萃取色谱法富集原子吸收法测定环境水中超痕量金属元素：两种…

本文研究并比较了分别以８－羟基喹啉和巯基苯骈噻唑为萃取剂，以活性硅胶为载体的柱式萃取色谱法对环境水中Ｚｎ、Ｃｕ、Ｐｂ、Ｃｄ、Ｆｅ、Ｃｏ、Ｎｉ和Ｍｎ的最佳富集和洗脱条件。     

轻质萃取剂的分散液液微萃取-石墨炉原子吸收光谱法测定生活用水中痕量Pb与Cd

以轻质溶剂辛醇为萃取剂,建立了分散液液微萃取-石墨炉原子吸收光谱分析法(LDS-DLLME-GFAAS),并应用于生活用水中痕量Pb及Cd的测定。在分散液液微萃取(DLLME)中,以二乙基二硫代氨基甲酸盐(DDTC)为螯合剂,用微量注射器将辛醇和甲醇的混合溶液快速注入到样品溶液中发生雾化分散现象,Pb2+和Cd2+与DDTC的络合物被萃取到辛醇微滴中。离心分离后,以GFAAS测定萃取至上层辛醇相中的分析物。实验考察了萃取剂种类和体积、分散剂种类和体积、pH、DDTC浓度、萃取时间等影响萃取效率的实验参数。在最优实验条件下,Pb和Cd的检出限分别为0.15和0.03 μg·L-1,富集倍数分别为87和48,具有良好的线性和精密度。该分析方法优势在于操作简便,快速,低成本,高富集倍数,萃取剂用量少,已成功应用于自来水、饮用水和南湖水中痕量Pb和Cd的检测。     

1-亚硝基-2-萘酚为配合剂流动注射固相富集原子吸收光谱法测定铜和钴

本文研究了用１－亚硝基－２－萘酚为配合剂，Ｃ１８键合硅胶为固相富集材料，流动注射在线固相萃取预富集火焰原子吸收测定痕量和钴的方法。该方法自动化程度高，选择性强，方法的采样速度达９０ｈ＾－１时，铜和钴的订九分别达２０倍和１８倍，检出限分别达１．８μｇ／Ｌ和３μｇ／Ｌ。用这一方法来测定生物样品淡菜、钢样ＮＢＳ－３６４和ＮＢＳ－３６２等标准样品，结果与标准值相符。     

纳米粒子修饰硅胶整体柱的制备及其在柱表面增强拉曼光谱应用研究

通过溶胶-凝胶法以四甲氧基硅烷(TMOS)和甲基三甲氧基硅烷(MTMS)作为混合的前体,聚乙二醇(PEG)为致孔剂,制备了具有贯通孔道结构的双孔硅胶整体柱,采用3-巯基丙基三甲氧基硅烷(MTPMS)对硅胶整体柱表面进行巯基化修饰后,分别将金、 银纳米粒子组装在整体柱材料表面。 利用透射电子显微镜(TEM)、 紫外-可见吸收光谱(UV-Vis)、 扫描电子显微镜(SEM)对金、 银纳米粒子形貌、 吸收光谱及组装金、 银纳米粒子前后整体柱的形貌进行了表征。 以对巯基苯胺(PATP)为探针分子,分别采用波长为633和532 nm的激发光作为激发光源,研究金和银纳米粒子修饰的硅胶整体柱的在柱表面增强拉曼光谱(SERS)性能。 结果表明,该基底呈现出很强的SERS活性,结合整体柱的分离富集优势将在食品/环境领域现场痕量检测方面具有广泛的应用前景。     

固相萃取富集高效液相色谱法测定卷烟烟气中的铅、镉和汞

研究了用固相萃取富集,柱前衍生高效液相色谱法测定卷烟烟气中的铅、镉、汞的方法.卷烟烟气样品经剑桥滤片捕集,用四-(对甲氧基苯基)-卟啉(T4 MPP)柱前衍生卷烟烟气中的重金属元素:铅、镉、汞.采用C18固相萃取小柱萃取富集铅、镉、汞的卟啉T4MPP络合物,以Waters Xterra RPl8色谱柱为固定相,甲醇和四氢呋喃为流动相梯度洗脱,用光二级管矩阵检测器检测.铅、隔、汞的捡出限在0.02-0.03μg/L之间.方法相对标准偏差小于2.3％,加标回收率为95％-102％.该方法用于测定卷烟烟气中的重金属元素铅、镉和汞,结果可靠,令人满意.     

