NHEXAS PHASE I REGION 5 STUDY--METALS IN BLOOD ANALYTICAL RESULTS

EPA Science Inventory

This data set includes analytical results for measurements of metals in 165 blood samples. These samples were collected to examine the relationships between personal exposure measurements, environmental measurements, and body burden. Venous blood samples were collected by venipun...

NHEXAS PHASE I REGION 5 STUDY--VOCS IN BLOOD ANALYTICAL RESULTS

EPA Science Inventory

This data set includes analytical results for measurements of VOCs (volatile organic compounds) in 145 blood samples. These samples were collected to examine the relationships between personal exposure measurements, environmental measurements, and body burden. Venous blood sample...

Sample Collection Information Document for Chemical & Radiochemical Analytes – Companion to Selected Analytical Methods for Environmental Remediation and Recovery (SAM) 2012

EPA Pesticide Factsheets

Sample Collection Information Document is intended to provide sampling information to be used during site assessment, remediation and clearance activities following a chemical or radiological contamination incident.

Empirical insights and considerations for the OBT inter-laboratory comparison of environmental samples.

PubMed

Kim, Sang-Bog; Roche, Jennifer

2013-08-01

Organically bound tritium (OBT) is an important tritium species that can be measured in most environmental samples, but has only recently been recognized as a species of tritium in these samples. Currently, OBT is not routinely measured by environmental monitoring laboratories around the world. There are no certified reference materials (CRMs) for environmental samples. Thus, quality assurance (QA), or verification of the accuracy of the OBT measurement, is not possible. Alternatively, quality control (QC), or verification of the precision of the OBT measurement, can be achieved. In the past, there have been differences in OBT analysis results between environmental laboratories. A possible reason for the discrepancies may be differences in analytical methods. Therefore, inter-laboratory OBT comparisons among the environmental laboratories are important and would provide a good opportunity for adopting a reference OBT analytical procedure. Due to the analytical issues, only limited information is available on OBT measurement. Previously conducted OBT inter-laboratory practices are reviewed and the findings are described. Based on our experiences, a few considerations were suggested for the international OBT inter-laboratory comparison exercise to be completed in the near future. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Two important limitations relating to the spiking of environmental samples with contaminants of emerging concern: How close to the real analyte concentrations are the reported recovered values?

PubMed

Michael, Costas; Bayona, Josep Maria; Lambropoulou, Dimitra; Agüera, Ana; Fatta-Kassinos, Despo

2017-06-01

Occurrence and effects of contaminants of emerging concern pose a special challenge to environmental scientists. The investigation of these effects requires reliable, valid, and comparable analytical data. To this effect, two critical aspects are raised herein, concerning the limitations of the produced analytical data. The first relates to the inherent difficulty that exists in the analysis of environmental samples, which is related to the lack of knowledge (information), in many cases, of the form(s) of the contaminant in which is present in the sample. Thus, the produced analytical data can only refer to the amount of the free contaminant ignoring the amount in which it may be present in other forms; e.g., as in chelated and conjugated form. The other important aspect refers to the way with which the spiking procedure is generally performed to determine the recovery of the analytical method. Spiking environmental samples, in particular solid samples, with standard solution followed by immediate extraction, as is the common practice, can lead to an overestimation of the recovery. This is so, because no time is given to the system to establish possible equilibria between the solid matter-inorganic and/or organic-and the contaminant. Therefore, the spiking procedure need to be reconsidered by including a study of the extractable amount of the contaminant versus the time elapsed between spiking and the extraction of the sample. This study can become an element of the validation package of the method.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koester, C J; Moulik, A

This article discusses developments in environmental analytical chemistry that occurred in the years of 2003 and 2004. References were found by searching the ''Science Citation Index and Current Contents''. As in our review of two years ago (A1), techniques are highlighted that represent current trends and state-of-the-art technologies in the sampling, extraction, separation, and detection of trace concentrations, low-part-per-billion and less, of organic, inorganic, and organometallic contaminants in environmental samples. New analytes of interest are also reviewed, the detections of which are made possible by recently developed analytical instruments and methods.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

PubMed

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

This purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year 1990. The ACL has four technical groups -- Chemical Analysis, Instrumental Analysis, Organic Analysis, and Environmental Analysis. The Chemical Analysis Group uses wet-chemical and instrumental methods for elemental, compositional, and isotopic analyses of solid, liquid, and gaseous samples and provides specialized analytical services. The Instrumental Analysis Group uses nuclear counting techniques in radiochemical analyses over a wide range of sample types from low-level environmental samples to samples of high radioactivity. The Organic Analysis Group uses amore » number of complementary techniques to separate and to quantitatively and qualitatively analyze complex organic mixtures and compounds at the trace level, including synthetic fuels, toxic substances, fossil-fuel residues and emissions, pollutants, biologically active compounds, pesticides, and drugs. The Environmental Analysis Group performs analyses of inorganic environmental and hazardous waste and coal samples.« less

A new tool for the evaluation of the analytical procedure: Green Analytical Procedure Index.

PubMed

Płotka-Wasylka, J

2018-05-01

A new means for assessing analytical protocols relating to green analytical chemistry attributes has been developed. The new tool, called GAPI (Green Analytical Procedure Index), evaluates the green character of an entire analytical methodology, from sample collection to final determination, and was created using such tools as the National Environmental Methods Index (NEMI) or Analytical Eco-Scale to provide not only general but also qualitative information. In GAPI, a specific symbol with five pentagrams can be used to evaluate and quantify the environmental impact involved in each step of an analytical methodology, mainly from green through yellow to red depicting low, medium to high impact, respectively. The proposed tool was used to evaluate analytical procedures applied in the determination of biogenic amines in wine samples, and polycyclic aromatic hydrocarbon determination by EPA methods. GAPI tool not only provides an immediately perceptible perspective to the user/reader but also offers exhaustive information on evaluated procedures. Copyright © 2018 Elsevier B.V. All rights reserved.

SAM Companion Documents

EPA Pesticide Factsheets

SAM Companion Documents and Sample Collection Procedures provide information intended to complement the analytical methods listed in Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

Seabird tissue archival and monitoring project: Protocol for collecting and banking seabird eggs

USGS Publications Warehouse

Weston-York, Geoff; Porter, Barbara J.; Pugh, Rebecca S.; Roseneau, David G.; Simac, Kristin S.; Becker, Paul R.; Thorsteinson, Lyman K.; Wise, Stephen A.

2001-01-01

Archiving biological and environmental samples for retrospective analysis is a major component of systematic environmental monitoring. The long-term storage of carefully selected, representative samples in an environmental specimen bank is an important complement to the real-time monitoring of the environment. These archived samples permit:The use of subsequently developed innovative analytical technology that was not available at the time the samples were archived, for clear state-of-art identification an~ quantification of analytes of interest,The identification and quantification of analytes that are of subsequent interest but that were not of interest at the time the samples were archived, andThe comparison of present and past analytical techniques and values, providing continued credibility of past analytical values, and allowing flexibility in environmental monitoring programs.Seabirds, including albatrosses, pelicans, cormorants, terns, kittiwakes, murres, guillemots, and puffins spend most of their lives at sea and have special adaptations for feeding in the marine environment, including the ability to excrete the excess salt obtained from ingesting seawater. Many species nest in dense groups (colonies) on steep, precipitous sea-cliffs and headlands.Seabirds are long-lived and slow to mature. They occupy high positions in the marine food web and are considered sensitive indicators for the marine environment (prey includes krill, small fish, and squid). Breeding success, timing of nesting, diets, and survival rates may provide early indications of changing environmental conditions (e.g., see Hatch et aI., 1993). Chemical analysis of seabird tissues, including egg contents, can be particularly useful in determining whether contaminants (and potential biological effects) associated with human industrial activities, such as offshore petroleum and mineral exploration and development, are accumulating in marine environments. The collection and archival of seabird tissues over a period of several years will be a resource for future analyses, providing samples that can be used to determine historical baseline contaminant levels.

Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

2012-10-24

This plan incorporates U.S. Department of Energy (DOE) Office of Legacy Management (LM) standard operating procedures (SOPs) into environmental monitoring activities and will be implemented at all sites managed by LM. This document provides detailed procedures for the field sampling teams so that samples are collected in a consistent and technically defensible manner. Site-specific plans (e.g., long-term surveillance and maintenance plans, environmental monitoring plans) document background information and establish the basis for sampling and monitoring activities. Information will be included in site-specific tabbed sections to this plan, which identify sample locations, sample frequencies, types of samples, field measurements, and associatedmore » analytes for each site. Additionally, within each tabbed section, program directives will be included, when developed, to establish additional site-specific requirements to modify or clarify requirements in this plan as they apply to the corresponding site. A flowchart detailing project tasks required to accomplish routine sampling is displayed in Figure 1. LM environmental procedures are contained in the Environmental Procedures Catalog (LMS/PRO/S04325), which incorporates American Society for Testing and Materials (ASTM), DOE, and U.S. Environmental Protection Agency (EPA) guidance. Specific procedures used for groundwater and surface water monitoring are included in Appendix A. If other environmental media are monitored, SOPs used for air, soil/sediment, and biota monitoring can be found in the site-specific tabbed sections in Appendix D or in site-specific documents. The procedures in the Environmental Procedures Catalog are intended as general guidance and require additional detail from planning documents in order to be complete; the following sections fulfill that function and specify additional procedural requirements to form SOPs. Routine revision of this Sampling and Analysis Plan will be conducted annually at the beginning of each fiscal year when attachments in Appendix D, including program directives and sampling location/analytical tables, will be reviewed by project personnel and updated. The sampling location/analytical tables in Appendix D, however, may have interim updates according to project direction that are not reflected in this plan. Deviations from location/analytical tables in Appendix D prior to sampling will be documented in project correspondence (e.g., startup letters). If significant changes to other aspects of this plan are required before the annual update, then the plan will be revised as needed.« less

Novel immunoassay formats for integrated microfluidic circuits: diffusion immunoassays (DIA)

NASA Astrophysics Data System (ADS)

Weigl, Bernhard H.; Hatch, Anson; Kamholz, Andrew E.; Yager, Paul

2000-03-01

Novel designs of integrated fluidic microchips allow separations, chemical reactions, and calibration-free analytical measurements to be performed directly in very small quantities of complex samples such as whole blood and contaminated environmental samples. This technology lends itself to applications such as clinical diagnostics, including tumor marker screening, and environmental sensing in remote locations. Lab-on-a-Chip based systems offer many *advantages over traditional analytical devices: They consume extremely low volumes of both samples and reagents. Each chip is inexpensive and small. The sampling-to-result time is extremely short. They perform all analytical functions, including sampling, sample pretreatment, separation, dilution, and mixing steps, chemical reactions, and detection in an integrated microfluidic circuit. Lab-on-a-Chip systems enable the design of small, portable, rugged, low-cost, easy to use, yet extremely versatile and capable diagnostic instruments. In addition, fluids flowing in microchannels exhibit unique characteristics ('microfluidics'), which allow the design of analytical devices and assay formats that would not function on a macroscale. Existing Lab-on-a-chip technologies work very well for highly predictable and homogeneous samples common in genetic testing and drug discovery processes. One of the biggest challenges for current Labs-on-a-chip, however, is to perform analysis in the presence of the complexity and heterogeneity of actual samples such as whole blood or contaminated environmental samples. Micronics has developed a variety of Lab-on-a-Chip assays that can overcome those shortcomings. We will now present various types of novel Lab- on-a-Chip-based immunoassays, including the so-called Diffusion Immunoassays (DIA) that are based on the competitive laminar diffusion of analyte molecules and tracer molecules into a region of the chip containing antibodies that target the analyte molecules. Advantages of this technique are a reduction in reagents, higher sensitivity, minimal preparation of complex samples such as blood, real-time calibration, and extremely rapid analysis.

Adjustment of pesticide concentrations for temporal changes in analytical recovery, 1992–2010

USGS Publications Warehouse

Martin, Jeffrey D.; Eberle, Michael

2011-01-01

Recovery is the proportion of a target analyte that is quantified by an analytical method and is a primary indicator of the analytical bias of a measurement. Recovery is measured by analysis of quality-control (QC) water samples that have known amounts of target analytes added ("spiked" QC samples). For pesticides, recovery is the measured amount of pesticide in the spiked QC sample expressed as a percentage of the amount spiked, ideally 100 percent. Temporal changes in recovery have the potential to adversely affect time-trend analysis of pesticide concentrations by introducing trends in apparent environmental concentrations that are caused by trends in performance of the analytical method rather than by trends in pesticide use or other environmental conditions. This report presents data and models related to the recovery of 44 pesticides and 8 pesticide degradates (hereafter referred to as "pesticides") that were selected for a national analysis of time trends in pesticide concentrations in streams. Water samples were analyzed for these pesticides from 1992 through 2010 by gas chromatography/mass spectrometry. Recovery was measured by analysis of pesticide-spiked QC water samples. Models of recovery, based on robust, locally weighted scatterplot smooths (lowess smooths) of matrix spikes, were developed separately for groundwater and stream-water samples. The models of recovery can be used to adjust concentrations of pesticides measured in groundwater or stream-water samples to 100 percent recovery to compensate for temporal changes in the performance (bias) of the analytical method.

The procedures manual of the Environmental Measurements Laboratory. Volume 2, 28. edition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chieco, N.A.

1997-02-01

This report contains environmental sampling and analytical chemistry procedures that are performed by the Environmental Measurements Laboratory. The purpose of environmental sampling and analysis is to obtain data that describe a particular site at a specific point in time from which an evaluation can be made as a basis for possible action.

Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

PubMed Central

Sosa-Ferrera, Zoraida; Mahugo-Santana, Cristina; Santana-Rodríguez, José Juan

2013-01-01

Endocrine-disruptor compounds (EDCs) can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented. PMID:23738329

Arsenic, Antimony, Chromium, and Thallium Speciation in Water and Sediment Samples with the LC-ICP-MS Technique

PubMed Central

Jabłońska-Czapla, Magdalena

2015-01-01

Chemical speciation is a very important subject in the environmental protection, toxicology, and chemical analytics due to the fact that toxicity, availability, and reactivity of trace elements depend on the chemical forms in which these elements occur. Research on low analyte levels, particularly in complex matrix samples, requires more and more advanced and sophisticated analytical methods and techniques. The latest trends in this field concern the so-called hyphenated techniques. Arsenic, antimony, chromium, and (underestimated) thallium attract the closest attention of toxicologists and analysts. The properties of those elements depend on the oxidation state in which they occur. The aim of the following paper is to answer the question why the speciation analytics is so important. The paper also provides numerous examples of the hyphenated technique usage (e.g., the LC-ICP-MS application in the speciation analysis of chromium, antimony, arsenic, or thallium in water and bottom sediment samples). An important issue addressed is the preparation of environmental samples for speciation analysis. PMID:25873962

Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

DOEpatents

Stark, Peter C [Los Alamos, NM; Zurek, Eduardo [Barranquilla, CO; Wheat, Jeffrey V [Fort Walton Beach, FL; Dunbar, John M [Santa Fe, NM; Olivares, Jose A [Los Alamos, NM; Garcia-Rubio, Luis H [Temple Terrace, FL; Ward, Michael D [Los Alamos, NM

2011-07-26

There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

Protocol for Detection of Yersinia pestis in Environmental ...

EPA Pesticide Factsheets

Methods Report This is the first ever open-access and detailed protocol available to all government departments and agencies, and their contractors to detect Yersinia pestis, the pathogen that causes plague, from multiple environmental sample types including water. Each analytical method includes sample processing procedure for each sample type in a step-by-step manner. It includes real-time PCR, traditional microbiological culture, and the Rapid Viability PCR (RV-PCR) analytical methods. For large volume water samples it also includes an ultra-filtration-based sample concentration procedure. Because of such a non-restrictive availability of this protocol to all government departments and agencies, and their contractors, the nation will now have increased laboratory capacity to analyze large number of samples during a wide-area plague incident.

Microbiological Detection Systems for Molecular Analysis of Environmental Water and Soil Samples

EPA Science Inventory

Multiple detection systems are being targeted to track various species and genotypes of pathogens found in environmental samples with the overreaching goal of developing analytical separation and detection techniques for Salmonella enterica Serovars Typhi, Cryptosporidium parvum,...

40 CFR 87.82 - Sampling and analytical procedures for measuring smoke exhaust emissions.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 20 2011-07-01 2011-07-01 false Sampling and analytical procedures for measuring smoke exhaust emissions. 87.82 Section 87.82 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) CONTROL OF AIR POLLUTION FROM AIRCRAFT AND AIRCRAFT ENGINES...

40 CFR 87.64 - Sampling and analytical procedures for measuring gaseous exhaust emissions.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 20 2011-07-01 2011-07-01 false Sampling and analytical procedures for measuring gaseous exhaust emissions. 87.64 Section 87.64 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) CONTROL OF AIR POLLUTION FROM AIRCRAFT AND AIRCRAFT ENGINES...

40 CFR 87.82 - Sampling and analytical procedures for measuring smoke exhaust emissions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 20 2010-07-01 2010-07-01 false Sampling and analytical procedures for measuring smoke exhaust emissions. 87.82 Section 87.82 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) CONTROL OF AIR POLLUTION FROM AIRCRAFT AND AIRCRAFT ENGINES...

40 CFR 87.64 - Sampling and analytical procedures for measuring gaseous exhaust emissions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 20 2010-07-01 2010-07-01 false Sampling and analytical procedures for measuring gaseous exhaust emissions. 87.64 Section 87.64 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) CONTROL OF AIR POLLUTION FROM AIRCRAFT AND AIRCRAFT ENGINES...

Dynamic fabric phase sorptive extraction for a group of pharmaceuticals and personal care products from environmental waters.

PubMed

Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Marcé, Rosa Maria; Fontanals, Núria

2016-07-22

This paper describes for the first time the use of a new extraction technique, based on fabric phase sorptive extraction (FPSE). This new mode proposes the extraction of the analytes in dynamic mode in order to reduce the extraction time. Dynamic fabric phase sorptive extraction (DFPSE) followed by liquid chromatography-tandem mass spectrometry was evaluated for the extraction of a group of pharmaceuticals and personal care products (PPCPs) from environmental water samples. Different parameters affecting the extraction were optimized and best conditions were achieved when 50mL of sample at pH 3 was passed through 3 disks and analytes retained were eluted with 10mL of ethyl acetate. The recoveries were higher than 60% for most of compounds with the exception of the most polar ones (between 8% and 38%). The analytical method was validated with environmental samples such as river water and effluent and influent wastewater, and good performance was obtained. The analysis of samples revealed the presence of some PPCPs at low ngL(-1) concentrations. Copyright © 2016 Elsevier B.V. All rights reserved.

Environmental monitoring of phenolic pollutants in water by cloud point extraction prior to micellar electrokinetic chromatography.

PubMed

Stege, Patricia W; Sombra, Lorena L; Messina, Germán A; Martinez, Luis D; Silva, María F

2009-05-01

Many aromatic compounds can be found in the environment as a result of anthropogenic activities and some of them are highly toxic. The need to determine low concentrations of pollutants requires analytical methods with high sensitivity, selectivity, and resolution for application to soil, sediment, water, and other environmental samples. Complex sample preparation involving analyte isolation and enrichment is generally necessary before the final analysis. The present paper outlines a novel, simple, low-cost, and environmentally friendly method for the simultaneous determination of p-nitrophenol (PNP), p-aminophenol (PAP), and hydroquinone (HQ) by micellar electrokinetic capillary chromatography after preconcentration by cloud point extraction. Enrichment factors of 180 to 200 were achieved. The limits of detection of the analytes for the preconcentration of 50-ml sample volume were 0.10 microg L(-1) for PNP, 0.20 microg L(-1) for PAP, and 0.16 microg L(-1) for HQ. The optimized procedure was applied to the determination of phenolic pollutants in natural waters from San Luis, Argentina.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and alpha-spectrometry.

PubMed

Goldstein, S J; Hensley, C A; Armenta, C E; Peters, R J

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for alpha-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of "real" environmental and bioassay samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of approximately 2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously.

Simultaneous analysis of multiple classes of antimicrobials in environmental water samples using SPE coupled with UHPLC-ESI-MS/MS and isotope dilution.

PubMed

Tran, Ngoc Han; Chen, Hongjie; Do, Thanh Van; Reinhard, Martin; Ngo, Huu Hao; He, Yiliang; Gin, Karina Yew-Hoong

2016-10-01

A robust and sensitive analytical method was developed for the simultaneous analysis of 21 target antimicrobials in different environmental water samples. Both single SPE and tandem SPE cartridge systems were investigated to simultaneously extract multiple classes of antimicrobials. Experimental results showed that good extraction efficiencies (84.5-105.6%) were observed for the vast majority of the target analytes when extraction was performed using the tandem SPE cartridge (SB+HR-X) system under an extraction pH of 3.0. HPLC-MS/MS parameters were optimized for simultaneous analysis of all the target analytes in a single injection. Quantification of target antimicrobials in water samples was accomplished using 15 isotopically labeled internal standards (ILISs), which allowed the efficient compensation of the losses of target analytes during sample preparation and correction of matrix effects during UHPLC-MS/MS as well as instrument fluctuations in MS/MS signal intensity. Method quantification limit (MQL) for most target analytes based on SPE was below 5ng/L for surface waters, 10ng/L for treated wastewater effluents, and 15ng/L for raw wastewater. The method was successfully applied to detect and quantify the occurrence of the target analytes in raw influent, treated effluent and surface water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

U.S. Geological Survey Standard Reference Sample Project: Performance Evaluation of Analytical Laboratories

USGS Publications Warehouse

Long, H. Keith; Daddow, Richard L.; Farrar, Jerry W.

1998-01-01

Since 1962, the U.S. Geological Survey (USGS) has operated the Standard Reference Sample Project to evaluate the performance of USGS, cooperator, and contractor analytical laboratories that analyze chemical constituents of environmental samples. The laboratories are evaluated by using performance evaluation samples, called Standard Reference Samples (SRSs). SRSs are submitted to laboratories semi-annually for round-robin laboratory performance comparison purposes. Currently, approximately 100 laboratories are evaluated for their analytical performance on six SRSs for inorganic and nutrient constituents. As part of the SRS Project, a surplus of homogeneous, stable SRSs is maintained for purchase by USGS offices and participating laboratories for use in continuing quality-assurance and quality-control activities. Statistical evaluation of the laboratories results provides information to compare the analytical performance of the laboratories and to determine possible analytical deficiences and problems. SRS results also provide information on the bias and variability of different analytical methods used in the SRS analyses.

METHOD DEVELOPMENT FOR THE DETERMINATION OF FORMALDEHYDE IN SAMPLES OF ENVIRONMENTAL ORIGIN

EPA Science Inventory

An analytical method was developed for the determination of formaldehyde in samples of environmental origin. After a review of the current literature, five candidate methods involving chemical derivatization were chosen for evaluation. The five derivatization reagents studied wer...

Detection of pyrethroid pesticides and their environmental degradation products in duplicate diet samples

EPA Science Inventory

The abstract is for an oral presentation at the Asilomar Conference on Mass Spectrometry: Mass Spectrometry in Environmental Chemistry, Toxicology, and Health. It describes analytical method development and sample results for determination of pyrethroid pesticides and environme...

Quality-assurance results for routine water analysis in US Geological Survey laboratories, water year 1991

USGS Publications Warehouse

Maloney, T.J.; Ludtke, A.S.; Krizman, T.L.

1994-01-01

The US. Geological Survey operates a quality- assurance program based on the analyses of reference samples for the National Water Quality Laboratory in Arvada, Colorado, and the Quality of Water Service Unit in Ocala, Florida. Reference samples containing selected inorganic, nutrient, and low ionic-strength constituents are prepared and disguised as routine samples. The program goal is to determine precision and bias for as many analytical methods offered by the participating laboratories as possible. The samples typically are submitted at a rate of approximately 5 percent of the annual environmental sample load for each constituent. The samples are distributed to the laboratories throughout the year. Analytical data for these reference samples reflect the quality of environmental sample data produced by the laboratories because the samples are processed in the same manner for all steps from sample login through data release. The results are stored permanently in the National Water Data Storage and Retrieval System. During water year 1991, 86 analytical procedures were evaluated at the National Water Quality Laboratory and 37 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic (major ion and trace metal) constituent data for water year 1991 indicated analytical imprecision in the National Water Quality Laboratory for 5 of 67 analytical procedures: aluminum (whole-water recoverable, atomic emission spectrometric, direct-current plasma); calcium (atomic emission spectrometric, direct); fluoride (ion-exchange chromatographic); iron (whole-water recoverable, atomic absorption spectrometric, direct); and sulfate (ion-exchange chromatographic). The results for 11 of 67 analytical procedures had positive or negative bias during water year 1991. Analytical imprecision was indicated in the determination of two of the five National Water Quality Laboratory nutrient constituents: orthophosphate as phosphorus and phosphorus. A negative or positive bias condition was indicated in three of five nutrient constituents. There was acceptable precision and no indication of bias for the 14 low ionic-strength analytical procedures tested in the National Water Quality Laboratory program and for the 32 inorganic and 5 nutrient analytical procedures tested in the Quality of Water Service Unit during water year 1991.

HSRP and HSRP Partner Analytical Methods and Protocols

EPA Pesticide Factsheets

HSRP has worked with various partners to develop and test analytical methods and protocols for use by laboratories charged with analyzing environmental and/or buildling material samples following contamination incident.

The Sampling and Analysis Plan, Galena Airport and Kalakaket Creek Radio Relay Station, Alaska. Addendum

DTIC Science & Technology

1994-09-08

information deactivated during 1993. Currently, approximately 30 required in a QAPP per the U.S. Environmental caretakers are present at the facility...the total analytical cost. A subset of those Galena Airport-The current environmental samples collected and screened will be sent to an investigative...sampling report United States Environmental Protection Agency (US preparation. EPA), USAF, state, and local requirements. Ms. Sandy Smith is

Clean Water Act Analytical Methods

EPA Pesticide Factsheets

EPA publishes laboratory analytical methods (test procedures) that are used by industries and municipalities to analyze the chemical, physical and biological components of wastewater and other environmental samples required by the Clean Water Act.

Hanford analytical sample projections FY 1998--FY 2002

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joyce, S.M.

1998-02-12

Analytical Services projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Projections are categorized by radiation level, protocol, sample matrix and program. Analyses requirements are also presented. This document summarizes the Hanford sample projections for fiscal years 1998 to 2002. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Waste Remediation Systems (TWRS), Solid Waste, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition, details on laboratory scale technology (development) work, Sample Management,more » and Data Management activities are included. This information will be used by Hanford Analytical Services (HAS) and the Sample Management Working Group (SMWG) to assure that laboratories and resources are available and effectively utilized to meet these documented needs.« less

The Savannah River Site`s groundwater monitoring program. Third quarter 1990

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1991-05-06

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site`s (SRS) Groundwater Monitoring Program. During third quarter 1990 (July through September) EPD/EMS conducted routine sampling of monitoring wells and drinking water locations. EPD/EMS established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria do not define contamination levels; instead they aid personnel in sample scheduling, interpretation of data, and trend identification. The flagging criteria are based on detection limits, background levels in SRS groundwater, and drinking water standards. All analytical results from third quarter 1990 are listed in thismore » report, which is distributed to all site custodians. One or more analytes exceeded Flag 2 in 87 monitoring well series. Analytes exceeded Flat 2 for the first since 1984 in 14 monitoring well series. In addition to groundwater monitoring, EPD/EMS collected drinking water samples from SRS drinking water systems supplied by wells. The drinking water samples were analyzed for radioactive constituents.« less

The Savannah River Site's groundwater monitoring program

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1991-05-06

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site's (SRS) Groundwater Monitoring Program. During third quarter 1990 (July through September) EPD/EMS conducted routine sampling of monitoring wells and drinking water locations. EPD/EMS established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria do not define contamination levels; instead they aid personnel in sample scheduling, interpretation of data, and trend identification. The flagging criteria are based on detection limits, background levels in SRS groundwater, and drinking water standards. All analytical results from third quarter 1990 are listed in thismore » report, which is distributed to all site custodians. One or more analytes exceeded Flag 2 in 87 monitoring well series. Analytes exceeded Flat 2 for the first since 1984 in 14 monitoring well series. In addition to groundwater monitoring, EPD/EMS collected drinking water samples from SRS drinking water systems supplied by wells. The drinking water samples were analyzed for radioactive constituents.« less

The Use and Abuse of Limits of Detection in Environmental Analytical Chemistry

PubMed Central

Brown, Richard J. C.

2008-01-01

The limit of detection (LoD) serves as an important method performance measure that is useful for the comparison of measurement techniques and the assessment of likely signal to noise performance, especially in environmental analytical chemistry. However, the LoD is only truly related to the precision characteristics of the analytical instrument employed for the analysis and the content of analyte in the blank sample. This article discusses how other criteria, such as sampling volume, can serve to distort the quoted LoD artificially and make comparison between various analytical methods inequitable. In order to compare LoDs between methods properly, it is necessary to state clearly all of the input parameters relating to the measurements that have been used in the calculation of the LoD. Additionally, the article discusses that the use of LoDs in contexts other than the comparison of the attributes of analytical methods, in particular when reporting analytical results, may be confusing, less informative than quoting the actual result with an accompanying statement of uncertainty, and may act to bias descriptive statistics. PMID:18690384

Analysis of Environmental Contamination resulting from ...

EPA Pesticide Factsheets

Catastrophic incidents can generate a large number of samples with analytically diverse types including forensic, clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urban building and infrastructure materials, and surface residue. Such samples may arise not only from contamination from the incident but also from the multitude of activities surrounding the response to the incident, including decontamination. This document summarizes a range of activities to help build laboratory capability in preparation for analysis following a catastrophic incident, including selection and development of fit-for-purpose analytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are those which have been selected to meet project specific data quality objectives. For example, methods could be fit for screening contamination in the early phases of investigation of contamination incidents because they are rapid and easily implemented, but those same methods may not be fit for the purpose of remediating the environment to safe levels when a more sensitive method is required. While the exact data quality objectives defining fitness-for-purpose can vary with each incident, a governing principle of the method selection and development process for environmental remediation and recovery is based on achieving high throughput while maintaining high quality analytical results. This paper illu

Analysis of environmental contamination resulting from catastrophic incidents: part 2. Building laboratory capability by selecting and developing analytical methodologies.

PubMed

Magnuson, Matthew; Campisano, Romy; Griggs, John; Fitz-James, Schatzi; Hall, Kathy; Mapp, Latisha; Mullins, Marissa; Nichols, Tonya; Shah, Sanjiv; Silvestri, Erin; Smith, Terry; Willison, Stuart; Ernst, Hiba

2014-11-01

Catastrophic incidents can generate a large number of samples of analytically diverse types, including forensic, clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urban building and infrastructure materials, and surface residue. Such samples may arise not only from contamination from the incident but also from the multitude of activities surrounding the response to the incident, including decontamination. This document summarizes a range of activities to help build laboratory capability in preparation for sample analysis following a catastrophic incident, including selection and development of fit-for-purpose analytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are those which have been selected to meet project specific data quality objectives. For example, methods could be fit for screening contamination in the early phases of investigation of contamination incidents because they are rapid and easily implemented, but those same methods may not be fit for the purpose of remediating the environment to acceptable levels when a more sensitive method is required. While the exact data quality objectives defining fitness-for-purpose can vary with each incident, a governing principle of the method selection and development process for environmental remediation and recovery is based on achieving high throughput while maintaining high quality analytical results. This paper illustrates the result of applying this principle, in the form of a compendium of analytical methods for contaminants of interest. The compendium is based on experience with actual incidents, where appropriate and available. This paper also discusses efforts aimed at adaptation of existing methods to increase fitness-for-purpose and development of innovative methods when necessary. The contaminants of interest are primarily those potentially released through catastrophes resulting from malicious activity. However, the same techniques discussed could also have application to catastrophes resulting from other incidents, such as natural disasters or industrial accidents. Further, the high sample throughput enabled by the techniques discussed could be employed for conventional environmental studies and compliance monitoring, potentially decreasing costs and/or increasing the quantity of data available to decision-makers. Published by Elsevier Ltd.

Sample Collection Procedures and Strategies

EPA Pesticide Factsheets

Individuals responsible for collecting environmental and building material samples following a contamination incident, can use these procedures to plan for and/or collect samples for analysis using the analytical methods listed in EPA's SAM

SIMULTANEOUS DETERMINATION OF ORGANOTIN, ORGANOLEAD, AND ORGANOMERCURY COMPOUNDS IN ENVIRONMENTAL SAMPLES USING CAPILLARY GAS CHROMATOGRAPHY WITH ATOMIC EMISSION DETECTION

EPA Science Inventory

As part of a continuing evaluation of new analytical and sample preparation techniques conducted by the US Environmental Protection Agency (EPA), the use of capillary gas chromatography with atomic emission detection (GC-AED) for the simultaneous determination of organotin, organ...

ION COMPOSITION ELUCIDATION (ICE): A HIGH RESOLUTION MASS SPECTROMETRIC TOOL FOR IDENTIFYING ORGANIC COMPOUNDS IN COMPLEX EXTRACTS OF ENVIRONMENTAL SAMPLES

EPA Science Inventory

Unidentified Organic Compounds. For target analytes, standards are purchased, extraction and clean-up procedures are optimized, and mass spectra and retention times for the chromatographic separation are obtained for comparison to the target compounds in environmental sample ...

On-line solid-phase microextraction of triclosan, bisphenol A, chlorophenols, and selected pharmaceuticals in environmental water samples by high-performance liquid chromatography-ultraviolet detection.

PubMed

Kim, Dalho; Han, Jungho; Choi, Yongwook

2013-01-01

A method using on-line solid-phase microextraction (SPME) on a carbowax-templated fiber followed by liquid chromatography (LC) with ultraviolet (UV) detection was developed for the determination of triclosan in environmental water samples. Along with triclosan, other selected phenolic compounds, bisphenol A, and acidic pharmaceuticals were studied. Previous SPME/LC or stir-bar sorptive extraction/LC-UV for polar analytes showed lack of sensitivity. In this study, the calculated octanol-water distribution coefficient (log D) values of the target analytes at different pH values were used to estimate polarity of the analytes. The lack of sensitivity observed in earlier studies is identified as a lack of desorption by strong polar-polar interactions between analyte and solid-phase. Calculated log D values were useful to understand or predict the interaction between analyte and solid phase. Under the optimized conditions, the method detection limit of selected analytes by using on-line SPME-LC-UV method ranged from 5 to 33 ng L(-1), except for very polar 3-chlorophenol and 2,4-dichlorophenol which was obscured in wastewater samples by an interfering substance. This level of detection represented a remarkable improvement over the conventional existing methods. The on-line SPME-LC-UV method, which did not require derivatization of analytes, was applied to the determination of TCS including phenolic compounds and acidic pharmaceuticals in tap water and river water and municipal wastewater samples.

Advances in organic-inorganic hybrid sorbents for the extraction of organic and inorganic pollutants in different types of food and environmental samples.

PubMed

Ng, Nyuk-Ting; Kamaruddin, Amirah Farhan; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Abdul Keyon, Aemi S

2018-01-01

The efficiency of the extraction and removal of pollutants from food and the environment has been an important issue in analytical science. By incorporating inorganic species into an organic matrix, a new material known as an organic-inorganic hybrid material is formed. As it possesses high selectivity, permeability, and mechanical and chemical stabilities, organic-inorganic hybrid materials constitute an emerging research field and have become popular to serve as sorbents in various separaton science methods. Here, we review recent significant advances in analytical solid-phase extraction employing organic-inorganic composite/nanocomposite sorbents for the extraction of organic and inorganic pollutants from various types of food and environmental matrices. The physicochemical characteristics, extraction properties, and analytical performances of sorbents are discussed; including morphology and surface characteristics, types of functional groups, interaction mechanism, selectivity and sensitivity, accuracy, and regeneration abilities. Organic-inorganic hybrid sorbents combined with extraction techniques are highly promising for sample preparation of various food and environmental matrixes with analytes at trace levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation of a polar monolithic stir bar based on methacrylic acid and divinylbenzene for the sorptive extraction of polar pharmaceuticals from complex water samples.

PubMed

Bratkowska, D; Fontanals, N; Cormack, P A G; Borrull, F; Marcé, R M

2012-02-17

A monolithic, hydrophilic stir bar coating based upon a copolymer of methacrylic acid and divinylbenzene [poly(MAA-co-DVB)] was synthesised and evaluated as a new polymeric phase for the stir bar sorptive extraction (SBSE) of polar compounds from complex environmental water samples. The experimental conditions for the extraction and liquid desorption in SBSE were optimised. Liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was used for the determination of a group of polar pharmaceuticals in environmental water matrices. The extraction performance of the poly(MAA-co-DVB) stir bar was compared to the extraction performance of a commercially available polydimethylsiloxane stir bar; it was found that the former gave rise to significantly higher extraction efficiency of polar analytes (% recovery values near to 100% for most of the studied analytes) than the commercial product. The developed method was applied to determine the studied analytes at low ng L⁻¹ in different complex environmental water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and {alpha}-Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goldstein, S.J.; Hensley, C.A.; Armenta, C.E.

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for {alpha}-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of `real` environmental and bioassaymore » samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of {approx}2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously. 24 refs., 2 figs., 2 tabs.« less

Application of enhanced gas chromatography/triple quadrupole mass spectrometry for monitoring petroleum weathering and forensic source fingerprinting in samples impacted by the Deepwater Horizon oil spill.

PubMed

Adhikari, Puspa L; Wong, Roberto L; Overton, Edward B

2017-10-01

Accurate characterization of petroleum hydrocarbons in complex and weathered oil residues is analytically challenging. This is primarily due to chemical compositional complexity of both the oil residues and environmental matrices, and the lack of instrumental selectivity due to co-elution of interferences with the target analytes. To overcome these analytical selectivity issues, we used an enhanced resolution gas chromatography coupled with triple quadrupole mass spectrometry in Multiple Reaction Monitoring (MRM) mode (GC/MS/MS-MRM) to eliminate interferences within the ion chromatograms of target analytes found in environmental samples. This new GC/MS/MS-MRM method was developed and used for forensic fingerprinting of deep-water and marsh sediment samples containing oily residues from the Deepwater Horizon oil spill. The results showed that the GC/MS/MS-MRM method increases selectivity, eliminates interferences, and provides more accurate quantitation and characterization of trace levels of alkyl-PAHs and biomarker compounds, from weathered oil residues in complex sample matrices. The higher selectivity of the new method, even at low detection limits, provides greater insights on isomer and homolog compositional patterns and the extent of oil weathering under various environmental conditions. The method also provides flat chromatographic baselines for accurate and unambiguous calculation of petroleum forensic biomarker compound ratios. Thus, this GC/MS/MS-MRM method can be a reliable analytical strategy for more accurate and selective trace level analyses in petroleum forensic studies, and for tacking continuous weathering of oil residues. Copyright © 2017 Elsevier Ltd. All rights reserved.

Environmental Response Laboratory Network (ERLN) Laboratory Requirements

EPA Pesticide Factsheets

The Environmental Response Laboratory Network requires its member labs follow specified quality systems, sample management, data reporting, and general, in order to ensure consistent analytical data of known and documented quality.

Green analytical chemistry--theory and practice.

PubMed

Tobiszewski, Marek; Mechlińska, Agata; Namieśnik, Jacek

2010-08-01

This tutorial review summarises the current state of green analytical chemistry with special emphasis on environmentally friendly sample preparation techniques. Green analytical chemistry is a part of the sustainable development concept; its history and origins are described. Miniaturisation of analytical devices and shortening the time elapsing between performing analysis and obtaining reliable analytical results are important aspects of green analytical chemistry. Solventless extraction techniques, the application of alternative solvents and assisted extractions are considered to be the main approaches complying with green analytical chemistry principles.

Comparison of two thin-film microextractions for the analysis of estrogens in aqueous tea extract and environmental water samples by high performance liquid chromatography-ultraviolet detection.

PubMed

Cai, Pei-Shan; Li, Dan; Chen, Jing; Xiong, Chao-Mei; Ruan, Jin-Lan

2015-04-15

Two thin-film microextractions (TFME), octadecylsilane (ODS)-polyacrylonitrile (PAN)-TFME and polar enhanced phase (PEP)-PAN-TFME have been proposed for the analysis of bisphenol-A, diethylstilbestrol and 17β-estradiol in aqueous tea extract and environmental water samples followed by high performance liquid chromatography-ultraviolet detection. Both thin-films were prepared by spraying. The influencing factors including pH, extraction time, desorption solvent, desorption volume, desorption time, ion strength and reusability were investigated. Under the optimal conditions, the two TFME methods are similar in terms of the analytical performance evaluated by standard addition method. The limits of detection for three estrogens in environmental water and aqueous tea extract matrix ranged from 1.3 to 1.6 and 2.8 to 7.1 ng mL(-1) by the two TFME methods, respectively. Both approaches were applied for the analysis of analytes in real aqueous tea extract and environmental water samples, presenting satisfactory recoveries ranged from 87.3% to 109.4% for the spiked samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

A sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

PubMed

Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

2015-05-01

The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies.

