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流动注射在线分离富集—火焰原子吸收光谱法测定硫酸镍电解液中的?… 总被引:6,自引:6,他引:0
采用微型分离柱流动注射在线分离富集火焰原子吸收法测定硫酸镍电解液中的铅。用本法分析含铅量为1.33mg/L的试样,相对标准偏并为3.4%,检出限为0.03mg/L 相似文献
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流动注射膜分离测定水中的苯胺 总被引:3,自引:0,他引:3
本文提出了用硅橡胶膜在线分离的流动注射紫外度法测定水样中的苯胺。该方法的检出限为1mg/L,苯胺含量在2-200mg/L范围内呈良好的线性,对50mg/L试样12次测定的相对标准偏差为1.2%,1h能测35个样品。用本方法测定了几种水样中苯胺的含量,回收率均达90%以上。 相似文献
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用离子色谱法测定环境样品中甲酸、乙酸、草酸 总被引:12,自引:0,他引:12
用离子色谱法分析环境样品中甲酸、乙酸、草酸,操作简便,灵敏度较好,线性范围宽。甲酸、乙酸、草酸的检出限分别为0.02mg/L、0.10mg/L、0.04mg/L;样品加标回收率分别为93%~106%、94%~108%、92%~108%;相对标准偏差分别为1.2%、2.4%、2.7%;工作曲线的线性范围分别为0.00~30mg/L、0.00~30mg/L、0.00~50mg/L。该法可用于酸雨、大气 相似文献
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硫化物沉淀分离富集原子吸收法测定钢铁废水中的铋 总被引:4,自引:1,他引:4
本文研究了硫化物沉淀分离富集原子吸收法分析微量铋的方法,实验表明:在62.8mg/L,S^2-和0.14mol/LHNO3条件下,Bi^3+可与S^2-形成难溶化合物而从溶液中定量分离富集出来,溶解后借助原子吸收法测定,可用于钢铁废水中秘的分析,方法对铋的最低分析浓度为0.05mg/L,加标回收率为93.8%~110.0%相对标准偏差为2.9%~4.3%。 相似文献
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本文用抑制型离子色谱,薄壳强碱性阴离子交换树脂为分离柱,柱温为30±1℃,在常规淋洗液NaHCO_3-Na_2CO_3中加入对-硝基苯酚作为有机改进剂,测定了I ̄-、SCN ̄-、离子。它们有良好的线性关系,三种离子的浓度在5.0~30.0mg/L范围内其相关系数分别为:0.9994、r_(SCN) ̄(-0.9906),检测限分别为:I ̄-0.17mg/L、SCN ̄-0.10mg/L、L。 相似文献
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用鲁米诺-双氧水-铬(Ⅲ)化学发光体系结合巯基棉对As(Ⅲ)的富集分离,建立了快速的测定化探样品中痕量砷的新方法,检测线性范围为1.0*10^-4-1.0*10^1mg/L,检出限为3.4*10^-5mg/L。用于实际化探样吕测定,相对标准偏差为5.5^-9.0%。 相似文献
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An improved method for tracking and reducing the void volume in nano HPLC–MS with micro trapping columns 总被引:1,自引:0,他引:1
Mitulović G Smoluch M Chervet JP Steinmacher I Kungl A Mechtler K 《Analytical and bioanalytical chemistry》2003,376(7):946-951
Tandem mass spectrometry coupled to HPLC is the state of the art technique in proteomic research. Here we describe a highly sensitive nano liquid chromatography system (nano HPLC) for analysis of protein digests. Using preconcentration in a column-switching set-up, we were able to inject large sample volumes (250 µL) without significant loss of sensitivity. The major problem with this type of preconcentration is usually the occurrence of void volumes. In order to diagnose void volumes a simple and easy test was developed by which the UV trace and the pressure profile in the separation column were monitored. Part by part replacement of connection tubing restored a void volume-free system. A major pre-requisite for handling samples in the femtomol range was found to be the use of protein/peptide-saturated columns tryptic digests of cytochrome C were injected directly onto the reversed-phase nano separation column (75 µm inner diameter) and the separation results were compared with chromatograms obtained from separations using column switching. By using column switching we were able to inject large sample volumes in a short time period without losing resolution. 相似文献
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Wuilloud RG González AH Marchevsky EJ Olsina RA Martinez LD 《Journal of AOAC International》2001,84(5):1555-1560
An on-line lead preconcentration and determination system implemented with inductively coupled plasma-atomic emission spectrometry (ICP-AES) with ultrasonic nebulization (USN) in association with flow injection was studied. For the preconcentration of lead, a Pb-quinolin-8-ol complex was formed on-line at pH 6.8 and retained on Amberlite XAD-16 resin. The lead was removed from the microcolumn by countercurrent elution with nitric acid. A total enhancement factor of 225 was obtained with respect to ICP-AES with pneumatic nebulization (15.0 for USN and 15.0 for the column). The detection limit for Pb for the preconcentration of a 10 mL wine sample was 0.15 microg/L. The precision for 10 replicate determinations at a Pb level of 25 microg/L was a relative standard deviation of 2.5%, calculated from the peak heights obtained. The calibration graph obtained by using the preconcentration system for lead was linear with a correlation coefficient of 0.9995 for levels near the detection limit up to > or = 1000 microg/L. The method was successfully applied to the determination of lead in wine samples. 相似文献
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Preconcentration of selenium compounds on a porous graphitic carbon column in view of HPLC-ICP-AES speciation analysis 总被引:1,自引:0,他引:1
Abbas-Ghaleb K Gilon N Crétier G Mermet JM 《Analytical and bioanalytical chemistry》2003,377(6):1026-1031
