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邻硝基苯基荧光酮褪色分光光度法测定痕量钴 总被引:6,自引:0,他引:6
研究了Co(Ⅱ)在碱性介质催化过化氢氧化邻硝基苯基荧光酮(o-NPF)这一主影响反应 因素,建立了测定痕量Co(Ⅱ)的新方法。灵敏度为4.3×106-10g/L;测定范围为0 ̄0.5ng/25mL方法简便快速,用于药物维生素B12中Co(Ⅱ)含量的测定,样品分析结果良好。 相似文献
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1,9-二(4-安替比林偶氮)嘌呤酮与钯的显色反应及其用于光度法测定钯 总被引:1,自引:0,他引:1
1引言 新合成的试剂1,9-二[4-安替比林偶氮]嘌呤酮(BAPD),在pH=4.50.的HAc-NaAc缓冲溶液中与Pd(Ⅱ)生成稳定的红色络合物,其λmax= 510 nm,把含量在0. 12~2.4 mg/L范围内与吸光度呈线性关系。据此建立了测定Pd(Ⅱ)的分析方法,并应用于电镀液和镀层中钯含量的测定。2实验部分2.1仪器与试剂 DU-7 HS型分光光度计(美国 Beckman公司);760 CRT型紫外-可见光分光光度计(上海第三分析仪器厂);HM-20E型酸度计(日本TOA公司)。钯标准溶液… 相似文献
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苯酚对固定在增塑的聚氯乙烯(PVC)敏感膜中的2,2,7,7,12,12,17,17-八甲基-21,22,23,24-四氧杂四烯(TOE)有可逆荧光增强作用,据此研制了测定水溶液中苯酚含量的荧光化学传感器。该敏感膜最佳组成为:50mg PVC、100mg癸二酸二异辛脂(DOS)、1.5 mg TOE。该传感器在pH7.4的 Tris/HCl缓冲溶液中,对苯酚的线性响应范围为4.47×l0~(-6)~4.17×10~(-3)mol/L;检出限为6.30×l0~(-7)mol/L;其响应时间小于30s。该传感器具有良好的重现性、可逆性和选择性,常见阴离子和阳离子不干扰测定。该传感器应用于工业废水中苯酚含量的测定,结果满意。 相似文献
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流动注射—氢化物发生—非色散原子荧光光谱法直接测定海水中的砷(Ⅲ)和砷( 总被引:7,自引:0,他引:7
用流动注射-氢化物发生-非色散原子荧光光谱法对海水中As(Ⅲ)和As(Ⅴ)的直接测定进行了研究,氢化物发生的最佳条件为:KHB4溶液浓度为5g.L^-1(含KOH5g.L^-1),流速10.0mL.min^-1;样品酸度为1.3mol.L^-1HCl,流速4.2mL.min^-1。对基体NaCl,MgCl2,CaCl2,Na2SO4以及微量共存金属离子(Cd,Zn,Pd,Cu)的干扰实验结果表明,基体和微量共存金属离子对As(Ⅲ)的测定没有干扰。样品中As(Ⅴ)的测定用硫脲进行预还原,通过总量和As(Ⅲ)的含量的差减得到As(Ⅴ)含量,在优化实验条件下下测量方法的检出限(3σ)为0.08ng.mL^-1;7次测定的相对标准偏差为0.48%-1.30%(8.0ng.mL^-1标准溶液)。标准曲线和标准加入法对海水 相似文献
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本文报告了在0.01mol/LCTAB体系中,以F-为掩蔽剂、苯芴酮显色、用分光光度法测定饮料食品中Ge-132含量,最低检测限0.054μg/mL;线性范围0.54~27.14μg/mL;回收率96.3%~101.5%,并确定了Ge-132摩尔吸收系数(ε)3.39×104。用本法测定了康寿茶、矿泉水和博士奶中Ge-132含量,灵敏度高、重现性和准确度好。用盐酸化本体系,研究了二氧化锗(Ge~(4+))的含量测定,其最低检测限0.021μg/mL;线性范围1.0~21.0μg/ml;回收率95.8%~102.8%,Ge-132不干扰。饮料食品中同时存在Ge-132和Ge(4+)时,本体系可分别测定两者含量。 相似文献
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A rapid and simple method is described for the simultaneous determination of methyl, ethyl, isopropyl, n-propyl, isobutyl and n-butyl p-hydroxybenzoic acid esters (parabens) in cosmetics by high-performance liquid chromatography (HPLC). The method involves a single extraction of parabens with diethyl ether and clean-up on a Sep-Pak Florisil cartridge. Fat-soluble excipients in the diethyl ether extracts are removed through the cartridges with hexane-chloroform (75:25). Parabens are then eluted from the cartridges with hexane-ethyl acetate (70:30) and determined by HPLC on a reversed-phase column with water-methanol (50:50) as the mobile phase using sec.-butylpraben as an internal standard. The method was applied to samples with complicated matrices such as cream, milk lotion, lotion and cleansing foam, and the recoveries were 99.0-102.3% with coefficients of variation of 0.3-1.2%. 相似文献
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液相色谱-大气压化学电离离子阱质谱法测定烟草中的游离茄尼醇 总被引:1,自引:0,他引:1
用液相色谱/大气压化学电离离子阱质谱建立了一种分析烟草中游离茄尼醇的方法。烟草样品用甲醇振荡提取30 min,在分析前无需进行其它前处理。在1.8μm快速分离C18色谱短柱上用V(甲醇)∶V(异丙醇)=85∶15等梯度洗脱实现了茄尼醇的快速分离。用不带碰撞能量的二级质谱全扫描选择监测离子m/z 613.6进行定量,检出限为0.4μg/L,RSD为1.1%,两种添加量的回收率分别为97%和99%。方法应用于不同烟草和烟草制品样品的检测分析。 相似文献
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高效液相色谱法测定烟叶提取物中茄尼醇的含量 总被引:29,自引:0,他引:29
采用硅胶色谱柱 ,以正己烷 异丙醇 (体积比为 98∶2 )混合液为流动相 ,在紫外检测波长设定为 2 15nm的高效液相色谱仪上测定了烟叶提取物中茄尼醇的含量。实验结果表明 :方法在茄尼醇进样量为 1μg~ 10 μg时有良好线性关系 (Y =16 6 2 0 4X - 32 5 3,r=0 9997) ;加标回收实验 (n =6 )的平均回收率为 98 1% ,RSD为 1 9% ;方法简便 ,有良好的精密度和准确性。 相似文献
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Guo Yu Xing Fan Xue‐Ming Dong Rui‐Yu Wang Yun‐Peng Zhao Hong‐Cun Bai Tian‐Sheng Zhao Qing‐Jie Guo Xian‐Yong Wei 《Journal of separation science》2020,43(4):839-846