Base Realignment and Closure Environmental Evaluation (BRAC EE) Fort Devens, Massachusetts

DTIC Science & Technology

1995-09-01

Not Sampled ......... 6 2.3.2 Transformer Sites Sampled ........................ 7 2.4 Soil Sampling Protocol and Analytical Program ...Evaluation (AREE) 66. The study included evaluating the current PCB Transformer Management Program administered by the Fort Devens Environmental Management...Office (EMO), the Fort Devens Spill Contingency Plan, and the ongoing transformer inspection program . Personnel in both the Fort Devens EMO and the Fort

Automating data analysis for two-dimensional gas chromatography/time-of-flight mass spectrometry non-targeted analysis of comparative samples.

PubMed

Titaley, Ivan A; Ogba, O Maduka; Chibwe, Leah; Hoh, Eunha; Cheong, Paul H-Y; Simonich, Staci L Massey

2018-03-16

Non-targeted analysis of environmental samples, using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC/ToF-MS), poses significant data analysis challenges due to the large number of possible analytes. Non-targeted data analysis of complex mixtures is prone to human bias and is laborious, particularly for comparative environmental samples such as contaminated soil pre- and post-bioremediation. To address this research bottleneck, we developed OCTpy, a Python™ script that acts as a data reduction filter to automate GC × GC/ToF-MS data analysis from LECO ® ChromaTOF ® software and facilitates selection of analytes of interest based on peak area comparison between comparative samples. We used data from polycyclic aromatic hydrocarbon (PAH) contaminated soil, pre- and post-bioremediation, to assess the effectiveness of OCTpy in facilitating the selection of analytes that have formed or degraded following treatment. Using datasets from the soil extracts pre- and post-bioremediation, OCTpy selected, on average, 18% of the initial suggested analytes generated by the LECO ® ChromaTOF ® software Statistical Compare feature. Based on this list, 63-100% of the candidate analytes identified by a highly trained individual were also selected by OCTpy. This process was accomplished in several minutes per sample, whereas manual data analysis took several hours per sample. OCTpy automates the analysis of complex mixtures of comparative samples, reduces the potential for human error during heavy data handling and decreases data analysis time by at least tenfold. Copyright © 2018 Elsevier B.V. All rights reserved.

A Modern Approach to College Analytical Chemistry.

ERIC Educational Resources Information Center

Neman, R. L.

1983-01-01

Describes a course which emphasizes all facets of analytical chemistry, including sampling, preparation, interference removal, selection of methodology, measurement of a property, and calculation/interpretation of results. Includes special course features (such as cooperative agreement with an environmental protection center) and course…

A soil sampling intercomparison exercise for the ALMERA network.

PubMed

Belli, Maria; de Zorzi, Paolo; Sansone, Umberto; Shakhashiro, Abduhlghani; Gondin da Fonseca, Adelaide; Trinkl, Alexander; Benesch, Thomas

2009-11-01

Soil sampling and analysis for radionuclides after an accidental or routine release is a key factor for the dose calculation to members of the public, and for the establishment of possible countermeasures. The IAEA organized for selected laboratories of the ALMERA (Analytical Laboratories for the Measurement of Environmental Radioactivity) network a Soil Sampling Intercomparison Exercise (IAEA/SIE/01) with the objective of comparing soil sampling procedures used by different laboratories. The ALMERA network is a world-wide network of analytical laboratories located in IAEA member states capable of providing reliable and timely analysis of environmental samples in the event of an accidental or intentional release of radioactivity. Ten ALMERA laboratories were selected to participate in the sampling exercise. The soil sampling intercomparison exercise took place in November 2005 in an agricultural area qualified as a "reference site", aimed at assessing the uncertainties associated with soil sampling in agricultural, semi-natural, urban and contaminated environments and suitable for performing sampling intercomparison. In this paper, the laboratories sampling performance were evaluated.

USGS Laboratory Review Program Ensures Analytical Quality

USGS Publications Warehouse

Erdmann, David E.

1995-01-01

The USGS operates a review program for laboratories that analyze samples for USGS environmental investigations. This program has been effective in providing QA feedback to laboratories while ensuring that analytical data are consistent, of satisfactory quality, and meet the data objectives of the investigation.

A New Approach to Standardize Multicenter Studies: Mobile Lab Technology for the German Environmental Specimen Bank

PubMed Central

Lermen, Dominik; Schmitt, Daniel; Bartel-Steinbach, Martina; Schröter-Kermani, Christa; Kolossa-Gehring, Marike; von Briesen, Hagen; Zimmermann, Heiko

2014-01-01

Technical progress has simplified tasks in lab diagnosis and improved quality of test results. Errors occurring during the pre-analytical phase have more negative impact on the quality of test results than errors encountered during the total analytical process. Different infrastructures of sampling sites can highly influence the quality of samples and therewith of analytical results. Annually the German Environmental Specimen Bank (ESB) collects, characterizes, and stores blood, plasma, and urine samples of 120–150 volunteers each on four different sampling sites in Germany. Overarching goal is to investigate the exposure to environmental pollutants of non-occupational exposed young adults combining human biomonitoring with questionnaire data. We investigated the requirements of the study and the possibility to realize a highly standardized sampling procedure on a mobile platform in order to increase the required quality of the pre-analytical phase. The results lead to the development of a mobile epidemiologic laboratory (epiLab) in the project “Labor der Zukunft” (future’s lab technology). This laboratory includes a 14.7 m2 reception area to record medical history and exposure-relevant behavior, a 21.1 m2 examination room to record dental fillings and for blood withdrawal, a 15.5 m2 biological safety level 2 laboratory to process and analyze samples on site including a 2.8 m2 personnel lock and a 3.6 m2 cryofacility to immediately freeze samples. Frozen samples can be transferred to their final destination within the vehicle without breaking the cold chain. To our knowledge, we herewith describe for the first time the implementation of a biological safety laboratory (BSL) 2 lab and an epidemiologic unit on a single mobile platform. Since 2013 we have been collecting up to 15.000 individual human samples annually under highly standardized conditions using the mobile laboratory. Characterized and free of alterations they are kept ready for retrospective analyses in their final archive, the German ESB. PMID:25141120

A new approach to standardize multicenter studies: mobile lab technology for the German Environmental Specimen Bank.

PubMed

Lermen, Dominik; Schmitt, Daniel; Bartel-Steinbach, Martina; Schröter-Kermani, Christa; Kolossa-Gehring, Marike; von Briesen, Hagen; Zimmermann, Heiko

2014-01-01

Technical progress has simplified tasks in lab diagnosis and improved quality of test results. Errors occurring during the pre-analytical phase have more negative impact on the quality of test results than errors encountered during the total analytical process. Different infrastructures of sampling sites can highly influence the quality of samples and therewith of analytical results. Annually the German Environmental Specimen Bank (ESB) collects, characterizes, and stores blood, plasma, and urine samples of 120-150 volunteers each on four different sampling sites in Germany. Overarching goal is to investigate the exposure to environmental pollutants of non-occupational exposed young adults combining human biomonitoring with questionnaire data. We investigated the requirements of the study and the possibility to realize a highly standardized sampling procedure on a mobile platform in order to increase the required quality of the pre-analytical phase. The results lead to the development of a mobile epidemiologic laboratory (epiLab) in the project "Labor der Zukunft" (future's lab technology). This laboratory includes a 14.7 m(2) reception area to record medical history and exposure-relevant behavior, a 21.1 m(2) examination room to record dental fillings and for blood withdrawal, a 15.5 m(2) biological safety level 2 laboratory to process and analyze samples on site including a 2.8 m(2) personnel lock and a 3.6 m2 cryofacility to immediately freeze samples. Frozen samples can be transferred to their final destination within the vehicle without breaking the cold chain. To our knowledge, we herewith describe for the first time the implementation of a biological safety laboratory (BSL) 2 lab and an epidemiologic unit on a single mobile platform. Since 2013 we have been collecting up to 15.000 individual human samples annually under highly standardized conditions using the mobile laboratory. Characterized and free of alterations they are kept ready for retrospective analyses in their final archive, the German ESB.

Determination of 18 veterinary antibiotics in environmental water using high-performance liquid chromatography-q-orbitrap combined with on-line solid-phase extraction.

PubMed

Kim, Chansik; Ryu, Hong-Duck; Chung, Eu Gene; Kim, Yongseok

2018-05-01

The use of antibiotics and their occurrence in the environment have received significant attention in recent years owing to the generation of antibiotic-resistant bacteria. Antibiotic residues in water near livestock farming areas should be monitored to establish effective strategies for reducing the use of veterinary antibiotics. However, environmental water contamination resulting from veterinary antibiotics has not been studied extensively. In this work, we developed an analytical method for the simultaneous determination of multiple classes of veterinary antibiotic residues in environmental water using on-line solid-phase extraction (SPE)-high performance liquid chromatography (HPLC)-high resolution mass spectrometry (HRMS). Eighteen popular antibiotics (eight classes) were selected as target analytes based on veterinary antibiotics sales in South Korea in 2015. The developed method was validated by calibration-curve linearities, precisions, relative recoveries, and method detection limits (MDLs)/limits of quantification (LOQs) of the selected antibiotics, and applied to the analysis of environmental water samples (groundwater, river water, and wastewater-treatment-plant effluent). All calibration curves exhibited r 2  > 0.995 with MDLs ranging from 0.2 to 11.9 ng/L. Relative recoveries were between 50 and 150% with coefficients of variation below 20% for all analytes (spiked at 500 ng/L) in groundwater and river water samples. Relative standard deviations (RSDs) of standard-spiked samples were lower than 7% for all antibiotics. The on-line SPE system eliminates human-based SPE errors and affords excellent method reproducibility. Amoxicillin, ampicillin, clopidol, fenbendazole, flumequine, lincomycin, sulfadiazine, and trimethoprim were detected in environmental water samples in concentrations ranging from 1.26 to 127.49 ng/L. The developed method is a reliable analytical technique for the potential routine monitoring of veterinary antibiotics. Copyright © 2018 Elsevier B.V. All rights reserved.

EPA Region 6 Laboratory Method Specific Analytical Capabilities with Sample Concentration Range

EPA Pesticide Factsheets

EPA Region 6 Environmental Services Branch (ESB) Laboratory is capable of analyzing a wide range of samples with concentrations ranging for low part-per trillion (ppt) to low percent () levels, depending on the sample matrix.

Evaluation of nutrient quality-assurance data for Alexanders and Mount Rock Spring basins, Cumberland County, Pennsylvania

USGS Publications Warehouse

Witt, E. C.; Hippe, D.J.; Giovannitti, R.M.

1992-01-01

A total of 304 nutrient samples were collected from May 1990 through September 1991 to determine concentrations and loads of nutrients in water discharged from two spring basins in Cumberland County, Pa. Fifty-four percent of these nutrient samples were for the evaluation of (1) laboratory consistency, (2) container and preservative cleanliness, (3) maintenance of analyte representativeness as affected by three different preservation methods, and (4) comparison of analyte results with the "Most Probable Value" for Standard Reference Water Samples. Results of 37 duplicate analyses indicate that the Pennsylvania Department of Environmental Resources, Bureau of Laboratories (principal laboratory) remained within its ±10 percent goal for all but one analyte. Results of the blank analysis show that the sampling containers did not compromise the water quality. However, mercuric-chloride-preservation blanks apparently contained measurable ammonium in four of five samples and ammonium plus organic nitrogen in two of five samples. Interlaboratory results indicate substantial differences in the determination of nitrate and ammonium plus organic nitrogen between the principal laboratory and the U.S. Geological Survey National Water-Quality Laboratory. In comparison with the U.S. Environmental Protection Agency Quality-Control Samples, the principal laboratory was sufficiently accurate in its determination of nutrient anafytes. Analysis of replicate samples indicated that sulfuric-acid preservative best maintained the representativeness of the anafytes nitrate and ammonium plus organic nitrogen, whereas, mercuric chloride best maintained the representativeness of orthophosphate. Comparison of nutrient analyte determinations with the Most Probable Value for each preservation method shows that two of five analytes with no chemical preservative compare well, three of five with mercuric-chloride preservative compare well, and three of five with sulfuricacid preservative compare well.

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

PubMed

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in biological or environmental samples. Due to low consumption of eluent (usually 0.3-1mL/run) mainly composed of water-alcohol binary mixtures, this method can be considered as environmentally friendly and green chemistry focused analytical tool, supplementary to analytical protocols involving column chromatography or planar micro-fluidic devices. Copyright © 2011 Elsevier Ltd. All rights reserved.

Analytical methodologies for aluminium speciation in environmental and biological samples--a review.

PubMed

Bi, S P; Yang, X D; Zhang, F P; Wang, X L; Zou, G W

2001-08-01

It is recognized that aluminium (Al) is a potential environmental hazard. Acidic deposition has been linked to increased Al concentrations in natural waters. Elevated levels of Al might have serious consequences for biological communities. Of particular interest is the speciation of Al in aquatic environments, because Al toxicity depends on its forms and concentrations. In this paper, advances in analytical methodologies for Al speciation in environmental and biological samples during the past five years are reviewed. Concerns about the specific problems of Al speciation and highlights of some important methods are elucidated in sections devoted to hybrid techniques (HPLC or FPLC coupled with ET-AAS, ICP-AES, or ICP-MS), flow-injection analysis (FIA), nuclear magnetic resonance (27Al NMR), electrochemical analysis, and computer simulation. More than 130 references are cited.

Detecting a wide range of environmental contaminants in human blood samples--combining QuEChERS with LC-MS and GC-MS methods.

PubMed

Plassmann, Merle M; Schmidt, Magdalena; Brack, Werner; Krauss, Martin

2015-09-01

Exposure to environmental pollution and consumer products may result in an uptake of chemicals into human tissues. Several studies have reported the presence of diverse environmental contaminants in human blood samples. However, previously developed multi-target methods for the analysis of human blood include a fairly limited amount of compounds stemming from one or two related compound groups. Thus, the sample preparation method QuEChERS (quick easy cheap effective rugged and safe) was tested for the extraction of 64 analytes covering a broad compound domain followed by detection using liquid and gas chromatography coupled to mass spectrometry (LC- and GC-MS). Forty-seven analytes showed absolute recoveries above 70% in the first QuEChERS step, being a simple liquid-liquid extraction (LLE) using acetonitrile and salt. The second QuEChERS step, being a dispersive solid phase extraction, did not result in an overall improvement of recoveries or removal of background signals. Using solely the LLE step, eight analytes could subsequently be detected in human blood samples from the German Environmental Specimen Bank. Using a LC-multiple reaction monitoring (MRM) method with a triple quadrupole instrument, better recoveries were achieved than with an older LC-high-resolution (HR) MS full scan orbitrap instrument, which required a higher concentration factor of the extracts. However, the application of HRMS full scan methods could be used for the detection of additional compounds retrospectively.

Analytical evaluation of BEA zeolite for the pre-concentration of polycyclic aromatic hydrocarbons and their subsequent chromatographic analysis in water samples.

PubMed

Wilson, Walter B; Costa, Andréia A; Wang, Huiyong; Dias, José A; Dias, Sílvia C L; Campiglia, Andres D

2012-07-06

The analytical performance of BEA - a commercial zeolite - is evaluated for the pre-concentration of fifteen Environmental Protection Agency - polycyclic aromatic hydrocarbons and their subsequent HPLC analysis in tap and lake water samples. The pre-concentration factors obtained with BEA have led to a method with excellent analytical figures of merit. One milliliter aliquots were sufficient to obtain excellent precision of measurements at the parts-per-trillion concentration level with relative standard deviations varying from 4.1% (dibenzo[a,h]anthracene) to 13.4% (pyrene). The limits of detection were excellent as well and varied between 1.1 (anthracene) and 49.9 ng L(-1) (indeno[1,2,3-cd]pyrene). The recovery values of all the studied compounds meet the criterion for regulated polycyclic aromatic hydrocarbons, which mandates relative standard deviations equal or lower than 25%. The small volume of organic solvents (100 μL per sample) and amount of BEA (2 mg per sample) makes sample pre-concentration environmentally friendly and cost effective. The extraction procedure is well suited for numerous samples as the small working volume (1 mL) facilitates the implementation of simultaneous sample extraction. These are attractive features when routine monitoring of numerous samples is contemplated. Copyright © 2012 Elsevier B.V. All rights reserved.

Three-phase double-arc plasma for spectrochemical analysis of environmental samples.

PubMed

Mohamed, M M; Ghatass, Z F; Shalaby, E A; Kotb, M M; El-Raey, M

2000-12-01

A new instrument, which uses a three-phase current to support a double-arc argon plasma torch for evaporation, atomization and excitation of solid or powder samples, is described. The sampling arc is ignited between the first and second electrode while the excitation arc is ignited between the second and third electrode. Aerosol generated from the sample (first electrode) is swept by argon gas, through a hole in the second electrode (carbon tubing electrode), into the excitation plasma. A tangential stream of argon gas is introduced through an inlet orifice as a coolant gas for the second electrode. This gas stream forces the excitation arc discharge to rotate reproducibly around the electrode surface. Discharge rotation increases the stability of the excitation plasma. Spectroscopic measurements are made directly in the current-carrying region of the excitation arc. An evaluation of each parameter influencing the device performance was performed. Analytical calibration curves were obtained for Fe, Al, K, and Pb. Finally, the present technique was applied for the analysis of environmental samples. The present method appears to have significant, low cost analytical utility for environmental measurements.

Spectral multivariate calibration without laboratory prepared or determined reference analyte values.

PubMed

Ottaway, Josh; Farrell, Jeremy A; Kalivas, John H

2013-02-05

An essential part to calibration is establishing the analyte calibration reference samples. These samples must characterize the sample matrix and measurement conditions (chemical, physical, instrumental, and environmental) of any sample to be predicted. Calibration usually requires measuring spectra for numerous reference samples in addition to determining the corresponding analyte reference values. Both tasks are typically time-consuming and costly. This paper reports on a method named pure component Tikhonov regularization (PCTR) that does not require laboratory prepared or determined reference values. Instead, an analyte pure component spectrum is used in conjunction with nonanalyte spectra for calibration. Nonanalyte spectra can be from different sources including pure component interference samples, blanks, and constant analyte samples. The approach is also applicable to calibration maintenance when the analyte pure component spectrum is measured in one set of conditions and nonanalyte spectra are measured in new conditions. The PCTR method balances the trade-offs between calibration model shrinkage and the degree of orthogonality to the nonanalyte content (model direction) in order to obtain accurate predictions. Using visible and near-infrared (NIR) spectral data sets, the PCTR results are comparable to those obtained using ridge regression (RR) with reference calibration sets. The flexibility of PCTR also allows including reference samples if such samples are available.

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... requirements. 141.22 Section 141.22 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Monitoring and Analytical Requirements... suppliers of water for both community and non-community water systems at a representative entry point(s) to...

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... requirements. 141.22 Section 141.22 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Monitoring and Analytical Requirements... suppliers of water for both community and non-community water systems at a representative entry point(s) to...

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... requirements. 141.22 Section 141.22 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Monitoring and Analytical Requirements... suppliers of water for both community and non-community water systems at a representative entry point(s) to...

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... requirements. 141.22 Section 141.22 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Monitoring and Analytical Requirements... suppliers of water for both community and non-community water systems at a representative entry point(s) to...

40 CFR 141.22 - Turbidity sampling and analytical requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... requirements. 141.22 Section 141.22 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Monitoring and Analytical Requirements... suppliers of water for both community and non-community water systems at a representative entry point(s) to...

Environmental Sampling & Analytical Methods (ESAM) Program - Home

EPA Pesticide Factsheets

ESAM is a comprehensive program to facilitate a coordinated response to a chemical, radiochemical, biotoxin or pathogen contamination incident focusing on sample collection, processing, and analysis to provide quality results to the field.

Lessons Learned for the Assessment of Children’s Pesticide Exposure: Critical Sampling and Analytical Issues for Future Studies

PubMed Central

Fenske, Richard A.; Bradman, Asa; Whyatt, Robin M.; Wolff, Mary S.; Barr, Dana B.

2005-01-01

In this article we examine sampling strategies and analytical methods used in a series of recent studies of children’s exposure to pesticides that may prove useful in the design and implementation of the National Children’s Study. We focus primarily on the experiences of four of the National Institute of Environmental Health Sciences/U.S. Environmental Protection Agency/ Children’s Centers and include University of Washington studies that predated these centers. These studies have measured maternal exposures, perinatal exposures, infant and toddler exposures, and exposure among young children through biologic monitoring, personal sampling, and environmental monitoring. Biologic monitoring appears to be the best available method for assessment of children’s exposure to pesticides, with some limitations. It is likely that a combination of biomarkers, environmental measurements, and questionnaires will be needed after careful consideration of the specific hypotheses posed by investigators and the limitations of each exposure metric. The value of environmental measurements, such as surface and toy wipes and indoor air or house dust samples, deserves further investigation. Emphasis on personal rather than environmental sampling in conjunction with urine or blood sampling is likely to be most effective at classifying exposure. For infants and young children, ease of urine collection (possible for extended periods of time) may make these samples the best available approach to capturing exposure variability of nonpersistent pesticides; additional validation studies are needed. Saliva measurements of pesticides, if feasible, would overcome the limitations of urinary metabolite-based exposure analysis. Global positioning system technology appears promising in the delineation of children’s time–location patterns. PMID:16203262

Quality-assurance results for routine water analyses in U.S. Geological Survey laboratories, water year 1998

USGS Publications Warehouse

Ludtke, Amy S.; Woodworth, Mark T.; Marsh, Philip S.

2000-01-01

The U.S. Geological Survey operates a quality-assurance program based on the analyses of reference samples for two laboratories: the National Water Quality Laboratory and the Quality of Water Service Unit. Reference samples that contain selected inorganic, nutrient, and low-level constituents are prepared and submitted to the laboratory as disguised routine samples. The program goal is to estimate precision and bias for as many analytical methods offered by the participating laboratories as possible. Blind reference samples typically are submitted at a rate of 2 to 5 percent of the annual environmental-sample load for each constituent. The samples are distributed to the laboratories throughout the year. The reference samples are subject to the identical laboratory handling, processing, and analytical procedures as those applied to environmental samples and, therefore, have been used as an independent source to verify bias and precision of laboratory analytical methods and ambient water-quality measurements. The results are stored permanently in the National Water Information System and the Blind Sample Project's data base. During water year 1998, 95 analytical procedures were evaluated at the National Water Quality Laboratory and 63 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic and low-level constituent data for water year 1998 indicated 77 of 78 analytical procedures at the National Water Quality Laboratory met the criteria for precision. Silver (dissolved, inductively coupled plasma-mass spectrometry) was determined to be imprecise. Five of 78 analytical procedures showed bias throughout the range of reference samples: chromium (dissolved, inductively coupled plasma-atomic emission spectrometry), dissolved solids (dissolved, gravimetric), lithium (dissolved, inductively coupled plasma-atomic emission spectrometry), silver (dissolved, inductively coupled plasma-mass spectrometry), and zinc (dissolved, inductively coupled plasma-mass spectrometry). At the National Water Quality Laboratory during water year 1998, lack of precision was indicated for 2 of 17 nutrient procedures: ammonia as nitrogen (dissolved, colorimetric) and orthophosphate as phosphorus (dissolved, colorimetric). Bias was indicated throughout the reference sample range for ammonia as nitrogen (dissolved, colorimetric, low level) and nitrate plus nitrite as nitrogen (dissolved, colorimetric, low level). All analytical procedures tested at the Quality of Water Service Unit during water year 1998 met the criteria for precision. One of the 63 analytical procedures indicated a bias throughout the range of reference samples: aluminum (whole-water recoverable, inductively coupled plasma-atomic emission spectrometry, trace).

Validation of a liquid chromatography-tandem mass spectrometry method for the detection of nicotine biomarkers in hair and an evaluation of wash procedures for removal of environmental nicotine.

PubMed

Miller, Eleanor I; Murray, Gordon J; Rollins, Douglas E; Tiffany, Stephen T; Wilkins, Diana G

2011-07-01

The aim of this exploratory study was to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for the quantification of nicotine, eight nicotine metabolites, and two minor tobacco alkaloids in fortified analyte-free hair and subsequently apply this method to hair samples collected from active smokers. An additional aim of the study was to include an evaluation of different wash procedures for the effective removal of environmentally deposited nicotine from tobacco smoke. An apparatus was designed for the purpose of exposing analyte-free hair to environmental tobacco smoke in order to deposit nicotine onto the hair surface. A shampoo/water wash procedure was identified as the most effective means of removing nicotine. This wash procedure was utilized for a comparison of washed and unwashed heavy smoker hair samples. Analytes and corresponding deuterated internal standards were extracted using a cation-exchange solid-phase cartridge. LC-MS-MS was carried out using an Acquity™ UPLC(®) system (Waters) and a Quattro Premier XE™ triple quadrupole MS (Waters) operated in electrospray positive ionization mode, with multiple reaction monitoring data acquisition. The developed method was applied to hair samples collected from heavy smokers (n = 3) and low-level smokers (n = 3) collected through IRB-approved protocols. Nicotine, cotinine, and nornicotine were quantified in both the washed and unwashed hair samples collected from three heavy smokers, whereas 3-hydroxycotinine was quantified in only one unwashed sample and nicotine-1'-oxide in the washed and unwashed hair samples from two heavy smokers. In contrast, nicotine-1'-oxide was quantified in one of the three low-level smoker samples; nicotine was quantified in the other two low-level smoker samples. No other analytes were detected in the hair of the three low-level smokers.

40 CFR 86.537-90 - Dynamometer test runs.

Code of Federal Regulations, 2014 CFR

2014-07-01

... “transient” formaldehyde exhaust sample, the “transient” dilution air sample bag, the “transient” methanol... start “transient” exhaust and dilution air bag samples to the analytical system and process the samples... Section 86.537-90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS...

40 CFR 86.537-90 - Dynamometer test runs.

Code of Federal Regulations, 2012 CFR

2012-07-01

... “transient” formaldehyde exhaust sample, the “transient” dilution air sample bag, the “transient” methanol... start “transient” exhaust and dilution air bag samples to the analytical system and process the samples... Section 86.537-90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS...

40 CFR 86.537-90 - Dynamometer test runs.

Code of Federal Regulations, 2013 CFR

2013-07-01

... “transient” formaldehyde exhaust sample, the “transient” dilution air sample bag, the “transient” methanol... start “transient” exhaust and dilution air bag samples to the analytical system and process the samples... Section 86.537-90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS...

Bee pollen as a bioindicator of environmental pesticide contamination.

PubMed

de Oliveira, Renata Cabrera; Queiroz, Sonia Claudia do Nascimento; da Luz, Cynthia Fernandes Pinto; Porto, Rafael Silveira; Rath, Susanne

2016-11-01

Honeybees and bee products are potential bioindicators of the presence of contaminants in the environment, enabling monitoring of large areas due to the long distances travelled by bees. This work evaluates the use of bee pollen as a bioindicator of environmental contamination by pesticides. A GC-MS/MS analytical method for multiresidue determination of 26 different pesticides in pollen was developed and validated in accordance with the recommendations of the European Union SANCO guide. Environmental monitoring was conducted using the analysis of 145 pollen samples collected from ten beehives in the experimental apiary of Embrapa in Jaguariúna (São Paulo State, Brazil). Bioallethrin and pendimethalin were identified in four and eighteen samples, respectively, at concentrations below the LOQ of the method (25 ng g(-1)). Passive sampling with polyurethane foam discs was used as a control, and no pesticides were found. The detection of pesticide residues in seven samples (33%) from commercial apiaries in Ribeirão Preto (São Paulo State) confirmed the efficiency of the analytical method and the need for environmental monitoring for the presence of pesticide residues. The results demonstrated the potential of bee pollen as a bioindicator of environmental contamination by pesticides. Copyright © 2016 Elsevier Ltd. All rights reserved.

ENVIRONMENTAL EVALUATION FOR UTILIZATION OF ASH IN SOIL STABILIZATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

David J. Hassett; Loreal V. Heebink

2001-08-01

The Minnesota Pollution Control Agency (MPCA) approved the use of coal ash in soil stabilization, indicating that environmental data needed to be generated. The overall project goal is to evaluate the potential for release of constituents into the environment from ash used in soil stabilization projects. Supporting objectives are: (1) To ensure sample integrity through implementation of a sample collection, preservation, and storage protocol to avoid analyte concentration or loss. (2) To evaluate the potential of each component (ash, soil, water) of the stabilized soil to contribute to environmental release of analytes of interest. (3) To use laboratory leaching methodsmore » to evaluate the potential for release of constituents to the environment. (4) To facilitate collection of and to evaluate samples from a field runoff demonstration effort. The results of this study indicated limited mobility of the coal combustion fly ash constituents in laboratory tests and the field runoff samples. The results presented support previous work showing little to negligible impact on water quality. This and past work indicates that soil stabilization is an environmentally beneficial CCB utilization application as encouraged by the U.S. Environmental Protection Agency. This project addressed the regulatory-driven environmental aspect of fly ash use for soil stabilization, but the demonstrated engineering performance and economic advantages also indicate that the use of CCBs in soil stabilization can and should become an accepted engineering option.« less

Improvements to sample processing and measurement to enable more widespread environmental application of tritium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moran, James; Alexander, Thomas; Aalseth, Craig

2017-08-01

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120 mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of T behavior in the environment.

Laser Induced Breakdown Spectroscopy for Elemental Analysis in Environmental, Cultural Heritage and Space Applications: A Review of Methods and Results

PubMed Central

Gaudiuso, Rosalba; Dell’Aglio, Marcella; De Pascale, Olga; Senesi, Giorgio S.; De Giacomo, Alessandro

2010-01-01

Analytical applications of Laser Induced Breakdown Spectroscopy (LIBS), namely optical emission spectroscopy of laser-induced plasmas, have been constantly growing thanks to its intrinsic conceptual simplicity and versatility. Qualitative and quantitative analysis can be performed by LIBS both by drawing calibration lines and by using calibration-free methods and some of its features, so as fast multi-elemental response, micro-destructiveness, instrumentation portability, have rendered it particularly suitable for analytical applications in the field of environmental science, space exploration and cultural heritage. This review reports and discusses LIBS achievements in these areas and results obtained for soils and aqueous samples, meteorites and terrestrial samples simulating extraterrestrial planets, and cultural heritage samples, including buildings and objects of various kinds. PMID:22163611

Laser induced breakdown spectroscopy for elemental analysis in environmental, cultural heritage and space applications: a review of methods and results.

PubMed

Gaudiuso, Rosalba; Dell'Aglio, Marcella; De Pascale, Olga; Senesi, Giorgio S; De Giacomo, Alessandro

2010-01-01

Analytical applications of Laser Induced Breakdown Spectroscopy (LIBS), namely optical emission spectroscopy of laser-induced plasmas, have been constantly growing thanks to its intrinsic conceptual simplicity and versatility. Qualitative and quantitative analysis can be performed by LIBS both by drawing calibration lines and by using calibration-free methods and some of its features, so as fast multi-elemental response, micro-destructiveness, instrumentation portability, have rendered it particularly suitable for analytical applications in the field of environmental science, space exploration and cultural heritage. This review reports and discusses LIBS achievements in these areas and results obtained for soils and aqueous samples, meteorites and terrestrial samples simulating extraterrestrial planets, and cultural heritage samples, including buildings and objects of various kinds.

Nutrient and pesticide contamination bias estimated from field blanks collected at surface-water sites in U.S. Geological Survey Water-Quality Networks, 2002–12

USGS Publications Warehouse

Medalie, Laura; Martin, Jeffrey D.

2017-08-14

Potential contamination bias was estimated for 8 nutrient analytes and 40 pesticides in stream water collected by the U.S. Geological Survey at 147 stream sites from across the United States, and representing a variety of hydrologic conditions and site types, for water years 2002–12. This study updates previous U.S. Geological Survey evaluations of potential contamination bias for nutrients and pesticides. Contamination is potentially introduced to water samples by exposure to airborne gases and particulates, from inadequate cleaning of sampling or analytic equipment, and from inadvertent sources during sample collection, field processing, shipment, and laboratory analysis. Potential contamination bias, based on frequency and magnitude of detections in field blanks, is used to determine whether or under what conditions environmental data might need to be qualified for the interpretation of results in the context of comparisons with background levels, drinking-water standards, aquatic-life criteria or benchmarks, or human-health benchmarks. Environmental samples for which contamination bias as determined in this report applies are those from historical U.S. Geological Survey water-quality networks or programs that were collected during the same time frame and according to the same protocols and that were analyzed in the same laboratory as field blanks described in this report.Results from field blanks for ammonia, nitrite, nitrite plus nitrate, orthophosphate, and total phosphorus were partitioned by analytical method; results from the most commonly used analytical method for total phosphorus were further partitioned by date. Depending on the analytical method, 3.8, 9.2, or 26.9 percent of environmental samples, the last of these percentages pertaining to all results from 2007 through 2012, were potentially affected by ammonia contamination. Nitrite contamination potentially affected up to 2.6 percent of environmental samples collected between 2002 and 2006 and affected about 3.3 percent of samples collected between 2007 and 2012. The percentages of environmental samples collected between 2002 and 2011 that were potentially affected by nitrite plus nitrate contamination were 7.3 for samples analyzed with the low-level method and 0.4 for samples analyzed with the standard-level method. These percentages increased to 14.8 and 2.2 for samples collected in 2012 and analyzed using replacement low- and standard-level methods, respectively. The maximum potentially affected concentrations for nitrite and for nitrite plus nitrate were much less than their respective maximum contamination levels for drinking-water standards. Although contamination from particulate nitrogen can potentially affect up to 21.2 percent and that from total Kjeldahl nitrogen can affect up to 16.5 percent of environmental samples, there are no critical or background levels for these substances.For total nitrogen, orthophosphate, and total phosphorus, contamination in a small percentage of environmental samples might be consequential for comparisons relative to impairment risks or background levels. At the low ends of the respective ranges of impairment risk for these nutrients, contamination in up to 5 percent of stream samples could account for at least 23 percent of measured concentrations of total nitrogen, for at least 40 or 90 percent of concentrations of orthophosphate, depending on the analytical method, and for 31 to 76 percent of concentrations of total phosphorus, depending on the time period.Twenty-six pesticides had no detections in field blanks. Atrazine with 12 and metolachlor with 11 had the highest number of detections, mostly occurring in spring or early summer. At a 99-percent level of confidence, contamination was estimated to be no greater than the detection limit in at least 98 percent of all samples for 38 of 40 pesticides. For metolachlor and atrazine, potential contamination was no greater than 0.0053 and 0.0093 micrograms per liter in 98 percent of samples. For 11 of 14 pesticides with at least one detection, the maximum potentially affected concentration of the environmental sample was less than their respective human-health or aquatic-life benchmarks. Small percentages of environmental samples had concentrations high enough that atrazine contamination potentially could account for the entire aquatic-life benchmark for acute effects on nonvascular plants, that dieldrin contamination could account for up to 100 percent of the cancer health-based screening level, or that chlorpyrifos contamination could account for 13 or 12 percent of the concentrations in the aquatic-life benchmarks for chronic effects on invertebrates or the criterion continuous concentration for chronic effects on aquatic life.

PFAS methods and guidance for sampling and analyzing water and other environmental media (Technical Brief)

EPA Pesticide Factsheets

EPA's methods for analyzing PFAS in environmental media are in various stages of development. This fact sheet summarizes EPA's analytical methods development for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids

Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

PubMed

Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

2012-03-05

Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

Results of quality-control sampling of water, bed sediment, and tissue in the Western Lake Michigan Drainages study unit of the National Water-Quality Assessment Program

USGS Publications Warehouse

Fitzgerald, S.A.

1997-01-01

This report contains the quality control results of the Western Lake Michigan Drainages study unit of the National Water Quality Assessment Program. Quality control samples were collected in the same manner and contemporaneously with environmental samples during the first highintensity study phase in the unit (1992 through 1995) and amounted to approximately 15 percent of all samples collected. The accuracy and precision of hundreds of chemical analyses of surface and ground-water, bed sediment, and tissue was determined through the collection and analysis of field blanks, field replicates and splits, matrix spikes, and surrogates. Despite the several detections of analytes in the field blanks, the concentrations of most constituents in the environmental samples will likely be an order of magnitude or higher than those in the blanks. However, frequent detections, and high concentrations, of dissolved organic carbon (DOC) in several surface and ground-water blanks are probably significant with respect to commonly measured environmental concentrations, and the environmental data will have to be qualified accordingly. The precision of sampling of water on a percent basis, as determined from replicates and splits, was generally proportional to the concentration of the constituents, with constituents present in relatively high concentrations generally having less sampling variability than those with relatively low concentrations. In general, analytes with relatively high variability between replicates were present at concentrations near the reporting limit or were associated with relatively small absolute concentration differences, or both. Precision of replicates compared to that for splits in bed sediment samples was similar, thus eliminating sampling as a major source of variability in analyte concentrations. In the case the phthalates in bed sediment, contamination in either the field or laboratory could have caused the relatively large variability between replicate samples and between split samples.Variability of analyte concentrations in tissue samples was relatively low, being 29 percent or less for all constituents. Recoveries of most laboratory schedule 2001/2010 pesticide spike compounds in surfacewater samples were reasonably good. Low intrinsic method recovery resulted in relatively low recovery forp,p'-DDE, metribuzin, and propargite. In the case of propargite, decomposition with the environmental sample matrices was also indicated. Recoveries of two compounds, cyanazine and thiobencarb, might have been biased high due to interferences. The one laboratory schedule 2050/2051 field matrix pesticide spike indicated numerous operational problems with this method that biased recoveries either low or high. Recoveries of pesticides from both pesticide schedules in field spikes of ground-water samples generally were similar to those of field matrix spikes of surface- water samples. High maximum recoveries were noted for tebuthiuron, disulfoton, DCPA, and permethrin, which indicates the possible presence of interferents in the matrices for these compounds. Problems in the recoveries of pesticides on schedule 2050/2051 from ground-water samples generally were the same as those for surfacewater samples. Recoveries of VOCs in field matrix spikes were reasonable when consideration was given for the use of the micropipettor that delivered only about 80 percent on average of the nominal mass of spiked analytes. Finally, the recoveries of most surrogate compounds in surface and ground-water samples were reasonable. Problems in sample handling (for example, spillage) were likely not the cause of any of the low recoveries of spiked compounds.

Optimization of Analytical Conditions for a Rapid Determination of Aniline in Environmental Water by Liquid Chromatography/Tandem Mass Spectrometry.

PubMed

Furukawa, Koji; Hashimoto, Makoto; Kaneco, Satoshi

2017-01-01

A rapid determination of aniline in environmental water was examined based on liquid chromatography/tandem mass spectrometry (LC/MS/MS). Environmental water samples were diluted 20-fold with Mill-Q water and measured by LC/MS/MS after adding a surrogate substance (aniline-d 5 ). In the results of the present study, the calibration curve of aniline showed good linearity in the range of 0.05 - 2.0 μg/L. Since the RSD (repeatability) by measuring repeatedly an aniline standard solution (0.05 μg/L, n = 7) was 3.2%, the repeatability of this work was very excellent. In addition, the recovery rate of aniline in environmental water was in the range of 99.0 - 102% with RSD 3.4 - 7.7%, and very good recovery test results were obtained. From these results, this analytical method was confirmed to be effective for aniline measurements of environmental water samples. Also, it is possible to conduct rapid analyses of aniline in environmental water without any solid-phase extraction process, compared to the solid-phase extraction-GC/MS method.

Simultaneous quantitative determination of benzene, toluene, and xylenes in water using mid-infrared evanescent field spectroscopy.

PubMed

Karlowatz, M; Kraft, M; Mizaikoff, B

2004-05-01

Attenuated total reflection mid-infrared spectroscopy is applied for simultaneous detection and quantification of the environmentally relevant analytes benzene, toluene, and the three xylene isomers. The analytes are enriched into a thin polymer membrane coated onto the surface of an internal reflection waveguide, which is exposed to the aqueous sample. Direct detection of analytes permeating into the polymer coating is performed by utilizing evanescent field spectroscopy in the fingerprint range (>10 microm) of the mid-infrared (MIR) spectrum (3-20 microm) without additional sample preparation. All investigated compounds are characterized by well-separated absorption features in the evaluated wavelength regime. Hence, data evaluation was performed by integration of the respective absorption peaks. Limits of detection lower than 20 ppb (v/v) for all xylene isomers, 45 ppb (v/v) for benzene, and 80 ppb (v/v) for toluene have been achieved. The straightforward experimental setup and the achieved detection limits for these environmentally relevant volatile organic compounds in the low-ppb concentration range reveal a substantial potential of MIR evanescent field sensing devices for on-line in situ environmental analysis.

Sample Collection Information Document for Pathogens and Biotoxins − Companion to Standardized Analytical Methods for Environmental Restoration Following Homeland Security Events (SAM) Revision 5.0

EPA Pesticide Factsheets

Sample Collection Information Document is intended to provide sampling information to be used during site assessment, remediation and clearance activities following a biological or biotoxin contamination incident.

