Cu(Ⅱ)-头孢羟氨苄的荧光光谱性质及应用

采用不同的表面活性剂对Cu(Ⅱ)与头孢羟氨苄生成的配合物在胶束体系中的荧光性质进行了研究,发现在pH6.2的Tris缓冲溶液中阴离子表面活性剂十二烷基硫酸钠对其配合物的荧光有显著的增敏作用,据此建立了胶束增敏荧光光谱法测定头孢羟氨苄的新方法。在最佳实验条件下其线性范围为0.03~1.14μg/mL,检出限为0.03μg/mL,经实际样品测定,其平均回收率为97.3%~101.4%,相对标准偏差为1.1%~1.3%。     

胶束增敏荧光光谱法测定恩诺沙星的含量

研究了恩诺沙星(EFLX)在胶束体系中的荧光特性,发现十二烷基硫酸钠(SDS)对EFLX有较强的增敏作用,据此建立了胶束增敏荧光光谱法测定恩诺沙星的新方法。方法的线性范围为0-0.64μg/mL,检出限为4.75 ng/mL。     

胶束增敏法测定盐酸左氧氟沙星的研究

研究了盐酸左氧氟沙星（OFLX）在胶束体系中的荧光性质,发现十二烷基硫酸钠对OFLX有较强的增敏作用,据此建立了胶束增敏荧光光谱法测定痕量OFLX的新方法。其线性范围为0～1．00μg/mL,检出限为4．73ng／mL。     

洛美沙星在胶束体系中的荧光特性研究及应用

研究了洛美沙星在胶束中的荧光特性,发现十二烷基磺酸钠(SDS)对洛美沙星的荧光有较强的增敏作用。据此,提出了胶束增敏荧光光谱法测定痕量洛美沙星的新方法,洛美沙星含量在0.04~4μg/mL范围内与其荧光强度线性关系良好,相关系数r=0.9995。方法的平均回收率为96.2%~100.8%。     

荧光分析法测定维生素C

维生素C经Cu2 氧化为脱氢抗坏血酸,与苯甲酸及十六烷基三甲基溴化铵产生荧光协同增敏作用。提出一种新的测定维生素C的高灵敏荧光分析法,建立了测定维生素C的适合条件。该方法的的线性范围为0.02~8.0μg/mL,检出限为0.006 5μg/mL。对3.0μg/mL的维生素C测定6次,测定结果的相对标准偏差为0.12%。将该法用于西红柿、果珍以及维生素C药片中维生素C含量的测定,加标回收率为96.7%~100.5%。     

荧光分析法测定荜茇有效成分荜茇宁

根据荜茇有效成分荜茇宁的荧光被表面活性剂OP-10显著增敏的特征,提出了胶束增敏荧光法测定蒙药荜茇中荜茇宁的荧光分析新方法.荜茇宁的含量在2.0～16.0μg/mL范围内,与其荧光强度呈良好的线性关系,相关系数为0.9992,方法的回收率为96.9%～104.5%.此方法适合蒙药荜茇中荜茇宁的测定.     

胶束增敏荧光光谱法测定吡哌酸

采用不同表面活性剂对吡哌酸在胶束体系中的荧光性质进行了研究，发现在酸性介质中十二烷基硫酸钠(SDS)对吡哌酸有较强的增敏作用，据此建立了胶束增敏荧光光谱法测定吡哌酸的新方法。方法线性范围为0．07-0．36μg／mL，检出限为0.04μg／mL，平均回收率为98．6％-101．3％，相对标准偏差为1．1％-1．2％。样品测定结果令人满意。     

碘化物-CTMAB体系共振光散射法测定电镀废水中的钯

用简易荧光计研究了在微酸性介质中钯-碘化钾-溴化十六烷基三甲基铵体系的共振光散射光谱,考查了光谱特征、影响因素和适宜的反应条件,确定了散射光强度与溶液中钯浓度的关系,提出了共振光散射法测定钯的方法。钯的线性范围为0.0~0.5μg/mL,检出限为0.005μg/mL。该法可用于电镀废水中钯浓度的测定。     