Dayan lignite was subjected to thermal dissolution sequentially with cyclohexane, acetone, and methanol. Each thermal dissolution extract was subjected to further separation/enrichment using column chromatography, which was sequentially eluted with petroleum ether, a mixture of ethyl acetate and petroleum ether (vol:vol = 1:1), and ethyl acetate. The three thermal dissolution extracts and nine enrichment subfractions were characterized by an Orbitrap mass spectrometry equipped with an atmospheric pressure chemical ionization ion source. The mass spectrometry data were also statistically analyzed by principal component analysis, which can reduce the dimensionality of data and classify multiple samples according to principal components. Identified compounds in the extracts and subfractions are classified into eight classes according to the heteroatom distribution. Hydrocarbon class is mainly presented in the petroleum ether fraction, and oxygen class, nitrogen class, and oxygen‐nitrogen class are distributed in both petroleum ether/ethyl acetate and ethyl acetate subfractions. The combination of different analytical methods enhances the understanding of coal at the molecular level and provides important data for downstream refining processes. 相似文献
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The infrared laser induced decomposition of mixtures of ethyl acetate and isopropyl bromide has been studied. The ratio of the yields of products ethylene and propylene, arising from the unimolecular decomposition reactions: ethyl acetate → ethylene + acetic acid, and isopropyl bromide → propylene + hydrogen bromide, were measured as a function of the ratio of ethyl acetate to isopropyl bromide and pressure of added helium. The results indicate clearly that in these systems non-equilibrium behavior is found up to the highest pressures used (about one atmosphere). A two level kinetic model is suggested which qualitatively explains the observations. 相似文献
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Qingqing Wang Mangmang Shen Rong Cheng Asan Yang Yanping Zheng 《Physics and Chemistry of Liquids》2017,55(1):38-50
The solubility of valsartan in ethyl acetate + (butanone, isopropyl ether) binary solvent mixtures was measured at temperatures T = 278.15–323.15 K and pressure p = 0.1 MPa with a laser monitoring dynamic technique by a synthetic method. The experimental data were regressed by the modified Apelblat equation, the general single model and the hybrid model. The experimental data are well correlated with the above models because the mean deviations (MDs) are less than 3.79%. The mole fraction solubility of valsartan increases with increase in temperature and enrichment in butanone content, while it decreases with increased mole fraction of isopropyl ether at constant temperature. In addition, thermodynamic studies, including Gibbs energy, entropy and enthalpy, were calculated by van’t Hoff analysis. The results showed that the dissolution of valsartan in mixed solvents is endothermic, spontaneous and entropy-driven. 相似文献
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Binary azeotropic data have been measured at different pressures for ethyl acetate + heptane, methyl acetate + heptane, isopropyl acetate + hexane and isopropyl acetate + heptane by means of a wire band column. Additionally activity coefficients at infinite dilution have been determined for ethyl acetate and isopropyl acetate in decane and dodecane in the temperature range between 303.15 and 333.15 K with the help of the dilutor technique. Furthermore excess enthalpies for the binary systems methyl acetate + hexane, methyl acetate + decane, ethyl acetate + hexane and ethyl acetate + decane at 363.15 and 413.15 K have been studied with the help of isothermal flow calorimetry. Finally solid–liquid equilibria for the systems ethyl myristate + benzene and ethyl myristate + p-xylene have been investigated by a visual technique. All these data have been used for the revision and extension of the group interaction parameters of the group contribution method modified UNIFAC (Dortmund) and the group contribution equation of state VTPR. The experimental data was compared with the results predicted using the group contribution method modified UNIFAC (Dortmund) and the group contribution equation of state VTPR. 相似文献