A Demonstration of Sample Segregation

ERIC Educational Resources Information Center

Fritz, Mark D.; Brumbach, Stephen B.; Hartman, JudithAnn R.

2005-01-01

The demonstration of sample segregation, which is simple, and visually compelling illustrates the importance of sample handling for students studying analytical chemistry and environmental chemistry. The mixture used in this demonstration has two components, which have big particle size, and different colors, which makes the segregation graphic.

Adjustment of Pesticide Concentrations for Temporal Changes in Analytical Recovery, 1992-2006

USGS Publications Warehouse

Martin, Jeffrey D.; Stone, Wesley W.; Wydoski, Duane S.; Sandstrom, Mark W.

2009-01-01

Recovery is the proportion of a target analyte that is quantified by an analytical method and is a primary indicator of the analytical bias of a measurement. Recovery is measured by analysis of quality-control (QC) water samples that have known amounts of target analytes added ('spiked' QC samples). For pesticides, recovery is the measured amount of pesticide in the spiked QC sample expressed as percentage of the amount spiked, ideally 100 percent. Temporal changes in recovery have the potential to adversely affect time-trend analysis of pesticide concentrations by introducing trends in environmental concentrations that are caused by trends in performance of the analytical method rather than by trends in pesticide use or other environmental conditions. This report examines temporal changes in the recovery of 44 pesticides and 8 pesticide degradates (hereafter referred to as 'pesticides') that were selected for a national analysis of time trends in pesticide concentrations in streams. Water samples were analyzed for these pesticides from 1992 to 2006 by gas chromatography/mass spectrometry. Recovery was measured by analysis of pesticide-spiked QC water samples. Temporal changes in pesticide recovery were investigated by calculating robust, locally weighted scatterplot smooths (lowess smooths) for the time series of pesticide recoveries in 5,132 laboratory reagent spikes; 1,234 stream-water matrix spikes; and 863 groundwater matrix spikes. A 10-percent smoothing window was selected to show broad, 6- to 12-month time scale changes in recovery for most of the 52 pesticides. Temporal patterns in recovery were similar (in phase) for laboratory reagent spikes and for matrix spikes for most pesticides. In-phase temporal changes among spike types support the hypothesis that temporal change in method performance is the primary cause of temporal change in recovery. Although temporal patterns of recovery were in phase for most pesticides, recovery in matrix spikes was greater than recovery in reagent spikes for nearly every pesticide. Models of recovery based on matrix spikes are deemed more appropriate for adjusting concentrations of pesticides measured in groundwater and stream-water samples than models based on laboratory reagent spikes because (1) matrix spikes are expected to more closely match the matrix of environmental water samples than are reagent spikes and (2) method performance is often matrix dependent, as was shown by higher recovery in matrix spikes for most of the pesticides. Models of recovery, based on lowess smooths of matrix spikes, were developed separately for groundwater and stream-water samples. The models of recovery can be used to adjust concentrations of pesticides measured in groundwater or stream-water samples to 100 percent recovery to compensate for temporal changes in the performance (bias) of the analytical method.

DETERMINATION OF CHLOROETHENES IN ENVIRONMENTAL BIOLOGICAL SAMPLES USING GAS CHROMATOGRAPHY COUPLED WITH SOLID PHASE MICRO EXTRACTION

EPA Science Inventory

An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase mi...

The Savannah River Site's Groundwater Monitoring Program, third quarter 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site's (SRS) Groundwater Monitoring Program. During third quarter 1991, EPD/EMS conducted extensive sampling of monitoring wells. Analytical results from third quarter 1991 are listed in this report.

Analytical techniques for steroid estrogens in water samples - A review.

PubMed

Fang, Ting Yien; Praveena, Sarva Mangala; deBurbure, Claire; Aris, Ahmad Zaharin; Ismail, Sharifah Norkhadijah Syed; Rasdi, Irniza

2016-12-01

In recent years, environmental concerns over ultra-trace levels of steroid estrogens concentrations in water samples have increased because of their adverse effects on human and animal life. Special attention to the analytical techniques used to quantify steroid estrogens in water samples is therefore increasingly important. The objective of this review was to present an overview of both instrumental and non-instrumental analytical techniques available for the determination of steroid estrogens in water samples, evidencing their respective potential advantages and limitations using the Need, Approach, Benefit, and Competition (NABC) approach. The analytical techniques highlighted in this review were instrumental and non-instrumental analytical techniques namely gas chromatography mass spectrometry (GC-MS), liquid chromatography mass spectrometry (LC-MS), enzyme-linked immuno sorbent assay (ELISA), radio immuno assay (RIA), yeast estrogen screen (YES) assay, and human breast cancer cell line proliferation (E-screen) assay. The complexity of water samples and their low estrogenic concentrations necessitates the use of highly sensitive instrumental analytical techniques (GC-MS and LC-MS) and non-instrumental analytical techniques (ELISA, RIA, YES assay and E-screen assay) to quantify steroid estrogens. Both instrumental and non-instrumental analytical techniques have their own advantages and limitations. However, the non-instrumental ELISA analytical techniques, thanks to its lower detection limit and simplicity, its rapidity and cost-effectiveness, currently appears to be the most reliable for determining steroid estrogens in water samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analytical and environmental aspects of the flame retardant tetrabromobisphenol-A and its derivatives.

PubMed

Covaci, Adrian; Voorspoels, Stefan; Abdallah, Mohamed Abou-Elwafa; Geens, Tinne; Harrad, Stuart; Law, Robin J

2009-01-16

The present article reviews the available literature on the analytical and environmental aspects of tetrabromobisphenol-A (TBBP-A), a currently intensively used brominated flame retardant (BFR). Analytical methods, including sample preparation, chromatographic separation, detection techniques, and quality control are discussed. An important recent development in the analysis of TBBP-A is the growing tendency for liquid chromatographic techniques. At the detection stage, mass-spectrometry is a well-established and reliable technology in the identification and quantification of TBBP-A. Although interlaboratory exercises for BFRs have grown in popularity in the last 10 years, only a few participating laboratories report concentrations for TBBP-A. Environmental levels of TBBP-A in abiotic and biotic matrices are low, probably due to the major use of TBBP-A as reactive FR. As a consequence, the expected human exposure is low. This is in agreement with the EU risk assessment that concluded that there is no risk for humans concerning TBBP-A exposure. Much less analytical and environmental information exists for the various groups of TBBP-A derivatives which are largely used as additive flame retardants.

Silicone rod extraction followed by liquid desorption-large volume injection-programmable temperature vaporiser-gas chromatography-mass spectrometry for trace analysis of priority organic pollutants in environmental water samples.

PubMed

Delgado, Alejandra; Posada-Ureta, Oscar; Olivares, Maitane; Vallejo, Asier; Etxebarria, Nestor

2013-12-15

In this study a priority organic pollutants usually found in environmental water samples were considered to accomplish two extraction and analysis approaches. Among those compounds organochlorine compounds, pesticides, phthalates, phenols and residues of pharmaceutical and personal care products were included. The extraction and analysis steps were based on silicone rod extraction (SR) followed by liquid desorption in combination with large volume injection-programmable temperature vaporiser (LVI-PTV) and gas chromatography-mass spectrometry (GC-MS). Variables affecting the analytical response as a function of the programmable temperature vaporiser (PTV) parameters were firstly optimised following an experimental design approach. The SR extraction and desorption conditions were assessed afterwards, including matrix modification, time extraction, and stripping solvent composition. Subsequently, the possibility of performing membrane enclosed sorptive coating extraction (MESCO) as a modified extraction approach was also evaluated. The optimised method showed low method detection limits (3-35 ng L(-1)), acceptable accuracy (78-114%) and precision values (<13%) for most of the studied analytes regardless of the aqueous matrix. Finally, the developed approach was successfully applied to the determination of target analytes in aqueous environmental matrices including estuarine and wastewater samples. © 2013 Elsevier B.V. All rights reserved.

Analytical results from an environmental investigation of six sites on Kirtland Air Force Base, New Mexico, 1993-94

USGS Publications Warehouse

Wilcox, Ralph

1995-01-01

The six sites investigated include silver recovery units; a buried caustic drain line; a neutralization pit; an evaporation/infiltration pond; the Manzano fire training area; and a waste oil underground storage tank. Environmental samples of soil, pond sediment, soil gas, and water and gas in floor drains were collected and analyzed. Field quality-control samples were also collected and analyzed in association with the environmental samples. The six sites were investigated because past or current activities could have resulted in contamination of soil, pond sediment, or water and sediment in drains.

STANDARD OPERATING PROCEDURE FOR QUALITY ASSURANCE IN ANALYTICAL CHEMISTRY METHODS DEVELOPMENT

EPA Science Inventory

The Environmental Protection Agency's (EPA) Office of Research and Development (ORD) is engaged in the development, demonstration, and validation of new or newly adapted methods of analysis for environmentally related samples. Recognizing that a "one size fits all" approach to qu...

The Savannah River Site`s Groundwater Monitoring Program, third quarter 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site`s (SRS) Groundwater Monitoring Program. During third quarter 1991, EPD/EMS conducted extensive sampling of monitoring wells. Analytical results from third quarter 1991 are listed in this report.

Validation of Rapid Radiochemical Method for Californium ...

EPA Pesticide Factsheets

Technical Brief In the event of a radiological/nuclear contamination event, the response community would need tools and methodologies to rapidly assess the nature and the extent of contamination. To characterize a radiologically contaminated outdoor area and to inform risk assessment, large numbers of environmental samples would be collected and analyzed over a short period of time. To address the challenge of quickly providing analytical results to the field, the U.S. EPA developed a robust analytical method. This method allows response officials to characterize contaminated areas and to assess the effectiveness of remediation efforts, both rapidly and accurately, in the intermediate and late phases of environmental cleanup. Improvement in sample processing and analysis leads to increased laboratory capacity to handle the analysis of a large number of samples following the intentional or unintentional release of a radiological/nuclear contaminant.

Literature Review on Processing and Analytical Methods for ...

EPA Pesticide Factsheets

Report The purpose of this report was to survey the open literature to determine the current state of the science regarding the processing and analytical methods currently available for recovery of F. tularensis from water and soil matrices, and to determine what gaps remain in the collective knowledge concerning F. tularensis identification from environmental samples.

40 CFR Appendix B to Part 136 - Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11

Code of Federal Regulations, 2012 CFR

2012-07-01

... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES... to a wide variety of sample types ranging from reagent (blank) water containing analyte to wastewater... times the standard deviation of replicate instrumental measurements of the analyte in reagent water. (c...

Metal-organic framework MIL-101 as sorbent based on double-pumps controlled on-line solid-phase extraction coupled with high-performance liquid chromatography for the determination of flavonoids in environmental water samples.

PubMed

Liu, Yue; Hu, Jia; Li, Yan; Li, Xiao-Shuang; Wang, Zhong-Liang

2016-10-01

A novel method with high sensitivity for the rapid determination of chrysin, apigenin and luteolin in environment water samples was developed by double-pumps controlled on-line solid-phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC). In the developed technique, metal organic framework MIL-101 was synthesized and applied as a sorbent for SPE. The as-synthesized MIL-101 was characterized by scanning electron microscope, X-ray diffraction spectrometry, thermal gravimetric analysis and micropore physisorption analysis. The MIL-101 behaved as a fast kinetics in the adsorption of chrysin, apigenin and luteolin. On-line SPE of chrysin, apigenin and luteolin was processed by loading a sample solution at a flow rate of 1.0 mL/min for 10 min. The extracted analytes were subsequently eluted into a ZORBAX Bonus-RP analytical column (25 cm long × 4.6 mm i.d.) for HPLC separation under isocratic condition with a mobile phase (MeOH: ACN: 0.02 M H 3 PO 4 = 35:35:30) at a flow rate of 1.0 mL/min. Experimental conditions, including ionic strength, sample pH, sample loading rates, sample loading time and desorption analytes time, were further optimized to obtain efficient preconcentration and high-precision determination of the analytes mentioned above. The method achieved the merits of simplicity, rapidity, sensitivity, wide linear range and high sample throughput. The possible mechanism for the adsorption of flavonoids on MIL-101 was proposed. The developed method has been applied to determine trace chrysin, apigenin and luteolin in a variety of environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

DETERMINATION OF PYRETHROID PESTICIDES IN COMPOSITE DIETARY SAMPLES

EPA Science Inventory

The U.S. Environmental Protection Agency's National Exposure Research Laboratory (NERL) conducts aggregate exposure studies for determining an individual's exposure to a broad range of target analytes in composite dietary samples. The objective of this work is to develop an anal...

40 CFR 86.160-00 - Exhaust emission test procedure for SC03 emissions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... simulates testing in an environmental test cell (see § 86.162-00 (a) for a discussion of simulation... exhaust and dilution air bag samples to the analytical system and process the samples according to § 86...

ERLN Technical Support for Labs

EPA Pesticide Factsheets

The Environmental Response Laboratory Network provides policies and guidance on lab and data requirements, Standardized Analytical Methods, and technical support for water and radiological sampling and analysis

Rapid sample preparation and fast GC-MS/MS for the analysis of pesticides and environmental contaminants in fish

USDA-ARS?s Scientific Manuscript database

A rapid high-throughput analytical method for the simultaneous determination of pesticides and environmental contaminants, including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs) and flame retardants (FRs) in fish was developed and ...

Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

PubMed

Popov, L

2016-09-01

Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microplastics in the environment: Challenges in analytical chemistry - A review.

PubMed

Silva, Ana B; Bastos, Ana S; Justino, Celine I L; da Costa, João P; Duarte, Armando C; Rocha-Santos, Teresa A P

2018-08-09

Microplastics can be present in the environment as manufactured microplastics (known as primary microplastics) or resulting from the continuous weathering of plastic litter, which yields progressively smaller plastic fragments (known as secondary microplastics). Herein, we discuss the numerous issues associated with the analysis of microplastics, and to a less extent of nanoplastics, in environmental samples (water, sediments, and biological tissues), from their sampling and sample handling to their identification and quantification. The analytical quality control and quality assurance associated with the validation of analytical methods and use of reference materials for the quantification of microplastics are also discussed, as well as the current challenges within this field of research and possible routes to overcome such limitations. Copyright © 2018 Elsevier B.V. All rights reserved.

The National Shipbuilding Research Program. Environmental Studies and Testing (Phase V)

DTIC Science & Technology

2000-11-20

development of an analytical procedure for toxic organic compounds, including TBT ( tributyltin ), whose turnaround time would be in the order of minutes...Cost of the Subtask was $20,000. Subtask #33 - Turnaround Analytical Method for TBT This Subtask performed a preliminary investigation leading to the...34Quick TBT Analytical Method" that will yield reliable results in 15 minutes, a veritable breakthrough in sampling technology. The Subtask was managed by

General statistical considerations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eberhardt, L L; Gilbert, R O

From NAEG plutonium environmental studies program meeting; Las Vegas, Nevada, USA (2 Oct 1973). The high sampling variability encountered in environmental plutonium studies along with high analytical costs makes it very important that efficient soil sampling plans be used. However, efficient sampling depends on explicit and simple statements of the objectives of the study. When there are multiple objectives it may be difficult to devise a wholly suitable sampling scheme. Sampling for long-term changes in plutonium concentration in soils may also be complex and expensive. Further attention to problems associated with compositing samples is recommended, as is the consistent usemore » of random sampling as a basic technique. (auth)« less

UNCERTAINTY IN SCALING NUTRIENT EXPORT COEFFICIENTS

EPA Science Inventory

The Innov-X XT400 portable XRF analyzer features a miniature, rugged x-ray tube excitation source for analyzing a wide variety of elements and sample materials, including alloys, environmental solids, and other analytical samples. The x-ray tube source and Light Element Analysis...

40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...

40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...

40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...

40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...

40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...

High temperature ion channels and pores

NASA Technical Reports Server (NTRS)

Cheley, Stephen (Inventor); Gu, Li Qun (Inventor); Bayley, Hagan (Inventor); Kang, Xiaofeng (Inventor)

2011-01-01

The present invention includes an apparatus, system and method for stochastic sensing of an analyte to a protein pore. The protein pore may be an engineer protein pore, such as an ion channel at temperatures above 55.degree. C. and even as high as near 100.degree. C. The analyte may be any reactive analyte, including chemical weapons, environmental toxins and pharmaceuticals. The analyte covalently bonds to the sensor element to produce a detectable electrical current signal. Possible signals include change in electrical current. Detection of the signal allows identification of the analyte and determination of its concentration in a sample solution. Multiple analytes present in the same solution may also be detected.

MEASUREMENT OF VOLATILE ORGANIC COMPOUNDS BY THE US ENVIRONMENTAL PROTECTION AGENCY COMPENDIUM METHOD TO-17 - EVALUATION OF PERFORMANCE CRITERIA

EPA Science Inventory

An evaluation of performance criteria for US Environmental Protection Agency Compendium Method TO-17 for monitoring volatile organic compounds (VOCs) in air has been accomplished. The method is a solid adsorbent-based sampling and analytical procedure including performance crit...

Residues of 2-hydroxy-3-phenylpyrazine, a degradation product of some β-lactam antibiotics, in environmental water in Vietnam.

PubMed

Sy, Nguyen Van; Harada, Kazuo; Asayama, Megumi; Warisaya, Minae; Dung, Le Hong; Sumimura, Yoshinori; Diep, Khong Thi; Ha, Le Viet; Thang, Nguyen Nam; Hoa, Tran Thi Tuyet; Phu, Tran Minh; Khai, Pham Ngoc; Phuong, Nguyen Thanh; Tuyen, Le Danh; Yamamoto, Yoshimasa; Hirata, Kazumasa

2017-04-01

Antibiotic-resistant bacteria have become a serious problem worldwide, caused in part by the excessive use and discharge of antibiotics into the environment. Ampicillin (ABPC) is a widely used antibiotic. However, this chemical rapidly decomposes in water containing divalent cations like Ca 2+ and Mg 2+ , thus, detection of ABPC in environmental water is difficult. This study was carried out to evaluate the presence of 2-hydroxy-3-phenylpyrazine (HPP), one of the degradation products of ABPC and β-lactam antibiotics with an ABPC substructure, in environmental water. An analytical method for HPP monitoring in environmental water was developed using liquid chromatography/tandem mass spectrometry. The analyte was extracted from water samples and enriched using a solid-phase extraction cartridge. The quantification limit was 1 ng L -1 . The HPP recovery rates from spiked water samples of 25 and 125 ng L -1 were 84.1 and 86.1%, respectively. The method was then used to determine HPP residue levels in 98 environmental water samples from rivers, household ponds, and aquacultural ponds in Vietnam. HPP residues were detected in 60 samples. The HPP detection rates in rivers and household ponds were 42 and 79%, respectively. HPP was not detected in aquacultural ponds. HPP residue concentrations in the samples ranged from 1.3 to 413.3 ng L -1 . The residue levels in rivers flowing through city centres were higher than levels in other sampling locations. The findings of this study suggest that HPP is a promising marker for assessing the discharge of ABPC and β-lactam antibiotics with an ABPC substructure into the environment around sampling sites. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analytical results and sample locations of reanalyzed NURE stream-sediment and soil samples for the Humboldt River basin mineral-environmental assessment, northern Nevada

USGS Publications Warehouse

Folger, H. W.

2000-01-01

The U.S. Geological Survey (USGS), in cooperation with the Bureau of Land Management (BLM), began a study in 1996 to describe to the geochemistry of the Humboldt River Basin. The principal sample media evaluated are stream-sediment and soil samples retrieved from the National Uranium Resource Evaluation (NURE) archives located in Denver, Colorado. Samples were retrieved from the Wells, McDermitt, Vya, Lovelock, Winnemucca, Elko, Ely, Millett, Reno, and Tonopah 1? x 2? quadrangles in northern Nevada. The data are appropriate for large-scale reconnaissance resource evaluations and landscape geochemical-geoenvironmental evaluations. The analytical results are presented in this report.

Miniaturization of environmental chemical assays in flowing systems: the lab-on-a-valve approach vis-à-vis lab-on-a-chip microfluidic devices.

PubMed

Miró, Manuel; Hansen, Elo Harald

2007-09-26

The analytical capabilities of the microminiaturized lab-on-a-valve (LOV) module integrated into a microsequential injection (muSI) fluidic system in terms of analytical chemical performance, microfluidic handling and on-line sample processing are compared to those of the micro total analysis systems (muTAS), also termed lab-on-a-chip (LOC). This paper illustrates, via selected representative examples, the potentials of the LOV scheme vis-à-vis LOC microdevices for environmental assays. By means of user-friendly programmable flow and the exploitation of the interplay between the thermodynamics and the kinetics of the chemical reactions at will, LOV allows accommodation of reactions which, at least at the present stage, are not feasible by application of microfluidic LOC systems. Thus, in LOV one may take full advantage of kinetic discriminations schemes, where even subtle differences in reactions are utilized for analytical purposes. Furthermore, it is also feasible to handle multi-step sequential reactions of divergent kinetics; to conduct multi-parametric determinations without manifold reconfiguration by utilization of the inherent open-architecture of the micromachined unit for implementation of peripheral modules and automated handling of a variety of reagents; and most importantly, it offers itself as a versatile front end to a plethora of detection schemes. Not the least, LOV is regarded as an emerging downscaled tool to overcome the dilemma of LOC microsystems to admit real-life samples. This is nurtured via its intrinsic flexibility for accommodation of sample pre-treatment schemes aimed at the on-line manipulation of complex samples. Thus, LOV is playing a prominent role in the environmental field, whenever the monitoring of trace level concentration of pollutants is pursued, because both matrix isolation and preconcentration of target analytes is most often imperative, or in fact necessary, prior to sample presentation to the detector.

Level 1 environmental assessment performance evaluation. Final report jun 77-oct 78

DOE Office of Scientific and Technical Information (OSTI.GOV)

Estes, E.D.; Smith, F.; Wagoner, D.E.

1979-02-01

The report gives results of a two-phased evaluation of Level 1 environmental assessment procedures. Results from Phase I, a field evaluation of the Source Assessment Sampling System (SASS), showed that the SASS train performed well within the desired factor of 3 Level 1 accuracy limit. Three sample runs were made with two SASS trains sampling simultaneously and from approximately the same sampling point in a horizontal duct. A Method-5 train was used to estimate the 'true' particulate loading. The sampling systems were upstream of the control devices to ensure collection of sufficient material for comparison of total particulate, particle sizemore » distribution, organic classes, and trace elements. Phase II consisted of providing each of three organizations with three types of control samples to challenge the spectrum of Level 1 analytical procedures: an artificial sample in methylene chloride, an artificial sample on a flyash matrix, and a real sample composed of the combined XAD-2 resin extracts from all Phase I runs. Phase II results showed that when the Level 1 analytical procedures are carefully applied, data of acceptable accuracy is obtained. Estimates of intralaboratory and interlaboratory precision are made.« less

New trends in the analytical determination of emerging contaminants and their transformation products in environmental waters.

PubMed

Agüera, Ana; Martínez Bueno, María Jesús; Fernández-Alba, Amadeo R

2013-06-01

Since the so-called emerging contaminants were established as a new group of pollutants of environmental concern, a great effort has been devoted to the knowledge of their distribution, fate and effects in the environment. After more than 20 years of work, a significant improvement in knowledge about these contaminants has been achieved, but there is still a large gap of information on the growing number of new potential contaminants that are appearing and especially of their unpredictable transformation products. Although the environmental problem arising from emerging contaminants must be addressed from an interdisciplinary point of view, it is obvious that analytical chemistry plays an important role as the first step of the study, as it allows establishing the presence of chemicals in the environment, estimate their concentration levels, identify sources and determine their degradation pathways. These tasks involve serious difficulties requiring different analytical solutions adjusted to purpose. Thus, the complexity of the matrices requires highly selective analytical methods; the large number and variety of compounds potentially present in the samples demands the application of wide scope methods; the low concentrations at which these contaminants are present in the samples require a high detection sensitivity, and high demands on the confirmation and high structural information are needed for the characterisation of unknowns. New developments on analytical instrumentation have been applied to solve these difficulties. Furthermore and not less important has been the development of new specific software packages intended for data acquisition and, in particular, for post-run analysis. Thus, the use of sophisticated software tools has allowed successful screening analysis, determining several hundreds of analytes, and assisted in the structural elucidation of unknown compounds in a timely manner.

Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

2018-04-01

In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent advances in analytical methods for the determination of 4-alkylphenols and bisphenol A in solid environmental matrices: A critical review.

PubMed

Salgueiro-González, N; Castiglioni, S; Zuccato, E; Turnes-Carou, I; López-Mahía, P; Muniategui-Lorenzo, S

2018-09-18

The problem of endocrine disrupting compounds (EDCs) in the environment has become a worldwide concern in recent decades. Besides their toxicological effects at low concentrations and their widespread use in industrial and household applications, these pollutants pose a risk for non-target organisms and also for public safety. Analytical methods to determine these compounds at trace levels in different matrices are urgently needed. This review critically discusses trends in analytical methods for well-known EDCs like alkylphenols and bisphenol A in solid environmental matrices, including sediment and aquatic biological samples (from 2006 to 2018). Information about extraction, clean-up and determination is covered in detail, including analytical quality parameters (QA/QC). Conventional and novel analytical techniques are compared, with their advantages and drawbacks. Ultrasound assisted extraction followed by solid phase extraction clean-up is the most widely used procedure for sediment and aquatic biological samples, although softer extraction conditions have been employed for the latter. The use of liquid chromatography followed by tandem mass spectrometry has greatly increased in the last five years. The majority of these methods have been employed for the analysis of river sediments and bivalve molluscs because of their usefulness in aquatic ecosystem (bio)monitoring programs. Green, simple, fast analytical methods are now needed to determine these compounds in complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

NASA Astrophysics Data System (ADS)

Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

2016-12-01

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples.

Green aspects, developments and perspectives of liquid phase microextraction techniques.

PubMed

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2014-02-01

Determination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte isolation/enrichment prior to analysis is required in many cases. In this work the newest trends and innovations in liquid phase microextraction, like: single-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME) have been discussed, including their critical evaluation and possible application in analytical practice. The described modifications of extraction techniques deal with system miniaturization and/or automation, the use of ultrasound and physical agitation, and electrochemical methods. Particular attention was given to pro-ecological aspects therefore the possible use of novel, non-toxic extracting agents, inter alia, ionic liquids, coacervates, surfactant solutions and reverse micelles in the liquid phase microextraction techniques has been evaluated in depth. Also, new methodological solutions and the related instruments and devices for the efficient liquid phase micoextraction of analytes, which have found application at the stage of procedure prior to chromatographic determination, are presented. © 2013 Published by Elsevier B.V.

Using model-based screening to help discover unknown environmental contaminants.

PubMed

McLachlan, Michael S; Kierkegaard, Amelie; Radke, Michael; Sobek, Anna; Malmvärn, Anna; Alsberg, Tomas; Arnot, Jon A; Brown, Trevor N; Wania, Frank; Breivik, Knut; Xu, Shihe

2014-07-01

Of the tens of thousands of chemicals in use, only a small fraction have been analyzed in environmental samples. To effectively identify environmental contaminants, methods to prioritize chemicals for analytical method development are required. We used a high-throughput model of chemical emissions, fate, and bioaccumulation to identify chemicals likely to have high concentrations in specific environmental media, and we prioritized these for target analysis. This model-based screening was applied to 215 organosilicon chemicals culled from industrial chemical production statistics. The model-based screening prioritized several recognized organosilicon contaminants and generated hypotheses leading to the selection of three chemicals that have not previously been identified as potential environmental contaminants for target analysis. Trace analytical methods were developed, and the chemicals were analyzed in air, sewage sludge, and sediment. All three substances were found to be environmental contaminants. Phenyl-tris(trimethylsiloxy)silane was present in all samples analyzed, with concentrations of ∼50 pg m(-3) in Stockholm air and ∼0.5 ng g(-1) dw in sediment from the Stockholm archipelago. Tris(trifluoropropyl)trimethyl-cyclotrisiloxane and tetrakis(trifluoropropyl)tetramethyl-cyclotetrasiloxane were found in sediments from Lake Mjøsa at ∼1 ng g(-1) dw. The discovery of three novel environmental contaminants shows that models can be useful for prioritizing chemicals for exploratory assessment.

Reliable quantification of phthalates in environmental matrices (air, water, sludge, sediment and soil): a review.

PubMed

Net, Sopheak; Delmont, Anne; Sempéré, Richard; Paluselli, Andrea; Ouddane, Baghdad

2015-05-15

Because of their widespread application, phthalates or phthalic acid esters (PAEs) are ubiquitous in the environment. Their presence has attracted considerable attention due to their potential impacts on ecosystem functioning and on public health, so their quantification has become a necessity. Various extraction procedures as well as gas/liquid chromatography and mass spectrometry detection techniques are found as suitable for reliable detection of such compounds. However, PAEs are ubiquitous in the laboratory environment including ambient air, reagents, sampling equipment, and various analytical devices, that induces difficult analysis of real samples with a low PAE background. Therefore, accurate PAE analysis in environmental matrices is a challenging task. This paper reviews the extensive literature data on the techniques for PAE quantification in natural media. Sampling, sample extraction/pretreatment and detection for quantifying PAEs in different environmental matrices (air, water, sludge, sediment and soil) have been reviewed and compared. The concept of "green analytical chemistry" for PAE determination is also discussed. Moreover useful information about the material preparation and the procedures of quality control and quality assurance are presented to overcome the problem of sample contamination and these encountered due to matrix effects in order to avoid overestimating PAE concentrations in the environment. Copyright © 2015 Elsevier B.V. All rights reserved.

A review of selected inorganic surface water quality-monitoring practices: are we really measuring what we think, and if so, are we doing it right?

USGS Publications Warehouse

Horowitz, Arthur J.

2013-01-01

Successful environmental/water quality-monitoring programs usually require a balance between analytical capabilities, the collection and preservation of representative samples, and available financial/personnel resources. Due to current economic conditions, monitoring programs are under increasing pressure to do more with less. Hence, a review of current sampling and analytical methodologies, and some of the underlying assumptions that form the bases for these programs seems appropriate, to see if they are achieving their intended objectives within acceptable error limits and/or measurement uncertainty, in a cost-effective manner. That evaluation appears to indicate that several common sampling/processing/analytical procedures (e.g., dip (point) samples/measurements, nitrogen determinations, total recoverable analytical procedures) are generating biased or nonrepresentative data, and that some of the underlying assumptions relative to current programs, such as calendar-based sampling and stationarity are no longer defensible. The extensive use of statistical models as well as surrogates (e.g., turbidity) also needs to be re-examined because the hydrologic interrelationships that support their use tend to be dynamic rather than static. As a result, a number of monitoring programs may need redesigning, some sampling and analytical procedures may need to be updated, and model/surrogate interrelationships may require recalibration.

One-calibrant kinetic calibration for on-site water sampling with solid-phase microextraction.

PubMed

Ouyang, Gangfeng; Cui, Shufen; Qin, Zhipei; Pawliszyn, Janusz

2009-07-15

The existing solid-phase microextraction (SPME) kinetic calibration technique, using the desorption of the preloaded standards to calibrate the extraction of the analytes, requires that the physicochemical properties of the standard should be similar to those of the analyte, which limited the application of the technique. In this study, a new method, termed the one-calibrant kinetic calibration technique, which can use the desorption of a single standard to calibrate all extracted analytes, was proposed. The theoretical considerations were validated by passive water sampling in laboratory and rapid water sampling in the field. To mimic the variety of the environment, such as temperature, turbulence, and the concentration of the analytes, the flow-through system for the generation of standard aqueous polycyclic aromatic hydrocarbons (PAHs) solution was modified. The experimental results of the passive samplings in the flow-through system illustrated that the effect of the environmental variables was successfully compensated with the kinetic calibration technique, and all extracted analytes can be calibrated through the desorption of a single calibrant. On-site water sampling with rotated SPME fibers also illustrated the feasibility of the new technique for rapid on-site sampling of hydrophobic organic pollutants in water. This technique will accelerate the application of the kinetic calibration method and also will be useful for other microextraction techniques.

Quality Control Guidelines for SAM Chemical Methods

EPA Pesticide Factsheets

Learn more about quality control guidelines and recommendations for the analysis of samples using the chemistry methods listed in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

Quality Control Guidelines for SAM Pathogen Methods

EPA Pesticide Factsheets

Learn more about quality control guidelines and recommendations for the analysis of samples using the biotoxin methods listed in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

Quality Control Guidelines for SAM Radiochemical Methods

EPA Pesticide Factsheets

Learn more about quality control guidelines and recommendations for the analysis of samples using the radiochemistry methods listed in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

General Quality Control (QC) Guidelines for SAM Methods

EPA Pesticide Factsheets

Learn more about quality control guidelines and recommendations for the analysis of samples using the methods listed in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

Quality Control Guidelines for SAM Biotoxin Methods

EPA Pesticide Factsheets

Learn more about quality control guidelines and recommendations for the analysis of samples using the pathogen methods listed in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

PubMed

Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

2016-05-15

A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

EPA Science Inventory

The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

GUIDANCE FOR OBTAINING REPRESENTATIVE ANALYTICAL LABORATORY SUBSAMPLES FROM PARTICULATE LABORATORY SAMPLES

EPA Science Inventory

An ongoing research program has been established to experimentally verify the application of the Gy theory to environmental samples, which serves as a supporting basis for -the material presented in this guidance. Research results from studies performed by the United
States E...

Environmental isotope investigation of groundwater flow in the Honey Lake Basin, California and Nevada

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rose, T.P.; Davisson, M.L.; Hudson, G.B.

The hydrology of Honey Lake Basin was studied using environmental isotope measurements of approximately 130 water samples collected during 1995 and 1996. The principal analytical methods included hydrogen, oxygen and carbon stable isotope ratio measurements, radiocarbon and tritium dating, and measurements of dissolved noble gas abundances.

Piezoelectric sensors based on molecular imprinted polymers for detection of low molecular mass analytes.

PubMed

Uludağ, Yildiz; Piletsky, Sergey A; Turner, Anthony P F; Cooper, Matthew A

2007-11-01

Biomimetic recognition elements employed for the detection of analytes are commonly based on proteinaceous affibodies, immunoglobulins, single-chain and single-domain antibody fragments or aptamers. The alternative supra-molecular approach using a molecularly imprinted polymer now has proven utility in numerous applications ranging from liquid chromatography to bioassays. Despite inherent advantages compared with biochemical/biological recognition (which include robustness, storage endurance and lower costs) there are few contributions that describe quantitative analytical applications of molecularly imprinted polymers for relevant small molecular mass compounds in real-world samples. There is, however, significant literature describing the use of low-power, portable piezoelectric transducers to detect analytes in environmental monitoring and other application areas. Here we review the combination of molecularly imprinted polymers as recognition elements with piezoelectric biosensors for quantitative detection of small molecules. Analytes are classified by type and sample matrix presentation and various molecularly imprinted polymer synthetic fabrication strategies are also reviewed.

Interim results of quality-control sampling of surface water for the Upper Colorado River National Water-Quality Assessment Study Unit, water years 1995-96

USGS Publications Warehouse

Spahr, N.E.; Boulger, R.W.

1997-01-01

Quality-control samples provide part of the information needed to estimate the bias and variability that result from sample collection, processing, and analysis. Quality-control samples of surface water collected for the Upper Colorado River National Water-Quality Assessment study unit for water years 1995?96 are presented and analyzed in this report. The types of quality-control samples collected include pre-processing split replicates, concurrent replicates, sequential replicates, post-processing split replicates, and field blanks. Analysis of the pre-processing split replicates, concurrent replicates, sequential replicates, and post-processing split replicates is based on differences between analytical results of the environmental samples and analytical results of the quality-control samples. Results of these comparisons indicate that variability introduced by sample collection, processing, and handling is low and will not affect interpretation of the environmental data. The differences for most water-quality constituents is on the order of plus or minus 1 or 2 lowest rounding units. A lowest rounding unit is equivalent to the magnitude of the least significant figure reported for analytical results. The use of lowest rounding units avoids some of the difficulty in comparing differences between pairs of samples when concentrations span orders of magnitude and provides a measure of the practical significance of the effect of variability. Analysis of field-blank quality-control samples indicates that with the exception of chloride and silica, no systematic contamination of samples is apparent. Chloride contamination probably was the result of incomplete rinsing of the dilute cleaning solution from the outlet ports of the decaport sample splitter. Silica contamination seems to have been introduced by the blank water. Sampling and processing procedures for water year 1997 have been modified as a result of these analyses.

Salicylic Acid and 4-Nitroaniline Removal from Water Using Magnetic Biochar: An Environmental and Analytical Experiment for the Undergraduate Laboratory

ERIC Educational Resources Information Center

Karunanayake, Akila G.; Dewage, Narada Bombuwala; Todd, Olivia Adele; Essandoh, Matthew; Anderson, Renel; Mlsna, Todd; Mlsna, Deb

2016-01-01

Adsorption studies of salicylic acid (SA) and 4-nitroaniline (4NA) from aqueous solutions were performed with magnetic biochar (MBC) in order to train students in analytical techniques such as standard calibration curves, UV-vis spectrophotometry, and chemical separations within the context of wastewater purification. Analysis of samples purified…

Determination of technetium-99 in environmental samples: a review.

PubMed

Shi, Keliang; Hou, Xiaolin; Roos, Per; Wu, Wangsuo

2012-01-04

Due to the lack of a stable technetium isotope, and the high mobility and long half-life, (99)Tc is considered to be one of the most important radionuclides in safety assessment of environmental radioactivity as well as nuclear waste management. (99)Tc is also an important tracer for oceanographic research due to the high technetium solubility in seawater as TcO(4)(-). A number of analytical methods, using chemical separation combined with radiometric and mass spectrometric measurement techniques, have been developed over the past decades for determination of (99)Tc in different environmental samples. This article summarizes and compares recently reported chemical separation procedures and measurement methods for determination of (99)Tc. Due to the extremely low concentration of (99)Tc in environmental samples, the sample preparation, pre-concentration, chemical separation and purification for removal of the interferences for detection of (99)Tc are the most important issues governing the accurate determination of (99)Tc. These aspects are discussed in detail in this article. Meanwhile, the different measurement techniques for (99)Tc are also compared with respect to advantages and drawbacks. Novel automated analytical methods for rapid determination of (99)Tc using solid extraction or ion exchange chromatography for separation of (99)Tc, employing flow injection or sequential injection approaches are also discussed. Copyright © 2011 Elsevier B.V. All rights reserved.

Environmental Response Laboratory Network Membership and Benefits

EPA Pesticide Factsheets

Member laboratories must meet core requirements including quality systems, policies and procedures, sample and data management, and analytical capabilities. Benefits include training and exercise opportunities, information sharing and technical support.

USGS Blind Sample Project: monitoring and evaluating laboratory analytical quality

USGS Publications Warehouse

Ludtke, Amy S.; Woodworth, Mark T.

1997-01-01

The U.S. Geological Survey (USGS) collects and disseminates information about the Nation's water resources. Surface- and ground-water samples are collected and sent to USGS laboratories for chemical analyses. The laboratories identify and quantify the constituents in the water samples. Random and systematic errors occur during sample handling, chemical analysis, and data processing. Although all errors cannot be eliminated from measurements, the magnitude of their uncertainty can be estimated and tracked over time. Since 1981, the USGS has operated an independent, external, quality-assurance project called the Blind Sample Project (BSP). The purpose of the BSP is to monitor and evaluate the quality of laboratory analytical results through the use of double-blind quality-control (QC) samples. The information provided by the BSP assists the laboratories in detecting and correcting problems in the analytical procedures. The information also can aid laboratory users in estimating the extent that laboratory errors contribute to the overall errors in their environmental data.

ERLN Regional Support

EPA Pesticide Factsheets

Regional labs play important roles in the Environmental Response Laboratory Network. They can serve as point of contact; coordinate sample flow, special analytical service requests, or training exercises; and partner with regional emergency/disaster staff.

A chemodynamic approach for estimating losses of target organic chemicals from water during sample holding time

USGS Publications Warehouse

Capel, P.D.; Larson, S.J.

1995-01-01

Minimizing the loss of target organic chemicals from environmental water samples between the time of sample collection and isolation is important to the integrity of an investigation. During this sample holding time, there is a potential for analyte loss through volatilization from the water to the headspace, sorption to the walls and cap of the sample bottle; and transformation through biotic and/or abiotic reactions. This paper presents a chemodynamic-based, generalized approach to estimate the most probable loss processes for individual target organic chemicals. The basic premise is that the investigator must know which loss process(es) are important for a particular analyte, based on its chemodynamic properties, when choosing the appropriate method(s) to prevent loss.

Gas chromatography coupled to tunable pulsed glow discharge time-of-flight mass spectrometry for environmental analysis.

