46g/g,在1.5P0压力下吸水倍率可达143g/g。     

高效液相色谱法测定地沟油中5种生物胺

本文建立了高效液相色谱柱前衍生化法测定地沟油中5种生物胺含量的方法。样品经0.5mol/L盐酸提取后用丹磺酰氯衍生,采用ZORBAX 80A Extend-C1(84.6×150mm5μm),以0.1mol/L乙酸铵和乙腈为流动相进行梯度洗脱,流速1.0mL/min,柱温30℃,检测波长260nm。该方法检测限为腐胺1.2μg/g,尸胺1.4μg/g,组胺1.3μg/g,酪胺、精胺1.5μg/g。样品添加浓度为10μg/g、20μg/g时,回收率为82%～89%,相对标准偏差为1.8%～3.5%。本法为地沟油的质量鉴定提供了简便、灵敏、可靠的检测方法。     

一种铁基复合材料的制备及其电容性能

采用微乳液法制备了铁基复合材料,研究了反应温度、十六烷基三甲基溴化铵(CTAB)用量对其电容性能的影响.结果表明,在温度为140℃,CTAB用量为1.5 g时,所制得的电极材料电容性能最佳:当电流密度为1 A/g时,比电容为202.5 F/g;电流密度为2 A/g时,比电容为123.0 F/g;电流密度为5 A/g时,比电容为78.0 F/g.     

氢化物原子荧光光谱法同时测定生活饮用水中砷和硒

建立了氢化物发生原子荧光光谱法同时测定生活饮用水中砷和硒的方法.测试结果表明砷和硒在质量浓度分别为0.00μg/L~10.00μg/L和0.00μg/L~40.00μg/L范围内呈线性关系,相关系数分别为(砷r=0.9998,硒r=0.9997)。仪器检出限为砷:0.03μg/L硒:0.05μg/L。本方法检出限砷为0.075μg/L;硒为0.125μg/L。水质样品中砷的回收率为92.6%~96.5%,精密度为0.8%~1.4%;硒的回收率为91.2%~97.4%,精密度为1.0%~1.6%。应用本方法测定生活饮用水中的砷和硒方法简便、快速,结果准确可靠,较好地提高了工作效率。     

罗丹明B酶联免疫分析方法的建立与应用

建立一种用于检测罗丹明B的间接竞争酶联免疫分析方法。该方法的IC50为1.3ng/m L,检测限为0.786ng/g。该方法检测豆瓣酱,加标浓度5 ng/g,平均回收率为83%,加标浓度10 ng/g,平均回收率为89%;检测辣椒酱,加标浓度5 ng/g,均回收率为88%,加标浓度10 ng/g,平均回收率为104%;检测辣椒油,加标浓度5 ng/g,平均回收率为94%,加标浓度10 ng/g,平均回收率为101%;检测辣椒粉,添加浓度5 ng/g,平均回收率为82%,加标浓度10 ng/g,平均回收率为90%。该方法的平均批内差为9.0%,批间差为10.5%,与其他常见染料未见交叉反应。该方法操作简便,结果准确,适用于罗丹明B的现场大量样品快速检测。     

化妆品中新补骨脂异黄酮、补骨脂二氢黄酮、补骨脂素和异补骨脂素含量的测量不确定度评定

用高效液相色谱法测定化妆品中新补骨脂异黄酮、补骨脂二氢黄酮、补骨脂素和异补骨脂素含量,建立数学模型,分析检测过程中不确定度的来源,给出量化结果,得到标准不确定度和扩展不确定度。结果表明,当取95%置信概率,包含因子k为2,被测样品中新补骨脂异黄酮、补骨脂二氢黄酮、补骨脂素和异补骨脂素的含量分别为42.61μg/g、44.04μg/g 、42.94μg/g和41.90μg/g时,相应的扩展不确定度为1.65μg/g、1.82μg/g、1.66μg/g和1.61μg/g。分析了测量不确定度的主要来源,并提出了改进建议。     

