New Photoluminescence Phenomena of Ge／SiO2 Glass Synthesized by Sol-gel Method

New Ge/SiO2 glasses have been synthesized by heating the GeO2/SiO2 dry gels under H2 gas at 700℃. The resulting fluorescence spectra show that this kind of Ge/SiO2 glasses emit strong photoluminescence at 392 nm (3.12 eV), medium strong photoluminescence at 600 nm (2.05 eV) and weak photoluminescence at 770 nm (1.60 eV) respectively. Possible photoluminescence mechanisms are also discussed based on the results of X-ray diffraction (XRD) and X-ray photoelectron spectra (XPS).     

采用溶胶-凝胶技术涂层的新型固相微萃取方法及其应用

将溶胶-凝胶技术应用于SPME固相涂层的制备,涂制的端羟基-聚二甲基硅氧烷固相涂层热稳定性好,萃取时间和解吸时间短,对极性化合物及非极性化合物均有较强的萃取富集能力。扫描电镜图显示涂层表面为多孔结构。采用该涂层的SPME方法在对环境样品的分析中获得了令人满意的效果。     

The Preparation of Perovskite Nano Powder by Sol-gel from DTPA and the Mechanism of Thermal Decomposition

Dy0.8Sr0.2FeO3 nano powder, a synthetic oxide, is made by sol-gel method from metal nitrate and diethylenetriaminepentaaeetic acid (DTPA), and the processing parameters are optimized.The process of the preparation, thermal decomposition and the property of the powder are studied by TG-DTA, IR, TEM, and XRD. The diameter of the average grain is about 70 nm. This new technique can be used in the preparation and the studying of ha‘no materials in the complex oxide system.     

Self-assembly of silica nanosheets on titanium fibers for solids-phase microex⁃traction of UV absorbers in environmental water samplesEI北大核心CSCD

Silica nanosheets （SiO2NSs）were successfully assembled on titanium （Ti）wires by sol-gel method. TiO2 nanosheets （TiO2NSs）were grown in situ on Ti wires using anodic oxidation in a fluoride-containing electrolyte to obtain Ti@TiO2NSs. The Ti@TiO2NSs@SiO2NSs fibers were obtained by coating Ti@TiO2NSs with SiO2NSs. It was characterized by scanning electron microscopy （SEM） and X-ray energy dispersive spectroscopy （EDS）. The fibers were used for solid-phase microextraction of ultraviolet absorbers （UVFs）. Under the optimized conditions, six UVFs presented good linearity with the correlation coefficients （R2） greater than 0.999, and the limits of detection （LODs）ranged from 9 to 59 ng/L. The intra-day and inter-day relative standard deviations （RSDs） were from 4.3% to 5.1% and 4.6% to 5.8% for a single fiber at the spiked level of 25 μg/L, respectively. The developed method was successfully applied to the selective enrichment and determination of target UVFs in environmental water samples with recoveries from 93.2% to 108.1% and RSDs from 4.5% to 7.1%. Moreover, the fiber can be fabricated in a precisely controllable manner and is stable for at least 200 extraction and desorption cycles. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

溶胶-凝胶固相微萃取涂层及其在农药残留分析中的应用

利用溶胶-凝胶(sol-gel)技术制备固相微萃取(SPME)涂层材料.通过硅醇盐前驱体与涂层聚合物羟基硅油(OH-TSO)的水解共聚的方法,成功地制备了聚二甲基硅氧烷sol-gel 涂层的SPME 萃取头,并以农药的混合标准水溶液为研究对象,用直接-固相微萃取-气相色谱法(GC)对涂层的性能进行考察,制成的萃取头适用于多种农药残留的萃取分离分析.     

溶胶-凝胶法制备SE-54固相微萃取探针

固相微萃取(SPME)是一种样品制备技术。用来对样品中的有机分子进行富集萃取,已被广泛应用于痕量分析。然而,市售的SPME石英探针的表面涂渍层的最高允许使用温度只有270℃,实际在温度达200℃时固定相已经明显流失。其使用寿命只有40~100次。这是由于较厚的涂层用自由基引发固定     