PubMed

Solà-Vázquez, Auristela; Lara-Gonzalo, Azucena; Costa-Fernández, José M; Pereiro, Rosario; Sanz-Medel, Alfredo

2010-05-01

A tuneable microsecond pulsed direct current glow discharge (GD)-time-of-flight mass spectrometer MS(TOF) developed in our laboratory was coupled to a gas chromatograph (GC) to obtain sequential collection of the mass spectra, at different temporal regimes occurring in the GD pulses, during elution of the analytes. The capabilities of this set-up were explored using a mixture of volatile organic compounds of environmental concern: BrClCH, Cl(3)CH, Cl(4)C, BrCl(2)CH, Br(2)ClCH, Br(3)CH. The experimental parameters of the GC-pulsed GD-MS(TOF) prototype were optimized in order to separate appropriately and analyze the six selected organic compounds, and two GC carrier gases, helium and nitrogen, were evaluated. Mass spectra for all analytes were obtained in the prepeak, plateau and afterpeak temporal regimes of the pulsed GD. Results showed that helium offered the best elemental sensitivity, while nitrogen provided higher signal intensities for fragments and molecular peaks. The analytical performance characteristics were also worked out for each analyte. Absolute detection limits obtained were in the order of ng. In a second step, headspace solid phase microextraction (HS SPME), as sample preparation and preconcentration technique, was evaluated for the quantification of the compounds under study, in order to achieve the required analytical sensitivity for trihalomethanes European Union (EU) environmental legislation. The analytical figures of merit obtained using the proposed methodology showed rather good detection limits (between 2 and 13 microg L(-1) depending on the analyte). In fact, the developed methodology met the EU legislation requirements (the maximum level permitted in tap water for the "total trihalomethanes" is set at 100 microg L(-1)). Real analysis of drinking water and river water were successfully carried out. To our knowledge this is the first application of GC-pulsed GD-MS(TOF) for the analysis of real samples. Its ability to provide elemental, fragments and molecular information of the organic compounds is demonstrated.

Analytical interferences of mercuric chloride preservative in environmental water samples: Determination of organic compounds isolated by continuous liquid-liquid extraction or closed-loop stripping

USGS Publications Warehouse

Foreman, W.T.; Zaugg, S.D.; Falres, L.M.; Werner, M.G.; Leiker, T.J.; Rogerson, P.F.

1992-01-01

Analytical interferences were observed during the determination of organic compounds in groundwater samples preserved with mercuric chloride. The nature of the interference was different depending on the analytical isolation technique employed. (1) Water samples extracted with dichloromethane by continuous liquid-liquid extraction (CLLE) and analyzed by gas chromatography/mass spectrometry revealed a broad HgCl2 'peak' eluting over a 3-5-min span which interfered with the determination of coeluting organic analytes. Substitution of CLLE for separatory funnel extraction in EPA method 508 also resulted in analytical interferences from the use of HgCl2 preservative. (2) Mercuric chloride was purged, along with organic contaminants, during closed-loop stripping (CLS) of groundwater samples and absorbed onto the activated charcoal trap. Competitive sorption of the HgCl2 by the trap appeared to contribute to the observed poor recoveries for spiked organic contaminants. The HgCl2 was not displaced from the charcoal with the dichloromethane elution solvent and required strong nitric acid to achieve rapid, complete displacement. Similar competitive sorption mechanisms might also occur in other purge and trap methods when this preservative is used.

Determination of insoluble soap in agricultural soil and sewage sludge samples by liquid chromatography with ultraviolet detection.

PubMed

Cantarero, Samuel; Zafra-Gómez, Alberto; Ballesteros, Oscar; Navalón, Alberto; Vílchez, José L; Crovetto, Guillermo; Verge, Coral; de Ferrer, Juan A

2010-11-01

We have developed a new analytical procedure for determining insoluble Ca and Mg fatty acid salts (soaps) in agricultural soil and sewage sludge samples. The number of analytical methodologies that focus in the determination of insoluble soap salts in different environmental compartments is very limited. In this work, we propose a methodology that involves a sample clean-up step with petroleum ether to remove soluble salts and a conversion of Ca and Mg insoluble salts into soluble potassium salts using tripotassium ethylenediaminetetraacetate salt and potassium carbonate, followed by the extraction of analytes from the samples using microwave-assisted extraction with methanol. An improved esterification procedure using 2,4-dibromoacetophenone before the liquid chromatography with ultraviolet detection analysis also has been developed. The absence of matrix effect was demonstrated with two fatty acid Ca salts that are not commercial and are never detected in natural samples (C₁₃:₀ and C₁₇:₀). Therefore, it was possible to evaluate the matrix effect because both standards have similar environmental behavior (adsorption and precipitation) to commercial soaps (C₁₀:₀) to C₁₈:₀). We also studied the effect of the different variables on the clean-up, the conversion of Ca soap, and the extraction and derivatization procedures. The quantification limits found ranged from 0.4 to 0.8 mg/kg. The proposed method was satisfactorily applied for the development of a study on soap behavior in agricultural soil and sewage sludge samples. © 2010 SETAC.

Lab-on-chip systems for integrated bioanalyses

PubMed Central

Madaboosi, Narayanan; Soares, Ruben R.G.; Fernandes, João Tiago S.; Novo, Pedro; Moulas, Geraud; Chu, Virginia

2016-01-01

Biomolecular detection systems based on microfluidics are often called lab-on-chip systems. To fully benefit from the miniaturization resulting from microfluidics, one aims to develop ‘from sample-to-answer’ analytical systems, in which the input is a raw or minimally processed biological, food/feed or environmental sample and the output is a quantitative or qualitative assessment of one or more analytes of interest. In general, such systems will require the integration of several steps or operations to perform their function. This review will discuss these stages of operation, including fluidic handling, which assures that the desired fluid arrives at a specific location at the right time and under the appropriate flow conditions; molecular recognition, which allows the capture of specific analytes at precise locations on the chip; transduction of the molecular recognition event into a measurable signal; sample preparation upstream from analyte capture; and signal amplification procedures to increase sensitivity. Seamless integration of the different stages is required to achieve a point-of-care/point-of-use lab-on-chip device that allows analyte detection at the relevant sensitivity ranges, with a competitive analysis time and cost. PMID:27365042

Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site-Working towards a toolbox for better assessment.

PubMed

Wroble, Julie; Frederick, Timothy; Frame, Alicia; Vallero, Daniel

2017-01-01

Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)'s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete ("grab") samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples.

Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site—Working towards a toolbox for better assessment

PubMed Central

2017-01-01

Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)’s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete (“grab”) samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples. PMID:28759607

Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods.

PubMed

Han, Lijun; Matarrita, Jessie; Sapozhnikova, Yelena; Lehotay, Steven J

2016-06-03

This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography - tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChERS extraction followed by use of EMR-Lipid ("enhanced matrix removal of lipids") and an additional salting out step for cleanup. The optimal amount of EMR-Lipid was determined to be 500mg for 2.5mL extracts for most of the analytes. The co-extractive removal efficiency by the EMR-Lipid cleanup step was 83-98% for fatty samples and 79% for kale, including 76% removal of chlorophyll. Matrix effects were typically less than ±20%, in part because analyte protectants were used in the LPGC-MS/MS analysis. The recoveries of polycyclic aromatic hydrocarbons and diverse pesticides were mostly 70-120%, whereas recoveries of nonpolar polybrominated diphenyl ethers and polychlorinated biphenyls were mostly lower than 70% through the cleanup procedure. With the use of internal standards, method validation results showed that 76-85 of the 117 analytes achieved satisfactory results (recoveries of 70-120% and RSD≤20%) in pork, avocado, and kale, while 53 analytes had satisfactory results in salmon. Detection limits were 5-10ng/g for all but a few analytes. EMR-Lipid is a new sample preparation tool that serves as another useful option for cleanup in multiresidue analysis, particularly of fatty foods. Published by Elsevier B.V.

The procedures manual of the Environmental Measurements Laboratory. Volume 1, 28. edition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chieco, N.A.

1997-02-01

This manual covers procedures and technology currently in use at the Environmental Measurements Laboratory. An attempt is made to be sure that all work carried out will be of the highest quality. Attention is focused on the following areas: quality assurance; sampling; radiation measurements; analytical chemistry; radionuclide data; special facilities; and specifications.

Ground-water-quality data in Pennsylvania: A compilation of computerized [electronic] databases, 1979-2004

USGS Publications Warehouse

Low, Dennis J.; Chichester, Douglas C.

2006-01-01

This study, by the U.S. Geological Survey (USGS) in cooperation with the Pennsylvania Department of Environmental Protection (PADEP), provides a compilation of ground-water-quality data for a 25-year period (January 1, 1979, through August 11, 2004) based on water samples from wells. The data are from eight source agencies唯orough of Carroll Valley, Chester County Health Department, Pennsylvania Department of Environmental Protection-Ambient and Fixed Station Network, Montgomery County Health Department, Pennsylvania Drinking Water Information System, Pennsylvania Department of Agriculture, Susquehanna River Basin Commission, and the U.S. Geological Survey. The ground-water-quality data from the different source agencies varied in type and number of analyses; however, the analyses are represented by 12 major analyte groups:biological (bacteria and viruses), fungicides, herbicides, insecticides, major ions, minor ions (including trace elements), nutrients (dominantly nitrate and nitrite as nitrogen), pesticides, radiochemicals (dominantly radon or radium), volatile organic compounds, wastewater compounds, and water characteristics (dominantly field pH, field specific conductance, and hardness).A summary map shows the areal distribution of wells with ground-water-quality data statewide and by major watersheds and source agency. Maps of 35 watersheds within Pennsylvania are used to display the areal distribution of water-quality information. Additional maps emphasize the areal distribution with respect to 13 major geolithologic units in Pennsylvania and concentration ranges of nitrate (as nitrogen). Summary data tables by source agency provide information on the number of wells and samples collected for each of the 35 watersheds and analyte groups. The number of wells sampled for ground-water-quality data varies considerably across Pennsylvania. Of the 8,012 wells sampled, the greatest concentration of wells are in the southeast (Berks, Bucks, Chester, Delaware, Lancaster, Montgomery, and Philadelphia Counties), in the vicinity of Pittsburgh, and in the northwest (Erie County). The number of wells sampled is relatively sparse in south-central (Adams, Cambria, Cumberland, and Franklin Counties), central (Centre, Indiana, and Snyder Counties), and north-central (Bradford, Potter, and Tioga Counties) Pennsylvania. Little to no data are available for approximately one-third of the state. Water characteristics and nutrients were the most frequently sampled major analyte groups; approximately 21,000 samples were collected for each group. Major and minor ions were the next most-frequently sampled major analyte groups; approximately 17,000 and 12,000 samples were collected, respectively. For the remaining eight major analyte groups, the number of samples collected ranged from a low of 307 samples (wastewater compounds) to a high of approximately 3,000 samples (biological).The number of samples that exceeded a maximum contaminant level (MCL) or secondary maximum contaminant level (SMCL) by major analyte group also varied. Of the 2,988 samples in the biological analyte group, 53 percent had water that exceeded an MCL. Almost 2,500 samples were collected and analyzed for volatile organic compounds; 14 percent exceeded an MCL. Other major analyte groups that frequently exceeded MCLs or SMCLs included major ions (17,465 samples and a 33.9 percent exceedence), minor ions (11,905 samples and a 17.1 percent exceedence), and water characteristics (21,183 samples and a 20.3 percent exceedence). Samples collected and analyzed for fungicides, herbicides, insecticides, and pesticides (4,062 samples), radiochemicals (1,628 samples), wastewater compounds (307 samples), and nutrients (20,822 samples) had the lowest exceedences of 0.3, 8.4, 0.0, and 8.8 percent, respectively.

Green Aspects of Techniques for the Determination of Currently Used Pesticides in Environmental Samples

PubMed Central

Stocka, Jolanta; Tankiewicz, Maciej; Biziuk, Marek; Namieśnik, Jacek

2011-01-01

Pesticides are among the most dangerous environmental pollutants because of their stability, mobility and long-term effects on living organisms. Their presence in the environment is a particular danger. It is therefore crucial to monitor pesticide residues using all available analytical methods. The analysis of environmental samples for the presence of pesticides is very difficult: the processes involved in sample preparation are labor-intensive and time-consuming. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solvent-less and solvent-minimized techniques are becoming popular. The application of Green Chemistry principles to sample preparation is primarily leading to the miniaturization of procedures and the use of solvent-less techniques, and these are discussed in the paper. PMID:22174632

An Overview of Conventional and Emerging Analytical Methods for the Determination of Mycotoxins

PubMed Central

Cigić, Irena Kralj; Prosen, Helena

2009-01-01

Mycotoxins are a group of compounds produced by various fungi and excreted into the matrices on which they grow, often food intended for human consumption or animal feed. The high toxicity and carcinogenicity of these compounds and their ability to cause various pathological conditions has led to widespread screening of foods and feeds potentially polluted with them. Maximum permissible levels in different matrices have also been established for some toxins. As these are quite low, analytical methods for determination of mycotoxins have to be both sensitive and specific. In addition, an appropriate sample preparation and pre-concentration method is needed to isolate analytes from rather complicated samples. In this article, an overview of methods for analysis and sample preparation published in the last ten years is given for the most often encountered mycotoxins in different samples, mainly in food. Special emphasis is on liquid chromatography with fluorescence and mass spectrometric detection, while in the field of sample preparation various solid-phase extraction approaches are discussed. However, an overview of other analytical and sample preparation methods less often used is also given. Finally, different matrices where mycotoxins have to be determined are discussed with the emphasis on their specific characteristics important for the analysis (human food and beverages, animal feed, biological samples, environmental samples). Various issues important for accurate qualitative and quantitative analyses are critically discussed: sampling and choice of representative sample, sample preparation and possible bias associated with it, specificity of the analytical method and critical evaluation of results. PMID:19333436

Development of a carbon-nanoparticle-coated stirrer for stir bar sorptive extraction by a simple carbon deposition in flame.

PubMed

Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

2016-03-01

Stir bar sorptive extraction is an environmentally friendly microextraction technique based on a stir bar with various sorbents. A commercial stirrer is a good support, but it has not been used in stir bar sorptive extraction due to difficult modification. A stirrer was modified with carbon nanoparticles by a simple carbon deposition process in flame and characterized by scanning electron microscopy and energy-dispersive X-ray spectrometry. A three-dimensional porous coating was formed with carbon nanoparticles. In combination with high-performance liquid chromatography, the stir bar was evaluated using five polycyclic aromatic hydrocarbons as model analytes. Conditions including extraction time and temperature, ionic strength, and desorption solvent were investigated by a factor-by-factor optimization method. The established method exhibited good linearity (0.01-10 μg/L) and low limits of quantification (0.01 μg/L). It was applied to detect model analytes in environmental water samples. No analyte was detected in river water, and five analytes were quantified in rain water. The recoveries of five analytes in two samples with spiked at 2 μg/L were in the range of 92.2-106% and 93.4-108%, respectively. The results indicated that the carbon nanoparticle-coated stirrer was an efficient stir bar for extraction analysis of some polycyclic aromatic hydrocarbons. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel approach to high-throughput determination of endocrine disruptors using recycled diatomaceous earth as a green sorbent phase for thin-film solid-phase microextraction combined with 96-well plate system.

PubMed

Kirschner, Nicolas; Dias, Adriana Neves; Budziak, Dilma; da Silveira, Cristian Berto; Merib, Josias; Carasek, Eduardo

2017-12-15

A sustainable approach to TF-SPME is presented using recycled diatomaceous earth, obtained from a beer purification process, as a green sorbent phase for the determination of bisphenol A (BPA), benzophenone (BzP), triclocarban (TCC), 4-methylbenzylidene camphor (4-MBC) and 2-ethylhexyl-p-methoxycinnamate (EHMC) in environmental water samples. TF-SPME was combined with a 96-well plate system allowing for high-throughput analysis due to the simultaneous extraction/desorption up to 96 samples. The proposed sorbent phase exhibited good stability in organic solvents, as well as satisfactory analytical performance. The optimized method consisted of 240 min of extraction at pH 6 with the addition of NaCl (15% w/v). A mixture of MeOH:ACN (50:50 v/v) was used for the desorption the analytes, using a time of 30 min. Limits of detection varied from 1 μg L -1 for BzP and TCC to 8 μg L -1 for the other analytes, and R 2 ranged from 0.9926 for 4-MBC to 0.9988 for BPA. This novel and straightforward approach offers an environmentally-friendly and very promising alternative for routine analysis. . The total sample preparation time per sample was approximately 2.8 min, which is a significant advantage when a large number of analytical run is required. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical Methods to Distinguish the Positive and Negative Spectra of Mineral and Environmental Elements Using Deep Ablation Laser-Induced Breakdown Spectroscopy (LIBS).

PubMed

Kim, Dongyoung; Yang, Jun-Ho; Choi, Soojin; Yoh, Jack J

2018-01-01

Environments affect mineral surfaces, and the surface contamination or alteration can provide potential information to understanding their regional environments. However, when investigating mineral surfaces, mineral and environmental elements appear mixed in data. This makes it difficult to determine their atomic compositions independently. In this research, we developed four analytical methods to distinguish mineral and environmental elements into positive and negative spectra based on depth profiling data using laser-induced breakdown spectroscopy (LIBS). The principle of the methods is to utilize how intensity varied with depth for creating a new spectrum. The methods were applied to five mineral samples exposed to four environmental conditions including seawater, crude oil, sulfuric acid, and air as control. The proposed methods are then validated by applying the resultant spectra to principal component analysis and data were classified by the environmental conditions and atomic compositions of mineral. By applying the methods, the atomic information of minerals and environmental conditions were successfully inferred in the resultant spectrum.

Monitoring the Presence of 13 Active Compounds in Surface Water Collected from Rural Areas in Northwestern Spain

PubMed Central

Iglesias, Alejandra; Nebot, Carolina; Vázquez, Beatriz I.; Coronel-Olivares, Claudia; Franco Abuín, Carlos M.; Cepeda, Alberto

2014-01-01

Drug residues are considered environmental contaminants, and their occurrence has recently become a matter of concern. Analytical methods and monitoring systems are therefore required to control the continuous input of these drug residues into the environment. This article presents a suitable HPLC-ESI-MS/MS method for the simultaneous extraction, detection and quantification of residues of 13 drugs (antimicrobials, glucocorticosteroids, anti-inflammatories, anti-hypertensives, anti-cancer drugs and triphenylmethane dyes) in surface water. A monitoring study with 549 water samples was carried out in northwestern Spain to detect the presence of drug residues over two sampling periods during 2010, 2011 and 2012. Samples were collected from rural areas with and without farming activity and from urban areas. The 13 analytes were detected, and 18% of the samples collected showed positive results for the presence of at least one analyte. More collection sites were located in rural areas than in urban areas. However, more positive samples with higher concentrations and a larger number of analytes were detected in samples collected from sites located after the discharge of a WWTP. Results indicated that the WWTPs seems to act as a concentration point. Positive samples were also detected at a site located near a drinking water treatment plant. PMID:24837665

Monitoring the presence of 13 active compounds in surface water collected from rural areas in northwestern Spain.

PubMed

Iglesias, Alejandra; Nebot, Carolina; Vázquez, Beatriz I; Coronel-Olivares, Claudia; Abuín, Carlos M Franco; Cepeda, Alberto

2014-05-15

Drug residues are considered environmental contaminants, and their occurrence has recently become a matter of concern. Analytical methods and monitoring systems are therefore required to control the continuous input of these drug residues into the environment. This article presents a suitable HPLC-ESI-MS/MS method for the simultaneous extraction, detection and quantification of residues of 13 drugs (antimicrobials, glucocorticosteroids, anti-inflammatories, anti-hypertensives, anti-cancer drugs and triphenylmethane dyes) in surface water. A monitoring study with 549 water samples was carried out in northwestern Spain to detect the presence of drug residues over two sampling periods during 2010, 2011 and 2012. Samples were collected from rural areas with and without farming activity and from urban areas. The 13 analytes were detected, and 18% of the samples collected showed positive results for the presence of at least one analyte. More collection sites were located in rural areas than in urban areas. However, more positive samples with higher concentrations and a larger number of analytes were detected in samples collected from sites located after the discharge of a WWTP. Results indicated that the WWTPs seems to act as a concentration point. Positive samples were also detected at a site located near a drinking water treatment plant.

Novel pollutants in the Moscow atmosphere in winter period: Gas chromatography-high resolution time-of-flight mass spectrometry study.

PubMed

Mazur, D M; Polyakova, O V; Artaev, V B; Lebedev, A T

2017-03-01

The most common mass spectrometry approach analyzing contamination of the environment deals with targeted analysis, i.e. detection and quantification of the selected (priority) pollutants. However non-targeted analysis is becoming more often the method of choice for environmental chemists. It involves implementation of modern analytical instrumentation allowing for comprehensive detection and identification of the wide variety of compounds of the environmental interest present in the sample, such as pharmaceuticals and their metabolites, musks, nanomaterials, perfluorinated compounds, hormones, disinfection by-products, flame retardants, personal care products, and many others emerging contaminants. The paper presents the results of detection and identification of previously unreported organic compounds in snow samples collected in Moscow in March 2016. The snow analysis allows evaluation of long-term air pollution in the winter period. Gas chromatography coupled to a high resolution time-of-flight mass spectrometer has enabled us with capability to detect and identify such novel analytes as iodinated compounds, polychlorinated anisoles and even Ni-containing organic complex, which are unexpected in environmental samples. Some considerations concerning the possible sources of origin of these compounds in the environment are discussed. Copyright © 2017 LECO. Published by Elsevier Ltd.. All rights reserved.

Stochastic sensing through covalent interactions

DOEpatents

Bayley, Hagan; Shin, Seong-Ho; Luchian, Tudor; Cheley, Stephen

2013-03-26

A system and method for stochastic sensing in which the analyte covalently bonds to the sensor element or an adaptor element. If such bonding is irreversible, the bond may be broken by a chemical reagent. The sensor element may be a protein, such as the engineered P.sub.SH type or .alpha.HL protein pore. The analyte may be any reactive analyte, including chemical weapons, environmental toxins and pharmaceuticals. The analyte covalently bonds to the sensor element to produce a detectable signal. Possible signals include change in electrical current, change in force, and change in fluorescence. Detection of the signal allows identification of the analyte and determination of its concentration in a sample solution. Multiple analytes present in the same solution may be detected.

Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

PubMed

Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

2014-12-01

An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection.

PubMed

Núñez, L; Turiel, E; Tadeo, J L

2007-04-06

A simple and rapid analytical method for the determination of nonylphenol (NP) and nonylphenol ethoxylates (NPEOx) in solid environmental samples has been developed. This method combines an ultrasonic-assisted extraction procedure in small columns and an enrichment step onto C(18) solid-phase extraction cartridges prior to separation using HPLC with fluorescence detection. Method optimization was carried out using soil samples fortified at different concentration levels (from 0.1 to 100 microg/g). Under optimum conditions, 2g of soil was placed in small glass columns and extraction was performed assisted by sonication (SAESC) at 45 degrees C in two consecutive steps of 15 min using a mixture of H(2)O/MeOH (30/70). The obtained extracts were collected, loaded onto 500 mg C(18) cartridges, and analytes were eluted with 3 x 1 ml of methanol and 1 ml of acetonitrile. Finally, sample extracts were evaporated under a nitrogen stream, redissolved in 500 microl H(2)O/AcN (50/50), and passed though a 0.45 microm nylon filter before final determination by HPLC-FL. The developed procedure allowed to achieve quantitative recoveries for NP and NPEOx, and was properly validated. Finally, the method was applied to the determination of these compounds in soils and other environmental solid samples such as sediments, compost and sludge.

Sample processing approach for detection of ricin in surface samples.

PubMed

Kane, Staci; Shah, Sanjiv; Erler, Anne Marie; Alfaro, Teneile

2017-12-01

With several ricin contamination incidents reported over the past decade, rapid and accurate methods are needed for environmental sample analysis, especially after decontamination. A sample processing method was developed for common surface sampling devices to improve the limit of detection and avoid false negative/positive results for ricin analysis. Potential assay interferents from the sample matrix (bleach residue, sample material, wetting buffer), including reference dust, were tested using a Time-Resolved Fluorescence (TRF) immunoassay. Test results suggested that the sample matrix did not cause the elevated background fluorescence sometimes observed when analyzing post-bleach decontamination samples from ricin incidents. Furthermore, sample particulates (80mg/mL Arizona Test Dust) did not enhance background fluorescence or interfere with ricin detection by TRF. These results suggested that high background fluorescence in this immunoassay could be due to labeled antibody quality and/or quantity issues. Centrifugal ultrafiltration devices were evaluated for ricin concentration as a part of sample processing. Up to 30-fold concentration of ricin was observed by the devices, which serve to remove soluble interferents and could function as the front-end sample processing step to other ricin analytical methods. The procedure has the potential to be used with a broader range of environmental sample types and with other potential interferences and to be followed by other ricin analytical methods, although additional verification studies would be required. Published by Elsevier B.V.

LC-MS/MS signal suppression effects in the analysis of pesticides in complex environmental matrices.

PubMed

Choi, B K; Hercules, D M; Gusev, A I

2001-02-01

The application of LC separation and mobile phase additives in addressing LC-MS/MS matrix signal suppression effects for the analysis of pesticides in a complex environmental matrix was investigated. It was shown that signal suppression is most significant for analytes eluting early in the LC-MS analysis. Introduction of different buffers (e.g. ammonium formate, ammonium hydroxide, formic acid) into the LC mobile phase was effective in improving signal correlation between the matrix and standard samples. The signal improvement is dependent on buffer concentration as well as LC separation of the matrix components. The application of LC separation alone was not effective in addressing suppression effects when characterizing complex matrix samples. Overloading of the LC column by matrix components was found to significantly contribute to analyte-matrix co-elution and suppression of signal. This signal suppression effect can be efficiently compensated by 2D LC (LC-LC) separation techniques. The effectiveness of buffers and LC separation in improving signal correlation between standard and matrix samples is discussed.

Some thoughts on problems associated with various sampling media used for environmental monitoring

USGS Publications Warehouse

Horowitz, A.J.

1997-01-01

Modern analytical instrumentation is capable of measuring a variety of trace elements at concentrations down into the single or double digit parts-per-trillion (ng l-1) range. This holds for the three most common sample media currently used in environmental monitoring programs: filtered water, whole-water and separated suspended sediment. Unfortunately, current analytical capabilities have exceeded the current capacity to collect both uncontaminated and representative environmental samples. The success of any trace element monitoring program requires that this issue be both understood and addressed. The environmental monitoring of trace elements requires the collection of calendar- and event-based dissolved and suspended sediment samples. There are unique problems associated with the collection and chemical analyses of both types of sample media. Over the past 10 years, reported ambient dissolved trace element concentrations have declined. Generally, these decreases do not reflect better water quality, but rather improvements in the procedures used to collect, process, preserve and analyze these samples without contaminating them during these steps. Further, recent studies have shown that the currently accepted operational definition of dissolved constituents (material passing a 0.45 ??m membrane filter) is inadequat owing to sampling and processing artifacts. The existence of these artifacts raises questions about the generation of accurate, precise and comparable 'dissolved' trace element data. Suspended sediment and associated trace elements can display marked short- and long-term spatial and temporal variability. This implies that spatially representative samples only can be obtained by generating composites using depth- and width-integrated sampling techniques. Additionally, temporal variations have led to the view that the determination of annual trace element fluxes may require nearly constant (e.g., high-frequency) sampling and subsequent chemical analyses. Ultimately, sampling frequency for flux estimates becomes dependent on the time period of concern (daily, weekly, monthly, yearly) and the amount of acceptable error associated with these estimates.

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

PubMed Central

Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

2016-01-01

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples. PMID:27924944

Pharmaceutical metabolites in the environment: analytical challenges and ecological risks.

PubMed

Celiz, Mary D; Tso, Jerry; Aga, Diana S

2009-12-01

The occurrence of human and veterinary pharmaceuticals in the environment has been a subject of concern for the past decade because many of these emerging contaminants have been shown to persist in soil and water. Although recent studies indicate that pharmaceutical contaminants can pose long-term ecological risks, many of the investigations regarding risk assessment have only considered the ecotoxicity of the parent drug, with very little attention given to the potential contributions that metabolites may have. The scarcity of available environmental data on the human metabolites excreted into the environment or the microbial metabolites formed during environmental biodegradation of pharmaceutical residues can be attributed to the difficulty in analyzing trace amounts of previously unknown compounds in complex sample matrices. However, with the advent of highly sensitive and powerful analytical instrumentations that have become available commercially, it is likely that an increased number of pharmaceutical metabolites will be identified and included in environmental risk assessment. The present study will present a critical review of available literature on pharmaceutical metabolites, primarily focusing on their analysis and toxicological significance. It is also intended to provide an overview on the recent advances in analytical tools and strategies to facilitate metabolite identification in environmental samples. This review aims to provide insight on what future directions might be taken to help scientists in this challenging task of enhancing the available data on the fate, behavior, and ecotoxicity of pharmaceutical metabolites in the environment.

Vortex-assisted magnetic β-cyclodextrin/attapulgite-linked ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the fast determination of four fungicides in water samples.

PubMed

Yang, Miyi; Xi, Xuefei; Wu, Xiaoling; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

2015-02-13

A novel microextraction technique combining magnetic solid-phase microextraction (MSPME) with ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) to determine four fungicides is presented in this work for the first time. The main factors affecting the extraction efficiency were optimized by the one-factor-at-a-time approach and the impacts of these factors were studied by an orthogonal design. Without tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimum conditions, good linearity and high enrichment factors were obtained for all analytes, with correlation coefficients ranging from 0.9998 to 1.0000 and enrichment factors ranging 135 and 159 folds. The recoveries for proposed approach were between 98% and 115%, the limits of detection were between 0.02 and 0.04 μg L(-1) and the RSDs changed from 2.96 to 4.16. The method was successfully applied in the analysis of four fungicides (azoxystrobin, chlorothalonil, cyprodinil and trifloxystrobin) in environmental water samples. The recoveries for the real water samples ranged between 81% and 109%. The procedure proved to be a time-saving, environmentally friendly, and efficient analytical technique. Copyright © 2015 Elsevier B.V. All rights reserved.

The Savannah River Site's Groundwater Monitoring Program: Second quarter 1992

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rogers, C.D.

1992-10-07

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site's (SRS) Groundwater Monitoring Program. During second quarter 1992, EPD/EMS conducted extensive sampling of monitoring wells. EPD/EMS established two sets of criteria to assist in the management of sample results. The flagging criteria do not define contamination levels; instead, they aid personnel in sample scheduling, interpretation of data, and trend identification. Since 1991, the flagging criteria have been based on the federal Environmental Protection Agency (EPA) drinking water standards and on method detection limits. A detailed explanation of the current flagging criteria is presented in the Flagging Criteria sectionmore » of this document. Analytical results from second quarter 1992 are listed in this report.« less

Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

PubMed

Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

2014-02-01

This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation. © 2013 Elsevier B.V. All rights reserved.

High Throughput Determination of Tetramine in Drinking ...

EPA Pesticide Factsheets

Report The sampling and analytical procedure (SAP) presented herein, describes a method for the high throughput determination of tetramethylene disulfotetramine in drinking water by solid phase extraction and isotope dilution gas chromatography/mass spectrometry. This method, which will be included in the SAM, is expected to provide the Water Laboratory Alliance, as part of EPA’s Environmental Response Laboratory Network, with a more reliable and faster means of analyte collection and measurement.

Environmental analysis of higher brominated diphenyl ethers and decabromodiphenyl ethane.

PubMed

Kierkegaard, Amelie; Sellström, Ulla; McLachlan, Michael S

2009-01-16

Methods for environmental analysis of higher brominated diphenyl ethers (PBDEs), in particular decabromodiphenyl ether (BDE209), and the recently discovered environmental contaminant decabromodiphenyl ethane (deBDethane) are reviewed. The extensive literature on analysis of BDE209 has identified several critical issues, including contamination of the sample, degradation of the analyte during sample preparation and GC analysis, and the selection of appropriate detection methods and surrogate standards. The limited experience with the analysis of deBDethane suggests that there are many commonalities with BDE209. The experience garnered from the analysis of BDE209 over the last 15 years will greatly facilitate progress in the analysis of deBDethane.

Development of Analytical Methods for Escort Herbicide in Forest Environment Samples

Treesearch

Joseph Fischer; Jerry Michael

1990-01-01

The USDA Forest Service laboratory in Auburn, Alabama, is engaged in research to determine the environmental fate and ecosystem inipadts of forestry herbicides. Much of the effort is associated with the conduct of field dissipation studies in which herbicides are applied to forest sites and then monitored over time in a variety of environmental matrices (soil, water,...

Reconnaissance-Level Assessment of Water Quality Near Flandreau, South Dakota

DTIC Science & Technology

2002-01-01

associations with adverse health effects have been established. Con- centrations of some selected analytes were less than U.S. Environmental ...unregulated synthetic organic compounds in aquatic environments . This study provides information concerning the occurrence of selected organic compounds...water sites. Selected data from various other investigations also are described. A total of 15 environmental samples, which included two sets of

The role of atomic fluorescence spectrometry in the automatic environmental monitoring of trace element analysis

PubMed Central

Stockwell, P. B.; Corns, W. T.

1993-01-01

Considerable attention has been drawn to the environmental levels of mercury, arsenic, selenium and antimony in the last decade. Legislative and environmental pressure has forced levels to be lowered and this has created an additional burden for analytical chemists. Not only does an analysis have to reach lower detection levels, but it also has to be seen to be correct. Atomic fluorescence detection, especially when coupled to vapour generation techniques, offers both sensitivity and specificity. Developments in the design of specified atomic fluorescence detectors for mercury, for the hydride-forming elements and also for cadmium, are described in this paper. Each of these systems is capable of analysing samples in the part per trillion (ppt) range reliably and economically. Several analytical applications are described. PMID:18924964

Test and Analysis Capabilities of the Space Environment Effects Team at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Finckenor, M. M.; Edwards, D. L.; Vaughn, J. A.; Schneider, T. A.; Hovater, M. A.; Hoppe, D. T.

2002-01-01

Marshall Space Flight Center has developed world-class space environmental effects testing facilities to simulate the space environment. The combined environmental effects test system exposes temperature-controlled samples to simultaneous protons, high- and low-energy electrons, vacuum ultraviolet (VUV) radiation, and near-ultraviolet (NUV) radiation. Separate chambers for studying the effects of NUV and VUV at elevated temperatures are also available. The Atomic Oxygen Beam Facility exposes samples to atomic oxygen of 5 eV energy to simulate low-Earth orbit (LEO). The LEO space plasma simulators are used to study current collection to biased spacecraft surfaces, arcing from insulators and electrical conductivity of materials. Plasma propulsion techniques are analyzed using the Marshall magnetic mirror system. The micro light gas gun simulates micrometeoroid and space debris impacts. Candidate materials and hardware for spacecraft can be evaluated for durability in the space environment with a variety of analytical techniques. Mass, solar absorptance, infrared emittance, transmission, reflectance, bidirectional reflectance distribution function, and surface morphology characterization can be performed. The data from the space environmental effects testing facilities, combined with analytical results from flight experiments, enable the Environmental Effects Group to determine optimum materials for use on spacecraft.

Standard reference materials (SRMs) for determination of organic contaminants in environmental samples.

PubMed

Wise, Stephen A; Poster, Dianne L; Kucklick, John R; Keller, Jennifer M; Vanderpol, Stacy S; Sander, Lane C; Schantz, Michele M

2006-10-01

For the past 25 years the National Institute of Standards and Technology (NIST) has developed certified reference materials (CRMs), known as standard reference materials (SRMs), for determination of organic contaminants in environmental matrices. Assignment of certified concentrations has usually been based on combining results from two or more independent analytical methods. The first-generation environmental-matrix SRMs were issued with certified concentrations for a limited number (5 to 10) of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs). Improvements in the analytical certification approach significantly expanded the number and classes of contaminants determined. Environmental-matrix SRMs currently available include air and diesel particulate matter, coal tar, marine and river sediment, mussel tissue, fish oil and tissue, and human serum, with concentrations typically assigned for 50 to 90 organic contaminants, for example PAHs, nitro-substituted PAHs, PCBs, chlorinated pesticides, and polybrominated diphenyl ethers (PBDEs).

Rapid detection of terbufos in stomach contents using desorption electrospray ionization mass spectrometry.

PubMed

Wilson, Christina R; Mulligan, Christopher C; Strueh, Kurt D; Stevenson, Gregory W; Hooser, Stephen B

2014-05-01

Desorption electrospray ionization mass spectrometry (DESI-MS) is an emerging analytical technique that permits the rapid and direct analysis of biological or environmental samples under ambient conditions. Highlighting the versatility of this technique, DESI-MS has been used for the rapid detection of illicit drugs, chemical warfare agents, agricultural chemicals, and pharmaceuticals from a variety of sample matrices. In diagnostic veterinary toxicology, analyzing samples using traditional analytical instrumentation typically includes extensive sample extraction procedures, which can be time consuming and labor intensive. Therefore, efforts to expedite sample analyses are a constant goal for diagnostic toxicology laboratories. In the current report, DESI-MS was used to directly analyze stomach contents from a dog exposed to the organophosphate insecticide terbufos. The total DESI-MS analysis time required to confirm the presence of terbufos and diagnose organophosphate poisoning in this case was approximately 5 min. This highlights the potential of this analytical technique in the field of veterinary toxicology for the rapid diagnosis and detection of toxicants in biological samples. © 2014 The Author(s).

Inorganic chemical analysis of environmental materials—A lecture series

USGS Publications Warehouse

Crock, J.G.; Lamothe, P.J.

2011-01-01

At the request of the faculty of the Colorado School of Mines, Golden, Colorado, the authors prepared and presented a lecture series to the students of a graduate level advanced instrumental analysis class. The slides and text presented in this report are a compilation and condensation of this series of lectures. The purpose of this report is to present the slides and notes and to emphasize the thought processes that should be used by a scientist submitting samples for analyses in order to procure analytical data to answer a research question. First and foremost, the analytical data generated can be no better than the samples submitted. The questions to be answered must first be well defined and the appropriate samples collected from the population that will answer the question. The proper methods of analysis, including proper sample preparation and digestion techniques, must then be applied. Care must be taken to achieve the required limits of detection of the critical analytes to yield detectable analyte concentration (above "action" levels) for the majority of the study's samples and to address what portion of those analytes answer the research question-total or partial concentrations. To guarantee a robust analytical result that answers the research question(s), a well-defined quality assurance and quality control (QA/QC) plan must be employed. This QA/QC plan must include the collection and analysis of field and laboratory blanks, sample duplicates, and matrix-matched standard reference materials (SRMs). The proper SRMs may include in-house materials and/or a selection of widely available commercial materials. A discussion of the preparation and applicability of in-house reference materials is also presented. Only when all these analytical issues are sufficiently addressed can the research questions be answered with known certainty.

Applications of derivatization reactions to trace organic compounds during sample preparation based on pressurized liquid extraction.

PubMed

Carro, Antonia M; González, Paula; Lorenzo, Rosa A

2013-06-28

Pressurized liquid extraction (PLE) is an exhaustive technique used for the extraction of analytes from solid samples. Temperature, pressure, solvent type and volume, and the addition of other reagents notably influence the efficiency of the extraction. The analytical applications of this technique can be improved by coupling with appropriate derivatization reactions. The aim of this review is to discuss the recent applications of the sequential combination of PLE with derivatization and the approaches that involve simultaneous extraction and in situ derivatization. The potential of the latest developments to the trace analysis of environmental, food and biological samples is also analyzed. Copyright © 2013 Elsevier B.V. All rights reserved.

Rugged large volume injection for sensitive capillary LC-MS environmental monitoring

NASA Astrophysics Data System (ADS)

Roberg-Larsen, Hanne; Abele, Silvija; Demir, Deniz; Dzabijeva, Diana; Amundsen, Sunniva F.; Wilson, Steven R.; Bartkevics, Vadims; Lundanes, Elsa

2017-08-01

A rugged and high throughput capillary column (cLC) LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL) solid phase extraction (SPE) for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g. injection of 100 non-filtrated water samples would did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 µm). In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for environmental water samples was demonstrated with various pharmaceutical products, which had detection limits (LOD) in the 0.05 - 12.5 ng/L range. Between-day and within-day repeatability of selected analytes were < 20% RSD.

Guidance for Data Useability in Risk Assessment (Part B-4), Final, May, 1992

EPA Pesticide Factsheets

This chapter provides guidance to the RPM and the risk assessor for designing an effective sampling plan and selecting suitable analytical methods to collect environmental data for use in baseline risk assessments.

Field comparison of analytical results from discrete-depth ground water samplers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zemo, D.A.; Delfino, T.A.; Gallinatti, J.D.

