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41.
A new method for the non-specific determination of iron-porphyrin-like complexes in natural waters has been developed. It is based on the chemiluminescent oxidation of the luminol in the presence of dioxygen (O2) at pH 13. The method has been implemented in a FIA manifold that allowed the direct injection of seawater. The limit of detection is 0.11 nM of equivalent hemin (Fe-protoporphyrin IX). Fe2+, Fe3+, H2O2, siderophore (deferoxamin mesylate), humic acid and phytic acid did not interfere when they were present at the concentrations expected in seawater. Metal free porphyrin and Mg, Cu, Co porphyrin complexes did not induce a significant chemiluminescent signal. Poisoned unfiltered samples could be stored for several weeks before analyses. The new method was successfully applied to the determination of the Fe-porphyrin complexes contained in cultured phytoplankton and in natural samples. 相似文献
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Farhat Waqar Saida Jan Bashir Mohammad Muhammad Hakim Shah Alam Wasim Yawar 《中国化学会会志》2009,56(2):335-340
An analytical method has been developed for the preconcentration of rare earth elements (REEs) in seawater for their determination by inductively coupled plasma optical emission spectrometry (ICP‐OES). An indigenously synthesized chelating resin was used for the preconcentration of (REEs) which was based on immobilization of fluorinated β‐diketone group on solid support styrene divinyl benzene. Sample solutions (adjusted to optimized pH) were passed through a polyethylene column packed with 250 mg of the resin. Experimental conditions consisting of pH, sample flow rate, sample volume and eluent concentration were optimized. The established method has been applied for the preconcentration of light, medium and heavy REEs in coastal sea water samples for their subsequent determination by (ICP‐OES). Percentage recoveries of La, Ce, Nd, Sm, Eu, Gd, Dy, Er, Yb and Lu were ≥ 95%, a preconcentration factor of 200 times, and relative standard deviations < 5% were achieved. 相似文献
44.
Luiz L. Mafra Jr. Claude Léger Stephen S. Bates Michael A. Quilliam 《Journal of chromatography. A》2009,1216(32):6003-6011
Quantitation of trace levels of domoic acid (DA) in seawater samples usually requires labour-intensive protocols involving chemical derivatization with 9-fluorenylmethylchloroformate and liquid chromatography with fluorescence detection (FMOC–LC–FLD). Procedures based on LC–MS have been published, but time-consuming and costly solid-phase extraction pre-concentration steps are required to achieve suitable detection limits. This paper describes an alternative, simple and inexpensive LC method with ultraviolet detection (LC–UVD) for the routine analysis of trace levels of DA in seawater without the use of sample pre-concentration or derivatization steps. Qualitative confirmation of DA identity in dubious samples can be achieved by mass spectrometry (LC–MS) using the same chromatographic conditions. Addition of an ion-pairing/acidifying agent (0.15% trifluoroacetic acid) to sample extracts and the use of a gradient elution permitted the direct analysis of large sample volumes (100 μl), resulting in both high selectivity and sensitivity (limit of detection = 42 pg ml−1 by LC–UVD and 15 pg ml−1 by LC–MS). Same-day precision varied between 0.4 and 5%, depending on the detection method and DA concentration. Mean recoveries of spiked DA in seawater by LC–UVD were 98.8% at 0.1–10 ng ml−1 and 99.8% at 50–1000 ng ml−1. LC–UVD exhibited strong correlation with FMOC–LC–FLD during inter-laboratory analysis of Pseudo-nitzschia multiseries cultures containing 60–2000 ng DA ml−1 (r2 > 0.99), but more variable results were obtained by LC–MS (r2 = 0.85). This new technique was used to confirm the presence of trace DA levels in low-toxicity Pseudo-nitzschia spp. isolates (0.2–1.6 ng ml−1) and in whole-water field samples (0.3–5.8 ng ml−1), even in the absence of detectable Pseudo-nitzschia spp. cells in the water column. 相似文献
45.