聚酰亚胺/SiO2杂化材料固相微萃取涂层的制备及其应用

本文采用溶胶-凝胶技术制备了PI/SiO2固相微萃取涂层。由均苯四甲酸酐(PMDA)和4,4-二氨基二苯醚(ODA)共聚得到的聚酰胺酸,与四乙氧基硅烷水解产生的羟基进行缩合反应,通过γ-氨丙基三乙氧基硅烷偶联剂键合在石英纤维表面,经过高温脱水环化生成聚酰亚胺/二氧化硅复合固相微萃取涂层。通过红外光谱、热重分析、扫描电子显微镜对涂层的结构、热稳定性、表面形貌进行了分析。采用顶空固相微萃取-气相色谱联用法测定了水中的一氯代苯、邻二氯苯、间二氯苯,色谱峰面积与浓度呈良好的线性关系,线性相关系数(r)分别为0.9977、0.9988、0.9985,最低检测限分别为0.08mg/L、0.03mg/L、0.05mg/L,相对标准偏差(n=6)分别为6.34%、4.39%、4.76%。     

自制SPME涂层顶空萃取-气相色谱法分析废水中的芳香胺类化合物

建立了顶空固相微萃取与毛细管气相色谱法(HS—SPME-GC)测定废水中芳香胺类化合物的新方法。采用溶胶-凝胶法,自制新型单苯并冠醚探针．对萃取温度,萃取时间、解吸时间、离子强度和pH值等实验条件进行了优化选择：结果表明,该方法精密度良好,在标准溶液为0．1mg／L时,相对标准偏差(RSD)为4．0％～7．8％,线性范围为0．05～100μg/L,检出限达到0．005～0．01μg/L,加标回收率在97％～105％之间。运用该法对药厂废水中芳香胺类化合物进行了检测,结果令人满意由此可见,对环境中的芳香胺化合物进行检测,固相微萃取是一种快速、经济、有效的方法。     

网络互穿的固相微萃取聚乙烯醇复合涂层的制备

通过反复冷冻-解冻和溶胶-凝胶方法制备了聚乙烯醇/SiO₂有机/无机双交联网络互穿的固相微萃取涂层, 并利用红外光谱(FTIR)、 热重分析(TGA)、 扫描电子显微镜(SEM)和气相色谱(GC)等方法对该涂层进行了结构及性能表征. 该固相微萃取涂层具有很好的热稳定性(T_d>300 ℃), 通过化学键合作用于玻璃或石英纤维表面, 稳定性好, 不易脱落. 对正丙醇、 正丁醇、 异戊醇和甲苯进行萃取, 结果表明, 该纤维涂层对带有羟基的极性物质有很好的选择性, 并且相对标准偏差(RSD, n=3)小于5.0%.     

Perpentylated （2, 3, 6-Tri-O-pentyl）-β-cyclodextrin Used as Capillary Gas Chromatographic Stationary Phase Prepared by Sol-gel Technology

Capillary column preparation using perpentylated (2,3,6-tri-O-pentyl)-β-cyclodextrin as stationary phase by sol-gel technology with simplicity and rapidity is described. Multiple preparation steps in conventional column technology were avoided. The prepared columns exhibit satisfactory chromatographic performances and pronounced selectivity for a wide range of test solutes, and have been successfully used for the separation of nitrotoluene, dimethoxybenzene,alcohols, alkanes, dimethylphenol and cresol isomers.     

新型固相微萃取涂层直接检测样品中的3种多氯酚

利用聚乙二醇2000(PEG 2000)合成了聚乙二醇硅酯预聚物,并通过溶胶-凝胶法制备了含键合聚乙二醇硅酯的固相微萃取涂层,其使用最高温度为340℃。无需衍生化的情况下,采用顶空固相微萃取结合GC/FID的方法测定3种多氯酚的检出限为0.11~0.18 ng/L;线性范围达0.1~103μg/L,相对标准偏差(RSD,n=5)为4.24%~6.44%。土样中痕量多氯酚的加标回收率分别为108%、93.5%和73.7%。     

溶胶-凝胶法制备C18固相微萃取头及其在有机氯农药残留检测中的应用

以十八烷基三乙氧基硅烷(C18-TEOS)、四乙氧基硅烷(TEOS)、乙醇、盐和水酸为原料,采用溶胶-凝胶法制备了十八烷基(C18)固相微萃取头,利用所制备萃取头实现了水样中11种有机氯农药的检测。在优化条件下,使用该萃取头对有机氯农药(OCPs)萃取后用气相色谱/电子捕获检测器(GC/ECD)测定,检出限为0.01～0.24μg/L,相对标准偏差为3.0%～13.3%。该方法用于鱼塘水、湖水及自来水中OCPs的检测,结果满意。所制备的萃取头在不同溶剂中浸泡后,对有机氯农药的萃取性能无明显变化。使用50次后,C18萃取头的萃取性能未变化。结果表明,所制备的C18固相微萃取头涂层均匀,具有多孔结构,稳定性高,有很好的实用价值。     

Sol-Gel Method for the Preparation of Solid-Phase Microextraction Fibers

ABSTRACT

A novel sol-gel method is applied for the preparation of solid-phase microextraction (SPME) fibers. Scanning electron microscopy experiments suggested a porous structure for the poly(dimethylsiloxane) (PDMS) coating. SPME-GC analysis provided evidence that the sol-gel fibers have some advantages, such as high thermal stability, efficient extraction rates, high velocities of mass transfer, and spacious range of application.     

