A simple gas chromatography method for the analysis of monoethanolamine in air

A simple method determining airborne monoethanolamine has been developed. Monoethanolamine determination has traditionally been difficult due to analytical separation problems. Even in recent sophisticated methods, this difficulty remains as the major issue often resulting in time-consuming sample preparations. Impregnated glass fiber filters were used for sampling. Desorption of monoethanolamine was followed by capillary GC analysis and nitrogen phosphorous selective detection. Separation was achieved using a specific column for monoethanolamines (35% diphenyl and 65% dimethyl polysiloxane). The internal standard was quinoline. Derivatization steps were not needed. The calibration range was 0.5-80 μg/mL with a good correlation (R(2) = 0.996). Averaged overall precisions and accuracies were 4.8% and -7.8% for intraday (n = 30), and 10.5% and -5.9% for interday (n = 72). Mean recovery from spiked filters was 92.8% for the intraday variation, and 94.1% for the interday variation. Monoethanolamine on stored spiked filters was stable for at least 4 weeks at 5°C. This newly developed method was used among professional cleaners and air concentrations (n = 4) were 0.42 and 0.17 mg/m(3) for personal and 0.23 and 0.43 mg/m(3) for stationary measurements. The monoethanolamine air concentration method described here was simple, sensitive, and convenient both in terms of sampling and analytical analysis.

Recent Advances in Valorization Methods of Inorganic/Organic Solid, Liquid, and Gas Wastes

The main goal of this special issue was to gather contributions dealing with the latest breakthrough methods for providing value compounds and energy/fuel from waste valorization. Valorization is a relatively new approach in the area of industrial wastes management, a key issue to promote sustainable development. In this field, the recovery of value-added substances, such as antioxidants, proteins, vitamins, and so forth, from the processing of agroindustrial byproducts, is worth mentioning. Another important valorization approach is the use of biogas from waste treatment plants for the production of energy. Several approaches involving physical and chemical processes, thermal and biological processes that ensure reduced emissions and energy consumptions were taken into account. The papers selected for this topical issue represent some of the mostly researched methods that currently promote the valorization of wastes to energy and useful materials ...

FY2014 Equipment and Vehicle Revolving Fund report

The Equipment and Vehicle Revolving Fund report covers all equipment and vehicle purchases through the highway materials and equipment revolving fund during FY 2014.

Gas analysis of exhumed cadavers buried for 30 years: a case report about long time alteration.

Due to important alteration caused by long time decomposition, the gases in human bodies buried for more than a year have not been investigated. For the first time, the results of gas analysis sampled from bodies recently exhumed after 30 years are presented. Adipocere formation has prevented the bodies from too important alteration, and gaseous areas were identified. The sampling was performed with airtight syringes assisted by multi-detector computed tomography (MDCT) in those specific areas. The important amount of methane (CH4), coupled to weak amounts of hydrogen (H2) and carbon dioxide (CO2), usual gaseous alteration indicators, have permitted to confirm methanogenesis mechanism for long period of alteration. H2 and CO2 produced during the first stages of the alteration process were consumed through anaerobic oxidation by methanogenic bacteria, generating CH4.

Development and validation of a gas chromatography-negative chemical ionization tandem mass spectrometry method for the determination of ethyl glucuronide in hair and its application to forensic toxicology.

Ethyl glucuronide (EtG) is a minor and direct metabolite of ethanol. EtG is incorporated into the growing hair allowing retrospective investigation of chronic alcohol abuse. In this study, we report the development and the validation of a method using gas chromatography-negative chemical ionization tandem mass spectrometry (GC-NCI-MS/MS) for the quantification of EtG in hair. EtG was extracted from about 30 mg of hair by aqueous incubation and purified by solid-phase extraction (SPE) using mixed mode extraction cartridges followed by derivation with perfluoropentanoic anhydride (PFPA). The analysis was performed in the selected reaction monitoring (SRM) mode using the transitions m/z 347-->163 (for the quantification) and m/z 347-->119 (for the identification) for EtG, and m/z 352-->163 for EtG-d(5) used as internal standard. For validation, we prepared quality controls (QC) using hair samples taken post mortem from 2 subjects with a known history of alcoholism. These samples were confirmed by a proficiency test with 7 participating laboratories. The assay linearity of EtG was confirmed over the range from 8.4 to 259.4 pg/mg hair, with a coefficient of determination (r(2)) above 0.999. The limit of detection (LOD) was estimated with 3.0 pg/mg. The lower limit of quantification (LLOQ) of the method was fixed at 8.4 pg/mg. Repeatability and intermediate precision (relative standard deviation, RSD%), tested at 4 QC levels, were less than 13.2%. The analytical method was applied to several hair samples obtained from autopsy cases with a history of alcoholism and/or lesions caused by alcohol. EtG concentrations in hair ranged from 60 to 820 pg/mg hair.

