John J. Richard

Use of macroreticular resins in the analysis of water for trace organic contaminants

Abstract Organic impurities in water can be isolated by sorption on a small column of a macroreticular resin. The organics are readily eluted by diethyl ether: the eluate is then concentrated by evaporation, and the organics are separated and determined by gas chromatography. Studies on a large number of model compounds added to water in the 10- to 100-ppb range (20 parts per trillion for pesticides) demonstrated that this method is accurate and reliable. An extensive study of the procedure revealed several critical steps where proper technique and conditions are essential to avoid serious error. These include resin purification and handling, preparation of standard samples containing organic impurities, and the technique and apparatus used in concentrating the XAD column eluate.

Solid phase extraction, GC separation and EC detection of tributyltin chloride

Abstract A new procedure for determining trace levels of tributyltin chloride (Bu 3 SnCl) present in seawater, without resorting to derivatization, has been developed. The stepwise approach involves: 1) solid phase extraction of Bu 3 SnCl from 100 ml of water using 100 mg of octadecyl (C-18) bonded porous silica; 2) elution with HCl treated ethyl acetate to collect 50 μl of the eluate; 3) on-column injection of 1 μl of the eluate and separation on a 15 m DB-5 fused silica capillary column; and 4) detection of pg quantities of Bu 3 SnCl by electron capture. Background and stability problems with both bonded porous and fused silica are described using test data from contrived and harbor water samples.

Chromatographic separation of copper with an α-hydroxyoxime

Abstract Two aliphatic α-hydroxyoximes have been synthesized and characterized. These reagents are highly selective for the extraction of copper(II) from weakly acidic aqueous solution. A column containing a hydroxyoxime on a solid support effects a quantitative separation of copper(II) from most other metal ions.

Adsorption of chlorinated pesticides from river water with XAD-2 resin

Pesticides in river water at levels as low as parts per billion (10(12)), can be recovered by sorption on a column of XAD-2 resin, followed by elution with acetonitrile. Water is added to the acetonitrile and the pesticides are extracted by petroleum ether and determined by gas chromatography. The new procedure is more convenient to use than the solvent extraction procedure and gives comparable results for dieldrin.

Applications of resins for extracting organic components from water

ZusammenfassungDie verwendeten Harze, die Extraktionsvorrichtungen, einige Leistungstests sowie die allgemeine Methodik werden kurz beschrieben. Neue Entwicklungen von einfachen und wirtschaftlichen Verfahren zur Überwachung interessierender Verschmutzungsstoffe werden besonders erwähnt. Als Beispiele werden Wasserverunreinigungen durch PVC-Röhren, durch Pesticide, Amine, halogenierte Kohlenwasserstoffe sowie Modellverbindungen diskutiert. Das Verfahren der Sorption an Harz wird mit der Sorption an Aktivkohle sowie mit der Lösungsmittelextraktion verglichen. Ein neu entwickeltes Kleingerät zur Probenahme wird beschrieben.SummaryThe discussion of the applications is prefaced by very brief descriptions of: 1) the resin characteristics, 2) the extraction device, 3) some efficiency tests, and 4) the general methodology. Recent developments of simple and inexpensive procedures for the monitoring of selected contaminants of concern are stressed. Examples are given of the contamination of water by PVC tubes and of the measurements of pesticides, amines, halocarbons, and model compounds in water. Practical comparisons of the resin sorption method to carbon sorption and solvent extraction procedures are presented and recently developed mini-samplers are discussed.

Solid phase versus solvent extraction of pesticides from water

The average recovery for 12 pesticides spiked into 100 ml of water at 0.1 ppb was 90% when cartridges containing 100 mg of C-18 bonded porous silica were used for adsorption. Flow rates of up to 200 bed volumes per minute were employed for the adsorption step. Quantitative desorption of the pesticides was accomplished with less than 100μl of solvent, thus eliminating the need for a solvent reduction step. The pesticides from samples of surface waters were adsorbed onto C-18 bonded porous silica at the sampling site and the cartridges containing the bonded phase were returned to the laboratory for elution and analysis. The analytical results obtained from use of this procedure agreed with those obtained for duplicate samples of the water that were processed in the laboratory using standard solvent extraction procedures.

Dioxins not detected in effluents from coal/refuse combustion

Abstract No 2, 3, 7, 8-tetrachlorodibenzo-p-dioxin was detected in effluents from a power plant burning coal supplemented with processed municipal wastes. These negative findings, in contrast with the many reports of the presence of dioxins from waste incineration, are proposed to be due to the high temperature of ∼1200°C for the combustion of small pieces of refuse with adequate oxygen for times sufficient to insure complete oxidation.

Organic emissions from combustion of combination coal/refuse to produce electricity

The compounds reported in the literatue by others and in this report are only some of the organic chemicals being emitted during production of electrical energy by combustion of coal and combination coal/refuse. The possible presence of more deleterious chemicals illustrates the need for a broader scope of analyses encompassing more accurate sampling and extraction schemes combined with improved separation and detection methods. Such developments are needed before accurate environmental impacts can be predicted. Classes of compounds reported include: polychlorinated biphenyls, other chlorinated compounds, polycyclic aromatic hydrocarbons, alkanes, carboxylic acids, phenols, phosphates, plasticizers, alkyl aromatics, and heterocyclic compounds.

Simplified determination of polycyclic aromatic hydrocarbons

Accurate quantitative analysis for selected polycyclic aromatic hydrocarbons present on urban dust can be obtained by using a simple procedure consisting of sonic-probe extraction with cyclohexane; clean-up with Florisil((R))-XAD-4((R)), and measurement by high-resolution gas chromatography with flame-ionization detection (HRGC/FID). The analysis can be further simplified by eliminating the clean-up step if HRGC/electron-impact mass-spectrometry (MS) is available. Both the FID and MS methods give results consistent with those obtained by standard procedures. The direct HRGC/MS procedure, combined with chemical ionization, can also be applied to the determination of polycyclic organic materials present in solvent-refined coal, shale oil and crude oil.

Comparison of analytical figures of merit of an active nitrogen afterglow and a flame ionization detector for gas chromatography

Abstract A comparison of the analytical figures of merit of an atmospheric pressure, active nitrogen afterglow and a conventional flame ionization detector revealed that the latter had slightly superior powers of detection and a considerably higher range of linear response. The selectivity of the afterglow detector was far superior because of its specific response to carbon-containing compounds and its potential, as previously demonstrated, of being a metal-specific, multielement detector as well.