The retention of organic selenium compounds on a porous graphitic carbon stationary phase was investigated. Different acids were studied as mobile phases to elute selenocystamine, selenoethionine, selenomethionine and selenocystine. Detection was achieved using inductively coupled plasma-atomic emission spectrometry to provide selenium-specific and sensitive detection. The separation of the four species was carried out using methanoic acid. An important on-column preconcentration was obtained when solutes were injected in nitric acid or trifluoroacetic acid (TFA) media. The large injection volume employed (2,500 µL) allowed us to reach low relative detection limits (2–6 µg/L). The method, employing TFA as injection solvent and methanoic acid as the eluent was found to be robust with respect to different matrices spiked with selenocompounds. 相似文献
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An on-line preconcentration method based on ion exchange solid phase extraction was developed for the determination of cationic analytes in capillary electrophoresis (CE). The preconcentration-separation system consisted of a preconcentration capillary bonded with carboxyl cation-exchange stationary phase, a separation capillary for zone electrophoresis and a tee joint interface of the capillaries. Two capillaries were connected closely inside a 0.3 mm i.d. polytetrafluoroethylene tube with a side opening and fixed together by the interface. The preparations of the preconcentration capillaries and interface were described in detail in this paper. The on-line preconcentration and separation procedure of the analysis system included washing and conditioning the capillaries, loading analytes, filling with buffer solution, eluting analytes and separating by capillary zone electrophoresis (CZE). Several analysis parameters, including sample loading flow rate and time, eluting solution and volume, inner diameter and length of preconcentration capillary etc., were investigated. The proposed method enhanced the detection sensitivity of CE-UV about 5000 times for propranolol and metoprolol compared with normally electrokinetic injection. The detection limits of propranolol and metoprolol were 0.02 and 0.1 microg/L with the proposed method respectively, whereas those were 0.1 and 0.5 mg/L with conventional electrokinetic injection. The experiment results demonstrate that the proposed technique can increase the preconcentration factor evidently. 相似文献
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建立了以香烟过滤嘴纤维作吸附剂,在线固相萃取-高效液相色谱(SPE—HPLC)测定水中邻硝基苯甲酸、对硝基苯胺、邻硝基苯酚、3-氯硝基苯四种硝基类化合物的方法。邻硝基苯甲酸、对硝基苯胺、邻硝基苯酚、3-氯硝基苯分别在0.006~4.80、0.003~2.40、0.002~1.60、0.002~1.60mg/L范围内峰面积与浓度呈线性关系,相关系数分别为0.9994、0.9996、0.9997和0.9996;检出限(S/N=3)分别为1.0、0.8、0.6,0.6μg/L;富集倍数分别为28.2、176.6、172.1、153.3。该法用于河水中四种硝基类化合物的测定,回收率为85.41%~116.44%,相对标准偏差在1.1%~5.4%范围内。 相似文献
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Procedures for the determination of polar pesticides in surface and ground water after their preconcentration by dispersive liquid-liquid microextraction and solid-phase extraction on Oasis® HLB (3 cc/60 mg) extraction cartridges are proposed. Conditions for the separation and determination of pesticides from the following classes by micellar electrokinetic chromatography were chosen: arylhydroxycarboxylic acids, sym-triazines, triazinones, urea derivatives, neonicotinoids, carbamates, triazoles, imidazoles, benzimidazoles, and organophosphorus compounds. The determination limits of pesticides in water were 0.5–20 μg/L with consideration for preconcentration. The relative standard deviation of the results of analysis was no higher than 10%. 相似文献
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建立了离子印迹壳聚糖/凹凸棒石(IICA)分离富集-火焰原子吸收光谱(FAAS)测定中药材中痕量Cd(Ⅱ)的新方法。在动态吸附条件下,系统研究了溶液pH值、流速、洗脱条件和干扰离子对痕量Cd(Ⅱ)分离富集的影响。研究表明,在pH为4.5,上样流速为0.60mL/min条件下,Cd(Ⅱ)能被IICA定量富集;吸附的Cd(Ⅱ)可用1.0mol/L HCl-0.1mol/L甲基异丁酮的乙醇溶液,在流速为0.96mL/min条件下完全洗脱。优化条件下,IICA对Cd(Ⅱ)的动态吸附容量为56.45mg/g。线性范围为0.00097~1.28mg/L,r=0.9994,检出限(3σ,n=11)为0.97μg/L,相对标准偏差为1.32%(n=6,c=0.08mg/L),回收率在96.5%~106.4%之间。该方法操作简便,灵敏度和精密度高,可应用于实际中药材样品中痕量镉的测定。 相似文献
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Aristidis N. Anthemidis Constantina MitaniPaschalia Balkatzopoulou Paraskevas D. Tzanavaras 《Analytica chimica acta》2012
A simple and fast preconcentration/separation dispersive liquid–liquid micro extraction (DLLME) method for metal determination based on the use of extraction solvent with lower density than water has been developed. For this purpose a novel micro-volume introduction system was developed enabling the on-line injection of the organic solvent into flame atomic absorption spectrometry (FAAS). The effectiveness and efficiency of the proposed system were demonstrated for lead and copper preconcentration in environmental water samples using di-isobutyl ketone (DBIK) as extraction solvent. Under the optimum conditions the enhancement factor for lead and copper was 187 and 310 respectively. For a sample volume of 10 mL, the detection limit (3 s) and the relative standard deviation were 1.2 μg L−1 and 3.3% for lead and 0.12 μg L−1 and 2.9% for copper respectively. The developed method was evaluated by analyzing certified reference material and it was applied successfully to the analysis of environmental water samples. 相似文献