Accuracy profile validation of a new analytical method for propane measurement using headspace-gas chromatography-mass spectrometry

Propane can be responsible for several types of lethal intoxication and explosions. Quantifying it would be very helpful to determine in some cases the cause of death. Some gas chromatography-mass spectrometry (GC-MS) methods of propane measurements do already exist. The main drawback of these GC-MS methods described in the literature is the absence of a specific propane internal standard necessary for accurate quantitative analysis. The main outcome of the following study was to provide an innovative Headspace-GC-MS method (HS-GC-MS) applicable to the routine determination of propane concentration in forensic toxicology laboratories. To date, no stable isotope of propane is commercially available. The development of an in situ generation of standards is thus presented. An internal-labeled standard gas (C3DH7) is generated in situ by the stoichiometric formation of propane by the reaction of deuterated water (D2O) with Grignard reagent propylmagnesium chloride (C3H7MgCl). The method aims to use this internal standard to quantify propane concentrations and, therefore, to obtain precise measurements. Consequently, a complete validation with an accuracy profile according to two different guidelines, the French Society of Pharmaceutical Sciences and Techniques (SFSTP) and the Gesellschaft für toxikologische und Forensische Chemie (GTFCh), is presented.

Automated Traffic/Truck Weight Monitoring Equipment (Weigh-in-Motion), HR-282, 1988

This report documents work undertaken in the demonstration of a low-cost Automatic Weight and Classification System (AWACS). An AWACS procurement specification and details of the results of the project are also included. The intent of the project is to support and encourage transferring research knowledge to state and local agencies and manufacturers through field demonstrations. Presently available, Weigh-in-Motion and Classification Systems are typically too expensive to permit the wide deployment necessary to obtain representative vehicle data. Piezo electric technology has been used in the United Kingdom and Europe and is believed to be the basic element in a low-cost AWACS. Low-cost systems have been installed at two sites, one in Portland Cement Concrete (PCC) pavement in Iowa and the other in Asphaltic Cement Concrete (ACC) pavement in Minnesota to provide experience with both types of pavement. The systems provide axle weights, gross vehicle weight, axle spacing, vehicle classification, vehicle speed, vehicle count, and time of arrival. In addition, system self-calibration and a method to predict contact tire pressure is included in the system design. The study has shown that in the PCC pavement, the AWACS is capable of meeting the needs of state and federal highway agencies, producing accuracies comparable to many current commercial WIM devices. This is being achieved at a procurement cost of substantially less than currently available equipment. In the ACC pavement the accuracies were less than those observed in the PCC pavement which is concluded to result from a low pavement rigidity at this site. Further work is needed to assess the AWACS performance at a range of sites in ACC pavements.

Identification of Wax Esters in Latent Print Residues by Gas Chromatography-Mass Spectromertry and Their Potential Use as Aging Parameters

Recent studies show that the composition of fingerprint residue varies significantly from the same donor as well as between donors. This variability is a major drawback in latent print dating issues. This study aimed, therefore, at the definition of a parameter that is less variable from print to print, using a ratio of peak area of a target compound degrading over time divided by the summed area of peaks of more stable compounds also found in latent print residues.Gas chromatography-mass spectrometry (GC/MS) analysis of the initial lipid composition of latent prints identifies four main classes of compounds that can be used in the definition of an aging parameter: fatty acids, sterols, sterol precursors, and wax esters (WEs). Although the entities composing the first three groups are quite well known, those composing WEs are poorly reported. Therefore, the first step of the present work was to identify WE compounds present in latent print residues deposited by different donors. Of 29 WEs recorded in the chromatograms, seven were observed in the majority of samples.The identified WE compounds were subsequently used in the definition of ratios in combination with squalene and cholesterol to reduce the variability of the initial composition between latent print residues from different persons and more particularly from the same person. Finally, the influence of a latent print enhancement process on the initial composition was studied by analyzing traces after treatment with magnetic powder, 1,2-indanedione, and cyanoacrylate.

Evaluation of Hot Mix Asphalt Moisture Sensitivity Using the Nottingham Asphalt Test Equipment, TR-555, 2010

Pavements are subjected to different stresses during their design lives. A properly designed pavement will perform adequately during its design life, and the distresses will not exceed the allowable limits; however, there are several factors that can lead to premature pavement failure. One such factor is moisture sensitivity. AASHTO T 283 is the standard test used in the moisture susceptibility evaluation of asphalt mixtures, but the results of the test are not very representative of the expected behavior of asphalt mixtures. The dynamic modulus test measures a fundamental property of the mixture. The results of the dynamic modulus test can be used directly in the Mechanistic-Empirical Pavement Design Guide (MEPDG) and are considered a very good representation of the expected field performance of the mixture. Further research is still needed to study how the dynamic modulus results are affected by moisture. The flow number test was studied in previous research as a candidate test for moisture-susceptibility evaluation, but the results of that research were not favorable. This research has four main objectives. The first objective of this research is to evaluate the usefulness of the dynamic modulus and flow number tests in moisture-susceptibility evaluation. The second objective is to compare the results to those achieved using the AASHTO T 283 test. The third objective is to study the effect of different methods of sample conditioning and testing conditions. The fourth objective of the research is to study the variability in the test results.