浊点萃取-石墨炉原子吸收光谱法测定环境水样中痕量镉的研究

提出了1-(2-噻唑偶氮)-2-萘酚(TAN)浊点萃取石墨炉原子吸收光谱法测定痕量镉的新方法.详细探讨了溶液pH,试剂浓度等实验条件对浊点萃取及测定灵敏度的影响.在最佳条件下.富集10mL样品溶液,用石墨炉原子吸收光谱法测定.镉的检出限为0.037ug/L,镉的富集倍率为20倍.该方法用于环境水样中痕量镉的测定.获得满意结果.     

微珠析相微萃取-石墨炉原子吸收法测定岩石样品中痕量铬

采用二苯碳酰二肼为络合剂,正戊醇为萃取剂,乙醇为助溶剂,建立了微珠析相微萃取-石墨炉原子吸收法测定地质样品中痕量Cr的分析方法。实验详细探讨了微珠析相微萃取的析相条件、石墨炉原子吸收工作参数及共存离子的干扰,优化了体系萃取条件。实验结果表明：微珠析相微萃取既起到了分离富集的作用,在石墨炉升温程序中又起到了基体改进剂的作用;当萃取剂用量为0.2～1.5 mL时,使之与水完全互溶所需助溶剂体积约为水相体积的0.2～0.5倍;方法线性范围为0～10 μg·L-1,检出限为0.057 μg·L-1,相对标准偏差（RSD）为3.3%（c= 2.5 μg·L-1,n=11）;当萃取剂用量为1.5 mL、水相体积15 mL时,与直接溶液进样相比其灵敏度可提高10倍。所建立的方法用于地质标准参考物质AGV-2和G-2中Cr的测定,测定值与参考值具有较好的一致性。     

萃取色谱在线预浓集流动注射原子吸收光谱测定地质样品中痕量银

选用三苯膦萃取色谱柱，在线预浓集与分离地质样品中痕量银、建立了流动注射火焰原子吸收光谱测定的方法。     

MBM新型螯合纤维素富集原子吸收测定痕量铅,镉,铜和镍

螯合纤维素制备工艺简单，性能优越，成本低廉。本文运用间接醚化法将优良的重金属螯合剂２－巯基苯并咪唑接枝于棉纤维上，合成了２－巯基苯并咪唑新型螯合纤维素（ＣＣ－ＭＢＭ），通过选择最佳条件，达到了在一个水样中同时富集和洗脱铅、镉、铜、镍、结果表明，ＣＣ－ＭＢＭ用于痕量元素的分离富集具有交换速度快易于解脱，富集倍数大，选择好性等优点，样品测定结果令人满意。     

巯基棉富集─火焰原子吸收分光光度法测定水中的微量铁

本文详细考查了巯基棉富集Ｆｅ（Ⅲ）的条件，发现微量铁（Ⅲ）在ｐＨ值为５－８的条件下能为巯基棉定量吸附．１ｍｏｌ／Ｌ盐酸５ｍＬ能将巯基棉吸附的Ｆｅ（Ⅲ）定量洗脱，０．１ｇ巯基棉的饱和吸附量为９０μｇ，样品分析测定结果的相对标准偏差小于３．４％，９８．４％－９８．８％。     

Release studies of corrosion inhibitors from cerium titanium oxide nanocontainers