钒(Ⅴ)-桑色素-溴化十六烷基三甲铵胶束增敏荧光光度法的研究和应用

研究了在 p H 2 .5的 HCl- Na Ac介质中 ,溴化十六烷基三甲铵( CTMAB)对桑色素 ( morin)和钒 ( )配合物荧光的增敏作用 ,建立了利用钒 ( ) - morin- CTMAB胶束增敏荧光反应测定痕量钒的荧光光度新方法。方法的检出限为 0 .92μg/L ,荧光强度与钒的含量在 0 .0 1 0～ 6.0μg/1 0 m L范围内呈线性关系 ,配合物中钒 ( )与桑色素的组成比为 :V( )∶ morin=1∶ 1。方法可应用于天然水和食品中微量钒的测定     

胶束增敏分光光度法测定赖氨酸

研究表明赖氨酸与甲酚红在水溶液中可形成紫色络合物,溴化十六烷基三甲基胺(CTMAB)对该络合物有显著的增敏增稳作用。据此建立了胶束增敏光度法测定赖氨酸含量的新方法,方法的线性范围为0.028~0.175μg/mL,检出限为0.015μg/mL。该法用于药物制剂中赖氨酸含量的测定,回收率在98.0%~101.7%之间。     

Determination of trace amounts of Pd(II) ions in water and road dust samples by flame atomic absorption spectrometry after preconcentration on modified organo nanoclay

This paper describes the application of organo nanoclay, an easily prepared and stable solid sorbent, to the preconcentration of trace amounts of palladium ions in aqueous solution. The organo nanoclay was prepared by adding tetradecyldimethylbenzylamonium chloride onto montmorillonite, which was then modified with 1-(2-pyridylazo)-2-naphthol. The modified nanoclay was used as a solid sorbent for separation and preconcentration of trace amounts of Pd(II) ions, and a simple, sensitive, and economical method was developed for determination of trace amounts of palladium by flame atomic absorption spectrometry. The sorption of Pd(II) ions was quantitative in the pH range of 1.5-5.0, whereas quantitative desorption occurred with 5.0 mL of a mixture containing 1.0 M thiourea and 1.0 M HCl. The RSD of the method was +/- 2.1% (n = 10; concn = 0.5 microg/mL), and the LOD (3sigma(bl); sigma = SD and bl = blank) was 0.1 ng/mL. The calibration curve was linear for concentrations of 0.5-8.0 microg/mL in the initial solution, and the preconcentration factor was 140. The maximum capacity of the sorbent was 2.4 mg Pd(II)/g modified organo nanoclay. The influences of the experimental parameters, including sample pH, eluant volume, eluant type, sample volume, and interfering ions, on the recoveries of the palladium ion were investigated. The proposed method was applied to the preconcentration and determination of palladium in different samples.     

Online Separation and Preconcentration of Gold and Palladium on Amidinothiourea Immobilized Glass Bead for Interference-Free Flame Atom Absorption Spectrometry Determination

Amidinothiourea immobilized glass bead (AGB) was applied as the microcolumn packing for the flow-injection online separation and preconcentration of Au(III) and Pd(II) coupled with FAAS determination. The peak-area absorbance (A) and the peak-height absorbance (H) were all used as the evaluating modes. Au(III) and Pd(II) in 0.50 M HCl solution were absorbed onto AGB completely and then eluted into AAS with thiourea solution. Base metal ions with a concentration of 2.0 mg/mL and anions with a concentration of 20.0 mg/mL caused no interference in the determination of Au(III) and Pd(II). The LODs of Au(III) and Pd(II) for a preconcentration time of 60 s with a sampling flow rate of 5.0 mL/min for 0.20 μg/mL of Au(III) and 0.30 μg/mL of Pd(II) were 2.7 and 6.5 ng/mL with the H mode and 4.6 and 10.2 ng/mL with the A mode, respectively. The RSD of seven replicate determinations of 0.20 μg/mL of Au(III) and 0.30 μg/mL of Pd(II) were 0.018 and 0.024 for the H mode and 0.013 and 0.018 for the A mode, respectively. The method was successfully applied to the determination of Au and Pd in real samples. __________ From Zhurnal Analiticheskoi Khimii, Vol. 60, No. 10, 2005, pp. 1023–1029. Original English Text Copyright ? 2005 by Liu, Pu, Su. The text was submitted by the authors in English.     