1995-07-01

Discrete-depth ground water samplers are used during environmental screening investigations to collect ground water samples in lieu of installing and sampling monitoring wells. Two of the most commonly used samplers are the BAT Enviroprobe and the QED HydroPunch I, which rely on differing sample collection mechanics. Although these devices have been on the market for several years, it was unknown what, if any, effect the differences would have on analytical results for ground water samples containing low to moderate concentrations of chlorinated volatile organic compounds (VOCs). This study investigated whether the discrete-depth ground water sampler used introduces statistically significant differencesmore » in analytical results. The goal was to provide a technical basis for allowing the two devices to be used interchangeably during screening investigations. Because this study was based on field samples, it included several sources of potential variability. It was necessary to separate differences due to sampler type from variability due to sampling location, sample handling, and laboratory analytical error. To statistically evaluate these sources of variability, the experiment was arranged in a nested design. Sixteen ground water samples were collected from eight random locations within a 15-foot by 15-foot grid. The grid was located in an area where shallow ground water was believed to be uniformly affected by VOCs. The data were evaluated using analysis of variance.« less

Steroid hormones in environmental matrices: extraction method comparison.

PubMed

Andaluri, Gangadhar; Suri, Rominder P S; Graham, Kendon

2017-11-09

The U.S. Environmental Protection Agency (EPA) has developed methods for the analysis of steroid hormones in water, soil, sediment, and municipal biosolids by HRGC/HRMS (EPA Method 1698). Following the guidelines provided in US-EPA Method 1698, the extraction methods were validated with reagent water and applied to municipal wastewater, surface water, and municipal biosolids using GC/MS/MS for the analysis of nine most commonly detected steroid hormones. This is the first reported comparison of the separatory funnel extraction (SFE), continuous liquid-liquid extraction (CLLE), and Soxhlet extraction methods developed by the U.S. EPA. Furthermore, a solid phase extraction (SPE) method was also developed in-house for the extraction of steroid hormones from aquatic environmental samples. This study provides valuable information regarding the robustness of the different extraction methods. Statistical analysis of the data showed that SPE-based methods provided better recovery efficiencies and lower variability of the steroid hormones followed by SFE. The analytical methods developed in-house for extraction of biosolids showed a wide recovery range; however, the variability was low (≤ 7% RSD). Soxhlet extraction and CLLE are lengthy procedures and have been shown to provide highly variably recovery efficiencies. The results of this study are guidance for better sample preparation strategies in analytical methods for steroid hormone analysis, and SPE adds to the choice in environmental sample analysis.

Glow discharge spectrometry for the characterization of nuclear and radioactively contaminated environmental samples

NASA Astrophysics Data System (ADS)

Betti, Maria; Aldave de las Heras, Laura

2004-09-01

Glow discharge (GD) spectrometry as applied to characterize nuclear samples as well as for the determination of radionuclides in environmental samples is reviewed. The use of instrumentation for direct current (d.c.) glow discharge mass spectrometry (GDMS) and radio frequency glow discharge optical emission spectrometry (rf GDOES), installed inside a glove-box for the handling of radioactive samples as well as the two installations and their analytical possibilities, is described in detail. The applications of GD techniques for the characterization of samples of nuclear concern both with respect to their major and trace elements, as well as to the matrix isotopic composition are presented. Procedures for quantitative determination of major, minor, and trace elements in conductive samples are reported. As for non-conductive samples three different approaches for their measurement can be followed. Namely, the use of rf sources, the mixing of the sample with a binder conducting host matrix, and the use of a secondary cathode. In the case of oxide-based samples, the employment of a tantalum secondary cathode, acting as an oxygen getter, reduces the availability of oxygen to form polyatomic species and to produce quenching. Considerations on the use of the relative sensitivity factors (RSFs) in different matrices are reported. The analytical capabilities of GDMS are compared with ICP-MS in terms of accuracy, precision, and detection limit for the determination of trace elements in uranium oxide specimens. As for the determination of isotopic composition, GDMS was found to be competitive with thermal ionisation mass spectrometry (TIMS) as well as for bulk determinations of major elements with titration methods. Applications of GDMS to the determination of radioisotopes in environmental samples, as well for depth profiling of trace elements in oxide layers, are discussed.

Role of microextraction sampling procedures in forensic toxicology.

PubMed

Barroso, Mário; Moreno, Ivo; da Fonseca, Beatriz; Queiroz, João António; Gallardo, Eugenia

2012-07-01

The last two decades have provided analysts with more sensitive technology, enabling scientists from all analytical fields to see what they were not able to see just a few years ago. This increased sensitivity has allowed drug detection at very low concentrations and testing in unconventional samples (e.g., hair, oral fluid and sweat), where despite having low analyte concentrations has also led to a reduction in sample size. Along with this reduction, and as a result of the use of excessive amounts of potentially toxic organic solvents (with the subsequent environmental pollution and costs associated with their proper disposal), there has been a growing tendency to use miniaturized sampling techniques. Those sampling procedures allow reducing organic solvent consumption to a minimum and at the same time provide a rapid, simple and cost-effective approach. In addition, it is possible to get at least some degree of automation when using these techniques, which will enhance sample throughput. Those miniaturized sample preparation techniques may be roughly categorized in solid-phase and liquid-phase microextraction, depending on the nature of the analyte. This paper reviews recently published literature on the use of microextraction sampling procedures, with a special focus on the field of forensic toxicology.

DOE Office of Scientific and Technical Information (OSTI.GOV)

King, A.G.

The Pacific Northwest Laboratory (PNL)/Analytical Chemistry Laboratory (ACL) and the Westinghouse Hanford Company (WHC)/Process Analytical Laboratory (PAL) provide analytical support services to various environmental restoration and waste management projects/programs at Hanford. In response to a US Department of Energy -- Richland Field Office (DOE-RL) audit, which questioned the comparability of analytical methods employed at each laboratory, the Sample Exchange/Exchange (SEE) program was initiated. The SEE Program is a selfassessment program designed to compare analytical methods of the PAL and ACL laboratories using sitespecific waste material. The SEE program is managed by a collaborative, the Quality Assurance Triad (Triad). Triad membershipmore » is made up of representatives from the WHC/PAL, PNL/ACL, and WHC Hanford Analytical Services Management (HASM) organizations. The Triad works together to design/evaluate/implement each phase of the SEE Program.« less

Improvements to sample processing and measurement to enable more widespread environmental application of tritium.

PubMed

Moran, James; Alexander, Thomas; Aalseth, Craig; Back, Henning; Mace, Emily; Overman, Cory; Seifert, Allen; Freeburg, Wilcox

2017-08-01

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. We identify a current quantification limit of 92.2 TU which, combined with our small sample sizes, correlates to as little as 0.00133Bq of total T activity. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of both natural and artificial T behavior in the environment. Copyright © 2017. Published by Elsevier Ltd.

Improvements to sample processing and measurement to enable more widespread environmental application of tritium

DOE PAGES

Moran, James; Alexander, Thomas; Aalseth, Craig; ...

2017-01-26

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. Here, we present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120 mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. We also identify a current quantification limit of 92.2 TU which, combined with our small sample sizes, correlates to as little as 0.00133 Bq of total T activity. Furthermore, this enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps inmore » our understanding of both natural and artificial T behavior in the environment.« less

Miniaturized Temperature-Controlled Planar Chromatography (Micro-TLC) as a Versatile Technique for Fast Screening of Micropollutants and Biomarkers Derived from Surface Water Ecosystems and During Technological Processes of Wastewater Treatment.

PubMed

Ślączka-Wilk, Magdalena M; Włodarczyk, Elżbieta; Kaleniecka, Aleksandra; Zarzycki, Paweł K

2017-07-01

There is increasing interest in the development of simple analytical systems enabling the fast screening of target components in complex samples. A number of newly invented protocols are based on quasi separation techniques involving microfluidic paper-based analytical devices and/or micro total analysis systems. Under such conditions, the quantification of target components can be performed mainly due to selective detection. The main goal of this paper is to demonstrate that miniaturized planar chromatography has the capability to work as an efficient separation and quantification tool for the analysis of multiple targets within complex environmental samples isolated and concentrated using an optimized SPE method. In particular, we analyzed various samples collected from surface water ecosystems (lakes, rivers, and the Baltic Sea of Middle Pomerania in the northern part of Poland) in different seasons, as well as samples collected during key wastewater technological processes (originating from the "Jamno" wastewater treatment plant in Koszalin, Poland). We documented that the multiple detection of chromatographic spots on RP-18W microplates-under visible light, fluorescence, and fluorescence quenching conditions, and using the visualization reagent phosphomolybdic acid-enables fast and robust sample classification. The presented data reveal that the proposed micro-TLC system is useful, inexpensive, and can be considered as a complementary method for the fast control of treated sewage water discharged by a municipal wastewater treatment plant, particularly for the detection of low-molecular mass micropollutants with polarity ranging from estetrol to progesterone, as well as chlorophyll-related dyes. Due to the low consumption of mobile phases composed of water-alcohol binary mixtures (less than 1 mL/run for the simultaneous separation of up to nine samples), this method can be considered an environmentally friendly and green chemistry analytical tool. The described analytical protocol can be complementary to those involving classical column chromatography (HPLC) or various planar microfluidic devices.

In vitro bioassays for detecting dioxin-like activity--application potentials and limits of detection, a review.

PubMed

Eichbaum, Kathrin; Brinkmann, Markus; Buchinger, Sebastian; Reifferscheid, Georg; Hecker, Markus; Giesy, John P; Engwall, Magnus; van Bavel, Bert; Hollert, Henner

2014-07-15

Use of in vitro assays as screening tool to characterize contamination of a variety of environmental matrices has become an increasingly popular and powerful toolbox in the field of environmental toxicology. While bioassays cannot entirely substitute analytical methods such as gas chromatography-mass spectrometry (GC-MS), the increasing improvement of cell lines and standardization of bioassay procedures enhance their utility as bioanalytical pre-screening tests prior to more targeted chemical analytical investigations. Dioxin-receptor-based assays provide a holistic characterization of exposure to dioxin-like compounds (DLCs) by integrating their overall toxic potential, including potentials of unknown DLCs not detectable via e.g. GC-MS. Hence, they provide important additional information with respect to environmental risk assessment of DLCs. This review summarizes different in vitro bioassay applications for detection of DLCs and considers the comparability of bioassay and chemical analytically derived toxicity equivalents (TEQs) of different approaches and various matrices. These range from complex samples such as sediments through single reference to compound mixtures. A summary of bioassay derived detection limits (LODs) showed a number of current bioassays to be equally sensitive as chemical methodologies, but moreover revealed that most of the bioanalytical studies conducted to date did not report their LODs, which represents a limitation with regard to low potency samples. Copyright © 2014 Elsevier B.V. All rights reserved.

EPA Contract Laboratory Program Statement of Work for Inorganic Superfund Methods Multi-Media, Multi-Concentration ISM02.3

EPA Pesticide Factsheets

This document contains analytical methods for the analysis of metals and cyanide in environmental samples. It also contains contractual requirements for laboratories participating in Superfund's Contract Laboratory Program.

EPA Contract Laboratory Program Statement of Work for Inorganic Superfund Methods Multi-Media, Multi-Concentration ISM02.4

EPA Pesticide Factsheets

This document contains analytical methods for the analysis of metals and cyanide in environmental samples. It also contains contractual requirements for laboratories participating in Superfund's Contract Laboratory Program.

Ionic liquid-based ultrasound-assisted emulsification microextraction coupled with high performance liquid chromatography for the determination of four fungicides in environmental water samples.

PubMed

Liang, Pei; Wang, Fang; Wan, Qin

2013-02-15

A highly efficient and environmentally friendly sample preparation method termed ionic liquid-based ultrasound-assisted emulsification microextraction (IL-USAEME) combined with high performance liquid chromatography has been developed for the determination of four fungicides (azoxystrobin, diethofencarb, pyrimethanil and kresoxim-methyl) in water samples. In this novel approach, ionic liquid (IL) was used as extraction solvent in place of the organic solvent used in conventional USAEME assay, and there is no need for using organic dispersive solvent which is typically required in the common dispersive liquid-liquid microextraction method. Various parameters that affect the extraction efficiency, such as the kind and volume of IL, ultrasound emulsification time, extraction temperature and salt addition were investigated and optimized. Under the optimum extraction condition, the linearities of calibration curves were in the range from 3 to 5000 ng mL(-1) for target analytes with the correlation coefficient higher than 0.9992. The enrichment factors and the limits of detection were in the range of 88-137 and 0.73-2.2 ng mL(-1), depending on the analytes. The environmental water samples were successfully analyzed using the proposed method, and the relative recoveries at fortified levels of 50 and 100 ng mL(-1) were in the range of 83.9%-116.2%. Copyright © 2012 Elsevier B.V. All rights reserved.

Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations.

PubMed

Soylak, Mustafa; Erdogan, Nilgun D

2006-09-21

A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 microg/l for iron-3.4 microg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey.

Sampling and monitoring for the mine life cycle

USGS Publications Warehouse

McLemore, Virginia T.; Smith, Kathleen S.; Russell, Carol C.

2014-01-01

Sampling and Monitoring for the Mine Life Cycle provides an overview of sampling for environmental purposes and monitoring of environmentally relevant variables at mining sites. It focuses on environmental sampling and monitoring of surface water, and also considers groundwater, process water streams, rock, soil, and other media including air and biological organisms. The handbook includes an appendix of technical summaries written by subject-matter experts that describe field measurements, collection methods, and analytical techniques and procedures relevant to environmental sampling and monitoring.The sixth of a series of handbooks on technologies for management of metal mine and metallurgical process drainage, this handbook supplements and enhances current literature and provides an awareness of the critical components and complexities involved in environmental sampling and monitoring at the mine site. It differs from most information sources by providing an approach to address all types of mining influenced water and other sampling media throughout the mine life cycle.Sampling and Monitoring for the Mine Life Cycle is organized into a main text and six appendices that are an integral part of the handbook. Sidebars and illustrations are included to provide additional detail about important concepts, to present examples and brief case studies, and to suggest resources for further information. Extensive references are included.

Selective pressurized liquid extraction of replacement and legacy brominated flame retardants from soil.

PubMed

McGrath, Thomas J; Morrison, Paul D; Ball, Andrew S; Clarke, Bradley O

2016-08-05

Polybrominated diphenyl ethers (PBDEs) are a class of flame retardant registered as UN POPs due to their persistence in the environment, bioaccumulation potential and toxicity. Replacement novel brominated flame retardants (NBFRs) have exhibited similar health hazards and environmental distribution, becoming recognized as significant contaminants. This work describes the development and validation of a sensitive and reliable method for the simultaneous quantitation of PBDEs and NBFRs in environmental soil samples using selective pressurized liquid extraction (S-PLE) and gas chromatography coupled to triple quadrupole mass spectrometry (GC-(EI)-MS/MS). Under optimal conditions, extraction of eight PBDEs (-28, -47, -99, -100, -153, -154, -183 and -209) and five NBFRs; pentabromotoluene (PBT), pentabromoethylbenzene (PBEB), hexabromobenzene (HBB), 2-ethylhexyl-2,3,4,5-tetrabromobenzoate (EH-TBB) and bis(2,4,6-tribromophenoxy)ethane (BTBPE) was performed at 100°C and 1500psi using a 1:1 mixture of hexane and dichloromethane. The method utilized 33mL capacity PLE cells containing, from bottom to top, a single cellulose filter, 3g activated Florisil, 6g acid silica (10% w/w), 3g Na2SO4, another cellulose filter, 2g activated copper powder and 3g soil sample dispersed in 2g Na2SO4 and 1g of Hydromatrix. The method was evaluated by repeated extraction and analysis of all analytes from 3g soil at three spike concentrations. Good recoveries were observed for most analytes at each of the spiking levels with RSD values generally below 20%. MDLs ranged from 0.01 to 4.8ng/g dw for PBDEs and 0.01-0.55ng/g dw for NBFRs. The described one-step combined extraction and cleanup method reduces sample processing times compared with traditional procedures, while delivering comparable analytical performance. The method was successfully applied to environmental soil samples (n=5), detecting PBDEs in each sample and providing the first account of NBFR contamination in Australian soils. Copyright © 2016 Elsevier B.V. All rights reserved.

Estimating the uncertainty from sampling in pollution crime investigation: The importance of metrology in the forensic interpretation of environmental data.

PubMed

Barazzetti Barbieri, Cristina; de Souza Sarkis, Jorge Eduardo

2018-07-01

The forensic interpretation of environmental analytical data is usually challenging due to the high geospatial variability of these data. The measurements' uncertainty includes contributions from the sampling and from the sample handling and preparation processes. These contributions are often disregarded in analytical techniques results' quality assurance. A pollution crime investigation case was used to carry out a methodology able to address these uncertainties in two different environmental compartments, freshwater sediments and landfill leachate. The methodology used to estimate the uncertainty was the duplicate method (that replicates predefined steps of the measurement procedure in order to assess its precision) and the parameters used to investigate the pollution were metals (Cr, Cu, Ni, and Zn) in the leachate, the suspect source, and in the sediment, the possible sink. The metal analysis results were compared to statutory limits and it was demonstrated that Cr and Ni concentrations in sediment samples exceeded the threshold levels at all sites downstream the pollution sources, considering the expanded uncertainty U of the measurements and a probability of contamination >0.975, at most sites. Cu and Zn concentrations were above the statutory limits at two sites, but the classification was inconclusive considering the uncertainties of the measurements. Metal analyses in leachate revealed that Cr concentrations were above the statutory limits with a probability of contamination >0.975 in all leachate ponds while the Cu, Ni and Zn probability of contamination was below 0.025. The results demonstrated that the estimation of the sampling uncertainty, which was the dominant component of the combined uncertainty, is required for a comprehensive interpretation of the environmental analyses results, particularly in forensic cases. Copyright © 2018 Elsevier B.V. All rights reserved.

Trends in hard X-ray fluorescence mapping: environmental applications in the age of fast detectors.

PubMed

Lombi, E; de Jonge, M D; Donner, E; Ryan, C G; Paterson, D

2011-06-01

Environmental samples are extremely diverse but share a tendency for heterogeneity and complexity. This heterogeneity poses methodological challenges when investigating biogeochemical processes. In recent years, the development of analytical tools capable of probing element distribution and speciation at the microscale have allowed this challenge to be addressed. Of these available tools, laterally resolved synchrotron techniques such as X-ray fluorescence mapping are key methods for the in situ investigation of micronutrients and inorganic contaminants in environmental samples. This article demonstrates how recent advances in X-ray fluorescence detector technology are bringing new possibilities to environmental research. Fast detectors are helping to circumvent major issues such as X-ray beam damage of hydrated samples, as dwell times during scanning are reduced. They are also helping to reduce temporal beamtime requirements, making particularly time-consuming techniques such as micro X-ray fluorescence (μXRF) tomography increasingly feasible. This article focuses on μXRF mapping of nutrients and metalloids in environmental samples, and suggests that the current divide between mapping and speciation techniques will be increasingly blurred by the development of combined approaches.

STATISTICAL ANALYSIS OF TANK 5 FLOOR SAMPLE RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, E.

2012-03-14

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primarymore » sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, radionuclide, inorganic, and anion concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed in Appendix A, and the results of this analysis are reported in Appendix B. The data were generally found to follow a normal distribution, and to be homogeneous across composite samples.« less

Statistical Analysis of Tank 5 Floor Sample Results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, E. P.

2013-01-31

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primarymore » sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide1, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed, and the results of this analysis are reported. The data were generally found to follow a normal distribution, and to be homogenous across composite samples.« less

Statistical Analysis Of Tank 5 Floor Sample Results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, E. P.

2012-08-01

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primarymore » sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed in Appendix A, and the results of this analysis are reported in Appendix B. The data were generally found to follow a normal distribution, and to be homogenous across composite samples.« less

Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

PubMed

Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

2017-03-10

This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

An Undergraduate Field Experiment for Measuring Exposure to Environmental Tobacco Smoke in Indoor Environments

NASA Astrophysics Data System (ADS)

Marsella, Adam M.; Huang, Jiping; Ellis, David A.; Mabury, Scott A.

1999-12-01

An undergraduate field experiment is described for the measurement of nicotine and various carbonyl compounds arising from environmental tobacco smoke. Students are introduced to practical techniques in HPLC-UV and GC-NPD. Also introduced are current methods in personal air sampling using small and portable field sampling pumps. Carbonyls (formaldehyde, acetaldehyde, acrolein, and acetone) are sampled with silica solid-phase extraction cartridges impregnated with 2,4-dinitrophenylhydrazine, eluted, and analyzed by HPLC-UV (360-380 nm). Nicotine is sampled using XAD-2 cartridges, extracted, and analyzed by GC-NPD. Students gain an appreciation for the problems associated with measuring ubiquitous pollutants such as formaldehyde, as well as the issue of chromatographic peak resolution when trying to resolve closely eluting peaks. By allowing the students to formulate their own hypothesis and sampling scheme, critical thinking and problem solving are developed in addition to analysis skills. As an experiment in analytical environmental chemistry, this laboratory introduces the application of field sampling and analysis techniques to the undergraduate lab.

Large outbreak of salmonella phage type 1 infection with high infection rate and severe illness associated with fast food premises.

PubMed

Giraudon, I; Cathcart, S; Blomqvist, S; Littleton, A; Surman-Lee, S; Mifsud, A; Anaraki, S; Fraser, G

2009-06-01

To describe the epidemiology of an outbreak of Salmonella enteritidis phage type 1 (PT1) infection associated with a fast food premises, and to identify the causative factors leading to an acute outbreak with high attack rate and severe illness including hospital admission. Integrated descriptive study of epidemiology, food and environmental microbiology, and professional environmental health assessment, supplemented by a case-case analytical study. Cases were identified through multiple sources and were interviewed to identify food items consumed. Descriptive epidemiology of all cases and a case-case analytical study of risk factors for severe illness were undertaken. Microbiological investigation included analysis and typing of pathogens from stools, blood and environmental surfaces. Professional environmental heath assessment of the premises was undertaken. S. enteritidis PT1 was recovered from two-thirds of faecal samples. Three cases had dual infection with enterotoxin-producing Clostridium perfringens. S. enteritidis PT1 was isolated from 14 of 40 food samples examined and C. perfringens was isolated from eight food samples. Environmental health inspection of the premises revealed multiple deficiencies, including deficits in food preparation and hygiene consistent with multiple cross-contamination, and time-temperature abuse of sauces widely used across menu items. Severe cases were associated with consumption of chips and salad. Outbreaks from fast food premises have been infrequently described. This outbreak demonstrates the potential for fast food premises, with multiple deficiencies in food preparation and hygiene, to produce large, intense community outbreaks with high attack rates and severe illness, highly confined in space and time.

Analytical method development for the determination of emerging contaminants in water using supercritical-fluid chromatography coupled with diode-array detection.

PubMed

Del Carmen Salvatierra-Stamp, Vilma; Ceballos-Magaña, Silvia G; Gonzalez, Jorge; Ibarra-Galván, Valentin; Muñiz-Valencia, Roberto

2015-05-01

An analytical method using supercritical-fluid chromatography coupled with diode-array detection for the determination of seven emerging contaminants-two pharmaceuticals (carbamazepine and glyburide), three endocrine disruptors (17α-ethinyl estradiol, bisphenol A, and 17β-estradiol), one bactericide (triclosan), and one pesticide (diuron)-was developed and validated. These contaminants were chosen because of their frequency of use and their toxic effects on both humans and the environment. The optimized chromatographic separation on a Viridis BEH 2-EP column achieved baseline resolution for all compounds in less than 10 min. This separation was applied to environmental water samples after sample preparation. The optimized sample treatment involved a preconcentration step by means of solid-phase extraction using C18-OH cartridges. The proposed method was validated, finding recoveries higher than 94 % and limits of detection and limits of quantification in the range of 0.10-1.59 μg L(-1) and 0.31-4.83 μg L(-1), respectively. Method validation established the proposed method to be selective, linear, accurate, and precise. Finally, the method was successfully applied to environmental water samples.

A sustainable on-line CapLC method for quantifying antifouling agents like irgarol-1051 and diuron in water samples: Estimation of the carbon footprint.

PubMed

Pla-Tolós, J; Serra-Mora, P; Hakobyan, L; Molins-Legua, C; Moliner-Martinez, Y; Campins-Falcó, P

2016-11-01

In this work, in-tube solid phase microextraction (in-tube SPME) coupled to capillary LC (CapLC) with diode array detection has been reported, for on-line extraction and enrichment of booster biocides (irgarol-1051 and diuron) included in Water Frame Directive 2013/39/UE (WFD). The analytical performance has been successfully demonstrated. Furthermore, in the present work, the environmental friendliness of the procedure has been quantified by means of the implementation of the carbon footprint calculation of the analytical procedure and the comparison with other methodologies previously reported. Under the optimum conditions, the method presents good linearity over the range assayed, 0.05-10μg/L for irgarol-1051 and 0.7-10μg/L for diuron. The LODs were 0.015μg/L and 0.2μg/L for irgarol-1051 and diuron, respectively. Precision was also satisfactory (relative standard deviation, RSD<3.5%). The proposed methodology was applied to monitor water samples, taking into account the EQS standards for these compounds. The carbon footprint values for the proposed procedure consolidate the operational efficiency (analytical and environmental performance) of in-tube SPME-CapLC-DAD, in general, and in particular for determining irgarol-1051 and diuron in water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Multifunctional Au NPs-polydopamine-polyvinylidene fluoride membrane chips as probe for enrichment and rapid detection of organic contaminants.

PubMed

Wang, Saihua; Niu, Hongyun; Cai, Yaqi; Cao, Dong

2018-05-01

High-throughput and rapid detection of hazardous compounds in complicated samples is essential for the solution of environmental problems. We have prepared a "pH-paper-like" chip which can rapidly "indicate" the occurrence of organic contaminants just through dipping the chip in water samples for short time followed by fast analysis with surface-assisted laser desorption/ionization time-of-flight mass spectrometry (SALDI-TOF MS). The chips are composed of polyvinylidene fluoride membrane (PVDFM), polydopamine (PDA) film and Au nanoparticles (Au NPs), which are layer-by-layer assembled according to the adhesion, self-polymerization and reduction property of dopamine. In the Au NPs loaded polydopamine-polyvinylidene fluoride membrane (Au NPs-PDA-PVDFM) chips, PVDFM combined with PDA film are responsible for the enrichment of organic analyte through hydrophobic interactions and π-π stacking; Au NPs serve as effective SALDI matrix for the rapid detection of target analyte. After dipping into water solution for minutes, the Au-PDA-PVDFM chips with enriched organic analytes can be detected directly with SALDI-TOF MS. The good solid-phase extraction performance of the PDA-PVDFM components, remarkable matrix effect of the loaded AuNPs, and sensitivity of the SALDI-TOF MS technique ensure excellent sensitivity and reproducibility for the quantification of trace levels of organic contaminants in environmental water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Geographic Clustering of Cardiometabolic Risk Factors in Metropolitan Centres in France and Australia

PubMed Central

Paquet, Catherine; Chaix, Basile; Howard, Natasha J.; Coffee, Neil T.; Adams, Robert J.; Taylor, Anne W.; Thomas, Frédérique; Daniel, Mark

2016-01-01

Understanding how health outcomes are spatially distributed represents a first step in investigating the scale and nature of environmental influences on health and has important implications for statistical power and analytic efficiency. Using Australian and French cohort data, this study aimed to describe and compare the extent of geographic variation, and the implications for analytic efficiency, across geographic units, countries and a range of cardiometabolic parameters (Body Mass Index (BMI) waist circumference, blood pressure, resting heart rate, triglycerides, cholesterol, glucose, HbA1c). Geographic clustering was assessed using Intra-Class Correlation (ICC) coefficients in biomedical cohorts from Adelaide (Australia, n = 3893) and Paris (France, n = 6430) for eight geographic administrative units. The median ICC was 0.01 suggesting 1% of risk factor variance attributable to variation between geographic units. Clustering differed by cardiometabolic parameters, administrative units and countries and was greatest for BMI and resting heart rate in the French sample, HbA1c in the Australian sample, and for smaller geographic units. Analytic inefficiency due to clustering was greatest for geographic units in which participants were nested in fewer, larger geographic units. Differences observed in geographic clustering across risk factors have implications for choice of geographic unit in sampling and analysis, and highlight potential cross-country differences in the distribution, or role, of environmental features related to cardiometabolic health. PMID:27213423

Optimizing liquid effluent monitoring at a large nuclear complex.

PubMed

Chou, Charissa J; Barnett, D Brent; Johnson, Vernon G; Olson, Phil M

2003-12-01

Effluent monitoring typically requires a large number of analytes and samples during the initial or startup phase of a facility. Once a baseline is established, the analyte list and sampling frequency may be reduced. Although there is a large body of literature relevant to the initial design, few, if any, published papers exist on updating established effluent monitoring programs. This paper statistically evaluates four years of baseline data to optimize the liquid effluent monitoring efficiency of a centralized waste treatment and disposal facility at a large defense nuclear complex. Specific objectives were to: (1) assess temporal variability in analyte concentrations, (2) determine operational factors contributing to waste stream variability, (3) assess the probability of exceeding permit limits, and (4) streamline the sampling and analysis regime. Results indicated that the probability of exceeding permit limits was one in a million under normal facility operating conditions, sampling frequency could be reduced, and several analytes could be eliminated. Furthermore, indicators such as gross alpha and gross beta measurements could be used in lieu of more expensive specific isotopic analyses (radium, cesium-137, and strontium-90) for routine monitoring. Study results were used by the state regulatory agency to modify monitoring requirements for a new discharge permit, resulting in an annual cost savings of US dollars 223,000. This case study demonstrates that statistical evaluation of effluent contaminant variability coupled with process knowledge can help plant managers and regulators streamline analyte lists and sampling frequencies based on detection history and environmental risk.

Focused Feasibility Study Final Field Sampling Plan

DTIC Science & Technology

1993-10-01

baseline of groundwater chemistry prior to commencing additional environmental investigations of the area. Work for Phase I of the FFS is designed lo...investigations and remedial feasibility investigations at Beach Point. The groundwater data will also be used to aid in the design of any groundwater extraction...approved laboratories. The analytical data will be the equivalent of EPA Level IV data. This level of data quality has been established for environmental

EPA Method 200.8: Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry

EPA Pesticide Factsheets

\\tEPA’s Selected Analytical Methods for Environmental Remediation and Recovery (SAM) lists this method for preparation and analysis of drinking water samples to detect and measure compounds containing arsenic, thallium and vanadium.

EVALUATION OF COMPUTER-CONTROLLED SCANNING ELECTRON MICROSCOPY APPLIED TO AN AMBIENT URBAN AEROSOL SAMPLE

EPA Science Inventory

Concerns about the environmental and public health effects of particulate matter (PM) have stimulated interest in analytical techniques capable of measuring the size and chemical composition of individual aerosol particles. Computer-controlled scanning electron microscopy (CCSE...

Fast identification of microplastics in complex environmental samples by a thermal degradation method.

PubMed

Dümichen, Erik; Eisentraut, Paul; Bannick, Claus Gerhard; Barthel, Anne-Kathrin; Senz, Rainer; Braun, Ulrike

2017-05-01

In order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-phase adsorber and subsequently analyzed by thermal desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow. Copyright © 2017 Elsevier Ltd. All rights reserved.

Multielemental analysis in small amounts of environmental reference materials with inductively coupled plasma mass spectrometry.

PubMed

Dombovári, J; Becker, J S; Dietze, H J

2000-07-01

The lowest possible sample weight for performing multielemental trace element analysis on environmental and biological samples by ICP-MS has been investigated. The certified reference materials Bovine Liver NIST SRM 1577b, Human Hair NCS DC 73347 and Oriental Tobacco Leaves CTA-OTL-1 were applied at sample weights (1, 5, 20 and 50 mg aliquots, n = 10) which were significantly lower than those recommended with most recoveries in the range of 95-110%. Samples were digested in a mixture of nitric acid, hydrogen peroxide and hydrogen fluoride by closed-vessel microwave digestion. Multielemental analysis was performed with an optimized ICP-QMS method. Aqueous standard solutions were applied for external calibration with rhodium as the internal standard element. The detection limits varied between 0.02-0.38 microg/g for Li, Na, Cr, Mn, Ni, Cu, Zn, Sr, Cd, Ba and Pb, and up to 1.92 microg/g for Mg, Al, Ca, Fe and Ni. Digested human plasma samples were spiked with multielemental solution (0.5-10 microg/L) to test the analytical method and the recoveries were 95-105% for most analytes. Our results show that in the case of homogeneous SRMs it is possible to use them in very low amounts (1-5 mg) for method development and quality control.

Chiral Drug Analysis in Forensic Chemistry: An Overview.

PubMed

Ribeiro, Cláudia; Santos, Cristiana; Gonçalves, Valter; Ramos, Ana; Afonso, Carlos; Tiritan, Maria Elizabeth

2018-01-28

Many substances of forensic interest are chiral and available either as racemates or pure enantiomers. Application of chiral analysis in biological samples can be useful for the determination of legal or illicit drugs consumption or interpretation of unexpected toxicological effects. Chiral substances can also be found in environmental samples and revealed to be useful for determination of community drug usage (sewage epidemiology), identification of illicit drug manufacturing locations, illegal discharge of sewage and in environmental risk assessment. Thus, the purpose of this paper is to provide an overview of the application of chiral analysis in biological and environmental samples and their relevance in the forensic field. Most frequently analytical methods used to quantify the enantiomers are liquid and gas chromatography using both indirect, with enantiomerically pure derivatizing reagents, and direct methods recurring to chiral stationary phases.

Recent Application of Solid Phase Based Techniques for Extraction and Preconcentration of Cyanotoxins in Environmental Matrices.

PubMed

Mashile, Geaneth Pertunia; Nomngongo, Philiswa N

2017-03-04

Cyanotoxins are toxic and are found in eutrophic, municipal, and residential water supplies. For this reason, their occurrence in drinking water systems has become a global concern. Therefore, monitoring, control, risk assessment, and prevention of these contaminants in the environmental bodies are important subjects associated with public health. Thus, rapid, sensitive, selective, simple, and accurate analytical methods for the identification and determination of cyanotoxins are required. In this paper, the sampling methodologies and applications of solid phase-based sample preparation methods for the determination of cyanotoxins in environmental matrices are reviewed. The sample preparation techniques mainly include solid phase micro-extraction (SPME), solid phase extraction (SPE), and solid phase adsorption toxin tracking technology (SPATT). In addition, advantages and disadvantages and future prospects of these methods have been discussed.

Critical and systematic evaluation of data for estimating human exposures to 2,4-dichlorophenoxyacetic acid (2,4-D) - quality and generalizability.

PubMed

LaKind, Judy S; Burns, Carol J; Naiman, Daniel Q; O'Mahony, Cian; Vilone, Giulia; Burns, Annette J; Naiman, Joshua S

2017-01-01

The herbicide 2,4-dichlorophenoxyacetic acid (2,4-D) has been commercially available since the 1940's. Despite decades of data on 2,4-D in food, air, soil, and water, as well as in humans, the quality the quality of these data has not been comprehensively evaluated. Using selected elements of the Biomonitoring, Environmental Epidemiology, and Short-lived Chemicals (BEES-C) instrument (temporal variability, avoidance of sample contamination, analyte stability, and urinary methods of matrix adjustment), the quality of 156 publications of environmental- and biomonitoring-based 2,4-D data was examined. Few publications documented steps were taken to avoid sample contamination. Similarly, most studies did not demonstrate the stability of the analyte from sample collection to analysis. Less than half of the biomonitoring publications reported both creatinine-adjusted and unadjusted urine concentrations. The scope and detail of data needed to assess temporal variability and sources of 2,4-D varied widely across the reviewed studies. Exposures to short-lived chemicals such as 2,4-D are impacted by numerous and changing external factors including application practices and formulations. At a minimum, greater transparency in reporting of quality control measures is needed. Perhaps the greatest challenge for the exposure community is the ability to reach consensus on how to address problems specific to short-lived chemical exposures in observational epidemiology investigations. More extensive conversations are needed to advance our understanding of human exposures and enable interpretation of these data to catch up to analytical capabilities. The problems defined in this review remain exquisitely difficult to address for chemicals like 2,4-D, with short and variable environmental and physiological half-lives and with exposures impacted by numerous and changing external factors.

Detection of Pesticides and Pesticide Metabolites Using the Cross Reactivity of Enzyme Immunoassays

USGS Publications Warehouse

Thurman, E.M.; Aga, D.S.

2001-01-01

Enzyme immunoassay is an important environmental analysis method that may be used to identify many pesticide analytes in water samples. Because of similarities in chemical structure between various members of a pesticide class, there often may be an unwanted response that is characterized by a percentage of cross reactivity. Also, there may be cross reactivity caused by degradation products of the target analyte that may be present in the sample. In this paper, the concept of cross reactivity caused by degradation products or by nontarget analytes is explored as a tool for identification of metabolites or structurally similar compounds not previously known to be present in water samples. Two examples are examined in this paper from various water quality studies. They are alachlor and its metabolite, alachlor ethane sulfonic acid, and atrazine and its class members, prometryn and propazine. A method for using cross reactivity for the detection of these compounds is explained in this paper.

The rise of environmental analytical chemistry as an interdisciplinary activity.

PubMed

Brown, Richard

2009-07-01

Modern scientific endeavour is increasingly delivered within an interdisciplinary framework. Analytical environmental chemistry is a long-standing example of an interdisciplinary approach to scientific research where value is added by the close cooperation of different disciplines. This editorial piece discusses the rise of environmental analytical chemistry as an interdisciplinary activity and outlines the scope of the Analytical Chemistry and the Environmental Chemistry domains of TheScientificWorldJOURNAL (TSWJ), and the appropriateness of TSWJ's domain format in covering interdisciplinary research. All contributions of new data, methods, case studies, and instrumentation, or new interpretations and developments of existing data, case studies, methods, and instrumentation, relating to analytical and/or environmental chemistry, to the Analytical and Environmental Chemistry domains, are welcome and will be considered equally.

Analytical chemistry of PCBs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Erickson, M.D.

Analytical Chemistry of PCBs offers a review of physical, chemical, commercial, environmental and biological properties of PCBs. It also defines and discusses six discrete steps of analysis: sampling, extraction, cleanup, determination, data reduction, and quality assurance. The final chapter provides a discussion on collaborative testing - the ultimate step in method evaluation. Dr. Erickson also provides a bibliography of over 1200 references, critical reviews of primary literature, and five appendices which present ancillary material on PCB nomen-clature, physical properties, composition of commercial mixtures, mass spectra characteristics, and PGC/ECD chromatograms.

A novel statistical methodology to overcome sampling irregularities in the forest inventory data and to model forest changes under dynamic disturbance regimes

Treesearch

Nikolay Strigul; Jean Lienard

2015-01-01

Forest inventory datasets offer unprecedented opportunities to model forest dynamics under evolving environmental conditions but they are analytically challenging due to irregular sampling time intervals of the same plot, across the years. We propose here a novel method to model dynamic changes in forest biomass and basal area using forest inventory data. Our...

Final report: survey and removal of radioactive surface contamination at environmental restoration sites, Sandia National Laboratories/New Mexico. Volume 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lambert, K.A.; Mitchell, M.M.; Jean, D.

1997-09-01

This report contains the Appendices A-L including Voluntary Corrective Measure Plans, Waste Management Plans, Task-Specific Health and Safety Plan, Analytical Laboratory Procedures, Soil Sample Results, In-Situ Gamma Spectroscopy Results, Radionuclide Activity Summary, TCLP Soil Sample Results, Waste Characterization Memoranda, Waste Drum Inventory Data, Radiological Risk Assessment, and Summary of Site-Specific Recommendations.

Quality of nutrient data from streams and ground water sampled during water years 1992-2001

USGS Publications Warehouse

Mueller, David K.; Titus, Cindy J.

2005-01-01

Proper interpretation of water-quality data requires consideration of the effects that bias and variability might have on measured constituent concentrations. In this report, methods are described to estimate the bias due to contamination of samples in the field or laboratory and the variability due to sample collection, processing, shipment, and analysis. Contamination can adversely affect interpretation of measured concentrations in comparison to standards or criteria. Variability can affect interpretation of small differences between individual measurements or mean concentrations. Contamination and variability are determined for nutrient data from quality-control samples (field blanks and replicates) collected as part of the National Water-Quality Assessment (NAWQA) Program during water years 1992-2001. Statistical methods are used to estimate the likelihood of contamination and variability in all samples. Results are presented for five nutrient analytes from stream samples and four nutrient analytes from ground-water samples. Ammonia contamination can add at least 0.04 milligram per liter in up to 5 percent of all samples. This could account for more than 22 percent of measured concentrations at the low range of aquatic-life criteria (0.18 milligram per liter). Orthophosphate contamination, at least 0.019 milligram per liter in up to 5 percent of all samples, could account for more than 38 percent of measured concentrations at the limit to avoid eutrophication (0.05 milligram per liter). Nitrite-plus-nitrate and Kjeldahl nitrogen contamination is less than 0.4 milligram per liter in 99 percent of all samples; thus there is no significant effect on measured concentrations of environmental significance. Sampling variability has little or no effect on reported concentrations of ammonia, nitrite-plus-nitrate, orthophosphate, or total phosphorus sampled after 1998. The potential errors due to sampling variability are greater for the Kjeldahl nitrogen analytes and for total phosphorus sampled before 1999. The uncertainty in a mean of 10 concentrations caused by sampling variability is within a small range (1 to 7 percent) for all nutrients. These results can be applied to interpretation of environmental data collected during water years 1992-2001 in 52 NAWQA study units.