Simultaneous determination of CFC-11, CFC-12 and CFC-113 in seawater samples using a purge and trap gas-chromatographic system 总被引:1,自引:0,他引:1
We have optimized the analytical parameters of a homemade instrument for the simultaneous measurement of the chlorofluorocarbons CCl2F2 (CFC-12), CCl3F (CFC-11) and C2Cl3F3 (CFC-113) in seawater. Seawater samples are flame sealed into 60 ml glass ampoules avoiding any contact with the atmosphere and stored in cold, dark condition until analysis. In the laboratory, after cracking the ampoule in an enclosed chamber filled with ultra-pure nitrogen, the seawater sample is transferred to a stripping chamber, where ultra-pure nitrogen is used to purge the dissolved CFCs from the seawater. The extracted gases are then cryogenically trapped, subsequently the trap is isolated and heated and the CFCs are transferred by a carrier gas stream into a precolumn and then are separated on a gaschromatographic packed column. To separate adequately CFC-12 from N2O, during the early part of the chromatographic run, the gas stream passes through a molecular sieve, which is then isolated and backflushed. The CFCs are detected on an electron capture detector (63Ni ECD). After a careful choice of the experimental conditions, the performances of the system were evaluated. The detection limits for seawater samples are: 0.0081 pmol kg−1 for CFC-12, 0.0073 pmol kg−1 for CFC-11 and 0.0043 pmol kg−1 for CFC-113. The reproducibility of replicate samples lies within 5% for the three CFCs. The system has been successfully employed for CFC measurements in seawater samples collected in the Ross Sea (Antarctica) in the framework of the Italian Antarctic research project. 相似文献
46.
Optical biosensor for the determination of BOD in seawater 总被引:1,自引:0,他引:1
An automatic sensing system was developed using an optical BOD sensing film. The sensing film consists of an organically modified silicate (ORMOSIL) film embedded with an oxygen-sensitive Ru complex. A multi-microorganisms immobilization method was developed for the BOD sensing film preparation. Three different kinds of microorganisms, Bacillus licheniformis, Dietzia maris and Marinobacter marinus from seawater, were immobilized on a polyvinyl alcohol ORMOSILs. After preconditioning, the BOD biosensor could steadily perform well up to 10 months. The linear fluctuant coefficients (R2) in the range of 0.3-40 mg L−1 was 0.985 when a glucose/glutamate BOD standard was applied. The reproducible response for the BOD sensing film could be obtained within ±2.3% of the mean value in a series of 10 samples in 5.0 mg L−1 BOD standard GGA solution. The effects of temperature, pH and sodium chloride concentration on the two microbial films were studied as well. The BOD sensing system was tested and applied for the BOD determination of seawater. 相似文献
47.
应用流动注射技术,用D412螯合树脂微柱富集海水中的铅(Ⅱ),并与火焰原子吸收光谱法相结合测定海水中铅(Ⅱ)。20mL海水样品以3mL.min-1流量进柱,被树脂螯合吸附富集,以0.2mol.L-1乙酸铵溶液5mL淋洗柱体去除干扰物,以4mol.L-1硝酸溶液4mL为洗脱剂(流量为7mL.min-1),洗脱液直接引入火焰原子吸收光谱仪雾化器,在线检测。当海水样进样20mL时,铅(Ⅱ)测定灵敏度可提高约35倍;检出限(3s)为1.3μg.L-1。实际应用于海水样品分析,加标回收率为94.5%,测定值的相对标准偏差(n=6)为2.2%。 相似文献
48.
Pascal Salaün Kristopher B. Gibbon-Walsh Georgina M.S. Alves Helena M.V.M. Soares Constant M.G. van den Berg 《Analytica chimica acta》2012
The oxidation potentials of As0/AsIII and Sb0/SbIII on the gold electrode are very close to each other due to their similar chemistry. Arsenic concentration in seawater is low (10–20 nM), Sb occurring at ∼0.1 time that of As. Methods are shown here for the electroanalytical speciation of inorganic arsenic and inorganic antimony in seawater using a solid gold microwire electrode. Anodic stripping voltammetry (ASV) and chronopotentiometry (ASC) are used at pH ≤ 2 and pH 8, using a vibrating gold microwire electrode. Under vibrations, the diffusion layer size at a 5 μm diameter wire is 0.7 μm. The detection limits for the AsIII and SbIII are below 0.1 nM using 2 min and 10 min deposition times respectively. AsIII and SbIII can be determined in acidic conditions (after addition of hydrazine) or at neutral pH. In the latter case, oxidation of As0 to AsIII was found to proceed through a transient AsIII species. Adsorption of this species on the gold electrode at potentials where SbIII diffused away is used for selective deposition of AsIII. Addition of EDTA removes the interfering effect of manganese when analysing AsIII. Imposition of a desorption step for SbIII analysis is required. Total inorganic arsenic (iAs = AsV + AsIII) can be determined without interference from Sb nor mono-methyl arsenious acid (MMA) at 1.6 < pH < 2 using Edep = −1 V. Total inorganic antimony (iSb = SbV + SbIII) is determined at pH 1 using Edep = −1.8 V without interference by As. 相似文献
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