Cerium titanium oxide nanocontainers were synthesized through a two-step process and then loaded with corrosion inhibitors 2-mercaptobenzothiazole (2-MB) and 8-hydroxyquinoline (8-HQ). First, polystyrene nanospheres (PS) were produced using polymerization in suspension. Second, the PS spheres were coated via the sol–gel method to form a cerium titanium oxide layer. Finally, the nanocontainers were made by calcination of the coated PS nanospheres. The size of the containers was 180 ± 10 nm as determined by Scanning Electron Microscopy (SEM). X-Ray Diffraction Analysis (XRD) showed that the nanocontainers consist of anatase and cerianite crystalline phases. The presence and loading of the inhibitors in the nanocontainers was confirmed with Fourier Transform Infrared Spectroscopy (FT–IR) and Thermo Gravimetric Analysis (TGA), respectively. TGA revealed the amount of 10.43 and 4.61% w/w for 2-MB and 8-HQ in the nanocontainers, respectively. Furthermore, the release kinetics of the inhibitors from the nanocontainers was studied in corrosive environment using electrochemical impedance spectroscopy (EIS) in the presence of aluminum alloys 2024-T3 (AA2024-T3).     

Synthesis and Characterization of 8-hydroxyquinoline Complexes of Tin(IV) and Their Application in Organic Light Emitting Diode

A series of 8-hydroxyquinoline complexes of tin, Q(2)SnCl(2) (Q?=?2-methyl-8-hydroxyquinoline, 8-hydroxyquinoline, 5,7-dibromo-8-hydroxyquinoline, 5-chloro-8-hydroxyquinoline, 5,7-dichloro-8-hydroxyquinoline and 5-nitro-8-hydroxyquinoline) were prepared by reacting stannous dichloride with 8-hydroxyquinoline and its derivatives. All complexes were characterized by elemental analysis, mass spectrometry and infrared, UV-vis and (1)H NMR spectroscopes. Furthermore, the molecular structure of a representative complex, dichlorido-bis(5-nitro-quinolin-8-olato-2N,O)tin(IV), was determined by single-crystal X-ray diffraction. The photoluminescence (PL) properties of all prepared compounds and electroluminescence (EL) property of a selected complex (Q?=?5-chloro-8-hydroxyquinoline) were investigated. The results showed that the emission wavelength can be tuned by electron donating or withdrawing group substituent on 8-hydroxyquinoline. Application of prepared complexes in fabrication of an OLED has been demonstrated.     

高相对分子质量8-羟基喹啉锂聚合物的制备和性能

高分子电致发光显示器(PLED)是近几年来国际、国内的研究热点,取得了很大的进展,其中高分子化金属配合物是一类很有价值的功能材料。通过甲基丙烯酸甲酯(MMA)、苯乙烯(S)和含有8-羟基喹啉的单体共聚合成模板聚合物,再与氢氧化锂作用,实现了8-羟基喹啉锂配合物的高分子化,获得了一种能够溶解在普通的溶剂中的高相对分子质量的含喹啉锂配合物的发光聚合物,并利用元素分析、¹H-NMR、FTIR、UV、PL光谱、DSC、TGA、GPC等方法对其结构和性能作了表征。紫外吸收和光致发光(PL)光谱说明合成共聚物的发光来自于Liq基团,引入的可聚合的链段以及共聚物中的甲基丙烯酸甲酯或苯乙烯链段,并没有影响发光波长的改变。亲核溶剂改变8-羟基喹啉金属配合物分子结构,使共聚物光谱明显红移20nm左右。     

铟(Ⅲ)荧光探针与核酸作用机理的光谱研究

应用荧光和紫外可见光谱技术 ,研究了铟 ( )荧光探针与核酸作用的影响因素 ,探讨了体系的作用机理。在 p H7.5和低离子强度条件下 ,荧光探针与核酸发生了沟内结合作用 ,对体系产生了明显的荧光增强作用     