Solid-phase Microextraction of Volatile Polar Compounds in Water

A method was developed for the analysis of volatile polar compounds in a water matrix using open cap vials Solid Phase Micro-Extraction (SPME) and Capillary Gas Chromatography (CGC). Both SPME techniques – direct sampling and headspace – were tested. Optimization of experimental conditions – exposure time, desorption time, with headspace SPME in addition the influence of the temperature and ionic strength of the sample solution on compound sorption, and finally GC response – were investigated. The analytes were extracted by directly immersing the 85 μm polyacrylate fiber in the aqueous sample or in the headspace. The linear range of the preconcentration process and the precision were examined. The amount of polar analytes sorbed on the fiber was determined and was found to be concentration dependent; it amounted to 0.014–0.64% in the concentration range of 0.00425–425 ppm studied in aqueous solution for direct sampling SPME and to 0.011–2.76% for solutions of concentration 0.0425–255 ppm for headspace SPME. The limits of determination were ascertained. Headspace SPME was applied to the analysis of real-life samples.     

固相微萃取-气相色谱联用技术分析饮用水中的氯仿

利用顶空固相微萃取与气相色谱联用技术（ＨＳ－ＳＰＭＥ－ＧＣ）对饮用水中的氯仿进行了分析,并探讨了ＳＰＭＥ萃取头、吸附和热解吸时间对测定结果的影响;聚丙烯酸酯（ＰＡ）萃取头对水中的氯仿有较佳的富集效果,方法具有较好的重现性（ＲＳＤ为５．２３％,ｎ＝８）,线性范围为５～１００μｇ／Ｌ,检出限为３．４５μｇ／Ｌ。     

SPME/GC-MS测定水中痕量二苯氯胂

采用衍生化固相微萃取/气相色谱-质谱(GC-MS),对水中痕量二苯氯胂进行测定,考察了衍生化试剂、萃取纤维、萃取时间等因素对方法灵敏度的影响。测定二苯氯胂的线性范围为1.8~216μg/L,检出限为0.3μg/L(S/N=3),相对标准偏差为7.63%,回收率为95%~103%。     

固相微萃取-气相色谱法测定塑料食品包装袋中的痕量挥发性有机物

采用固相微萃取与气相色谱联用技术，对塑料制品-保鲜薄膜、牛奶包装袋中的痕量挥发性有机物异丙醇、乙酸乙酯、丁酮、甲苯进行定量测定．该方法的线性范围大于l0^2数量级，检出限低于4．4ng/mL水平，相对标准偏差为2.3％-4．7％．方法灵敏度高、重现性较好．     

固相微萃取与气相色谱质谱联用快速监测水中的萘及硝基萘

采用涂有聚二甲基硅酮的纤维快速吸附水中的萘、１－硝基萘和２－硝基萘，再利用气相色谱的气化室温度热解析纤维上的待测物。方法简单、灵敏，不需要使用任何有机萃取溶剂。该种类型纤维可较好地吸附萘及硝基萘。加入硫酸钠可改善样品的基质，增加纤维吸附量。监测水中的萘、１－硝基萘和２－硝基萘的方法检出限可分别达０．２５、０．３０、０．２０μｇ／Ｌ。     

羟基聚甲基苯基硅氧烷固相微萃取纤维的制备及在蔬菜中农药残留分析的应用

通过合成羟基聚甲基苯基硅氧烷(PMPS-OH)材料,制备固相微萃取(SPME)纤维涂层.通过与商品化聚二甲基硅氧烷(PDMS)、聚丙烯酸酯(PA)和PDMS/聚二乙烯基苯(DVB)纤维对六六六异构体(α,β,γ,δ-BHC)、DDT及其衍生物(p,p′-DDD,p,p′-DDE,o,p′-DDT,p,p′-DDT)、联苯菊酯、甲氰菊酯、高效氟氯氰菊酯、三氟氯氰菊酯、氯氰菊酯和氰戊菊酯等选定农药萃取效果的比较,所制备的PMPS-OH纤维具有更好的萃取效率.对SPME实验条件进行了研究和优化,测定方法对各种农药的线性范围多在0.01～2 ng/g之间,相应的检出限在0.001～0.05 ng/g范围,回收率在50.5%～103%.方法已被应用于蔬菜样品中农残的检测.