Water analysis extraction

RAPID PHOTOMETRIC METHODS FOR WATER ANALYSIS IN FIELD. EXTRACTION-FREE RAPID PROCEDURES FOR THE DETERMINATION OF TRACES OF REGULATED METALS WITH l-(2-PYRIDYLAZO)-NAPHTOL-2... 

Development of extraction-free photometric procedures for the determination of traces of metals for which hygienic and environmental regulations have been established is an urgent problem. For solution of this problem we used as an organic reagent l-(2- pyridylazo)-naphtol-2 (PAN) which forms intensely coloured complex compounds with many metals and is frequently used for their extraction-photometric determination however these procedures did not find wide application in water analysis due to lack of selectivity and necessity of using organic solvents. 

Methoxy-cis-19-norpregna-l,3,5(10),17(20)-tetraene A solution of 31 g (109 mmolesi of estrone methyl ether in 600 ml of benzene is added rapidly to a solution of 469 mmoles of ethylidenetriphenylphosphorane in 1.2 liters of DMSO. After heating under nitrogen at 60° overnight, the reaction is cooled, poured into ice water, and extracted with three portions of hexane, backwashed with three portions of water and the hexane removed. The crude product, dissolved in petroleum ether (bp, 30-60°), is filtered through 225 g of alumina (activity I). The residue from the eluate consists of 95 % cis- and 5 % tran5-isomers, as determined by vpc analysis. After recrystallization from ether-methanol, 26.3 g (82%) of cw-isomer is obtained mp 76.5-77.5° [a]o 60°. 

Analysis of water directly extraction of soil with methanol followed by dilution of extract with water... 

An advantage of the microbore gas chromatrography/time-of-flight mass spectrometry (GC/TOFMS) method over the other two approaches is that separation efficiency need not be compromised for speed of analysis. The rapid deconvolution of spectra ( scan rate ) with TOFMS makes it the only MS approach to achieve several data points across a narrow peak in full-scan operation. However, the injection of complex extracts deteriorates performance of microbore columns quickly, and an increased LOD and decreased ruggedness result. Microbore columns may be used in water analysis if the LOD is sufficiently low, but they can rarely be used in real-life applications to complicated extracts. 

IEC continues to have numerous applications to the detection and quantification of various inorganic ions.1 1 This is particularly true in water analysis.5-14 Inorganic ions in a variety of other sample types, such as food and beverages,1518 rocks,19-23 biological fluids, (blood, urine, etc.),24-31 pharmaceutical substances,32 33 concentrated acids,34 alcohols,35 and cleanroom air36 have also been analyzed by IEC. IEC has also been employed in isotopic separation of ions,37 including the production of radioisotopes for therapeutic purposes.3839 Typical IEC sample matrices are complex, and may contain substances that interfere with measurement of the ion(s) of interest. The low detection limits required for many IEC separations demand simple extraction procedures and small volumes to avoid over-dilution. Careful choice and manipulation of the eluent(s) may be needed to achieve the desired specificity, especially when multiple ions are to be determined in a single sample. 

A method for sediment involves Soxhlet extraction followed by filtration, and concentration to 5 mL. The residue is diluted with water, acidified, extracted with methylene chloride, and then the extracts are dried and evaporated to dryness. The residue is cleaned up on an alumina column. Analysis is performed by GC/NPD. Good recovery (81-97%) and precision (>15% RSD) were reported detection limits were not reported (Muir et al. 1981). 

Leoni [366] observed that in the extraction preconcentration of organochlo-rine insecticides and PCB s from surface and coastal waters in the presence of other pollutants such as oil, surface active substances, etc., the results obtained with an absorption column of Tenax-Celite are equivalent to those obtained with the continuous liquid-liquid extraction technique. For non-saline waters that contain solids in suspension that absorb pesticides, it may be necessary to filter the water before extraction with Tenax and then to extract the suspended solids separately. Analyses of river and estuarine sea waters, filtered before extraction, showed the effectiveness of Tenax, and the extracts obtained for pesticide analysis prove to be much less contaminated by interfering substances than corresponding extracts obtained by the liquid-liquid technique. Leoni et al. [365] showed that for the extraction of organic micro pollutants such as pesticides and aromatic polycyclic hydrocarbons from waters, the recoveries of these substances from unpolluted waters (mineral and potable waters) when added at the level of 1 xg/l averaged 90%. 

All filtering and extraction systems must be checked for compatibility with the analyte of interest. Some or all of the analytes may be absorbed or otherwise lost during the extraction process, and this must be known beforehand. Carbon may be lost by high vacuum differentials between sampler and soil water. Long extraction times may lead to distortions in the results of the sample analysis [5],... 

A city s water supply is found to be contaminated with carbon tetrachloride. The chemical analysis procedure involves the extraction of the carbon tetrachloride from the water with hexane. A 4.00-L sample of water is extracted with 10 mL of hexane. If this hexane solution is diluted from 1 to 25 mL and the concentration of carbon tetrachloride in the diluted solution found to be 10.4 ppm, what is the concentration in the original water ... 

The overall method includes sample collection and storage, extraction, and analysis steps. Sampling strategy is an important step in the overall process. Care must be taken to assure that the samples collected are representative of the environmental medium and that they are collected without contamination. There is an extensive list of test methods for water analysis (Tables 8.2, 8.3, and 8.4), which includes numerous modifications of the original methods, but most involve alternative extraction methods developed to improve overall method performance for the analysis. Solvent extraction methods with hexane are also in use. 

Reding, R. Kollman, W.B. Weisner, M.J. Brass, H.J., "Trihalomethanes in Drinking Water Analysis by Liquid-Liquid Extraction and a Comparison to Purge and Trap", Measurement of Organic Pollutants in Water and Wastewater, ASTM STP 686, C.E. Van Hall, Ed., American Society for Testing and Materials, Philadelphia, PA, 1979, pp. 36-41. 

Workup, in air, is begun by adding 250 mL of water and acidification to pH 5 with 1 M HC1. The reaction mixture is transferred to a 2-L separatory funnel with the assistance of 250 mL of diethyl ether. The aqueous phase is drawn off and set aside. The organic layer is washed twice with 300-mL portions of saturated aqueous Na2S203 and saturated aqueous NaCl. This is followed by a wash with two 200-mL portions of water. The extract is dried over MgS04, and concentrated in vacuo. Analysis by gas chromato-... 

The solubility of NHDC in hot water, alcohol, aqueous alkali, acetonitrile, dimethyl sulfoxide, and alcohol/water mixture facilitates its selective extraction from food samples (20,91,94). It is extracted from jams, fruit juices, and dairy products with methanol (66,93) or acetone (95) and filtered or centrifuged. Chewing gum samples are dissolved in chloroform and extracted with water. The extract is centrifuged, and the clear supernatant is injected into the HPLC (95). If necessary, sample cleanup and concentration may be achieved by selective adsorption or desorption (20) on Sep-Pak Cl8 (96). Tomas-Barberan et al. (93) used Amberlite XAD-2 resin for purification of jam extract. Sugars, pectin, and other polar compounds were eluted with water, and NHDC was eluted with methanol. After concentration, the extract was further purified on a Sephadex LH-20 column prior to HPLC analysis. 

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