Perchlorate in water via US Environmental Protection Agency Method 331 Determination of method uncertainties, lowest concentration minimum reporting levels, and Hubaux-Vos detection limits in reagent water and simulated drinking water

US Environmental Protection Agency (EPA) Method 331 determines perchlorate in drinking water using non-suppressed ion chromatography with tandem mass spectrometry. This study reports the results of calibration and recovery studies in reagent water, as well as of a recovery study in simulated drinking water (i.e., total dissolved solids are 500 mg/mL each of chloride, sulfate, and bicarbonate). The perchlorate concentrations in the study ranged from 0.05 to 64 ng/mL. At 95% confidence, the Hubaux-Vos detection limit (H-V DL) was 0.04 ng/mL for the calibration study and the simulated-drinking-water recovery study, and 0.03 ng/mL for the reagent-water recovery study. The lowest concentration minimum reporting level was 0.03 ng/mL for reagent water and 0.0 7 ng/mL for simulated drinking water, again at 95% confidence.     

Evaluation of Colilert-18 for detection and enumeration of fecal coliform bacteria in wastewater using the U.S. Environmental Protection Agency Alternative Test procedure Protocol

This study compared recovery of fecal coliform bacteria from sewage by Colilert-18 and Standard Methods 9222D (membrane-Fecal Coliform medium) in accordance with the U.S. Environmental Protection Agency (EPA) Alternative Test Protocol (ATP). Samples were collected from 10 different wastewater treatment plants in the northeastern United States and tested in a single laboratory. Twenty replicates of each sample were analyzed by each method, and 200 positive and 200 negative responses were confirmed for each method. Recovery of fecal coliforms by Colilert-18 was significantly higher than (8 of 10 sites) or statistically equivalent to (1 of 10 sites) recovery by the reference method (Standard Methods 9222D) for samples from all but one site. Both methods had low false-positive rates (< 2%); however, the false-negative rate observed with Standard Methods 9222D (21.5%) was substantially higher than that observed with Colilert-18 (7%). The accuracy rates of the two methods were calculated as 96.5 and 88.9% for Colilert-18 and Standard Methods 9222D, respectively. The results of this study demonstrate that Colilert-18 meets the acceptance criteria for alternative methods specified in the EPA ATP.     

Quantitative determination of wine highly volatile sulfur compounds by using automated headspace solid-phase microextraction and gas chromatography-pulsed flame photometric detection. Critical study and optimization of a new procedure

The quantitative determination of wine volatile sulfur compounds by automated headspace solid-phase microextraction (HS-SPME) with a carboxen-polydimethylsiloxane (CAR-PDMS) fiber and subsequent gas chromatography-pulsed flame photometric detection (GC-PFPD) has been evaluated. The direct extraction of the sulfur compounds in 5 ml of wine has been found to suffer from matrix effects and short linear ranges, problems which could not be solved by the use of different internal standards or by multiple headspace SPME. These problems were attributed to saturation of the fiber and to competitive effects between analytes, internal standards and other wine volatiles. Another problem was the oxidation of analytes during the procedure. The reduction in sample volume by a factor 50 (0.1 ml diluted with water or brine) brought about a reduction in the amount of sulfur compounds taken in the fiber by a factor just 3.3. Consequently, a new procedure has been proposed. In a sealed vial containing 4.9 ml of saturated NaCl brine, the air is thoroughly displaced with nitrogen, and the wine (0.1 ml) and the internal standards (0.02 ml) are further introduced with a syringe through the vial septum. This sample is extracted at 35 degrees C for 20 min. This procedure makes a satisfactory determination possible of hydrogen sulfide, methanethiol, ethanethiol, dimethyl sulfide, diethyl sulfide and dimethyl disulfide. The linear dynamic ranges cover the normal ranges of occurrence of these analytes in wine with typical r2 between 0.9823 and 0.9980. Reproducibility in real samples ranges from 10 to 20% and repeatability is better than 10% in most cases. The method accuracy is satisfactory, with errors below 20% for hydrogen sulfide and mostly below 10% for the other compounds. The proposed method has been applied to the analysis of 34 Spanish wines.