CZE separation of amitrol and triazine herbicides in environmental water samples with acid-assisted on-column preconcentration

A simple analytical scheme for the detection and quantification of amitrol and triazine herbicides (atrazine, ametryn and atraton) and degradation product (2‐hydroxyatrazine) in environmental water samples by CZE is reported. On‐column preconcentration of analytes from untreated water samples (mineral, spring, tap and river water) is accomplished by introducing an acid plug (200 mM citrate of pH 2.0) after the sample and then proceeding with the CZE separation, using 100 mM formiate buffer of pH 3.5 as running buffer and 25.0 KV as separation voltage. UV detection at 200 nm provides LODs from 50 to 300 nM in untreated samples and they were lowered tenfold by sample preconcentration by evaporation. Calculated recoveries were typically higher than 90%. Minimal detectable concentration of the electroactive amitrol could be decreased about 20‐fold when electrochemical detection was employed by monitoring the amperometric signal at +800 mV using a carbon paste electrode (LOD of 9.6 nM, 0.81 μg/L, versus 170 nM, 14.3 μg/L, using amperometric and UV detection, respectively) in untreated water samples.     

On-column polymer-imbedded graphite inlet electrode for capillary electrophoresis coupled on-line with flow injection analysis in a poly(dimethylsiloxane) interface

A method for coupling an electrophoretic driven separation to a liquid flow, using conventional fused-silica capillaries and a soft polymeric interface is presented. A novel design of the electrode providing high voltage to the electrophoretic separation was also developed. The electrode consisted of a conductive polyimide/graphite imbedded coating immobilized onto the capillary electrophoresis (CE) column inlet. This integrated electrode gave the same separation performance as a commonly used platinum electrode. The on-column electrode also showed good electrochemical stability in chronoamperometric experiments. In addition, with this electrode design, the electrode position relative to the inlet end of the CE column will always be constant and well defined. The on-line flow injection analysis (FIA)-CE system was used with electrospray ionization (ESI)-time of flight (TOF)-mass spectrometry detection. The preparation of the PDMS (poly(dimethylsiloxane)) interface for FIA-CE is described in detail and used for initial tests of the on-column polymer-imbedded graphite inlet electrode. In this interface, a pressure-driven liquid flow, a make up CE electrolyte and a CE column inlet meet in a two-level cross (95 microm ID) in the PDMS structure, enabling independent flow characterization.     

微型柱在线分离-ICP-MS法测定高纯氧化铕中的14个稀土杂质

研究了微型柱在线分离-电感耦合等离子质谱法（ICP-MS）测定高纯Eu2O3中痕量Tm的方法，研制了Cyanex272负载树脂微型分离柱，优化了分离Eu2O3基体的实验条件，在线分离测定时间为25min。建立了在线柱分离测定Tm，内标补偿法直接测定其余稀土杂质的高纯Eu2O3中14个稀土杂质的ICP-MS分析方法。方法检出限为0.01μg/g-0.15μg/g，加标回收率为91.5%-110%,相对标准偏差为1.7%-4.9%。可满足快速测定99.999%Eu2O3中14个稀土杂质的要求。     

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。     

Experimental study of the retention properties of a cyclo olefin polymer pillar array column in reversed-phase mode

Experimental measurements to study the retention capacity and band broadening under retentive conditions using micromachined non-porous pillar array columns fabricated in cyclo olefin polymer are presented. In particular, three columns with different depths but with the same pillar structure have been fabricated via hot embossing and pressure-assisted thermal bonding. Separations of a mixture of four coumarins using varying mobile phase compositions have been monitored to study the relation between the retention factor and the ratio of organic solvent in the aqueous mobile phase. Moreover, the linear relation between the retention and the surface/volume ratio predicted in theory has been observed, achieving retention factors up to k=2.5. Under the same retentive conditions, minimal reduced plate height values of h(min)=0.4 have been obtained at retention factors of k=1.2. These experimental results are compared with the case of non-porous and porous silicon pillars. Similar results for the plate heights are achieved while retention factors are higher than the non-porous silicon column and considerably smaller than the porous pillar column, given the non-porous nature of the used cyclo olefin polymer. The feasibility of using this polymer column as an alternative to the pillar array silicon columns is corroborated.     

流动注射在线液-液萃取火焰原子吸收法测定水中痕量铅

提出了一种流动注射在线液－液萃取火焰原子吸收直接测定水中痕量铅的分析方法。实验以APDC为螯合剂,用MIBK为萃取剂,研究了在线萃取中各种实验参数、酸度条件的影响,考察了共存元素的干扰。方法的RSD（n=12)为2．7％,测定检出限为3．1μg/L,回收率为96％－106％。     

Aspects of trapping efficiency and matrix effects in the development of a restricted‐access‐media‐based trap‐and‐elute liquid chromatography with mass spectrometry method

Online restricted access media with liquid chromatography and tandem mass spectrometry for the direct analysis of small molecules in biological fluids represents an interesting alternative to time‐demanding traditional sample preparation techniques. In this study, important considerations concerning the development of a restricted access media with liquid chromatography and tandem mass spectrometry method for the analysis of dansylated estrogens in biological matrix are presented. Parameters influencing peak tailing and trapping efficiency were evaluated. The key factors included the ion strength of the mobile phase, a loading flow rate of the sample onto the trap column, and selection of a proper stationary phase of the trap column for a given set of analytes. These parameters have proven to be essential for minimizing any unwanted chromatographic peak tailing. The bulk derivatization of the analytes in the biological fluids and its relationship to the observed matrix effects was evaluated as well.     

Electrochemical detection of nitrate,nitrite and ammonium for on-site water quality monitoring

This review examines the most recent electrochemical developments for nitrate, nitrite and ammonium detection for on-site water monitoring. There remains a high demand for effective field-based detection of the dissolved inorganic nitrogen (DIN) analytes to aid in mitigating nitrogen loading. Electrochemical approaches show increasing potential to fill this role as advancements in nanotechnology continually improve analytical performance and on-site applicability. However, translating these improvements into the field still faces the resonating challenges of reaching analytical proficiency (selectivity, sensitivity, robustness, stability), practical end-user functionality, minimal matrix interferences and cost effectiveness. Herein, we elaborate on these challenges via a critical evaluation of current studies and examine how realistic the prospects of on-site nitrate, nitrite and ammonium are. We also present recommendations in addressing these gaps to conclude the review.     

Ag NPs decked GO composite as a competent and reusable catalyst for ‘ON WATER’ chemoselective synthesis of pyrano[2,3-c:6,5-c′]dipyrazol]-2-ones

We have synthesized and characterized Ag NPs decked GO composite and studied its role as reusable catalyst for the ‘ON WATER’ chemoselective synthesis of pyranodipyrazolones via the reaction of different carbonyl compounds with 3-methyl-1-phenyl-1H-pyrazol-5(4H)-one. This method illustrates significant selectivity for pyranodipyrazolones over arylmethylene bispyrazolols and arylmethylenepyrazolones. Synergistic effect of heterogenic nature of water with reactants and Ag NPs/GO had profuse outcome on reaction as indicated by high TOF (18.03 × 10^?5 mol g^?1 min^?1). Furthermore, catalyst was recycled for 7-times without significant loss of activity.