亮绿褪色反应用于微量季铵盐型阳离子表面活性剂的分光光度法测定研究

在 p H 7.0 0 Tris- HCl缓冲介质中 ,微量季铵盐型阳离子表面活性剂溴化十六烷基三甲胺 ( CTMAB)和溴化十六烷基吡啶 ( CPB)能使亮绿 ( Brilliant Green,简称 BG)产生灵敏的褪色反应 ,发现其褪色程度ΔA (ΔA =A0 - Ai)与 CTMAB及 CPB用量存在定量关系。研究了该褪色反应的最佳条件 ,探讨了反应机理 ,拟定了利用该反应用于微量 CTMAB和 CPB的测定方法 ,CTMAB和 CPB的浓度分别在0～ 6× 1 0 - 5mol/ L ,0～ 8× 1 0 - 5mol/ L范围内符合比耳定律。拟定的方法用于电镀废液样品中微量 CTMAB的测定 ,结果满意     

Sorption preconcentration and separation of Palladium(II) and Platinum(IV) for visual test and densitometric determination

We have demonstrated the advantages of the dynamic preconcentration and separation of Pd(II) and Pt(IV) on paper carriers modified with 3-methyl-2,6-dimercapto-1,4-thiopyrone. The optimal conditions of the solid-phase reaction have been determined in Pd(II) sorption; after its separation Pt(IV), has been preconcentrated by sorption as its dimercaptides. Test scales have been produced for the visual determination of 0.5–40 μg Pd(II) and 1–195 μg Pt(IV) in 10- and 100 mL-samples, respectively. In addition, a procedure of their sorption-chromaticity densitometry determination from a single aliquot portion has been developed with detection limits of 5 and 1 ng/mL, respectively, and a procedure of Pd(II) determination using a test strip (c _min = 0.40 mg/L) has been proposed. The procedures have been applied to the determination of palladium and platinum in electrolytes, sludges, and alloys.     

1-(5-萘酚-7-磺酸)-3-[4-(苯基偶氮)苯基]-三氮烯的合成及与阳离子表面活性剂的显色反应

报道了1-（5-萘酚-7-磺酸）-3-[4-（苯基偶氮）苯基]-三氮烯（NASAPAPT）的合成，研究了该试剂与阳离子表面活性剂溴化十二烷基二甲基苄铵（DDMBAB），溴化十六烷基三甲铵（CTMAB）、溴化十六烷基吡啶（CPB）、溴化十四烷基吡啶（TPB）显色反应的条件。测定了显色反应的灵敏度，符合比尔定律的范围。建立了光度法测定微量阳离子表面活性剂的新方法。     

二正辛基亚砜萃取钯(II)和金(III)的动力学研究

应用连续自动测定的恒界面池装置, 研究了二正辛基亚砜(DOSO)在盐酸介质中萃取钯(II)和金(III)的动力学行为。得以了各自的萃取速率方程和表观活化能。测定了DOSO的两相分配和界面吸附性能。结果表明, DOSO萃取钯(II)为界面配本取代反应控制类型, 而萃取金(III)则为扩散或混合控制类型。     

表面活性剂对脂肪酶活性和选择性的影响

考察了几种表面活性剂对lipaseOF粗酶和纯化酶催化拆分酮基布洛芬的影响。除吐温-80,吐温-60和壬基酚聚氧乙烯醚外,大部分表面活性剂对酶活性有抑制作用,其中只有吐温-80能显著提高酶的立体选择性。酶的活性和选择性与表面活性剂浓度有关。在表面活性剂浓度为最佳(20mg/mL吐温-80或30mg/mL壬基酚聚氧乙烯醚)时lipaseOF粗酶的活性可分别提高13和15倍。加入80mg/mL吐温-80,粗酶和纯化酶的对映体选择率(E值)分别由1.1和8.0增至6.7和>100。     