7 CFR 91.23 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... Methods for the Analysis of Pesticide Residues in Human and Environmental Samples, EPA 600/9-80-038, U.S... Examination of Foods, Carl Vanderzant and Don Splittstoesser (Editors), American Public Health Association... Methods for the Examination of Dairy Products, American Public Health Association, 1015 Fifteenth Street...

7 CFR 91.23 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... Methods for the Analysis of Pesticide Residues in Human and Environmental Samples, EPA 600/9-80-038, U.S... Examination of Foods, Carl Vanderzant and Don Splittstoesser (Editors), American Public Health Association... Methods for the Examination of Dairy Products, American Public Health Association, 1015 Fifteenth Street...

VACUUM DISTILLATION COUPLED WITH GAS CHROMATOGRAPHY/MASS SPECTROMETRY FOR THE ANALYSIS OF ENVIRONMENTAL SAMPLES

EPA Science Inventory

A procedure is presented that uses a vacuum distillation/gas chromatography/mass spectrometry system for analysis of problematic matrices of volatile organic compounds. The procedure compensates for matrix effects and provides both analytical results and confidence intervals from...

The Specter of Cancer

ERIC Educational Resources Information Center

Environmental Science and Technology, 1975

1975-01-01

Increasing manmade pollutants seem to be correlated with increasing illnesses such as cancer and cardiovascular and respiratory diseases. Sensitive analytic methods have detected known or suspected carcinogenic chemicals in many environmental samples. Lower life forms could be used to monitor pollutants and indicate potential hazards to man. (MR)

COULOMETRIC DETERMINATION OF TOTAL SULFUR AND REDUCED INORGANIC SULFUR FRACTIONS IN ENVIRONMENTAL SAMPLES

EPA Science Inventory

Evaluation of the solid-phase partitioning of sulfur is frequently an important analytical component of risk assessments at hazardous waste sites because minerals containing reduced-sulfur can significantly affect the transport and fate of organic and inorganic contaminants in na...

Enantiomer fractions of polychlorinated biphenyls in three selected Standard Reference Materials.

PubMed

Morrissey, Joshua A; Bleackley, Derek S; Warner, Nicholas A; Wong, Charles S

2007-01-01

The enantiomer composition of six chiral polychlorinated biphenyls (PCBs) were measured in three different certified Standard Reference Materials (SRMs) from the US National Institute of Standards and Technology (NIST): SRM 1946 (Lake Superior fish tissue), SRM 1939a (PCB Congeners in Hudson River Sediment), and SRM 2978 (organic contaminants in mussel tissue--Raritan Bay, New Jersey) to aid in quality assurance/quality control methodologies in the study of chiral pollutants in sediments and biota. Enantiomer fractions (EFs) of PCBs 91, 95, 136, 149, 174, and 183 were measured using a suite of chiral columns by gas chromatography/mass spectrometry. Concentrations of target analytes were in agreement with certified values. Target analyte EFs in reference materials were measured precisely (<2% relative standard deviation), indicating the utility of SRM in quality assurance/control methodologies for analyses of chiral compounds in environmental samples. Measured EFs were also in agreement with previously published analyses of similar samples, indicating that similar enantioselective processes were taking place in these environmental matrices.

Local versus field scale soil heterogeneity characterization - a challenge for representative sampling in pollution studies

NASA Astrophysics Data System (ADS)

Kardanpour, Z.; Jacobsen, O. S.; Esbensen, K. H.

2015-06-01

This study is a contribution to development of a heterogeneity characterisation facility for "next generation" sampling aimed at more realistic and controllable pesticide variability in laboratory pots in experimental environmental contaminant assessment. The role of soil heterogeneity on quantification of a set of exemplar parameters, organic matter, loss on ignition (LOI), biomass, soil microbiology, MCPA sorption and mineralization is described, including a brief background on how heterogeneity affects sampling/monitoring procedures in environmental pollutant studies. The Theory of Sampling (TOS) and variographic analysis has been applied to develop a fit-for-purpose heterogeneity characterization approach. All parameters were assessed in large-scale profile (1-100 m) vs. small-scale (0.1-1 m) replication sampling pattern. Variographic profiles of experimental analytical results concludes that it is essential to sample at locations with less than a 2.5 m distance interval to benefit from spatial auto-correlation and thereby avoid unnecessary, inflated compositional variation in experimental pots; this range is an inherent characteristic of the soil heterogeneity and will differ among soils types. This study has a significant carrying-over potential for related research areas e.g. soil science, contamination studies, and environmental monitoring and environmental chemistry.

Best-Matched Internal Standard Normalization in Liquid Chromatography-Mass Spectrometry Metabolomics Applied to Environmental Samples.

PubMed

Boysen, Angela K; Heal, Katherine R; Carlson, Laura T; Ingalls, Anitra E

2018-01-16

The goal of metabolomics is to measure the entire range of small organic molecules in biological samples. In liquid chromatography-mass spectrometry-based metabolomics, formidable analytical challenges remain in removing the nonbiological factors that affect chromatographic peak areas. These factors include sample matrix-induced ion suppression, chromatographic quality, and analytical drift. The combination of these factors is referred to as obscuring variation. Some metabolomics samples can exhibit intense obscuring variation due to matrix-induced ion suppression, rendering large amounts of data unreliable and difficult to interpret. Existing normalization techniques have limited applicability to these sample types. Here we present a data normalization method to minimize the effects of obscuring variation. We normalize peak areas using a batch-specific normalization process, which matches measured metabolites with isotope-labeled internal standards that behave similarly during the analysis. This method, called best-matched internal standard (B-MIS) normalization, can be applied to targeted or untargeted metabolomics data sets and yields relative concentrations. We evaluate and demonstrate the utility of B-MIS normalization using marine environmental samples and laboratory grown cultures of phytoplankton. In untargeted analyses, B-MIS normalization allowed for inclusion of mass features in downstream analyses that would have been considered unreliable without normalization due to obscuring variation. B-MIS normalization for targeted or untargeted metabolomics is freely available at https://github.com/IngallsLabUW/B-MIS-normalization .

Environmental Survey of the B-3 and Ford’s Farm Ranges,

DTIC Science & Technology

1983-08-01

reported have an estimated analytical error of *35% unless noted otherwise. 14 Isotopic Analysis The isotopic uranium analysis procedure used by UST...sulfate buffer and elec- trodeposited on a stainless steel disc, and isotopes of uranium (234U, 23 5U, and 2 38U) were determined by pulse height analysis ...measurements and some environmental sampling. Several special studies were also conducted, including analyses of the isotopic composition of uranium in

Determination of nanomolar chromate in drinking water with solid phase extraction and a portable spectrophotometer.

PubMed

Ma, Jian; Yang, Bo; Byrne, Robert H

2012-06-15

Determination of chromate at low concentration levels in drinking water is an important analytical objective for both human health and environmental science. Here we report the use of solid phase extraction (SPE) in combination with a custom-made portable light-emitting diode (LED) spectrophotometer to achieve detection of chromate in the field at nanomolar levels. The measurement chemistry is based on a highly selective reaction between 1,5-diphenylcarbazide (DPC) and chromate under acidic conditions. The Cr-DPC complex formed in the reaction can be extracted on a commercial C18 SPE cartridge. Concentrated Cr-DPC is subsequently eluted with methanol and detected by spectrophotometry. Optimization of analytical conditions involved investigation of reagent compositions and concentrations, eluent type, flow rate (sample loading), sample volume, and stability of the SPE cartridge. Under optimized conditions, detection limits are on the order of 3 nM. Only 50 mL of sample is required for an analysis, and total analysis time is around 10 min. The targeted analytical range of 0-500 nM can be easily extended by changing the sample volume. Compared to previous SPE-based spectrophotometric methods, this analytical procedure offers the benefits of improved sensitivity, reduced sample consumption, shorter analysis time, greater operational convenience, and lower cost. Copyright © 2012 Elsevier B.V. All rights reserved.

Development of Novel Method for Rapid Extract of Radionuclides from Solution Using Polymer Ligand Film

NASA Astrophysics Data System (ADS)

Rim, Jung H.

Accurate and fast determination of the activity of radionuclides in a sample is critical for nuclear forensics and emergency response. Radioanalytical techniques are well established for radionuclides measurement, however, they are slow and labor intensive, requiring extensive radiochemical separations and purification prior to analysis. With these limitations of current methods, there is great interest for a new technique to rapidly process samples. This dissertation describes a new analyte extraction medium called Polymer Ligand Film (PLF) developed to rapidly extract radionuclides. Polymer Ligand Film is a polymer medium with ligands incorporated in its matrix that selectively and rapidly extract analytes from a solution. The main focus of the new technique is to shorten and simplify the procedure necessary to chemically isolate radionuclides for determination by alpha spectrometry or beta counting. Five different ligands were tested for plutonium extraction: bis(2-ethylhexyl) methanediphosphonic acid (H2DEH[MDP]), di(2-ethyl hexyl) phosphoric acid (HDEHP), trialkyl methylammonium chloride (Aliquat-336), 4,4'(5')-di-t-butylcyclohexano 18-crown-6 (DtBuCH18C6), and 2-ethylhexyl 2-ethylhexylphosphonic acid (HEH[EHP]). The ligands that were effective for plutonium extraction further studied for uranium extraction. The plutonium recovery by PLFs has shown dependency on nitric acid concentration and ligand to total mass ratio. H2DEH[MDP] PLFs performed best with 1:10 and 1:20 ratio PLFs. 50.44% and 47.61% of plutonium were extracted on the surface of PLFs with 1M nitric acid for 1:10 and 1:20 PLF, respectively. HDEHP PLF provided the best combination of alpha spectroscopy resolution and plutonium recovery with 1:5 PLF when used with 0.1M nitric acid. The overall analyte recovery was lower than electrodeposited samples, which typically has recovery above 80%. However, PLF is designed to be a rapid field deployable screening technique and consistency is more important than recovery. PLFs were also tested using blind quality control samples and the activities were accurately measured. It is important to point out that PLFs were consistently susceptible to analytes penetrating and depositing below the surface. The internal radiation within the body of PLF is mostly contained and did not cause excessive self-attenuation and peak broadening in alpha spectroscopy. The analyte penetration issue was beneficial in the destructive analysis. H2DEH[MDP] PLF was tested with environmental samples to fully understand the capabilities and limitations of the PLF in relevant environments. The extraction system was very effective in extracting plutonium from environmental water collected from Mortandad Canyon at Los Alamos National Laboratory with minimal sample processing. Soil samples were tougher to process than the water samples. Analytes were first leached from the soil matrixes using nitric acid before processing with PLF. This approach had a limitation in extracting plutonium using PLF. The soil samples from Mortandad Canyon, which are about 1% iron by weight, were effectively processed with the PLF system. Even with certain limitations of the PLF extraction system, this technique was able to considerably decrease the sample analysis time. The entire environmental sample was analyzed within one to two days. The decrease in time can be attributed to the fact that PLF is replacing column chromatography and electrodeposition with a single step for preparing alpha spectrometry samples. The two-step process of column chromatography and electrodeposition takes a couple days to a week to complete depending on the sample. The decrease in time and the simplified procedure make this technique a unique solution for application to nuclear forensics and emergency response. A large number of samples can be quickly analyzed and selective samples can be further analyzed with more sensitive techniques based on the initial data. The deployment of a PLF system as a screening method will greatly reduce a total analysis time required to gain meaningful isotopic data for the nuclear forensics application. (Abstract shortened by UMI.)

Reference Standardization for Mass Spectrometry and High-resolution Metabolomics Applications to Exposome Research.

PubMed

Go, Young-Mi; Walker, Douglas I; Liang, Yongliang; Uppal, Karan; Soltow, Quinlyn A; Tran, ViLinh; Strobel, Frederick; Quyyumi, Arshed A; Ziegler, Thomas R; Pennell, Kurt D; Miller, Gary W; Jones, Dean P

2015-12-01

The exposome is the cumulative measure of environmental influences and associated biological responses throughout the lifespan, including exposures from the environment, diet, behavior, and endogenous processes. A major challenge for exposome research lies in the development of robust and affordable analytic procedures to measure the broad range of exposures and associated biologic impacts occurring over a lifetime. Biomonitoring is an established approach to evaluate internal body burden of environmental exposures, but use of biomonitoring for exposome research is often limited by the high costs associated with quantification of individual chemicals. High-resolution metabolomics (HRM) uses ultra-high resolution mass spectrometry with minimal sample preparation to support high-throughput relative quantification of thousands of environmental, dietary, and microbial chemicals. HRM also measures metabolites in most endogenous metabolic pathways, thereby providing simultaneous measurement of biologic responses to environmental exposures. The present research examined quantification strategies to enhance the usefulness of HRM data for cumulative exposome research. The results provide a simple reference standardization protocol in which individual chemical concentrations in unknown samples are estimated by comparison to a concurrently analyzed, pooled reference sample with known chemical concentrations. The approach was tested using blinded analyses of amino acids in human samples and was found to be comparable to independent laboratory results based on surrogate standardization or internal standardization. Quantification was reproducible over a 13-month period and extrapolated to thousands of chemicals. The results show that reference standardization protocol provides an effective strategy that will enhance data collection for cumulative exposome research. In principle, the approach can be extended to other types of mass spectrometry and other analytical methods. © The Author 2015. Published by Oxford University Press on behalf of the Society of Toxicology. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

Reference Standardization for Mass Spectrometry and High-resolution Metabolomics Applications to Exposome Research

PubMed Central

Go, Young-Mi; Walker, Douglas I.; Liang, Yongliang; Uppal, Karan; Soltow, Quinlyn A.; Tran, ViLinh; Strobel, Frederick; Quyyumi, Arshed A.; Ziegler, Thomas R.; Pennell, Kurt D.; Miller, Gary W.; Jones, Dean P.

2015-01-01

The exposome is the cumulative measure of environmental influences and associated biological responses throughout the lifespan, including exposures from the environment, diet, behavior, and endogenous processes. A major challenge for exposome research lies in the development of robust and affordable analytic procedures to measure the broad range of exposures and associated biologic impacts occurring over a lifetime. Biomonitoring is an established approach to evaluate internal body burden of environmental exposures, but use of biomonitoring for exposome research is often limited by the high costs associated with quantification of individual chemicals. High-resolution metabolomics (HRM) uses ultra-high resolution mass spectrometry with minimal sample preparation to support high-throughput relative quantification of thousands of environmental, dietary, and microbial chemicals. HRM also measures metabolites in most endogenous metabolic pathways, thereby providing simultaneous measurement of biologic responses to environmental exposures. The present research examined quantification strategies to enhance the usefulness of HRM data for cumulative exposome research. The results provide a simple reference standardization protocol in which individual chemical concentrations in unknown samples are estimated by comparison to a concurrently analyzed, pooled reference sample with known chemical concentrations. The approach was tested using blinded analyses of amino acids in human samples and was found to be comparable to independent laboratory results based on surrogate standardization or internal standardization. Quantification was reproducible over a 13-month period and extrapolated to thousands of chemicals. The results show that reference standardization protocol provides an effective strategy that will enhance data collection for cumulative exposome research. In principle, the approach can be extended to other types of mass spectrometry and other analytical methods. PMID:26358001

Superhydrophobic Analyte Concentration Utilizing Colloid-Pillar Array SERS Substrates

DOE PAGES

Wallace, Ryan A.; Charlton, Jennifer J.; Kirchner, Teresa B.; ...

2014-11-04

In order to detect a few molecules present in a large sample it is important to know the trace components in the medicinal and environmental sample. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. Moreover, the following work involves superhydrophobic surfaces that includes silicon pillar arrays formed by lithographic and dewetting protocols. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added tomore » the functionalized pillar array system via soaking. The pillars are used native and with hydrophobic modification. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 10-12 M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up applications in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.« less

Superhydrophobic Analyte Concentration Utilizing Colloid-Pillar Array SERS Substrates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wallace, Ryan A.; Charlton, Jennifer J.; Kirchner, Teresa B.

In order to detect a few molecules present in a large sample it is important to know the trace components in the medicinal and environmental sample. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. Moreover, the following work involves superhydrophobic surfaces that includes silicon pillar arrays formed by lithographic and dewetting protocols. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added tomore » the functionalized pillar array system via soaking. The pillars are used native and with hydrophobic modification. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 10-12 M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up applications in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.« less

Quantification of 226Ra at environmental relevant levels in natural waters by ICP-MS: Optimization, validation and limitations of an extraction and preconcentration approach.

PubMed

Lagacé, François; Foucher, Delphine; Surette, Céline; Clarisse, Olivier

2017-05-15

Radium (Ra) at environmental relevant levels in natural waters was determined by ICP-MS after an off-line pre-concentration procedure. The latter consisted of Ra selective elution from potential interfering elements (i.e. other alkaline earth cations: Ba 2+ , Sr 2+ , Ca 2+ , Mg 2+ ) on a series of two different ion exchange resins (AG50W-X8 and Sr-resin). The overall analytical method was optimized according to the instrumental performance, the volume of water sample loaded on resins, and the sample salinity. Longer acquisition time (up to 150 s) was required to ensure stable measurement of Ra by ICP-MS at ultra trace level (1.0pgL -1 ). For a synthetic groundwater spiked with Ra at 10.0pgL -1 , the analytical procedure demonstrated efficient separation of the analyte from its potential interfering elements and a complete recovery, independent of the sample volume tested from 10 up to 100mL. For synthetic seawater spiked at a level of 10.0pgL -1 of Ra, the total load of salts on the two resins should not exceed 0.35g in order to ensure a complete separation and recovery of Ra. The method was validated on natural waters (i.e. groundwater, freshwater and seawater samples) spiked with Ra at different levels (0.0, 0.5, 1.0 and 5.0pgL -1 ). Absolute Ra detection limits were determined at 0.020pgL -1 (0.73mBqL -1 ) and 0.12pgL -1 (4.4mBqL -1 ) respectively for 60.0mL of freshwater sample and for 10.0mL of seawater. Copyright © 2017 Elsevier B.V. All rights reserved.

Trace analysis of surfactants in Corexit oil dispersant formulations and seawater

NASA Astrophysics Data System (ADS)

Place, Benjamin J.; Perkins, Matt J.; Sinclair, Ewan; Barsamian, Adam L.; Blakemore, Paul R.; Field, Jennifer A.

2016-07-01

After the April 2010 explosion on the Deepwater Horizon oil rig, and subsequent release of millions of barrels of oil, two Corexit oil dispersant formulations were used in unprecedented quantities both on the surface and sub-surface of the Gulf of Mexico. Although the dispersant formulations contain four classes of surfactants, current studies to date focus on the anionic surfactant, bis-(2-ethylhexyl) sulfosuccinate (DOSS). Factors affecting the integrity of environmental and laboratory samples for Corexit analysis have not been systematically investigated. For this reason, a quantitative analytical method was developed for the detection of all four classes of surfactants, as well as the hydrolysis products of DOSS, the enantiomeric mixture of α- and β-ethylhexyl sulfosuccinate (α-/β-EHSS). The analytical method was then used to evaluate which practices for sample collection, storage, and analysis resulted in high quality data. Large volume, direct injection of seawater followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) minimized analytical artifacts, analysis time, and both chemical and solid waste. Concentrations of DOSS in the seawater samples ranged from 71 to 13,000 ng/L, while the nonionic surfactants including Span 80, Tween 80, Tween 85 were detected infrequently (26% of samples) at concentrations from 840 to 9100 ng/L. The enantiomers α-/β-EHSS were detected in seawater, at concentrations from 200 to 1900 ng/L, and in both Corexit dispersant formulations, indicating α-/β-EHSS were applied to the oil spill and may be not unambiguous indicator of DOSS degradation. Best practices are provided to ensure sample integrity and data quality for environmental monitoring studies and laboratory that require the detection and quantification of Corexit-based surfactants in seawater.

Development of a low-cost method of analysis for the qualitative and quantitative analysis of butyltins in environmental samples.

PubMed

Bangkedphol, Sornnarin; Keenan, Helen E; Davidson, Christine; Sakultantimetha, Arthit; Songsasen, Apisit

2008-12-01

Most analytical methods for butyltins are based on high resolution techniques with complicated sample preparation. For this study, a simple application of an analytical method was developed using High Performance Liquid Chromatography (HPLC) with UV detection. The developed method was studied to determine tributyltin (TBT), dibutyltin (DBT) and monobutyltin (MBT) in sediment and water samples. The separation was performed in isocratic mode on an ultra cyanopropyl column with a mobile phase of hexane containing 5% THF and 0.03% acetic acid. This method was confirmed using standard GC/MS techniques and verified by statistical paired t-test method. Under the experimental conditions used, the limit of detection (LOD) of TBT and DBT were 0.70 and 0.50 microg/mL, respectively. The optimised extraction method for butyltins in water and sediment samples involved using hexane containing 0.05-0.5% tropolone and 0.2% sodium chloride in water at pH 1.7. The quantitative extraction of butyltin compounds in a certified reference material (BCR-646) and naturally contaminated samples was achieved with recoveries ranging from 95 to 108% and at %RSD 0.02-1.00%. This HPLC method and optimum extraction conditions were used to determine the contamination level of butyltins in environmental samples collected from the Forth and Clyde canal, Scotland, UK. The values obtained severely exceeded the Environmental Quality Standard (EQS) values. Although high resolution methods are utilised extensively for this type of research, the developed method is cheaper in both terms of equipment and running costs, faster in analysis time and has comparable detection limits to the alternative methods. This is advantageous not just as a confirmatory technique but also to enable further research in this field.

The Savannah River Site's Groundwater Monitoring Program

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1989-01-01

The Environmental Monitoring Section of the Environmental and Health Protection (EHP) Department administers the Savannah River Site's Groundwater Monitoring Program. During fourth quarter 1989 (October--December), EHP conducted routine sampling of monitoring wells and drinking water locations. EHP collected the drinking water samples from Savannah River Site (SRS) drinking water systems supplied by wells. EHP established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria aid personnel in sample scheduling, interpretation of data, and trend identification. An explanation of flagging criteria for the fourth quarter is presented in the Flagging Criteria sectionmore » of this document. All analytical results from fourth quarter 1989 are listed in this report, which is distributed to all waste-site custodians.« less

The Savannah River Site`s Groundwater Monitoring Program. Fourth quarter, 1989

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1989-12-31

The Environmental Monitoring Section of the Environmental and Health Protection (EHP) Department administers the Savannah River Site`s Groundwater Monitoring Program. During fourth quarter 1989 (October--December), EHP conducted routine sampling of monitoring wells and drinking water locations. EHP collected the drinking water samples from Savannah River Site (SRS) drinking water systems supplied by wells. EHP established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria aid personnel in sample scheduling, interpretation of data, and trend identification. An explanation of flagging criteria for the fourth quarter is presented in the Flagging Criteria sectionmore » of this document. All analytical results from fourth quarter 1989 are listed in this report, which is distributed to all waste-site custodians.« less

Matrix-enhanced degradation of p,p'-DDT during gas chromatographic analysis: A consideration

USGS Publications Warehouse

Foreman, W.T.; Gates, Paul M.

1997-01-01

Analysis of p,p‘-DDT in environmental samples requires monitoring the GC-derived breakdown of this insecticide, which produces p,p‘-DDD and/or p,p‘-DDE, both also primary environmental degradation products. A performance evaluation standard (PES) containing p,p‘-DDT but notp,p‘-DDD or p,p‘-DDE can be injected at regular intervals throughout an analytical sequence to monitor GC degradation. Some U.S. EPA methods limit GC breakdown of DDT in the PES to ≤20%. GC/MS analysis of large-volume natural water samples fortified with deuterium- and 13C-labeled p,p‘-DDT exhibited up to 65% DDT breakdown by the GC inlet. These matrix-enhanced GC degradation amounts substantially exceeded the <20% breakdown levels indicated by bracketing injections of the PES containing unlabeled and labeled DDT. Substantial matrix-enhanced GC degradation was not observed during analysis of a limited number of fractionated bed-sediment extracts containing labeled DDT. Use of isotopically labeled DDT seems to provide an effective tool for monitoring sample-specific DDT breakdown during GC/MS analysis. However, analyte co-elutions render impractical their use in GC/ECD analysis. The oc currence of matrix-enhanced GC degradation might have important implications on data quality and the resultant interpretations of the environmental degradation of DDT and other thermolabile contaminants.

[Simultaneous determination of 22 typical pharmaceuticals and personal care products in environmental water using ultra performance liquid chromatography- triple quadrupole mass spectrometry].

PubMed

Wu, Chunying; Gu, Feng; Bai, Lu; Lu, Wenlong

2015-08-01

An analytical method for simultaneous determination of 22 typical pharmaceuticals and personal care products (PPCPs) in environmental water samples was developed by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). An Oasis HLB solid phase extraction cartridge, methanol as washing solution, water containing 0. 1% formic acid-methanol (7:3, v/v) as the mobile phases were selected for sample pretreatment and chromatographic separation. Based on the optimized sample pretreatment procedures and separation condition, the target recoveries ranged from 73% to 125% in water with the relative standard deviations ( RSDs) from 8.8% to 17.5%, and the linear ranges were from 2 to 2 000 µg/L with correlation coefficients (R2) not less than 0.997. The method can be applied to simultaneous determination of the 22 typical PPCPs in environmental water samples because of its low detection limits and high recoveries. It can provide support and help for the related research on water environmental risk assessment and control of the micro-organic pollutants.

[Recent Development of Atomic Spectrometry in China].

PubMed

Xiao, Yuan-fang; Wang, Xiao-hua; Hang, Wei

2015-09-01

As an important part of modern analytical techniques, atomic spectrometry occupies a decisive status in the whole analytical field. The development of atomic spectrometry also reflects the continuous reform and innovation of analytical techniques. In the past fifteen years, atomic spectrometry has experienced rapid development and been applied widely in many fields in China. This review has witnessed its development and remarkable achievements. It contains several directions of atomic spectrometry, including atomic emission spectrometry (AES), atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS), X-ray fluorescence spectrometry (XRF), and atomic mass spectrometry (AMS). Emphasis is put on the innovation of the detection methods and their applications in related fields, including environmental samples, biological samples, food and beverage, and geological materials, etc. There is also a brief introduction to the hyphenated techniques utilized in atomic spectrometry. Finally, the prospects of atomic spectrometry in China have been forecasted.

Immunoanalysis Methods for the Detection of Dioxins and Related Chemicals

PubMed Central

Tian, Wenjing; Xie, Heidi Qunhui; Fu, Hualing; Pei, Xinhui; Zhao, Bin

2012-01-01

With the development of biotechnology, approaches based on antibodies, such as enzyme-linked immunosorbent assay (ELISA), active aryl hydrocarbon immunoassay (Ah-I) and other multi-analyte immunoassays, have been utilized as alternatives to the conventional techniques based on gas chromatography and mass spectroscopy for the analysis of dioxin and dioxin-like compounds in environmental and biological samples. These screening methods have been verified as rapid, simple and cost-effective. This paper provides an overview on the development and application of antibody-based approaches, such as ELISA, Ah-I, and multi-analyte immunoassays, covering the sample extraction and cleanup, antigen design, antibody preparation and immunoanalysis. However, in order to meet the requirements for on-site fast detection and relative quantification of dioxins in the environment, further optimization is needed to make these immuno-analytical methods more sensitive and easy to use. PMID:23443395

Diaion HP-2MG modified with 2-(2,6-dichlorobenzylideneamino) benzenethiol as new adsorbent for solid phase extraction and flame atomic absorption spectrometric determination of metal ions.

PubMed

Ghaedi, M; Montazerozohori, M; Haghdoust, S; Zaare, F; Soylak, M

2013-04-01

A solid phase extraction method for enrichment-separation and the determination of cobalt (Co(2+)), copper (Cu(2+)), nickel (Ni(2+)), zinc (Zn(2+)) and lead (Pb(2+)) ions in real samples has been proposed. The influences of some analytical parameters like pH, flow rate, eluent type and interference of matrix ions on recoveries of analytes were optimized. The limits of detection were found in the range of 1.6-3.9 µg L(-1), while preconcentration factor for all understudy metal ions were found to be 166 with loading half time (t 1/2) less than 10 min. The procedure was applied for the enrichment-separation of analyte ions in environmental samples with recoveries higher than 94.8% and relative SD <4.9% (N = 5).

Hydrogel nanoparticle based immunoassay

DOEpatents

Liotta, Lance A; Luchini, Alessandra; Petricoin, Emanuel F; Espina, Virginia

2015-04-21

An immunoassay device incorporating porous polymeric capture nanoparticles within either the sample collection vessel or pre-impregnated into a porous substratum within fluid flow path of the analytical device is presented. This incorporation of capture particles within the immunoassay device improves sensitivity while removing the requirement for pre-processing of samples prior to loading the immunoassay device. A preferred embodiment is coreshell bait containing capture nanoparticles which perform three functions in one step, in solution: a) molecular size sieving, b) target analyte sequestration and concentration, and c) protection from degradation. The polymeric matrix of the capture particles may be made of co-polymeric materials having a structural monomer and an affinity monomer, the affinity monomer having properties that attract the analyte to the capture particle. This device is useful for point of care diagnostic assays for biomedical applications and as field deployable assays for environmental, pathogen and chemical or biological threat identification.

14 CFR 34.82 - Sampling and analytical procedures for measuring smoke exhaust emissions.

Code of Federal Regulations, 2011 CFR

2011-01-01

..., DEPARTMENT OF TRANSPORTATION AIRCRAFT FUEL VENTING AND EXHAUST EMISSION REQUIREMENTS FOR TURBINE ENGINE POWERED AIRPLANES Test Procedures for Engine Smoke Emissions (Aircraft Gas Turbine Engines) § 34.82..., Environmental Protection, Volume II, Aircraft Engine Emissions, Second Edition, July 1993, effective July 26...

14 CFR 34.82 - Sampling and analytical procedures for measuring smoke exhaust emissions.

Code of Federal Regulations, 2010 CFR

2010-01-01

..., DEPARTMENT OF TRANSPORTATION AIRCRAFT FUEL VENTING AND EXHAUST EMISSION REQUIREMENTS FOR TURBINE ENGINE POWERED AIRPLANES Test Procedures for Engine Smoke Emissions (Aircraft Gas Turbine Engines) § 34.82..., Environmental Protection, Volume II, Aircraft Engine Emissions, Second Edition, July 1993, effective July 26...

GUIDELINES FOR THE APPLICATION OF SEM/EDX ANALYTICAL TECHNIQUES FOR FINE AND COARSE PM SAMPLES

EPA Science Inventory

Scanning Electron Microscopy (SEM) coupled with Energy-Dispersive X-ray analysis (EDX) is a powerful tool in the characterization and source apportionment of environmental particulate matter (PM), providing size, chemistry, and morphology of particles as small as a few tenths ...

Surface Environmental Surveillance Project: Locations Manual Volume 1 – Air and Water Volume 2 – Farm Products, Soil & Vegetation, and Wildlife

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fritz, Brad G.; Patton, Gregory W.; Stegen, Amanda

2009-01-01

This report describes all environmental monitoring locations associated with the Surface Environmental Surveillance Project. Environmental surveillance of the Hanford site and surrounding areas is conducted by the Pacific Northwest National Laboratory (PNNL) for the U.S. Department of Energy (DOE). Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 450.1, Environmental Protection Program, and DOE Order 5400.5, Radiation Protection of the Public and the Environment. The environmental surveillance sampling design is described in the Hanford Site Environmental Monitoring Plan, United States Department of Energy, Richland Operation Office (DOE/RL-91-50). This documentmore » contains the locations of sites used to collect samples for the Surface Environmental Surveillance Project (SESP). Each section includes directions, maps, and pictures of the locations. A general knowledge of roads and highways on and around the Hanford Site is necessary to successfully use this manual. Supplemental information (Maps, Gazetteer, etc.) may be necessary if user is unfamiliar with local routes. The SESP is a multimedia environmental surveillance effort to measure the concentrations of radionuclides and chemicals in environmental media to demonstrate compliance with applicable environmental quality standards and public exposure limits, and assessing environmental impacts. Project personnel annually collect selected samples of ambient air, surface water, agricultural products, fish, wildlife, and sediments. Soil and vegetation samples are collected approximately every 5 years. Analytical capabilities include the measurement of radionuclides at very low environmental concentrations and, in selected media, nonradiological chemicals including metals, anions, volatile organic compounds, and total organic carbon.« less

Inorganic trace analysis by mass spectrometry

NASA Astrophysics Data System (ADS)

Becker, Johanna Sabine; Dietze, Hans-Joachim

1998-10-01

Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g -1 concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of high-purity materials and environmental samples) is used in order to improve the detection limits of trace elements. Furthermore, the determination of chemical elements in the trace and ultratrace concentration range is often difficult and can be disturbed through mass interferences of analyte ions by molecular ions at the same nominal mass. By applying double-focusing sector field mass spectrometry at the required mass resolution—by the mass spectrometric separation of molecular ions from the analyte ions—it is often possible to overcome these interference problems. Commercial instrumental equipment, the capability (detection limits, accuracy, precision) and the analytical application fields of mass spectrometric methods for the determination of trace and ultratrace elements and for surface analysis are discussed.

Tracking Matrix Effects in the Analysis of DNA Adducts of Polycyclic Aromatic Hydrocarbons

PubMed Central

Klaene, Joshua J.; Flarakos, Caroline; Glick, James; Barret, Jennifer T.; Zarbl, Helmut; Vouros, Paul

2015-01-01

LC-MS using electrospray ionization is currently the method of choice in bio-organic analysis covering a wide range of applications in a broad spectrum of biological media. The technique is noted for its high sensitivity but one major limitation which hinders achievement of its optimal sensitivity is the signal suppression due to matrix inferences introduced by the presence of co-extracted compounds during the sample preparation procedure. The analysis of DNA adducts of common environmental carcinogens is particularly sensitive to such matrix effects as sample preparation is a multistep process which involves “contamination” of the sample due to the addition of enzymes and other reagents for digestion of the DNA in order to isolate the analyte(s). This problem is further exacerbated by the need to reach low levels of quantitation (LOQ in the ppb level) while also working with limited (2-5 μg) quantities of sample. We report here on the systematic investigation of ion signal suppression contributed by each individual step involved in the sample preparation associated with the analysis of DNA adducts of polycyclic aromatic hydrocarbon (PAH) using as model analyte dG-BaP, the deoxyguanosine adduct of benzo[a]pyrene (BaP). The individual matrix contribution of each one of these sources to analyte signal was systematically addressed as were any interactive effects. The information was used to develop a validated analytical protocol for the target biomarker at levels typically encountered in vivo using as little as 2 μg of DNA and applied to a dose response study using a metabolically competent cell line. PMID:26607319

Recent Trends in Rapid Environmental Monitoring of Pathogens and Toxicants: Potential of Nanoparticle-Based Biosensor and Applications

PubMed Central

Koedrith, Preeyaporn; Thasiphu, Thalisa; Weon, Jong-Il; Boonprasert, Rattana; Tuitemwong, Kooranee; Tuitemwong, Pravate

2015-01-01

Of global concern, environmental pollution adversely affects human health and socioeconomic development. The presence of environmental contaminants, especially bacterial, viral, and parasitic pathogens and their toxins as well as chemical substances, poses serious public health concerns. Nanoparticle-based biosensors are considered as potential tools for rapid, specific, and highly sensitive detection of the analyte of interest (both biotic and abiotic contaminants). In particular, there are several limitations of conventional detection methods for water-borne pathogens due to low concentrations and interference with various enzymatic inhibitors in the environmental samples. The increase of cells to detection levels requires long incubation time. This review describes current state of biosensor nanotechnology, the advantage over conventional detection methods, and the challenges due to testing of environmental samples. The major approach is to use nanoparticles as signal reporter to increase output rather than spending time to increase cell concentrations. Trends in future development of novel detection devices and their advantages over other environmental monitoring methodologies are also discussed. PMID:25884032

Application of dispersion-solidification liquid-liquid microextraction for the determination of triazole fungicides in environmental water samples by high-performance liquid chromatography.

PubMed

Wang, Chun; Wu, Qiuhua; Wu, Chunxia; Wang, Zhi

2011-01-15

A simple, rapid and environmentally friendly method has been developed for the determination of four triazole fungicides (myclobutanil, tebuconazole, triadimenol, hexaconazole) in water samples by dispersion-solidification liquid-liquid microextraction coupled with high performance liquid chromatography-diode array detection. Several variables that affect the extraction efficiencies, including the type and volume of the extraction solvent and dispersive solvent, extraction time, effect of pH and salt addition, were investigated and optimized. Under the optimum conditions, the proposed method is sensitive and shows a good linearity within a range of 0.5-200 ng mL(-1), with the correlation coefficients (r) varying from 0.9992 to 0.9998. High enrichment factors were achieved ranging from 190 to 450. The recoveries of the target analytes from water samples at spiking levels of 1.0, 5.0 and 50.0 ng mL(-1) were between 84.8% and 110.2%. The limits of detection (LODs) for the analytes were ranged in 0.06-0.1 ng mL(-1), and the relative standard deviations (RSD) varied from 3.9% to 5.7%. The proposed method has been successfully applied for the determination of the triazole fungicides in real water samples. Copyright © 2010 Elsevier B.V. All rights reserved.

Ultrafast Screening and Quantitation of Pesticides in Food and Environmental Matrices by Solid-Phase Microextraction-Transmission Mode (SPME-TM) and Direct Analysis in Real Time (DART).

PubMed

Gómez-Ríos, Germán Augusto; Gionfriddo, Emanuela; Poole, Justen; Pawliszyn, Janusz

2017-07-05

The direct interface of microextraction technologies to mass spectrometry (MS) has unquestionably revolutionized the speed and efficacy at which complex matrices are analyzed. Solid Phase Micro Extraction-Transmission Mode (SPME-TM) is a technology conceived as an effective synergy between sample preparation and ambient ionization. Succinctly, the device consists of a mesh coated with polymeric particles that extracts analytes of interest present in a given sample matrix. This coated mesh acts as a transmission-mode substrate for Direct Analysis in Real Time (DART), allowing for rapid and efficient thermal desorption/ionization of analytes previously concentrated on the coating, and dramatically lowering the limits of detection attained by sole DART analysis. In this study, we present SPME-TM as a novel tool for the ultrafast enrichment of pesticides present in food and environmental matrices and their quantitative determination by MS via DART ionization. Limits of quantitation in the subnanogram per milliliter range can be attained, while total analysis time does not exceed 2 min per sample. In addition to target information obtained via tandem MS, retrospective studies of the same sample via high-resolution mass spectrometry (HRMS) were accomplished by thermally desorbing a different segment of the microextraction device.

The Savannah River Site`s Groundwater Monitoring Program. Second quarter, 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1992-01-10

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site`s (SRS) Groundwater Monitoring Program. During second quarter 1991 EPD/EMS conducted extensive sampling of monitoring wells. EPD/EMS established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria do not define contamination levels; instead, they aid personnel in sample scheduling, interpretation of data, and trend identification. Beginning in 1991, the flagging criteria are based on EPA drinking water standards and method detection limits. A detailed explanation of the current flagging criteria is presented in the Flagging Criteria section of this document.more » Analytical results from second quarter 1991 are listed in this report.« less

The Savannah River Site's Groundwater Monitoring Program

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1992-01-10

The Environmental Protection Department/Environmental Monitoring Section (EPD/EMS) administers the Savannah River Site's (SRS) Groundwater Monitoring Program. During second quarter 1991 EPD/EMS conducted extensive sampling of monitoring wells. EPD/EMS established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria do not define contamination levels; instead, they aid personnel in sample scheduling, interpretation of data, and trend identification. Beginning in 1991, the flagging criteria are based on EPA drinking water standards and method detection limits. A detailed explanation of the current flagging criteria is presented in the Flagging Criteria section of this document.more » Analytical results from second quarter 1991 are listed in this report.« less

Portable capillary electrophoresis-system for on-site food analysis with lab-on-a-chip based contactless conductivity detection

NASA Astrophysics Data System (ADS)

Gärtner, Claudia; Sewart, René; Klemm, Richard; Becker, Holger

2014-06-01

A portable analytical system for the characterization of liquid environmental samples and beverages in food control was realized. The key element is the implementation of contactless conductivity detection on lab-on-a-chip basis ensuring the system to be operated in a label free mode. Typical target molecules such as small ionic species like Li+, Na+, K+, SO4 2- or NO3-, organic acids in wine whose concentration and ratio to each other documents the wine quality, or caffeine or phosphate in coke were detected. Results from sample matrices like various beverages as water, cola, tea, wine and milk, water from heaters, environmental samples and blood will be presented.

Correlated Raman micro-spectroscopy and scanning electron microscopy analyses of flame retardants in environmental samples: a micro-analytical tool for probing chemical composition, origin and spatial distribution.