人造金刚石表面化学镀W/Ni-P层的工艺优选及镀层质量

为改进人造金刚石的表面性能,先在其上化学镀W,再化学镀Ni-P,制备了W/Ni-P包覆人造金刚石粉末。以镀液稳定性和镀层与基体结合力为评价标准,用正交试验和单因素试验优选工艺,并用扫描电镜(SEM)、能谱仪和粒度分析仪考察了优化W/Ni-P复合镀层的组织结构和镀后粉末的粒度分布。结果表明:最优化学镀W工艺为50 g/L钨酸钠,32 g/L次亚磷酸钠,25 g/L柠檬酸三钠,0.002 0 g/L硫脲,p H值为8.5,温度为90℃,时间为1 h;最优化学镀Ni-P工艺为35 g/L硫酸镍,32 g/L次亚磷酸钠,25 g/L柠檬酸三钠,0.002 0 g/L硫脲,p H值为4.5,温度为80℃,时间为1 h;优化W/Ni-P层均匀细致,与金刚石结合良好,镀覆后的金刚石粉末粒度更均匀。     

石墨炉原子吸收光谱测定三甲基镓中痕量元素

介绍一种石墨炉原子吸收光谱测定三甲基镓的方法。用乙醇分解三甲基镓,分解产物的水解溶液用于检测四种痕量元素Cu、Fe、Ms、Si。分解和测定过程的相对标准偏差小于24.0％。检测限:Cu为0.4μg/g,Fe为0.4μg/g,Mg为0.09μg/g,Si为0.4μg/g。     

用火焰原子吸收光谱法测中草药中的金属元素

在微波消解罐内用硝酸消化样品,采用火焰原子吸收光谱法对9种中草药中的K、Na、Mg、Mn、Fe、Zn、Cu七种金属元素进行分析测定,并研究了最佳实验条件。在选定条件下,钾的检测限为0.0019μg/mL,钠的检测限为0.0077μg/mL,镁的检测限为0.0024μg/mL,铁检出限为0.0047μg/mL,锌检出限为0.0032μg/mL,铜检出限为0.0052μg/mL,锰检出限为0.0028μg/mL,相对标准偏差为0.54%～3.2%,回收率为94.8%～101.7%。用于中草药中金属元素的测定,简便、省时、准确,结果满意。     

4-叔丁基苯乙烯/三元乙丙橡胶悬浮共聚树脂的制备及表征

以EPDM(三元乙丙橡胶)、tBS(4-叔丁基苯乙烯)为单体,BPO(过氧化苯甲酰)为引发剂,DVB(二乙烯苯)为交联剂,明胶和磷酸三钙为分散稳定剂,甲苯和环己烷为溶剂,采用悬浮法合成新型功能高分子材料P(tBS/EPDM).采用SEM、FTIR、DSC等方法对其结构和性能进行表征,结果表明:所合成的粒状树脂中存在小而均匀的多孔结构,具有较高的比表面积.P(tBS/EPDM)对油品具有良好吸收性能,对四氯甲烷的最大吸油率为51.68g/g,氯仿35g/g,环己烷25.83g/g,煤油27.50g/g,甲苯22.8g/g,对甲苯和煤油最大吸油速率为66.64和199.93h-1.     

Importance of H(2)O(2)/Fe(2+) ratio in Fenton's treatment of a carpet dyeing wastewater

The effectiveness of the Fenton's reagent (H(2)O(2)/Fe(2+)) in the treatment of carpet dyeing wastewater was investigated under different operational conditions, namely, H(2)O(2) and FeSO(4) concentrations, initial pH and temperature. Up to 95% COD removal efficiency was attained using 5.5 g/l FeSO(4) and 385 g/l H(2)O(2) at a pH of 3, temperature of 50 degrees C. The H(2)O(2)/Fe(2+) ratio (g/g) was found to be between 95 and 290 for maximum COD removal. It was noteworthy that, keeping H(2)O(2)/Fe(2+) ratio constant within the range of 95-290, it became possible to decrease FeSO(4) concentration to 1.1 g/l and H(2)O(2) concentration to 96.3 g/l, still achieving nearly the same COD removal efficiency. The relative efficiencies of Fenton's oxidation and coagulation stages revealed that Fenton's coagulation removed organic compounds which were not removed by Fenton's oxidation, indicating that the Fenton's coagulation acted as a polishing step.     