废水中的阴离子表面活性剂的测定

十六烷基三甲基溴化铵 ( CTMAB)、溴甲酚紫 ( BCP)和阴离子表面活性剂三者在 p H 7.0 0的条件下可形成有色离子缔合物 ,据此建立了 CTMAB- BCP分光光度法测定阴离子表面活性剂的方法。在 75μg CTMAB存在下 ,十二烷基硫酸钠 ( SDS)在 0～ 5 0 μg范围内符合比耳定律 ,其表观摩尔吸光系数是 2 .74× 1 0 4 L· mol- 1·cm- 1,并用标准加入法和主成分回归法不分离干扰可直接测定。应用此方法测定了河水、池塘水和生活污水中的阴离子表面活性剂 (以 SDS计 )并与亚甲蓝法进行比较 ,结果满意     

Bi(Ⅲ)-茜素红-CTMAB体系共振散射光谱法测定环境水样中痕量铋

在pH=4.1的HCl溶液中,Bi(Ⅲ)与茜素红和十六烷基三甲基溴化铵（CTMAB）缔合形成粒径较大的疏水性三元离子缔合物（结合比为n(Bi(Ⅲ))∶n(AR)∶n(CTMAB)=1∶3∶3）,该反应导致共振光散射显著增强,最大散射峰位于364 nm。 研究了反应介质、pH值、共振探针浓度等对散射体系的影响,考察了该散射反应的稳定性及共存物质的影响,并对该三元离子缔合物的反应机理进行了探讨。 在2.5 mL 1.0×10-4 mol/L茜素红和2.0 mL 1.0×10-4 mol/L CTMAB最优试验条件下,Bi(Ⅲ)质量浓度与共振光散射强度ΔI364 nm在0～0.384 mg/L范围内呈良好线性关系,检测限为5.898×10-8 g/L,对含量为0.18 mg/L Bi(Ⅲ)溶液进行11次平行测定,其相对标准偏差为2.2%。 将该方法用于环境水样中痕量铋(质量浓度为0.552～0.831 μg/L)的测定,加标回收率为99.5%～100.2%,测定偏差小于2.7%。 基于Bi(Ⅲ)-AR-CTMAB三元离子缔合物的共振光散射光谱,建立了以茜素红染料为光谱探针的痕量Bi(Ⅲ)共振光散射检测新方法。     

Interference-free determination of trace levels of gold and palladium in geological and metallurgical samples by flame atomic absorption spectrometry coupled with a flow injection on-line microcolumn preconcentration and separation system

A simple and highly selective method was developed for the routine determination of trace or ultratrace amounts of gold and palladium in geological and metallurgical samples. The method uses flow injection on-line preconcentration and separation with determination by flame atomic absorption spectrometry. Au and Pd in the sample are adsorbed on a 2-mercaptopyrimidine chemically modified silica gel (MPMSG) packed microcolumn in a 0.50M HCl medium and then eluted with 0.5 or 1.0% thiourea solution. The eluates are introduced into the flame atomic absorption spectrometer directly. With the use of a 0.85 mL microcolumn (about 0.14 g MPMSG packed), the present system tolerated concentrations of common base metal ions up to 25.0 mg/mL and concentrations of anions up to 100.0 mg/mL when Au(III) at 0.100 microg/mL and Pd(II) at 0.200 microg/mL were preconcentrated for 60 s with a sample flow rate of 5.0 mL/min. The limits of detection were 3.1 ng/mL for Au(III) and 6.1 ng/mL for Pd(II) with relative standard deviations of < or = 2.5%. The analytical results obtained by the proposed method for geological and metallurgical samples were in good agreement with the certified values.