PubMed

Ghosal, Sutapa; Wagner, Jeff

2013-07-07

We present correlated application of two micro-analytical techniques: scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and Raman micro-spectroscopy (RMS) for the non-invasive characterization and molecular identification of flame retardants (FRs) in environmental dusts and consumer products. The SEM/EDS-RMS technique offers correlated, morphological, molecular, spatial distribution and semi-quantitative elemental concentration information at the individual particle level with micrometer spatial resolution and minimal sample preparation. The presented methodology uses SEM/EDS analyses for rapid detection of particles containing FR specific elements as potential indicators of FR presence in a sample followed by correlated RMS analyses of the same particles for characterization of the FR sub-regions and surrounding matrices. The spatially resolved characterization enabled by this approach provides insights into the distributional heterogeneity as well as potential transfer and exposure mechanisms for FRs in the environment that is typically not available through traditional FR analysis. We have used this methodology to reveal a heterogeneous distribution of highly concentrated deca-BDE particles in environmental dust, sometimes in association with identifiable consumer materials. The observed coexistence of deca-BDE with consumer material in dust is strongly indicative of its release into the environment via weathering/abrasion of consumer products. Ingestion of such enriched FR particles in dust represents a potential for instantaneous exposure to high FR concentrations. Therefore, correlated SEM/RMS analysis offers a novel investigative tool for addressing an area of important environmental concern.

Tracermodel1- Excel workbook for calculation and presentation of environmental tracer data for simple groundwater mixtures: Use of chlorofluorocarbons in hydrology - a guidebook; Section III.10.3

USGS Publications Warehouse

Böhlke, John Karl

2006-01-01

Atmospheric environmental tracers commonly used to date groundwater on timescales of years to decades include CFC-11, CFC-12, CFC-113, SF6, 85Kr, 3 H and 3 H/3 H0 , where 3 H0 refers to initial tritium (3 H + tritiogenic 3 He) (Cook and Herczeg, 2000). Interpretation of age from environmental tracer data may be relatively simple for a water sample with a single age, but the interpretation is more complex for a sample that is a mixture of waters of varying ages. A mixture can be a natural result of convergence of flow lines to a discharge area such as a spring or stream, or it can be an artefact of sampling a long-screen well. TRACERMODEL1 contains a worksheet that can be used to determine hypothetical concentrations of atmospheric environmental tracers in water samples with several different age distributions. It is designed to permit plotting of ages and tracer concentrations in a variety of different combinations to facilitate interpretation of measurements. TRACERMODEL1 includes several different types of graphs that are linked to the calculations. The spreadsheet and accompanying graphs can be modified for specific applications. For example, the selection of atmospheric environmental tracers can be changed to reflect analytes of interest, the input tracer data can be modified to reflect local conditions or different timescales, and the analytes of interest can include other types of non-point-source contaminants, such as nitrate (Böhlke, 2002). Previous versions of this workbook have been used to evaluate field data in studies of groundwater residence time and agricultural contamination (Böhlke and Denver, 1995; Focazio et al., 1998; Katz et al., 1999; Katz et al., 2001; Plummer et al., 2001; Böhlke and Krantz, 2003; Lindsey et al., 2003).

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

USGS Publications Warehouse

Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

1996-01-01

In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

Evaluation of carbon aerogel-based solid-phase extraction sorbent for the analysis of sulfur mustard degradation products in environmental water samples.

PubMed

Jõul, Piia; Vaher, Merike; Kuhtinskaja, Maria

2018-05-01

In this study, SPE method using a carbon aerogel(CA)-based sorbent was developed and evaluated for the simultaneous extraction of sulfur mustard (HD) degradation products from environmental water samples. Applied CAs proved to be very promising materials for use as SPE sorbents, due to their high porosity, very low density and a large specific surface area. 10 degradation products of HD, both aliphatic and cyclic (thiodiglycol (TDG), TDG sulfoxide, TDG sulfone, 3,5-dithia-1,7-heptanediol, 3,6-dithia-1,8-octanediol, 1,4-thioxane, 1,3-dithiolane, 1,4-dithiane, 1,2,5-trithiepane, and 1,4,5-oxadithiepane) were extracted on a CA-based SPE cartridge. The concentrations of target analytes in the eluate were determined by HPLC-DAD and CE-DAD. Several parameters affecting the extraction efficiency, including the kind and volume of the eluting solvent, sample loading flow rate, volume and ionic strength as well as the reusability of the cartridge, were investigated and optimized to achieve the best performance for the analytes. A series of quantitative parameters such as linear range, coefficient of determination, LOD, LOQ and precision were examined under the optimized conditions. High sensitivity (LODs 0.17-0.50 μM) and high precision (intraday RSD = 2.0-7.7% and interday RSD = 2.7-9.9%) for all the analytes were achieved. The performance of the CA-based sorbent was compared with that of commonly used SPE sorbents. Applied for the analysis of spiked pore water samples collected from the Bornholm Basin, one of the largest chemical warfare dumping sites in the Baltic Sea, the proposed method allowed high SPE recoveries of all the analytes ranging from 83.5 to 99.7% to be obtained. Copyright © 2018 Elsevier Ltd. All rights reserved.

Review of Processing and Analytical Methods for Francisella ...

EPA Pesticide Factsheets

Journal Article The etiological agent of tularemia, Francisella tularensis, is a resilient organism within the environment and can be acquired many ways (infectious aerosols and dust, contaminated food and water, infected carcasses, and arthropod bites). However, isolating F. tularensis from environmental samples can be challenging due to its nutritionally fastidious and slow-growing nature. In order to determine the current state of the science regarding available processing and analytical methods for detection and recovery of F. tularensis from water and soil matrices, a review of the literature was conducted. During the review, analysis via culture, immunoassays, and genomic identification were the most commonly found methods for F. tularensis detection within environmental samples. Other methods included combined culture and genomic analysis for rapid quantification of viable microorganisms and use of one assay to identify multiple pathogens from a single sample. Gaps in the literature that were identified during this review suggest that further work to integrate culture and genomic identification would advance our ability to detect and to assess the viability of Francisella spp. The optimization of DNA extraction, whole genome amplification with inhibition-resistant polymerases, and multiagent microarray detection would also advance biothreat detection.

Environmental 90Sr measurements

USGS Publications Warehouse

Paul, M.; Berkovits, D.; Cecil, L.D.; Feldstein, H.; Hershkowitz, A.; Kashiv, Y.; Vogt, S.

1997-01-01

90Sr (T1/2 = 28.5 years) is a long-lived radionuclide produced in nuclear fission. Fast radiochemical detection of 90Sr in environmental samples is not feasible using current analytical methods. Accelerator Mass Spectrometry (AMS) measurements of 90Sr were made with the Rehovot 14UD Pelletron accelerator at a terminal voltage of 11 or 12 MV using our standard detection system. Injection of hydride ions (SrH3-) was chosen owing to high beam intensity and low Coulomb explosion effects. 90Sr ions were identified and discriminated from isobaric 90Zr by measuring time of flight, total energy and three independent energy-loss signals in an ionization chamber. A reference sample and a ground-water sample were successfully measured. The detection limit determined for a laboratory blank by the residual counts in the 90Sr region is 90Sr/Sr = 3 ?? 10-13, corresponding in practice to (2-4) ?? 10790Sr atoms or about 0.5-1 pCi/L in environmental water samples.

NATIONAL PERFORMANCE AUDIT PROGRAM: 1979 PROFICIENCY SURVEYS FOR SULFUR DIOXIDE, NITROGEN DIOXIDE, CARBON MONOXIDE, SULFATE, NITRATE, LEAD AND HIGH VOLUME FLOW

EPA Science Inventory

The Quality Assurance Division of the Environmental Monitoring Systems Laboratory, Research Triangle Park, North Carolina, administers semiannual Surveys of Analytical Proficiency for sulfur dioxide, nitrogen dioxide, carbon monoxide, sulfate, nitrate and lead. Sample material, s...

ION-EXCLUSION CHROMATOGRAPHIC DETERMINATION OF CARBOXYLIC ACIDS USED TO SUPPORT THE MICROBIALLY MEDIATED REDUCTIVE DECHLORINATION OF TETRACHLOROETHENE

EPA Science Inventory

An analytical method was developed for the determination of lactic acid, formic acid, acetic acid, propionic acid, and butyric acid in environmental microcosm samples using ion-exclusion chromatography. The chromatographic behavior of various eluents was studied to determine the ...

EPA Method 538: Determination of Selected Organic Contaminants in Drinking Water by Direct Aqueous Injection-Liquid Chromatography/Tandem Mass Spectrometry (DAI-LC/MS/MS)

EPA Pesticide Factsheets

EPA’s Selected Analytical Methods for Environmental Remediation and Recovery (SAM) lists this method for preparation and analysis of drinking water samples to detect and measure acephate, diisopropyl methylphosphonate (DIMP), methamidophos and thiofanox.

ANALYSIS OF THE ENANTIOMERS OF CHIRAL PESTICIDES AND OTHER POLLUTANTS IN ENVIRONMENTAL SAMPLES BY CAPILLARY ELECTROPHORESIS

EPA Science Inventory

The generic method described here involves typical capillary electrophoresis (CE) techniques, with the addition of cyclodextrin chiral selectors to the electrolyte for enantiomer separation and also, in the case of neutral analytes, the further addition of a micelle forming comp...

40 CFR 86.1863-07 - Optional chassis certification for diesel vehicles.

Code of Federal Regulations, 2014 CFR

2014-07-01

... be tested using the test fuels, sampling systems, or analytical systems specified for diesel engines... diesel vehicles. 86.1863-07 Section 86.1863-07 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) CONTROL OF EMISSIONS FROM NEW AND IN-USE HIGHWAY VEHICLES AND ENGINES...

SIMULTANEOUS DTERMINATION OF CHROMATE AND AROMATIC HYDROCARBONS IN ENVIRONMENTAL SAMPLES BY CAPILLARY ELECTROPHORESIS

EPA Science Inventory

An analytical method was developed to determine simultaneously, the inorganic anion CrO2-4, and organic aromatic compounds including benzoate, 2-Cl-benzoate, phenol, m-cresol and o-/p-cresol by capillary electrophoresis (CE). Chromate and the aromatics were separated in a relativ...

Materials and Methods for Streamlined Laboratory Analysis of Environmental Samples, FY 2016 Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Addleman, Raymond S.; Naes, Benjamin E.; McNamara, Bruce K.

The International Atomic Energy Agency (IAEA) relies upon laboratory analysis of environmental samples (typically referred to as “swipes”) collected during on-site inspections of safeguarded facilities to support the detection and deterrence of undeclared activities. Unfortunately, chemical processing and assay of the samples is slow and expensive. A rapid, effective, and simple extraction process and analysis method is needed to provide certified results with improved timeliness at reduced costs (principally in the form of reduced labor), while maintaining or improving sensitivity and efficacy. To address these safeguard needs the Pacific Northwest National Laboratory (PNNL) explored and demonstrated improved methods for environmentalmore » sample (ES) analysis. Improvements for both bulk and particle analysis were explored. To facilitate continuity and adoption, the new sampling materials and processing methods will be compatible with existing IAEA protocols for ES analysis. PNNL collaborated with Oak Ridge National Laboratory (ORNL), which performed independent validation of the new bulk analysis methods and compared performance to traditional IAEA’s Network of Analytical Laboratories (NWAL) protocol. ORNL efforts are reported separately. This report describes PNNL’s FY 2016 progress, which was focused on analytical application supporting environmental monitoring of uranium enrichment plants and nuclear fuel processing. In the future the technology could be applied to other safeguard applications and analytes related to fuel manufacturing, reprocessing, etc. PNNL’s FY 2016 efforts were broken into two tasks and a summary of progress, accomplishments and highlights are provided below. Principal progress and accomplishments on Task 1, Optimize Materials and Methods for ICP-MS Environmental Sample Analysis, are listed below. • Completed initial procedure for rapid uranium extraction from ES swipes based upon carbonate-peroxide chemistry (delivered to ORNL for evaluation). • Explored improvements to carbonate-peroxide rapid uranium extraction chemistry. • Evaluated new sampling materials and methods (in collaboration with ORNL). • Demonstrated successful ES extractions from standard and novel swipes for a wide range uranium compounds of interest including UO 2F 2 and UO 2(NO 3) 2, U 3O 8 and uranium ore concentrate. • Completed initial discussions with commercial suppliers of PTFE swipe materials. • Submitted one manuscript for publication. Two additional drafts are being prepared. Principal progress and accomplishments on Task 2, Optimize Materials and Methods for Direct SIMS Environmental Sample Analysis, are listed below. • Designed a SIMS swipe sample holder that retrofits into existing equipment and provides simple, effective, and rapid mounting of ES samples for direct assay while enabling automation and laboratory integration. • Identified preferred conductive sampling materials with better performance characteristics. • Ran samples on the new PNNL NWAL equivalent Cameca 1280 SIMS system. • Obtained excellent agreement between isotopic ratios for certified materials and direct SIMS assay of very low levels of LEU and HEU UO 2F 2 particles on carbon fiber sampling material. Sample activities range from 1 to 500 CPM (uranium mass on sample is dependent upon specific isotope ratio but is frequently in the subnanogram range). • Found that the presence of the UF molecular ions, as measured by SIMS, provides chemical information about the particle that is separate from the uranium isotopics and strongly suggests that those particles originated from an UF6 enrichment activity. • Submitted one manuscript for publication. Another manuscript is in preparation.« less

A new high-speed hollow fiber based liquid phase microextraction method using volatile organic solvent for determination of aromatic amines in environmental water samples prior to high-performance liquid chromatography.

PubMed

Sarafraz-Yazdi, A; Mofazzeli, F; Es'haghi, Z

2009-07-15

A new and fast hollow fiber based liquid phase microextraction (HF-LPME) method using volatile organic solvents coupled with high-performance liquid chromatography (HPLC) was developed for determination of aromatic amines in the environmental water samples. Analytes including 3-nitroaniline, 3-chloroaniline and 4-bromoaniline were extracted from 6 mL basic aqueous sample solution (donor phase, NaOH 1 mol L(-1)) into the thin film of organic solvent that surrounded and impregnated the pores of the polypropylene hollow fiber wall (toluene, 20 microL), then back-extracted into the 6 mL acidified aqueous solution (acceptor phase, HCl 0.5 mol L(-1)) in the lumen of the two-end sealed hollow fiber. After the extraction, 5 microL of the acceptor phase was withdrawn into the syringe and injected directly into the HPLC system for the analysis. The parameters influencing the extraction efficiency including the kind of organic solvent and its volume, composition of donor and acceptor phases and the volume ratio between them, extraction time, stirring rate, salt addition and the effect of the analyte complexation with 18-crown-6 ether were investigated and optimized. Under the optimal conditions (donor phase: 6 mL of 1 mol L(-1) NaOH with 10% NaCl; organic phase: 20 microL of toluene; acceptor phase: 6 microL of 0.5 mol L(-1) HCl and 600 mmol L(-1) 18-crown-6 ether; pre-extraction and back-extraction times: 75 s and 10 min, respectively; stirring rate: 800 rpm), the obtained EFs were between 259 and 674, dynamic linear ranges were 0.1-1000 microg L(-1) (R>0.9991), and also the limits of detection were in the range of 0.01-0.1 micro gL(-1). The proposed procedure worked very well for real environmental water samples with microgram per liter level of the analytes, and good relative recoveries (91-102%) were obtained for the spiked sample solutions.

Background-free coherent anti-stokes Raman scattering of gas- and liquid-phase samples in a mesoporous silica aerogel host.

PubMed

Konorov, Stanislav O; Turner, Robin F B; Blades, Michael W

2007-05-01

Efficient time-resolved coherent anti-Stokes Raman scattering (CARS) of atmospheric nitrogen and ethanol trapped in a nanoporous silica aerogel matrix is demonstrated. Silica aerogel hosts are attractive for analytical CARS spectroscopy due to their high porosity/low density, low refractive index, and low scattering cross-section. Differences between the resonant and nonresonant parts of the nonlinear optical susceptibilities lead to much longer relaxation times for analytes compared to the matrix. Time-resolved CARS can then be used to obtain a nearly background-free measurement at characteristic vibrations of the analyte. These results demonstrate the potential of this approach for rapid, sensitive, background-free analyses of analytes entrapped in the aerogel pores, which may be advantageous for some environmental, chemical, and biological sensing applications.

Environmental behavior and analysis of agricultural sulfur.

PubMed

Griffith, Corey M; Woodrow, James E; Seiber, James N

2015-11-01

Sulfur has been widely used for centuries as a staple for pest and disease management in agriculture. Presently, it is the largest-volume pesticide in use worldwide. This review describes the sources and recovery methods for sulfur, its allotropic forms and properties and its agricultural uses, including development and potential advantages of nanosulfur as a fungicide. Chemical and microbial reactivity, interactions in soil and water and analytical methods for determination in environmental samples and foodstuffs, including inexpensive analytical methods for sulfur residues in wine, beer and other food/beverage substrates, will be reviewed. The toxicology of sulfur towards humans and agriculturally important fungi is included, with some restrictions on use to promote safety. The review concludes with areas for which more research is warranted. © 2015 Society of Chemical Industry.

Dispersive liquid-liquid microextraction applied to isolation and concentration of alkylphenols and their short-chained ethoxylates in water samples.

PubMed

Zgoła-Grześkowiak, Agnieszka

2010-03-12

Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography with fluorescence detector was applied for the determination of alkylphenols and their short-chained ethoxylates in water samples. Development of DLLME procedure included optimisation of some important parameters such as kind and volume of extracting and dispersing solvents. Under optimised conditions 50 microL of trichloroethylene in 1.5 mL of acetone were rapidly injected into 5 mL of a water sample. After centrifuging the organic phase containing the analytes was taken for evaporation with a gentle nitrogen purge and reconstituted to 50 microL of acetonitrile. The aliquot of this solution was analysed with the use of HPLC. For octylphenol (OP) and octylphenol ethoxylates (OPEOs) linearity was satisfactory in the range 8-1000 microg L(-1) and for nonylphenol (NP) and nonylphenol ethoxylates (NPEOs) linearity was in the range from 50 to about 3000 microg L(-1). Limit of quantitation was 0.1 microg L(-1) for OP and OPEOs and 0.3 microg L(-1) for NP and NPEOs. Satisfactory recoveries between 66 and 79% were obtained for environmental samples. The results showed that DLLME is a simple, rapid and sensitive analytical method for the preconcentration of trace amounts of alkylphenols and their ethoxylates in environmental water samples. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Application of a dispersive solid-phase extraction method using an amino-based silica-coated nanomagnetic sorbent for the trace quantification of chlorophenoxyacetic acids in water samples.

PubMed

Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali; Sobhi, Hamid Reza

2017-09-01

Herein, an amino-based silica-coated nanomagnetic sorbent was applied for the effective extraction of two chlorophenoxyacetic acids (2-methyl-4-chlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid) from various water samples. The sorbent was successfully synthesized and subsequently characterized by scanning electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy. The analytes were extracted by the sorbent mainly through ionic interactions. Once the extraction of analytes was completed, they were desorbed from the sorbent and detected by high-performance liquid chromatography with ultraviolet detection. A number of factors affecting the extraction and desorption of the analytes were investigated in detail and the optimum conditions were established. Under the optimum conditions, the calibration curves were linear over the concentration range of 1-250, and based on a signal-to-noise ratio of 3, the method detection limits were determined to be 0.5 μg/L for both analytes. Additionally, a preconcentration factor of 314 was achieved for the analytes. The average relative recoveries obtained from the fortified water samples varied in the range of 91-108% with relative standard deviations of 2.9-8.3%. Finally, the method was determined to be robust and effective for environmental water analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biological Matrix Effects in Quantitative Tandem Mass Spectrometry-Based Analytical Methods: Advancing Biomonitoring

PubMed Central

Panuwet, Parinya; Hunter, Ronald E.; D’Souza, Priya E.; Chen, Xianyu; Radford, Samantha A.; Cohen, Jordan R.; Marder, M. Elizabeth; Kartavenka, Kostya; Ryan, P. Barry; Barr, Dana Boyd

2015-01-01

The ability to quantify levels of target analytes in biological samples accurately and precisely, in biomonitoring, involves the use of highly sensitive and selective instrumentation such as tandem mass spectrometers and a thorough understanding of highly variable matrix effects. Typically, matrix effects are caused by co-eluting matrix components that alter the ionization of target analytes as well as the chromatographic response of target analytes, leading to reduced or increased sensitivity of the analysis. Thus, before the desired accuracy and precision standards of laboratory data are achieved, these effects must be characterized and controlled. Here we present our review and observations of matrix effects encountered during the validation and implementation of tandem mass spectrometry-based analytical methods. We also provide systematic, comprehensive laboratory strategies needed to control challenges posed by matrix effects in order to ensure delivery of the most accurate data for biomonitoring studies assessing exposure to environmental toxicants. PMID:25562585

Validation of the ANSR Salmonella method for detection of Salmonella spp. in selected foods and environmental samples.

PubMed

Mozola, Mark; Norton, Paul; Alles, Susan; Gray, R Lucas; Tolan, Jerry; Caballero, Oscar; Pinkava, Lisa; Hosking, Edan; Luplow, Karen; Rice, Jennifer

2013-01-01

ANSR Salmonella is a new molecular diagnostic assay for detection of Salmonella spp. in foods and environmental samples. The test is based on the nicking enzyme amplification reaction (NEAR) isothermal nucleic acid amplification technology. The assay platform features simple instrumentation, minimal labor, and, following a single-step 10-24 h enrichment (depending on sample type), an extremely short assay time of 30 min, including sample preparation. Detection is real-time using fluorescent molecular beacon probes. Inclusivity testing was performed using a panel of 113 strains of S. enterica and S. bongori, representing 109 serovars and all genetic subgroups. With the single exception of the rare serovar S. Weslaco, all serovars and genetic subgroups were detected. Exclusivity testing of 38 non-salmonellae, mostly Enterobacteriaceae, yielded no evidence of cross-reactivity. In comparative testing of chicken carcass rinse, raw ground turkey, raw ground beef, hot dogs, and oat cereal, there were no statistically significant differences in the number of positive results obtained with the ANSR and the U.S. Department of Agriculture-Food Safety and Inspection Service or U.S. Food and Drug Administration/Bacteriological Analytical Manual reference culture methods. In testing of swab or sponge samples from five different environmental surfaces, four trials showed no statistically significant differences in the number of positive results by the ANSR and the U.S. Food and Drug Administration/ Bacteriological Analytical Manual reference methods; in the trial with stainless steel surface, there were significantly more positive results by the ANSR method. Ruggedness experiments showed a high degree of assay robustness when deviations in reagent volumes and incubation times were introduced.

Spacelab Charcoal Analyses

NASA Technical Reports Server (NTRS)

Slivon, L. E.; Hernon-Kenny, L. A.; Katona, V. R.; Dejarme, L. E.

1995-01-01

This report describes analytical methods and results obtained from chemical analysis of 31 charcoal samples in five sets. Each set was obtained from a single scrubber used to filter ambient air on board a Spacelab mission. Analysis of the charcoal samples was conducted by thermal desorption followed by gas chromatography/mass spectrometry (GC/MS). All samples were analyzed using identical methods. The method used for these analyses was able to detect compounds independent of their polarity or volatility. In addition to the charcoal samples, analyses of three Environmental Control and Life Support System (ECLSS) water samples were conducted specifically for trimethylamine.

A solid phase extraction-ion chromatography with conductivity detection procedure for determining cationic surfactants in surface water samples.

PubMed

Olkowska, Ewa; Polkowska, Żaneta; Namieśnik, Jacek

2013-11-15

A new analytical procedure for the simultaneous determination of individual cationic surfactants (alkyl benzyl dimethyl ammonium chlorides) in surface water samples has been developed. We describe this methodology for the first time: it involves the application of solid phase extraction (SPE-for sample preparation) coupled with ion chromatography-conductivity detection (IC-CD-for the final determination). Mean recoveries of analytes between 79% and 93%, and overall method quantification limits in the range from 0.0018 to 0.038 μg/mL for surface water and CRM samples were achieved. The methodology was applied to the determination of individual alkyl benzyl quaternary ammonium compounds in environmental samples (reservoir water) and enables their presence in such types of waters to be confirmed. In addition, it is a simpler, less time-consuming, labour-intensive, avoiding use of toxic chloroform and significantly less expensive methodology than previously described approaches (liquid-liquid extraction coupled with liquid chromatography-mass spectrometry). Copyright © 2013 Elsevier B.V. All rights reserved.

Coupling pervaporation to AAS for inorganic and organic mercury determination. A new approach to speciation of Hg in environmental samples.

PubMed

Fernandez-Rivas, C; Muñoz-Olivas, R; Camara, C

2001-12-01

The design and development of a new approach for Hg speciation in environmental samples is described in detail. This method, consisting of the coupling of pervaporation and atomic absorption spectrometry, is based on a membrane phenomenon that combines the evaporation of volatile analytes and their diffusion through a polymeric membrane. It is proposed here as an alternative to gas chromatography for speciation of inorganic and organic Hg compounds, as the latter compounds are volatile and can be separated by applying the principles mentioned above. The interest of this method lies in its easy handling, low cost, and rapidity for the analysis of liquid and solid samples. This method has been applied to Hg speciation in a compost sample provided by a waste water treatment plant.

Evaluation of Quality-Assurance/Quality-Control Data Collected by the U.S. Geological Survey from Wells and Springs between the Southern Boundary of the Idaho National Engineering and Environmental Laboratory and the Hagerman Area, Idaho, 1989 through 1995

DOE Office of Scientific and Technical Information (OSTI.GOV)

Williams, L.M.; Bartholomay, R.C.; Campbell, L.J.

1998-10-01

The U.S. Geological (USGS) and the Idaho Department of Water Resources, in cooperation with the U.S. Department of Energy, collected and analyzed water samples to monitor the water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering and Environmental Laboratory to the Hagerman area, Idaho. Concurrently, replicate samples and blank samples were collected and analyzed as part of the quality-assurance/quality-control program. Samples were analyzed from inorganic constituents, gross radioactivity and radionuclides, organic constituents, and stable isotopes. To evaluate the precision of field and laboratory methods, analytical results of the water-quality and replicate samplesmore » were compared statistically for equivalence on the basis of the precision associated with each result. Statistical comparisons of the data indicated that 95 percent of the results of the replicate pairs were equivalent. Blank-sample analytical results indicated th at the inorganic blank water and volatile organic compound blank water from the USGS National Water Quality Laboratory and the distilled water from the Idaho Department of Water Resources were suitable for blanks; blank water from other sources was not. Equipment-blank analytical results were evaluated to determine if a bias had been introduced and possible sources of bias. Most equipment blanks were analyzed for trace elements and volatile organic compounds; chloroform was found in one equipment blank. Two of the equipment blanks were prepared after collection and analyses of the water-quality samples to determine whether contamination had been introduced during the sampling process. Results of one blank indicated that a hose used to divert water away from pumps and electrical equipment had contaminated the samples with some volatile organic compounds. Results of the other equipment blank, from the apparatus used to filter dissolved organic carbon samples, indicated that the filtering apparatus did not affect water-quality samples.« less

Ionic liquids: solvents and sorbents in sample preparation.

PubMed

Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

2018-01-01

The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Virginia Finley; Sheneman, Robert S.; Levine, Jerry D.

Contained in the following report are data for radioactivity in the environment collected and analyzed by Princeton Plasma Physics Laboratory’s Princeton Environmental, Analytical, and Radiological Laboratory (PEARL). The PEARL is located on-site and is certified for analyzing radiological and non-radiological parameters through the New Jersey Department of Environmental Protection’s Laboratory Certification Program, Certification Number 12471. Non-radiological surface and ground water samples are analyzed by NJDEP certified subcontractor laboratories – QC, Inc. and Accutest Laboratory. To the best of our knowledge, these data, as contained in the “Annual Site Environmental Report for 2011,” are documented and certified to be correct.

Considerations for estimating microbial environmental data concentrations collected from a field setting

PubMed Central

Silvestri, Erin E; Yund, Cynthia; Taft, Sarah; Bowling, Charlena Yoder; Chappie, Daniel; Garrahan, Kevin; Brady-Roberts, Eletha; Stone, Harry; Nichols, Tonya L

2017-01-01

In the event of an indoor release of an environmentally persistent microbial pathogen such as Bacillus anthracis, the potential for human exposure will be considered when remedial decisions are made. Microbial site characterization and clearance sampling data collected in the field might be used to estimate exposure. However, there are many challenges associated with estimating environmental concentrations of B. anthracis or other spore-forming organisms after such an event before being able to estimate exposure. These challenges include: (1) collecting environmental field samples that are adequate for the intended purpose, (2) conducting laboratory analyses and selecting the reporting format needed for the laboratory data, and (3) analyzing and interpreting the data using appropriate statistical techniques. This paper summarizes some key challenges faced in collecting, analyzing, and interpreting microbial field data from a contaminated site. Although the paper was written with considerations for B. anthracis contamination, it may also be applicable to other bacterial agents. It explores the implications and limitations of using field data for determining environmental concentrations both before and after decontamination. Several findings were of interest. First, to date, the only validated surface/sampling device combinations are swabs and sponge-sticks on stainless steel surfaces, thus limiting availability of quantitative analytical results which could be used for statistical analysis. Second, agreement needs to be reached with the analytical laboratory on the definition of the countable range and on reporting of data below the limit of quantitation. Finally, the distribution of the microbial field data and statistical methods needed for a particular data set could vary depending on these data that were collected, and guidance is needed on appropriate statistical software for handling microbial data. Further, research is needed to develop better methods to estimate human exposure from pathogens using environmental data collected from a field setting. PMID:26883476

EXAMPLES OF THE ROLE OF ANALYTICAL CHEMISTRY IN ENVIRONMENTAL RISK MANAGEMENT RESEARCH

EPA Science Inventory

Analytical chemistry is an important tier of environmental protection and has been traditionally linked to compliance and/or exposure monitoring activities for environmental contaminants. The adoption of the risk management paradigm has led to special challenges for analytical ch...

Liquid chromatography-tandem mass spectrometry analysis of perfluorooctane sulfonate and perfluorooctanoic Acid in fish fillet samples.

PubMed

Paiano, Viviana; Fattore, Elena; Carrà, Andrea; Generoso, Caterina; Fanelli, Roberto; Bagnati, Renzo

2012-01-01

Perfluorooctane sulfonate (PFOS) and perfluorooctanoic (PFOA) acid are persistent contaminants which can be found in environmental and biological samples. A new and fast analytical method is described here for the analysis of these compounds in the edible part of fish samples. The method uses a simple liquid extraction by sonication, followed by a direct determination using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The linearity of the instrumental response was good, with average regression coefficients of 0.9971 and 0.9979 for PFOS and PFOA, respectively, and the coefficients of variation (CV) of the method ranged from 8% to 20%. Limits of detection (LOD) were 0.04 ng/g for both the analytes and recoveries were 90% for PFOS and 76% for PFOA. The method was applied to samples of homogenized fillets of wild and farmed fish from the Mediterranean Sea. Most of the samples showed little or no contamination by perfluorooctane sulfonate and perfluorooctanoic acid, and the highest concentrations detected among the fish species analyzed were, respectively, 5.96 ng/g and 1.89 ng/g. The developed analytical methodology can be used as a tool to monitor and to assess human exposure to perfluorinated compounds through sea food consumption.

Analysis of CL-20 in environmental matrices: water and soil.

PubMed

Larson, Steven L; Felt, Deborah R; Davis, Jeffrey L; Escalon, Lynn

2002-04-01

Analytical techniques for the detection of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo(5.5.0.05,9.03,11)dodecane (CL-20) in water and soil are developed by adapting methods traditionally used for the analysis of nitroaromatics. CL-20 (a new explosives compound) is thermally labile, exhibits high polarity, and has low solubility in water. These constraints make the use of specialized sample handling, preparation, extraction, and analysis necessary. The ability to determine the concentrations of this new explosive compound in environmental matrices is helpful in understanding the environmental fate and effects of CL-20; understanding the physical, chemical, and biological fate of CL-20; and can be used in developing remediation technologies and determining their efficiency. The toxicity and mobility of new explosives in soil and groundwater are also of interest, and analytical techniques for quantitating CL-20 and its degradation products in soil and natural waters make these investigations possible.

Per- and Polyfluoroalkyl Substances (PFAS): Sampling ...

EPA Pesticide Factsheets

Per- and polyfluoroalkyl substances (PFAS) are a large group of manufactured compounds used in a variety of industries, such as aerospace, automotive, textiles, and electronics, and are used in some food packaging and firefighting materials. For example, they may be used to make products more resistant to stains, grease and water. In the environment, some PFAS break down very slowly, if at all, allowing bioaccumulation (concentration) to occur in humans and wildlife. Some have been found to be toxic to laboratory animals, producing reproductive, developmental, and systemic effects in laboratory tests. EPA's methods for analyzing PFAS in environmental media are in various stages of development. This technical brief summarizes the work being done to develop robust analytical methods for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids. The U.S. Environmental Protection Agency’s (EPA) methods for analyzing PFAS in environmental media are in various stages of development. EPA is working to develop robust analytical methods for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids.

Nitrate biosensors and biological methods for nitrate determination.

PubMed

Sohail, Manzar; Adeloju, Samuel B

2016-06-01

The inorganic nitrate (NO3‾) anion is present under a variety of both natural and artificial environmental conditions. Nitrate is ubiquitous within the environment, food, industrial and physiological systems and is mostly present as hydrated anion of a corresponding dissolved salt. Due to the significant environmental and toxicological effects of nitrate, its determination and monitoring in environmental and industrial waters are often necessary. A wide range of analytical techniques are available for nitrate determination in various sample matrices. This review discusses biosensors available for nitrate determination using the enzyme nitrate reductase (NaR). We conclude that nitrate determination using biosensors is an excellent non-toxic alternative to all other available analytical methods. Over the last fifteen years biosensing technology for nitrate analysis has progressed very well, however, there is a need to expedite the development of nitrate biosensors as a suitable alternative to non-enzymatic techniques through the use of different polymers, nanostructures, mediators and strategies to overcome oxygen interference. Copyright © 2016 Elsevier B.V. All rights reserved.

Superhydrophobic analyte concentration utilizing colloid-pillar array SERS substrates.

PubMed

Wallace, Ryan A; Charlton, Jennifer J; Kirchner, Teresa B; Lavrik, Nickolay V; Datskos, Panos G; Sepaniak, Michael J

2014-12-02

The ability to detect a few molecules present in a large sample is of great interest for the detection of trace components in both medicinal and environmental samples. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. The following work involves superhydrophobic surfaces that have as a framework deterministic or stochastic silicon pillar arrays formed by lithographic or metal dewetting protocols, respectively. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added to the functionalized pillar array system via soaking. Native pillars and pillars with hydrophobic modification are used. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A ≥ 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 × 10(-12) M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up uses in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.

Stir bar sorptive extraction and liquid chromatography-tandem mass spectrometry determination of polar and non-polar emerging and priority pollutants in environmental waters.

PubMed

Aparicio, Irene; Martín, Julia; Santos, Juan Luis; Malvar, José Luis; Alonso, Esteban

2017-06-02

An analytical method based on stir bar sorptive extraction (SBSE) was developed and validated for the determination of environmental concern pollutants in environmental waters by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Target compounds include six water and oil repellents (perfluorinated compounds), four preservatives (butylated hydroxytoluene and three parabens), two plasticizers (bisphenol A and di(2-ethylhexyl)phthalate), seven surfactants (four linear alkylbenzene sulfonates, nonylphenol and two nonylphenol ethoxylates), a flame retardant (hexabromocyclododecane), four hormones, fourteen pharmaceutical compounds, an UV-filter (2-ethylhexyl 4-methoxycinnamate) and nine pesticides. To achieve the simultaneous extraction of polar and non-polar pollutants two stir bar coatings were tested, the classic polydimethylsiloxane (PDMS) coating and the novel ethylene glycol modified silicone (EG-silicone). The best extraction recoveries were obtained using EG-silicone coating. The effects of sample pH, volume and ionic strength and extraction time on extraction recoveries were evaluated. The analytical method was validated for surface water and tap water samples. The method quantification limits ranged from 7.0ngL -1 to 177ngL -1 . The inter-day precision, expressed as relative standard deviation, was lower than 20%. Accuracy, expressed as relative recovery values, was in the range from 61 to 130%. The method was applied for the determination of the 48 target compounds in surface and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Screening Complex Effluents for Estrogenic Activity with the T47D-Kbluc Cell Bioassay: Assay Optimization and Comparison to In Vivo Responses in Fish

EPA Science Inventory

The endocrine activity of complex mixtures of chemicals associated with wastewater treatment plant effluents, runoff from concentrated animal feeding operations (CAFOs), and/or other environmental samples can be difficult to characterize based on analytical chemistry. In vitro bi...

Trace analysis of endocrine disrupting compounds in environmental water samples by use of solid-phase extraction and gas chromatography with mass spectrometry detection.

PubMed

Azzouz, Abdelmonaim; Ballesteros, Evaristo

2014-09-19

A novel analytical method using a continuous solid-phase extraction system in combination with gas chromatography-mass spectrometry for the simultaneous separation and determination of endocrine disrupting compounds (EDCs) is reported. The method was applied to major EDCs of various types including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in water. Samples were preconcentrated by using an automatic solid-phase extraction module containing a sorbent column, and retained analytes eluted with acetonitrile for derivatization with a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane. A number of variables potentially influencing recovery of the target compounds such as the type of SPE sorbent (Silica gel, Florisil, RP-C18, Amberlite XAD-2 and XAD-4, Oasis HLB and LiChrolut EN), eluent and properties of the water including pH and ionic strength, were examined. LiChrolut EN was found to be the most efficient sorbent for retaining the analytes, with ∼100% efficiency. The ensuing method was validated with good analytical results including low limits of detection (0.01-0.08ng/L for 100mL of sample) and good linearity (r(2)>0.997) throughout the studied concentration ranges. The method exhibited good accuracy (recoveries of 90-101%) and precision (relative standard deviations less than 7%) in the determination of EDCs in drinking, river, pond, well, swimming pool and waste water. Waste water samples were found to contain the largest number and highest concentrations of analytes (3.2-390ng/L). Copyright © 2014 Elsevier B.V. All rights reserved.

Application of microwave plasma atomic emission spectrometry (MP-AES) for environmental monitoring of industrially contaminated sites in Hyderabad city.

PubMed

Kamala C T; Balaram V; Dharmendra V; Satyanarayanan M; Subramanyam K S V; Krishnaiah A

2014-11-01

Recently introduced microwave plasma-atomic emission spectroscopy (MP-AES) represents yet another and very important addition to the existing array of modern instrumental analytical techniques. In this study, an attempt is made to summarize the performance characteristics of MP-AES and its potential as an analytical tool for environmental studies with some practical examples from Patancheru and Uppal industrial sectors of Hyderabad city. A range of soil, sediment, water reference materials, particulate matter, and real-life samples were chosen to evaluate the performance of this new analytical technique. Analytical wavelengths were selected considering the interference effects of other concomitant elements present in different sample solutions. The detection limits for several elements were found to be in the range from 0.05 to 5 ng/g. The trace metals analyzed in both the sectors followed the topography with more pollution in the low-lying sites. The metal contents were found to be more in ground waters than surface waters. Since a decade, the pollutants are transfered from Patancheru industrial area to Musi River. After polluting Nakkavagu and turning huge tracts of agricultural lands barren besides making people residing along the rivulet impotent and sick, industrialists of Patancheru are shifting the effluents to downstream of Musi River through an 18-km pipeline from Patancheru. Since the effluent undergoes primary treatment at Common Effluent Treatment Plant (CETP) at Patanchru and travels through pipeline and mixes with sewage, the organic effluents will be diluted. But the inorganic pollutants such as heavy and toxic metals tend to accumulate in the environmental segments near and downstreams of Musi River. The data generated by MP-AES of toxic metals like Zn, Cu, and Cr in the ground and surface waters can only be attributed to pollution from Patancheru since no other sources are available to Musi River.

"EMERGING" POLLUTANTS, AND COMMUNICATING THE ...

EPA Pesticide Factsheets

This paper weaves a rnulti-dimensioned perspective of mass spectrometry as a career against the backdrop of mass spectrometry's key role in the past and future of environmental chemistry. Along the way, some insights are offered for better focusing the spotlight on the discipline of mass spectrometry. A Foundation for Environmental Science-Mass Spectrometry Historically fundamental to our understanding of environmental processes and chemical pollution is mass spectrometry. This branch of analytical chemistry is the workhorse which supplies much of the definitive data to environmental scientists and engineers for identifying the molecular compositions, and ultimately the structures, of chemicals. This is not to ignore the complementary and critical roles played by the adjunct practices of sample enrichment (e.g., to lower method detection limits via any of various means of selective extraction) and analyte separation (e.g., to lessen contaminant interferences via the myriad forms of chromatography and electrophoresis). While the power of mass spectrometry has long been highly visible to the practicing environmental chemist, it borders on continued obscurity to the lay public and most non-chemists. Even though mass spectrometry has played a long, historic and Largely invisible role in establishing or undergirding our existing knowledge about environmental processes and pollution, what recognition it does enjoy is usually relegated to that of a tool. It is usually

Bioanalytical challenge: A review of environmental and pharmaceuticals contaminants in human milk.