Preparation and photocatalytic activity of iron oxide-loaded potassium titanate layered compounds

Iron oxide-loaded hydrous potassium tetratitanate (K0.3Ti4O7.3(OH)1.7) compounds consisting of 1.48 wt% (sample 'B'), 1.87 wt% (sample 'C') and 5.60 wt% (sample 'D') of iron oxide were synthesized by suspending the K0.3Ti4O7.3(OH)1.7 (sample 'A') in Fe2(SO4)3 solution for 24 h, followed by washing several times with deionized water and then dried at 120 degrees C for 24 h. The K0.3Ti4O7.3(OH)1.7 was synthesized by refluxing the K2Ti4O9 x 2H2O in 1 M HNO3 solution. Band-gap energies of the K0.3Ti4O7.3(OH)1.7 and the iron oxide-loaded samples are 3.12 +/- 0.6 eV and 2.23 +/- 0.09 eV, respectively. Photooxidation activity towards methylene blue decomposition under fluorescence irradiation was found to decrease as follow: sample 'B' > sample 'C' > Sample 'A' > sample 'D' > commercial Fe2O3-Blank. The photoactivity under sunlight irradiation was found to decrease as follow: sample 'B' > sample 'A' > Sample 'C' > sample 'D' > commercial Fe2O3-Blank.     

ACF负载TiO2光催化清除低浓度气态苯的实验研究

为有效清除密闭环境中低浓度气态苯,以钛酸丁酯为前驱物,采用sol -gel法和浸渍-提拉法制备了TiO2/ACF复合材料.采用正交试验研究了溶胶凝胶工艺参数中去离子水、无水乙醇、冰醋酸的加入量以及TiO2/ACF煅烧温度对ACF/TiO2光催化性能的影响,在动态试验装置中,考察了TiO2/ACF对低浓度气态苯清除效果,...     

溶剂对溶胶-凝胶燃烧法合成YAG粉体的影响

以Y(NO3)3.6H2O、Al(NO3)3.9H2O和柠檬酸为原料,分别以去离子水和无水乙醇为溶剂,采用溶胶-凝胶燃烧法合成YAG粉体。借助FT-IR、XRD、SEM等分析仪器研究了溶胶-凝胶燃烧法合成YAG粉体的过程,重点讨论了前躯体溶液不同溶剂对溶胶-凝胶燃烧法合成过程及合成产物的影响。结果表明:去离子水和无水乙醇对合成的YAG粉体的形貌和分散性有重要的影响。     

Modified solid-state reaction synthesized cathode lithium iron phosphate (LiFePO4) from different phosphate sources

A modified solid-state method was used to prepare LiFePO4. With the aid of deionized water, a mixture containing Fe2O3, NH4H2PO4 (or (NH4)2HPO4), LiOH, glucose and oxalic acid was prepared into fluffy powders, which were heated in a carbon-coated crucible at 700 degrees C for 3 hours to synthesize LiFePO4 without any inert gas flow. For the first time, the roles of NH4H2PO4 and (NH4)2HPO4 on the preparation of LiFePO4 were systematically investigated. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS), revealing that the crystallinity of the LiFePO4 sample prepared from NH4H2PO4 is superior to that prepared from (NH4)2HPO4 and the particle size of the sample prepared from NH4H2PO4 is smaller than that prepared from (NH4)2HPO4. The specific capacity, cycle property and rate capabilities were also compared between the as-prepared LiFePO4 samples. A better electrochemical performance was observed in the sample prepared from NH4H2PO4.     

