Direct determination of halogenated POPs in aqueous samples by in-tube SPME, focalization and GC-ECD analysis

RSC Advances ◽  
2015 ◽  
Vol 5 (14) ◽  
pp. 10418-10423 ◽  
Author(s):  
M. V. Russo ◽  
P. Avino ◽  
E. Veschetti

A rapid analytical screening method allowing simultaneous analysis of few halogenated persistent organic pollutants (POPs) in water samples at ultra-trace levels was developed.

1992 ◽  
Vol 25 (11) ◽  
pp. 205-212 ◽  
Author(s):  
S. Yamasaki ◽  
A. Tsumura

A specially designed high resolution ICP-MS was combined with an ultrasonic nebulizer to analyze trace amounts of various inorganic contaminants contained in water samples. It was confirmed that the detection limits of most elements obtained by the proposed method were well under 1 ppt. The Standard Reference Material 1643b (trace elements in water) provided by NIST (National Institute of Standards and Technology, formerly U. S. National Bureau of Standards) was also analyzed. Concentration values obtained by this work were in good agreement with certified values for all the elements examined except for Cu. It can be concluded from the foregoing that the combination of the above two instruments materializes an extraordinarily sensitive method and paves the way for direct determination of a considerable number of trace and ultra-trace elements in water samples with acceptable speed and accuracy.


2021 ◽  
pp. 174751982110273
Author(s):  
Quan Han ◽  
Yanyan Huo ◽  
Xiaohui Yang ◽  
Xing Yao

A highly sensitive method for the determination of ultra-trace levels of palladium in water samples by cloud point extraction and graphite furnace atomic absorption spectrometry is developed. The procedure is based on complexation of palladium with a laboratory-prepared novel chelating agent, 2-(5-bromo-4-methyl-2-pyridylazo)-5-dimethylaminoaniline (5-Br-4-CH3-PADMA) and subsequent micelle-mediated extraction of the product using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) as an extracting agent. Analytical parameters affecting the separation and detection process, such as pH, concentration of the chelating agent and surfactant, equilibration temperature, and time are investigated. The optimized conditions are as follows: pH 6.0 HAc–NaAc buffer solution, 1 × 10−5 mol L−1 5-Br-4-CH3-PADMA, and 0.1% (w/v) Triton X-114. Under the optimized conditions, the calibration graph is linear in the range of 0.1–12 ng/mL, the detection limit is 0.05 ng/mL for palladium, and the relative standard deviation is 2.9% ( c = 1.0 ng/mL, n = 10). The enrichment factor, defined as the ratio of the aqueous solution volume to that of the surfactant-rich phase volume after dilution with HNO3–methanol solution, is 200. The proposed method is applied to the determination of palladium in water samples with satisfactory results.


2018 ◽  
Vol 229 (12) ◽  
Author(s):  
Juliana Bazzan Arsand ◽  
Rodrigo Barcellos Hoff ◽  
Louíse Jank ◽  
Alexsandro Dallegrave ◽  
Carolina Galeazzi ◽  
...  

2020 ◽  
Vol 35 (8) ◽  
pp. 1632-1640
Author(s):  
Vikas Kumar Shukla ◽  
Sangita Dhara ◽  
N. L. Mishra

A total reflection X-ray fluorescence (TXRF) method in conjugation with dispersive liquid–liquid micro-extraction (DLLME) was developed for the determination of uranium present at ultra-trace levels in water samples.


1992 ◽  
Vol 75 (4) ◽  
pp. 720-724 ◽  
Author(s):  
Toshinari Suzuki ◽  
Satoru Watanabe

Abstract A liquid chromatographic method for screening 9 chlorophenoxy acids (2,4-D; 2,4-DP; 2,4-DB; MCPA; MCPP; MCPB; 2,4,5-T; 2,4,5-TP; and 2,4,5-TB) and their ethyl esters in ground- and tap water is presented. The water samples are acidified and subjected to either liquid-liquid or solid-phase extraction. The extracts obtained are saponified in 0.03N NaOH-50% methanol (1+1) and the acidic compounds are re-extracted with ethyl acetate-n-hexane (8 + 2) after acidification and derivatized with 9- anthryldiazomethane. Derivatized compounds are analyzed using reversed-phase column chromatography with fluorescence detection (excitation, 365 nm; emission, 412 nm). Recoveries of analytes from 20 mL water samples were greater than 90%, and the average coefficient of variation was within 5.0% at 0.5 ppb for both extraction methods. These methods are simple and useful for the determination of small amounts of chlorophenoxy herbicides. Solid-phase extraction is suitable for screening a large number of samples simultaneously, and liquid extraction for separate determination of the acids and ethyl esters of the herbicides was improved by introducing a saponification step.


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