Investigation of Materials for the Reduction and Prevention of Corrosion on Highway Maintenance Equipment, TR-472, 2009

The issue of corrosion of winter maintenance equipment is becoming of greater concern because of the increased use of liquid solutions of ice control chemicals, as opposed to their application in solid form. Being in liquid form, the ice control chemicals can more easily penetrate into the nooks and crannies on equipment and avoid being cleansed from the vehicle. Given this enhanced corrosive ability, methods must be found to minimize corrosion. The methods may include coatings, additives, cleansing techniques, other methods, and may also include doing nothing, and accepting a reduced equipment lifetime as a valid (perhaps) trade off with the enhanced benefits of using liquid ice control chemicals. In reality, some combination of these methods may prove to be optimal. Whatever solutions are selected, they must be relatively cheap and durable. The latter point is critical because of the environment in which maintenance trucks operate, in which scrapes, scratches and dents are facts of life. Protection methods that are not robust simply will not work. The purpose of this study is to determine how corrosion occurs on maintenance trucks, to find methods that would minimize the major corrosion mechanisms, and to

Effects of Implements of Husbandry (Farm Equipment) on Pavement Performance, TR-563, 2012

The effects of farm equipment on the structural behavior of flexible and rigid pavements were investigated in this study. The project quantified the difference in pavement behavior caused by heavy farm equipment as compared to a typical 5-axle, 80 kip semi-truck. This research was conducted on full scale pavement test sections designed and constructed at the Minnesota Road Research facility (MnROAD). The testing was conducted in the spring and fall seasons to capture responses when the pavement is at its weakest state and when agricultural vehicles operate at a higher frequency, respectively. The flexible pavement sections were heavily instrumented with strain gauges and earth pressure cells to measure essential pavement responses under heavy agricultural vehicles, whereas the rigid pavement sections were instrumented with strain gauges and linear variable differential transducers (LVDTs). The full scale testing data collected in this study were used to validate and calibrate analytical models used to predict relative damage to pavements. The developed procedure uses various inputs (including axle weight, tire footprint, pavement structure, material characteristics, and climatic information) to determine the critical pavement responses (strains and deflections). An analysis was performed to determine the damage caused by various types of vehicles to the roadway when there is a need to move large amounts agricultural product.

Ink dating using thermal desorption and gas chromatography / mass spectrometry: comparison of results obtained in two laboratories

Recent ink dating methods focused mainly on changes in solvent amounts occurring over time. A promising method was developed at the Landeskriminalamt of Munich using thermal desorption (TD) followed by gas chromatography / mass spectrometry (GC/MS) analysis. Sequential extractions of the phenoxyethanol present in ballpoint pen ink entries were carried out at two different temperatures. This method is applied in forensic practice and is currently implemented in several laboratories participating to the InCID group (International Collaboration on Ink Dating). However, harmonization of the method between the laboratories proved to be a particularly sensitive and time consuming task. The main aim of this work was therefore to implement the TD-GC/MS method at the Bundeskriminalamt (Wiesbaden, Germany) in order to evaluate if results were comparable to those obtained in Munich. At first validation criteria such as limits of reliable measurements, linearity and repeatability were determined. Samples were prepared in three different laboratories using the same inks and analyzed using two TDS-GC/MS instruments (one in Munich and one in Wiesbaden). The inter- and intra-laboratory variability of the ageing parameter was determined and ageing curves were compared. While inks stored in similar conditions yielded comparable ageing curves, it was observed that significantly different storage conditions had an influence on the resulting ageing curves. Finally, interpretation models, such as thresholds and trend tests, were evaluated and discussed in view of the obtained results. Trend tests were considered more suitable than threshold models. As both approaches showed limitations, an alternative model, based on the slopes of the ageing curves, was also proposed.

Health consultation : Sub-Slab Gas and Air Sampling Data Alcoa – Davenport Works CERCLIS No. IAD005270160 Riverdale, Scott County, Iowa (2005)

The U.S. Environmental Protection Agency (EPA), the Alcoa – Davenport Works Facility (Alcoa), and concerned citizens and community leaders of Riverdale, Iowa requested the Iowa Department of Public Health (IDPH) Hazardous Waste Site Health Assessment Program to evaluate the health impacts of exposures to volatile organic vapors detected within residences located immediately to the west of the Alcoa property. This health consultation addresses inhalation exposure to individuals that may have occupied the currently vacant residences in which the air sampling was completed.