三元配合物H[Ni（C7H4O4）（C9H6NO）]·2.5H2O的合成与表征

以2,4-二羟基苯甲酸和8-羟基喹啉为配体,以Ni2+作为中心原子,合成了一种新的三元固体配合物H[Ni(C7H4O4)(C9H6NO)]·2.5H2O,并采用元素分析、IR光谱和TG-DSC分析对它的结构进行了表征。结果表明,在该配合物中,2,4-二羟基苯甲酸配体以羧基O原子和一个羟基O原子与中心原子配位,8-羟基喹啉配体以羟基O原子和喹啉N原子与中心原子配位,配合物的配位数为4。     

Effect of Gamma Radiation on the IR Spectra of Some Divalent and Trivalent 8-Hydroxyquinoline Complexes

The I R spectra of ten elements chelated with 8-hydroxyquinoline were measured before and after gamma irradiation with different doses (7–518 Mrd) and discussed. It was found that the rate of decrease, K, of the absorbancy of M—O and (C—O)-M stretching vibration bands depends on the chelated cation. Moreover, the Cu 8-hydroxyquinoline complex is suggested as gamma dosimeter for doses ranging from 4.8 to 160 Mrd.     

Formation of mono(8-hydroxyquinoline) lithium(I) complex in smectites by solid-solid reactions

Lithium quinolate including mono(8-hydroxyquinoline) lithium(I) complex (Liq) formed in the interlayer spaces of two smectites via solid-solid reactions and in situ complex formation by reacting Li-smectites (Li(I)-synthetic saponite and Li(I)-montmorillonite) with 8-hydroxyquinoline at room temperature. The incorporation of 8-hydroxyquinoline into Li(I)-smectites was proved by powder X-ray diffraction, infrared spectroscopy, thermal and elemental (CHN) analysis. UV-vis absorption and photoluminescence spectra indicated that 8-hydroxyquinoline ligand formed Liq chelate in the interlayer spaces of smectites. The higher luminescence intensity of the Liq complex in synthetic saponite confirmed the very low content of quenching impurities such as iron in the synthetic saponite. The variation of the photoluminescence bands supported the difference in molecular packing and/or crystal structure of the complex formed in the interlayer spaces of smectites.     

发光性质可调的金属-有机骨架材料 的合成及发光性质

以对苯二甲酸(H₂BDC)为配体,以锌为中心离子,采用沉淀法合成了具有一维结构的金属配合物 纳米晶,将化合物分散到不同浓度的8-羟基喹啉(8-Hq)溶液中,得到系列配位聚合物 。分别用FT-IR和XRD对目标产物的结构进行了表征。固态发光性质研究显示: 及其配位聚合物具有强的发光,配位聚合物随着8-Hq量的增加,其发光发射光谱有规律地红移,表明该配位聚合物能够通过改变8-Hq与骨架材料间的量的比实现对材料发光性质的调控。     

8－羟基喹啉稀土螯合物有机薄膜电致发光研究

自1989年C.W.Tang的高性能有机电致发光(Electro-luminescence,即EL)器件工作发表以来[1],有机薄膜EL有可能成为一种新型的大面积平板显示器件.     

In situ formation of bis(8-hydroxyquinoline) zinc(II) complex in the interlayer spaces of smectites by solid–solid reactions

Bis(8-hydroxyquinoline) zinc(II) complex (Znq₂), an electroluminescent material used for organic light emitting devices (OLEDS), formed in the interlayer spaces of smectites by solid–solid reactions between Zn(II)-smectites (Zn(II)-synthetic saponite and Zn(II)-montmorillonite) and 8-hydroxyquinoline at ambient condition. The intercalation of 8-hydroxyquinoline molecules into Zn(II)-smectites and the in situ complex formation of Znq₂ chelate in smectites were confirmed by powder XRD, FT-IR, TG–DTA, UV–vis absorption and photoluminescence spectroscopies, and elemental (CHN) analysis. The photoluminescence intensity of the Znq₂ complex in synthetic saponite was higher than that of the complex in montmorillonite, suggesting the very low content of quenching impurities in synthetic saponite. The difference in the luminescence bands were thought to be caused by the different molecular structure and molecular packing of the complex formed in the interlayer spaces.