Salt-assisted Low Temperature Solid State Synthesis of High Surface Area CoFe2O4 Nanoparticles

A novel salt-assisted low temperature solid state method using CoCl2·6H2O, FeCl3·6H2O and NaOH as pre-cursor and using NaCl as a dispersant to synthesize high surface area CoFe2O4 nanoparticles, has been investigated. The effects of the molar ratio of added salt and calcination temperature on the characteristics of the products were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and Brunauer, Emmett and Teller (BET) surface area analysis. Results showed that the introduction of leachable inert inorganic salt as a hard agglomeration inhibitor in the mixture precursorled to the formation of high dispersive CoFe2O4 nanoparticles; and the increase in specific surface area from 28.28 to 73.97 m2/g, and the saturation magnetization is 84.6 emu/g.     

前驱溶液的碱浓度对BiVO4粉体的微波水热法制备及光催化性能的影响

以Bi(NO3)3·5H2O和NH4VO3为原料,采用微波水热法在200℃不同前驱液碱浓度下制备了BiVO4粉体。利用XRD、FE-SEM、BET、UV-Vis等手段研究了前驱液碱浓度对BiVO4晶型、结构及形貌的影响,并对不同前驱液碱浓度下合成粉体的光催化性能进行了研究。溶于纯水获得的粉体是单斜相和四方相1～3μm八面体结构的BiVO4混晶。溶于HNO3和NaOH溶液时制得粉体为纯单斜相3μm大小球状BiVO4,NaOH增加到4mol/L时为2μm大小鱼排骨状BiVO4的混晶。光催化结果表明,紫外光下光催化活性顺序为:BiVO4(纯水)>BiVO4(4mol/L NaOH)>BiVO4(2mol/L NaOH),可见光下光催化活性顺序为:BiVO4(4mol/L NaOH)>BiVO4(纯水)>BiVO4(2mol/L NaOH)。     

6061铝合金表面硅烷-镧盐杂化膜制备工艺参数的正交优化

为探索硅烷-稀土盐复合膜的最佳制备工艺,以La(NO_3)_3·6H_2O为成膜物质,H_2O_2为促进剂,在铝合金表面制备硅烷-镧盐杂化膜,以膜层的极化电阻作为评价指标,采用正交试验法对制备工艺进行优选,采用电化学极化曲线和交流阻抗谱分析膜层的耐腐蚀性能,采用扫描电镜观察膜层的形貌,并与单一硅烷膜和镧盐膜的性能进行比较。结果表明:杂化膜的最佳制备工艺中镧盐沉积条件为10 g/L La(NO_3)_3·6H_2O,15 mL/L H_2O_2,成膜温度50℃,成膜时间40 min;镧盐掺杂有效提高了膜层的均匀度与致密度;杂化膜较单一硅烷膜和镧盐膜具有更好的致密性和疏水性,且能明显发挥镧盐膜和硅烷膜的协同作用,可有效降低6061铝合金的腐蚀速率,提高其耐蚀性。     

机械活化木薯淀粉接枝丙烯酸-丙烯酰胺制备高吸水性树脂的研究

以机械活化木薯淀粉和丙烯酸-丙烯酰胺为原料,以过硫酸铵-亚硫酸钠为引发剂,用水溶液聚合法制得淀粉基高吸水性树脂。最佳工艺条件为:淀粉1.00g,丙烯酸13.50mL,丙烯酰胺1.50g,去离子水25.00mL,引发剂质量比为过硫酸铵∶亚硫酸钠=3∶2,反应温度70℃,反应时间1h,中和度80%。在该条件下,所制得的样品的吸液率为:吸去离子水为2503g/g,吸0.9%NaCl盐水为324g/g。     

溶胶-凝胶法制备尖晶石型LiMn_2O_4正极材料

采用溶胶-凝胶法制备了锂离子电池正极材料锂锰氧化物。以Mn(NO3)2(50%)、LiOH·2H2O为原料,以柠檬酸为螯合剂制得前驱体,400℃预烧6h,再经750、850℃分别焙烧并保温6h得到粉体产物。XRD分析表明,所合成的产物为尖晶石型LiMn2O4;SEM观察结果表明,合成产物颗粒均匀,形貌规则。用其组装的电池经恒电流充放电测试,表明其初始比容量可达118.76mAh/g,具有良好的循环性能。