PubMed

Lopes, Bianca Rebelo; Barreiro, Juliana Cristina; Cass, Quezia Bezerra

2016-10-25

An overview of bioanalytical methods for the determination of environmental and pharmaceutical contaminants in human milk is presented. The exposure of children to these contaminants through lactation has been widely investigated. The human milk contains diverse proteins, lipids, and carbohydrates and the concentration of these components is drastically altered during the lactation period providing a high degree of an analytical challenge. Sample collection and pretreatment are still considered the Achilles' heel. This review presents liquid chromatographic methods developed in the last 10 years for this complex matrix with focuses in the extraction and quantification steps. Green sample preparation protocols have been emphasized. Copyright © 2016 Elsevier B.V. All rights reserved.

The EPA National Fuels Surveillance Network. I. Trace constituents in gasoline and commercial gasoline fuel additives.

PubMed Central

Jungers, R H; Lee, R E; von Lehmden, D J

1975-01-01

A National Fuels Surveillance Network has been established to collect gasoline and other fuels through the 10 regional offices of the Environmental Protection Agency. Physical, chemical, and trace element analytical determinations are made on the collected fuel samples to detect components which may present an air pollution hazard or poison exhaust catalytic control devices. A summary of trace elemental constituents in over 50 gasoline samples and 18 commercially marketed consumer purchased gasoline additives is presented. Quantities of Mn, Ni, Cr, Zn, Cu, Fe, Sb, B, Mg, Pb, and S were found in most regular and premium gasoline. Environmental implications of trace constituents in gasoline are discussed. PMID:1157783

Rapid quantification of pharmaceuticals and pesticides in passive samplers using ultra high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Wille, Klaas; Claessens, Michiel; Rappé, Karen; Monteyne, Els; Janssen, Colin R; De Brabander, Hubert F; Vanhaecke, Lynn

2011-12-23

The presence of both pharmaceuticals and pesticides in the aquatic environment has become a well-known environmental issue during the last decade. An increasing demand however still exists for sensitive and reliable monitoring tools for these rather polar contaminants in the marine environment. In recent years, the great potential of passive samplers or equilibrium based sampling techniques for evaluation of the fate of these contaminants has been shown in literature. Therefore, we developed a new analytical method for the quantification of a high number of pharmaceuticals and pesticides in passive sampling devices. The analytical procedure consisted of extraction using 1:1 methanol/acetonitrile followed by detection with ultra-high performance liquid chromatography coupled to high resolution and high mass accuracy Orbitrap mass spectrometry. Validation of the analytical method resulted in limits of quantification and recoveries ranging between 0.2 and 20 ng per sampler sheet and between 87.9 and 105.2%, respectively. Determination of the sampler-water partition coefficients of all compounds demonstrated that several pharmaceuticals and most pesticides exert a high affinity for the polydimethylsiloxane passive samplers. Finally, the developed analytical methods were used to measure the time-weighted average (TWA) concentrations of the targeted pollutants in passive samplers, deployed at eight stations in the Belgian coastal zone. Propranolol, carbamazepine and seven pesticides were found to be very abundant in the passive samplers. These obtained long-term and large-scale TWA concentrations will contribute in assessing the environmental and human health risk of these emerging pollutants. Copyright © 2011 Elsevier B.V. All rights reserved.

External quality-assurance results for the National Atmospheric Deposition Program/National Trends Network, 2002-03

USGS Publications Warehouse

Wetherbee, Gregory A.; Latysh, Natalie E.; Burke, Kevin P.

2005-01-01

Six external quality-assurance programs were operated by the U.S. Geological Survey (USGS) External Quality-Assurance (QA) Project for the National Atmospheric Deposition Program/National Trends Network (NADP/NTN) from 2002 through 2003. Each program measured specific components of the overall error inherent in NADP/NTN wet-deposition measurements. The intersite-comparison program assessed the variability and bias of pH and specific conductance determinations made by NADP/NTN site operators twice per year with respect to accuracy goals. The percentage of site operators that met the pH accuracy goals decreased from 92.0 percent in spring 2002 to 86.3 percent in spring 2003. In these same four intersite-comparison studies, the percentage of site operators that met the accuracy goals for specific conductance ranged from 94.4 to 97.5 percent. The blind-audit program and the sample-handling evaluation (SHE) program evaluated the effects of routine sample handling, processing, and shipping on the chemistry of weekly NADP/NTN samples. The blind-audit program data indicated that the variability introduced by sample handling might be environmentally significant to data users for sodium, potassium, chloride, and hydrogen ion concentrations during 2002. In 2003, the blind-audit program was modified and replaced by the SHE program. The SHE program was designed to control the effects of laboratory-analysis variability. The 2003 SHE data had less overall variability than the 2002 blind-audit data. The SHE data indicated that sample handling buffers the pH of the precipitation samples and, in turn, results in slightly lower conductivity. Otherwise, the SHE data provided error estimates that were not environmentally significant to data users. The field-audit program was designed to evaluate the effects of onsite exposure, sample handling, and shipping on the chemistry of NADP/NTN precipitation samples. Field-audit results indicated that exposure of NADP/NTN wet-deposition samples to onsite conditions tended to neutralize the acidity of the samples by less than 1.0 microequivalent per liter. Onsite exposure of the sampling bucket appeared to slightly increase the concentration of most of the analytes but not to an extent that was environmentally significant to NADP data users. An interlaboratory-comparison program was used to estimate the analytical variability and bias of the NADP Central Analytical Laboratory (CAL) during 2002-03. Bias was identified in the CAL data for calcium, magnesium, sodium, potassium, ammonium, chloride, nitrate, sulfate, hydrogen ion, and specific conductance, but the absolute value of the bias was less than analytical minimum detection limits for all constituents except magnesium, nitrate, sulfate, and specific conductance. Control charts showed that CAL results were within statistical control approximately 90 percent of the time. Data for the analysis of ultrapure deionized-water samples indicated that CAL did not have problems with laboratory contamination. During 2002-03, the overall variability of data from the NADP/NTN precipitation-monitoring system was estimated using data from three collocated monitoring sites. Measurement differences of constituent concentration and deposition for paired samples from the collocated samplers were evaluated to compute error terms. The medians of the absolute percentage errors (MAEs) for the paired samples generally were larger for cations (approximately 8 to 50 percent) than for anions (approximately 3 to 33 percent). MAEs were approximately 16 to 30 percent for hydrogen-ion concentration, less than 10 percent for specific conductance, less than 5 percent for sample volume, and less than 8 percent for precipitation depth. The variability attributed to each component of the sample-collection and analysis processes, as estimated by USGS quality-assurance programs, varied among analytes. Laboratory analysis variability accounted for approximately 2 percent of the

Rainfall, Discharge, and Water-Quality Data During Stormwater Monitoring, July 1, 2008, to June 30, 2009 - Halawa Stream Drainage Basin and the H-1 Storm Drain, Oahu, Hawaii

USGS Publications Warehouse

Presley, Todd K.; Jamison, Marcael T.J.

2009-01-01

Storm runoff water-quality samples were collected as part of the State of Hawaii Department of Transportation Stormwater Monitoring Program. The program is designed to assess the effects of highway runoff and urban runoff on Halawa Stream, and to assess the effects from the H-1 storm drain on Manoa Stream. For this program, rainfall data were collected at three stations, continuous discharge data at five stations, and water-quality data at six stations, which include the five continuous discharge stations. This report summarizes rainfall, discharge, and water-quality data collected between July 1, 2008, and June 30, 2009. Within the Halawa Stream drainage area, three storms (October 25 and December 11, 2008, and February 3, 2009) were sampled during July 1, 2008, to June 30, 2009. A total of 43 environmental samples were collected during these three storms. During the storm of October 25, 2009, 31 samples were collected and analyzed individually for metals only. The other 12 samples from the other two storms were analyzed for some or all of the following analytes: total suspended solids, total dissolved solids, nutrients, chemical oxygen demand, and selected trace metals (cadmium, chromium, copper, lead, and zinc). Additionally, grab samples were analyzed for some or all of the following analytes: oil and grease, total petroleum hydrocarbons, fecal coliform, and biological oxygen demand. Some grab and composite samples were analyzed for only a partial list of these analytes, either because samples could not be delivered to the laboratory in a timely manner, or an insufficient volume of sample was collected by the automatic samplers. Two quality-assurance/quality-control samples were collected after cleaning automatic sampler lines to verify that the sampling lines were not contaminated. Four environmental samples were collected at the H-1 Storm Drain during July 1, 2008, to June 30, 2009. An oil and grease sample and a composite sample were collected during the storm on November 15, 2008, and two composite samples were collected during the January 11, 2009, storm. All samples at this site were collected using an automatic sampler. Samples were analyzed for some or all of the following analytes: total suspended solids, nutrients, oil and grease, total petroleum hydrocarbons, and selected trace metals (cadmium, chromium, copper, lead, nickel, and zinc). One qualityassurance/quality-control sample was collected after cleaning automatic sampler lines to verify that the sampling lines were not contaminated. During the storm of January 11, 2009, the two composite samples collected at H-1 Storm Drain were collected about three hours apart. Higher constituent concentrations were detected in the first 2 composite sample relative to the second composite sample, although the average discharge was higher during the period when the second sample was collected.

REVIEW ARTICLE: Environmental applications of analytical biosensors

NASA Astrophysics Data System (ADS)

Marco, María-Pilar; Barceló, Damià

1996-11-01

A review of the fundamental aspects and environmental applications of biosensors is presented. The bases of different transducer principles such as electrochemical, optical and piezoelectric are discussed. Various examples are given of the applications of such principles to develop immunosensor devices to determine common environmental contaminants. Attention is also paid to catalytic biosensors, using enzymes as sensing elements. Biosensor devices based on the use of cholinesterase and various oxidase enzymes such as tyrosinase, laccase, peroxidase and aldehyde dehydrogenase are reported. Some examples are given of the applications of other biomolecules such as whole cells, DNA or proteins, to determine pollution. Validation studies are presented comparing biosensors with chromatographic techniques to determine organophosphorus pesticides and phenolic compounds in environmental samples.

Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

PubMed

Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

2013-10-21

A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

Monitoring of emerging pollutants in Guadiamar River basin (South of Spain): analytical method, spatial distribution and environmental risk assessment.

PubMed

Garrido, Eva; Camacho-Muñoz, Dolores; Martín, Julia; Santos, Antonio; Santos, Juan Luis; Aparicio, Irene; Alonso, Esteban

2016-12-01

Guadiamar River is located in the southwest of the Iberian Peninsula and connects two protected areas in the South of Spain: Sierra Morena and Doñana National Park. It is sited in an area affected by urban, industrial and agriculture sewage pollution and with tradition on intensive mining activities. Most of the studies performed in this area have been mainly focused on the presence of heavy metals and, until now, little is known about the occurrence of other contaminants such as emerging organic pollutants (EOPs). In this work, an analytical method has been optimized and validated for monitoring of forty-seven EOPs in surface water. The analytical method has been applied to study the distribution and environmental risk of these pollutants in Guadiamar River basin. The analytical method was based on solid-phase extraction and determination by liquid chromatography-triple quadrupole-tandem mass spectrometry. The 60 % of the target compounds were found in the analyzed samples. The highest concentrations were found for two plasticizers (bisphenol A and di(2-ethyhexyl)phthalate, mean concentration up to 930 ng/L) and two pharmaceutical compounds (caffeine (up to 623 ng/L) and salicylic acid (up to 318 ng/L)). This study allowed to evaluate the potential sources (industrial or urban) of the studied compounds and the spatial distribution of their concentrations along the river. Environmental risk assessment showed a major risk on the south of the river, mainly due to discharges of wastewater effluents.

Bar adsorptive microextraction technique - application for the determination of pharmaceuticals in real matrices.

PubMed

Almeida, Carlos; Ahmad, Samir M; Nogueira, José Manuel F

2017-03-01

In the present work, bar adsorptive microextraction using miniaturized devices (7.5 × 3.0 mm) coated with suitable sorbent phases, combined with microliquid desorption (100 μL) followed by high-performance liquid chromatography with diode array detection (BAμE-μLD/HPLC-DAD), is proposed for the determination of trace level of six pharmaceuticals (furosemide, mebeverine, ketoprofen, naproxen, diclofenac and mefenamic acid) in environmental water and urine matrices. By comparing ten distinct sorbent materials (five polymeric and five activated carbons), the polymer P5 proved to be the most suitable to achieve the best selectivity and efficiency. The solvent volume minimization in the liquid desorption stage demonstrated remarkable effectiveness, being more environmentally friendly, and simultaneously increased the microextraction enrichment factor two-fold. Assays performed through BAμE(P5, 0.9 mg)-μLD(100 μL)/HPLC-DAD on 25 mL of ultrapure water samples spiked at the 4.0 μg/L level yielded average recoveries ranging from 91.4% (furosemide) to 101.0% (ketoprofen) with good precision (RSD < 10.6%), under optimized experimental conditions. The analytical performance showed convenient detection limits (25.0 - 120.0 ng/L), good linear dynamic ranges (0.1 to 24.0 μg/L), appropriate determination coefficients (r 2 > 0.9983), and excellent repeatability through intraday (RSD < 10.4%)) and interday (RSD < 10.0%) assays. By using the standard addition methodology, the application of the present analytical approach on environmental waters and urine samples revealed the occurrence of trace levels of some pharmaceuticals. The solvent minimization during the back-extraction step associated with the miniaturization of BAμE devices proved to be a very promising analytical technology for static microextraction analysis. Graphical abstract BAμE operating under the floating sampling technology for the determination of pharmaceuticals in aqueous media.

Environmental Monitoring and the Gas Industry: Program Manager Handbook

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gregory D. Gillispie

1997-12-01

This document has been developed for the nontechnical gas industry manager who has the responsibility for the development of waste or potentially contaminated soil and groundwater data or must make decisions based on such data for the management or remediation of these materials. It explores the pse of common analytical chemistry instrumentation and associated techniques for identification of environmentally hazardous materials. Sufficient detail is given to familiarize the nontechnical reader with the principles behind the operation of each technique. The scope and realm of the techniques and their constituent variations are portrayed through a discussion of crucial details and, wheremore » appropriate, the depiction of real-life data. It is the author's intention to provide an easily understood handbook for gas industry management. Techniques which determine the presence, composition, and quantification of gas industry wastes are discussed. Greater focus is given to traditional techniques which have been the mainstay of modem analytical benchwork. However, with the continual advancement of instrumental principles and design, several techniques have been included which are likely to receive greater attention in fiture considerations for waste-related detection. Definitions and concepts inherent to a thorough understanding of the principles common to analytical chemistry are discussed. It is also crucial that gas industry managers understand the effects of the various actions which take place before, during, and after the actual sampling step. When a series of sample collection, storage, and transport activities occur, new or inexperienced project managers may overlook or misunderstand the importance of the sequence. Each step has an impact on the final results of the measurement process; errors in judgment or decision making can be costly. Specific techniques and methodologies for the collection, storage, and transport of environmental media samples are not described or discussed in detail in thk handbook. However, the underlying philosophy regarding the importance of proper collection, storage, and transport practices, as well as pertinent references, are presented.« less

Rapid Radiochemical Analyses in Support of Fukushima Nuclear Accident - 13196

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples [1, 2]. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and datamore » assessment teams were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90}Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation [3, 4]. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride precipitations, followed by Sr-Resin separation and gas flow proportional counting. To achieve a lower detection limit for analysis of some of the Japanese soil samples, a 10 gram aliquot of soil was taken, acid-leached and processed with similar preconcentration chemistry. The MDA using this approach was ∼0.03 pCi/g (1.1 mBq/g)/, which is less than the 0.05-0.10 pCi/g {sup 90}Sr levels found in soil as a result of global fallout. The chemical yields observed for the Japanese soil samples was typically 75-80% and the laboratory control sample (LCS) and matrix spike (MS) results looked very good for this work Individual QC results were well within the ± 25% acceptable range and the average of these results does not show significant bias. Additional data for a radiostrontium in soil method for 50 gram samples will also be presented, which appears to be a significant step forward based on looking at the current literature, with higher chemical yields for even larger sample aliquots and lower MDA [5, 6, 7] Hou et al surveyed a wide range of separation methods for Pu in waters and environmental solid samples [8]. While there are many actinide methods in the scientific literature, few would be considered rapid due to the tedious and time-consuming steps involved. For actinide analyses in soil, a new rapid method for the determination of actinide isotopes in soil samples using both alpha spectrometry and inductively-coupled plasma mass spectrometry was employed. The new rapid soil method utilizes an acid leaching method, iron/titanium hydroxide precipitation, a lanthanum fluoride soil matrix removal step, and a rapid column separation process with TEVA Resin. The large soil matrix is removed easily and rapidly using these two simple precipitations with high chemical recoveries and effective removal of interferences. [9, 10] Vacuum box technology and rapid flow rates were used to reduce analytical time. Challenges associated with the mineral content in the volcanic soil will be discussed. Air filter samples were reported within twenty-four (24) hours of receipt using rapid techniques published previously. [11] The rapid reporting of high quality analytical data arranged through the U.S. Department of Energy Consequence Management Home Team was critical to allow the government of Japan to readily evaluate radiological impacts from the nuclear reactor incident to both personnel and the environment. SRNL employed unique rapid methods capability for radionuclides to support Japan that can also be applied to environmental, bioassay and waste management samples. New rapid radiochemical techniques for radionuclides in soil and other environmental matrices as well as some of the unique challenges associated with this work will be presented that can be used for application to environmental monitoring, environmental remediation, decommissioning and decontamination activities. (authors)« less

RAPID RADIOCHEMICAL ANALYSES IN SUPPORT OF FUKUSHIMA NUCLEAR ACCIDENT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S.

2012-11-07

There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and data assessment teamsmore » were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90} Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride precipitations, followed by Sr-Resin separation and gas flow proportional counting. To achieve a lower detection limit for analysis of some of the Japanese soil samples, a 10 gram aliquot of soil was taken, acid-leached and processed with similar preconcentration chemistry. The MDA using this approach was ~0.03 pCi/g (1.1 mBq/g)/, which is less than the 0.05-0.10 pCi/g {sup 90}Sr levels found in soil as a result of global fallout. The chemical yields observed for the Japanese soil samples was typically 75-80% and the laboratory control sample (LCS) and matrix spike (MS) results looked very good for this work Individual QC results were well within the ± 25% acceptable range and the average of these results does not show significant bias. Additional data for a radiostrontium in soil method for 50 gram samples will also be presented, which appears to be a significant step forward based on looking at the current literature, with higher chemical yields for even larger sample aliquots and lower MDA. Hou et al surveyed a wide range of separation methods for Pu in waters and environmental solid samples. While there are many actinide methods in the scientific literature, few would be considered rapid due to the tedious and time-consuming steps involved. For actinide analyses in soil, a new rapid method for the determination of actinide isotopes in soil samples using both alpha spectrometry and inductively-coupled plasma mass spectrometry was employed. The new rapid soil method utilizes an acid leaching method, iron/titanium hydroxide precipitation, a lanthanum fluoride soil matrix removal step, and a rapid column separation process with TEVA Resin. The large soil matrix is removed easily and rapidly using these two simple precipitations with high chemical recoveries and effective removal of interferences. Vacuum box technology and rapid flow rates were used to reduce analytical time. Challenges associated with the mineral content in the volcanic soil will be discussed. Air filter samples were reported within twenty-four (24) hours of receipt using rapid techniques published previously. The rapid reporting of high quality analytical data arranged through the U.S. Department of Energy Consequence Management Home Team was critical to allow the government of Japan to readily evaluate radiological impacts from the nuclear reactor incident to both personnel and the environment. SRNL employed unique rapid methods capability for radionuclides to support Japan that can also be applied to environmental, bioassay and waste management samples. New rapid radiochemical techniques for radionuclides in soil and other environmental matrices as well as some of the unique challenges associated with this work will be presented that can be used for application to environmental monitoring, environmental remediation, decommissioning and decontamination activities.« less

An overview of the main foodstuff sample preparation technologies for tetracycline residue determination.

PubMed

Pérez-Rodríguez, Michael; Pellerano, Roberto Gerardo; Pezza, Leonardo; Pezza, Helena Redigolo

2018-05-15

Tetracyclines are widely used for both the treatment and prevention of diseases in animals as well as for the promotion of rapid animal growth and weight gain. This practice may result in trace amounts of these drugs in products of animal origin, such as milk and eggs, posing serious risks to human health. The presence of tetracycline residues in foods can lead to the transmission of antibiotic-resistant pathogenic bacteria through the food chain. In order to ensure food safety and avoid exposure to these substances, national and international regulatory agencies have established tolerance levels for authorized veterinary drugs, including tetracycline antimicrobials. In view of that, numerous sensitive and specific methods have been developed for the quantification of these compounds in different food matrices. One will note, however, that the determination of trace residues in foods such as milk and eggs often requires extensive sample extraction and preparation prior to conducting instrumental analysis. Sample pretreatment is usually the most complicated step in the analytical process and covers both cleaning and pre-concentration. Optimal sample preparation can reduce analysis time and sources of error, enhance sensitivity, apart from enabling unequivocal identification, confirmation and quantification of target analytes. The development and implementation of more environmentally friendly analytical procedures, which involve the use of less hazardous solvents and smaller sample sizes compared to traditional methods, is a rapidly increasing trend in analytical chemistry. This review seeks to provide an updated overview of the main trends in sample preparation for the determination of tetracycline residues in foodstuffs. The applicability of several extraction and clean-up techniques employed in the analysis of foodstuffs, especially milk and egg samples, is also thoroughly discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

Impact of pesticide use by smallholder farmers on water quality in the Wakiso District, Uganda

NASA Astrophysics Data System (ADS)

Oltramare, Christelle; Weiss, Frederik T.; Atuhaire, Aggrey; Staudacher, Philipp; Niwagaba, Charles; Stamm, Christian

2017-04-01

As in many tropical countries, farmers of the Wakiso District rely on heavy use of pesticides to protect crops and animals. This may impair human and environmental health due to poor application techniques, misuse of pesticide bins or diffuse pesticide losses from the treated fields during intense tropical rainstorms. The extent of pollution in different environmental compartments however, are generally only poorly documented. The same holds true for quantitative data on the relevance of different transport pathways of pesticides into the environment. Part of the limited knowledge is caused by the demanding sampling and analytical techniques that are necessary to obtain robust data on the actual pollution status. Especially in surface waters, pesticide concentration may vary rapidly in time such that grab samples may yield a very incomplete picture. This incompleteness was often enhanced because of limited analytical windows that covered only a small fraction of the pesticides actually used. In this presentation, we describe an approach to overcome these limitations to a large extent by using three different passive sampling devices and two broad analytical techniques (GC-MS/MS, LC HR-MS) that allow the quantification of about 260 different pesticides. We will present how these approaches are implemented in the catchment area of the Wakiso District in Uganda. This area is intensively used by smallholder farmers who grow a large set of different crops. Diffuse losses are expected to occur mainly during the two rainy seasons (March to May and September to November). Accordingly, the study will focus on this situation.

The role of field auditing in environmental quality assurance management.

PubMed

Claycomb, D R

2000-01-01

Environmental data quality improvement continues to focus on analytical laboratoryperformance with little, if any, attention given to improving the performance of field consultants responsible for sample collection. Many environmental professionals often assume that the primary opportunity for data error lies within the activities conducted by the laboratory. Experience in the evaluation of environmental data and project-wide quality assurance programs indicates that an often-ignored factor affecting environmental data quality is the manner in which a sample is acquired and handled in the field. If a sample is not properly collected, preserved, stored, and transported in the field, even the best laboratory practices and analytical methods cannot deliver accurate and reliable data (i.e., bad data in equals bad data out). Poor quality environmental data may result in inappropriate decisions regarding site characterization and remedial action. Field auditing is becoming an often-employed technique for examining the performance of the environmental sampling field team and how their performance may affect data quality. The field audits typically focus on: (1) verifying that field consultants adhere to project control documents (e.g., Work Plans and Standard Operating Procedures [SOPs]) during field operations; (2) providing third-party independent assurance that field procedures, quality assurance/ quality control (QA/QC)protocol, and field documentation are sufficient to produce data of satisfactory quality; (3) providing a defense in the event that field procedures are called into question; and (4) identifying ways to reduce sampling costs. Field audits are typically most effective when performed on a surprise basis; that is, the sampling contractor may be aware that a field audit will be conducted during some phase of sampling activities but is not informed of the specific day(s) that the audit will be conducted. The audit also should be conducted early on in the sampling program such that deficiencies noted during the audit can be addressed before the majority of field activities have been completed. A second audit should be performed as a follow-up to confirm that the recommended changes have been implemented. A field auditor is assigned to the project by matching, as closely as possible, the auditor's experience with the type of field activities being conducted. The auditor uses a project-specific field audit checklist developed from key information contained in project control documents. Completion of the extensive audit checklist during the audit focuses the auditor on evaluating each aspect of field activities being performed. Rather than examine field team performance after sampling, a field auditor can do so while the samples are being collected and can apply real-time corrective action as appropriate. As a result of field audits, responsible parties often observe vast improvements in their consultant's field procedures and, consequently, receive more reliable and representative field data at a lower cost. The cost savings and improved data quality that result from properly completed field audits make the field auditing process both cost-effective and functional.

An approach toward quantification of organic compounds in complex environmental samples using high-resolution electrospray ionization mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nguyen, Tran B.; Nizkorodov, Sergey; Laskin, Alexander

2013-01-07

Quantitative analysis of individual compounds in complex mixtures using high-resolution electrospray ionization mass spectrometry (HR-ESI-MS) is complicated by differences in the ionization efficiencies of analyte molecules in the mixture, resulting in signal suppression during ionization. However, the ability to obtain concentration estimates of compounds in an environmental sample is important for data interpretation and comparison. We introduce an approach for estimating mass concentrations of analytes observed in a multicomponent mixture by HR-ESI-MS, without prior separation. The approach relies on a calibration of the instrument using appropriate standards added to the mixture of studied analytes. An illustration of how the proposedmore » calibration can be applied in practice is provided for aqueous extracts of isoprene photooxidation organic aerosol, with multifunctional organic acids standards. We show that the observed ion sensitivities in ESI-MS are positively correlated with the “adjusted mass,” defined as a product of the molecular mass and the H/C ratio in the molecule (adjusted mass = H/C x molecular mass). The correlation of the observed ESI sensitivity with adjusted mass is justified by considering trends of the physical and chemical properties of organic compounds that affect ionization in the positive ion mode, i.e., gas-phase basicity, polarizability, and molecular size.« less

Homeland Security Research Improves the Nation's Ability to ...

EPA Pesticide Factsheets

Technical Brief Homeland Security (HS) Research develops data, tools, and technologies to minimize the impact of accidents, natural disasters, terrorist attacks, and other incidents that can result in toxic chemical, biological or radiological (CBR) contamination. HS Research develops ways to detect contamination, sampling strategies, sampling and analytical methods, cleanup methods, waste management approaches, exposure assessment methods, and decision support tools (including water system models). These contributions improve EPA’s response to a broad range of environmental disasters.

Speciation of chromium in environmental samples by dual electromembrane extraction system followed by high performance liquid chromatography.

PubMed

Safari, Meysam; Nojavan, Saeed; Davarani, Saied Saeed Hosseiny; Morteza-Najarian, Amin

2013-07-30

This study proposes the dual electromembrane extraction followed by high performance liquid chromatography for selective separation-preconcentration of Cr(VI) and Cr(III) in different environmental samples. The method was based on the electrokinetic migration of chromium species toward the electrodes with opposite charge into the two different hollow fibers. The extractant was then complexed with ammonium pyrrolidinedithiocarbamate for HPLC analysis. The effects of analytical parameters including pH, type of organic solvent, sample volume, stirring rate, time of extraction and applied voltage were investigated. The results showed that Cr(III) and Cr(VI) could be simultaneously extracted into the two different hollow fibers. Under optimized conditions, the analytes were quantified by HPLC instrument, with acceptable linearity ranging from 20 to 500 μg L(-1) (R(2) values≥0.9979), and repeatability (RSD) ranging between 9.8% and 13.7% (n=5). Also, preconcentration factors of 21.8-33 that corresponded to recoveries ranging from 31.1% to 47.2% were achieved for Cr(III) and Cr(VI), respectively. The estimated detection limits (S/N ratio of 3:1) were less than 5.4 μg L(-1). Finally, the proposed method was successfully applied to determine Cr(III) and Cr(VI) species in some real water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Design, characterization and comparison of materials based on β and γ cyclodextrin covalently connected to microporous silica for environmental analysis.

PubMed

Belenguer-Sapiña, Carolina; Pellicer-Castell, Enric; El Haskouri, Jamal; Guillem, Carmen; Simó-Alfonso, Ernesto Francisco; Amorós, Pedro; Mauri-Aucejo, Adela

2018-08-17

Determination of organic pollutants in environmental samples presents great difficulties due to the lack of sensitivity and selectivity in many of the existing analytical methods. In this work, the efficiency of materials based on silica structures containing bounded γ-cyclodextrin has been evaluated to determinate phenolic compounds and polycyclic aromatic hydrocarbons in air and water samples, respectively, in comparison with materials made of β-cyclodextrin. According to the results obtained for the material characterization, the new γ-cyclodextrin solid phase does not apparently present any porosity when used in air samples, but it has been shown to work efficiently for the preconcentration of polycyclic aromatic hydrocarbons in water, with recoveries around 80%. In addition, the use of the β-cyclodextrin material for phenolic compounds sampling can be highlighted with recoveries between 83% and 95%, and recoveries for 4-vinylphenol and 2-methoxy-4-vinylphenol have been especially improved in comparison with the use of materials containing trapped β-cyclodextrin in our previous researches. The observed phenomena can be explained on the basis of the analyte molecules size and the diameter of the cyclodextrin cavities, the influence of the cyclodextrin type in the material structure as well as on the interactions taking place with the pollutants and the influence of the matrix type in the retention and desorption mechanisms. Copyright © 2018 Elsevier B.V. All rights reserved.

Trace level detection of compounds related to the chemical weapons convention by 1H-detected 13C NMR spectroscopy executed with a sensitivity-enhanced, cryogenic probehead.

PubMed

Cullinan, David B; Hondrogiannis, George; Henderson, Terry J

2008-04-15

Two-dimensional 1H-13C HSQC (heteronuclear single quantum correlation) and fast-HMQC (heteronuclear multiple quantum correlation) pulse sequences were implemented using a sensitivity-enhanced, cryogenic probehead for detecting compounds relevant to the Chemical Weapons Convention present in complex mixtures. The resulting methods demonstrated exceptional sensitivity for detecting the analytes at trace level concentrations. 1H-13C correlations of target analytes at < or = 25 microg/mL were easily detected in a sample where the 1H solvent signal was approximately 58,000-fold more intense than the analyte 1H signals. The problem of overlapping signals typically observed in conventional 1H spectroscopy was essentially eliminated, while 1H and 13C chemical shift information could be derived quickly and simultaneously from the resulting spectra. The fast-HMQC pulse sequences generated magnitude mode spectra suitable for detailed analysis in approximately 4.5 h and can be used in experiments to efficiently screen a large number of samples. The HSQC pulse sequences, on the other hand, required roughly twice the data acquisition time to produce suitable spectra. These spectra, however, were phase-sensitive, contained considerably more resolution in both dimensions, and proved to be superior for detecting analyte 1H-13C correlations. Furthermore, a HSQC spectrum collected with a multiplicity-edited pulse sequence provided additional structural information valuable for identifying target analytes. The HSQC pulse sequences are ideal for collecting high-quality data sets with overnight acquisitions and logically follow the use of fast-HMQC pulse sequences to rapidly screen samples for potential target analytes. Use of the pulse sequences considerably improves the performance of NMR spectroscopy as a complimentary technique for the screening, identification, and validation of chemical warfare agents and other small-molecule analytes present in complex mixtures and environmental samples.

Groundwater-quality and quality-control data for two monitoring wells near Pavillion, Wyoming, April and May 2012

USGS Publications Warehouse

Wright, Peter R.; McMahon, Peter B.; Mueller, David K.; Clark, Melanie L.

2012-01-01

In June 2010, the U.S. Environmental Protection Agency installed two deep monitoring wells (MW01 and MW02) near Pavillion, Wyoming, to study groundwater quality. During April and May 2012, the U.S Geological Survey, in cooperation with the Wyoming Department of Environmental Quality, collected groundwater-quality data and quality-control data from monitoring well MW01 and, following well redevelopment, quality-control data for monitoring well MW02. Two groundwater-quality samples were collected from well MW01—one sample was collected after purging about 1.5 borehole volumes, and a second sample was collected after purging 3 borehole volumes. Both samples were collected and processed using methods designed to minimize atmospheric contamination or changes to water chemistry. Groundwater-quality samples were analyzed for field water-quality properties (water temperature, pH, specific conductance, dissolved oxygen, oxidation potential); inorganic constituents including naturally occurring radioactive compounds (radon, radium-226 and radium-228); organic constituents; dissolved gasses; stable isotopes of methane, water, and dissolved inorganic carbon; and environmental tracers (carbon-14, chlorofluorocarbons, sulfur hexafluoride, tritium, helium, neon, argon, krypton, xenon, and the ratio of helium-3 to helium-4). Quality-control sample results associated with well MW01 were evaluated to determine the extent to which environmental sample analytical results were affected by bias and to evaluate the variability inherent to sample collection and laboratory analyses. Field documentation, environmental data, and quality-control data for activities that occurred at the two monitoring wells during April and May 2012 are presented.

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

PubMed

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of alternative preservatives in cosmetic products by chromophoric derivatization followed by vortex-assisted liquid-liquid semimicroextraction and liquid chromatography.

PubMed

Miralles, Pablo; Vrouvaki, Ilianna; Chisvert, Alberto; Salvador, Amparo

2016-07-01

An analytical method for the simultaneous determination of phenethyl alcohol, methylpropanediol, phenylpropanol, caprylyl glycol, and ethylhexylglycerin, which are used as alternative preservatives in cosmetic products, has been developed. The method is based on liquid chromatography with UV spectrophotometric detection after chromophoric derivatization with benzoyl chloride and vortex-assisted liquid-liquid semimicroextraction. Different chromatographic parameters, derivatization conditions, and sample preparation variables were studied. Under optimized conditions, the limits of detection values for the analytes ranged from 0.02 to 0.06µgmL(-1). The method was validated with good recovery values (84-118%) and precision values (3.9-9.5%). It was successfully applied to 10 commercially available cosmetic samples. The good analytical features of the proposed method besides of its environmentally-friendly characteristics, make it useful to carry out the quality control of cosmetic products containing the target compounds as preservative agents. Copyright © 2016 Elsevier B.V. All rights reserved.

Halogenated hydrocarbon pesticides and other volatile organic contaminants provide analytical challenges in global trading.

PubMed

Budnik, Lygia T; Fahrenholtz, Svea; Kloth, Stefan; Baur, Xaver

2010-04-01

Protection against infestation of a container cargo by alien species is achieved by mandatory fumigation with pesticides. Most of the effective fumigants are methyl and ethyl halide gases that are highly toxic and are a risk to both human health and the environment. There is a worldwide need for a reliable and robust analytical screening procedure for these volatile chemicals in a multitude of health and environmental scenarios. We have established a highly sensitive broad spectrum mass spectrometry method combined with thermal desorption gas chromatography to detect, identify and quantify volatile pesticide residues. Using this method, 1201 random ambient air samples taken from freight containers arriving at the biggest European ports of Hamburg and Rotterdam were analyzed over a period of two and a half years. This analytical procedure is a valuable strategy to measure air pollution from these hazardous chemicals, to help in the identification of pesticides in the new mixtures/formulations that are being adopted globally and to analyze expired breath samples after suspected intoxication in biomonitoring.

Cork-based activated carbons as supported adsorbent materials for trace level analysis of ibuprofen and clofibric acid in environmental and biological matrices.

PubMed

Neng, N R; Mestre, A S; Carvalho, A P; Nogueira, J M F

2011-09-16

In this contribution, powdered activated carbons (ACs) from cork waste were supported for bar adsorptive micro-extraction (BAμE), as novel adsorbent phases for the analysis of polar compounds. By combining this approach with liquid desorption followed by high performance liquid chromatography with diode array detection (BAμE(AC)-LD/HPLC-DAD), good analytical performance was achieved using clofibric acid (CLOF) and ibuprofen (IBU) model compounds in environmental and biological matrices. Assays performed on 30 mL water samples spiked at the 25.0 μg L(-1) level yielded recoveries around 80% for CLOF and 95% for IBU, under optimized experimental conditions. The ACs textural and surface chemistry properties were correlated with the results obtained. The analytical performance showed good precision (<15%), suitable detection limits (0.24 and 0.78 μg L(-1) for CLOF and IBU, respectively) and good linear dynamic ranges (r(2)>0.9922) from 1.0 to 600.0 μg L(-1). By using the standard addition methodology, the application of the present approach to environmental water and urine matrices allowed remarkable performance at the trace level. The proposed methodology proved to be a viable alternative for acidic pharmaceuticals analysis, showing to be easy to implement, reliable, sensitive and requiring low sample volume to monitor these priority compounds in environmental and biological matrices. Copyright © 2011 Elsevier B.V. All rights reserved.

The Savannah River Site`s Groundwater Monitoring Program, first quarter 1989

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The Environmental Monitoring Section of the Environmental and Health Protection (EHP) Department administers the Savannah River Site`s Groundwater Monitoring Program. During first quarter 1989 (January--March), EHP conducted routine sampling of monitoring wells and drinking water locations. EHP collected the drinking water samples from Savannah River Site (SRS) drinking water systems supplied by wells. EHP established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria aid personnel in sample scheduling, interpretation of data, and trend identification. The flagging criteria are based on detection limits, background levels in SRS groundwater, and drinking watermore » standards. An explanation of flagging criteria for the first quarter is presented in the Flagging Criteria section of this document. All analytical results from first quarter 1989 are listed in this report, which is distributed to all waste-site custodians.« less

The Savannah River Site`s Groundwater Monitoring Program, third quarter 1989

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The Environmental Monitoring Section of the Environmental and Health Protection (EHP) Department administers the Savannah River Site`s Groundwater Monitoring Program. During third quarter 1989 (July--September), EHP conducted routine sampling of monitoring wells and drinking water locations. EHP collected the drinking water samples from Savannah River Site (SRS) drinking water systems supplied by wells. EHP established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria do not define contamination levels; instead they aid personnel in sample scheduling, interpretation of data, and trend identification. The flagging criteria are based on detection limits, backgroundmore » levels in SRS groundwater, and drinking water standards. An explanation of flagging criteria for the third quarter is presented in the Flagging Criteria section of this document. All analytical results from third quarter 1989 are listed in this report, which is distributed to all waste-site custodians.« less

The Savannah River Site's Groundwater Monitoring Program, third quarter 1989

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The Environmental Monitoring Section of the Environmental and Health Protection (EHP) Department administers the Savannah River Site's Groundwater Monitoring Program. During third quarter 1989 (July--September), EHP conducted routine sampling of monitoring wells and drinking water locations. EHP collected the drinking water samples from Savannah River Site (SRS) drinking water systems supplied by wells. EHP established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria do not define contamination levels; instead they aid personnel in sample scheduling, interpretation of data, and trend identification. The flagging criteria are based on detection limits, backgroundmore » levels in SRS groundwater, and drinking water standards. An explanation of flagging criteria for the third quarter is presented in the Flagging Criteria section of this document. All analytical results from third quarter 1989 are listed in this report, which is distributed to all waste-site custodians.« less

The Savannah River Site's Groundwater Monitoring Program, first quarter 1989

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The Environmental Monitoring Section of the Environmental and Health Protection (EHP) Department administers the Savannah River Site's Groundwater Monitoring Program. During first quarter 1989 (January--March), EHP conducted routine sampling of monitoring wells and drinking water locations. EHP collected the drinking water samples from Savannah River Site (SRS) drinking water systems supplied by wells. EHP established two sets of flagging criteria in 1986 to assist in the management of sample results. The flagging criteria aid personnel in sample scheduling, interpretation of data, and trend identification. The flagging criteria are based on detection limits, background levels in SRS groundwater, and drinking watermore » standards. An explanation of flagging criteria for the first quarter is presented in the Flagging Criteria section of this document. All analytical results from first quarter 1989 are listed in this report, which is distributed to all waste-site custodians.« less

Validation of an advanced analytical procedure applied to the measurement of environmental radioactivity.

PubMed

Thanh, Tran Thien; Vuong, Le Quang; Ho, Phan Long; Chuong, Huynh Dinh; Nguyen, Vo Hoang; Tao, Chau Van

2018-04-01

In this work, an advanced analytical procedure was applied to calculate radioactivity in spiked water samples in a close geometry gamma spectroscopy. It included MCNP-CP code in order to calculate the coincidence summing correction factor (CSF). The CSF results were validated by a deterministic method using ETNA code for both p-type HPGe detectors. It showed that a good agreement for both codes. Finally, the validity of the developed procedure was confirmed by a proficiency test to calculate the activities of various radionuclides. The results of the radioactivity measurement with both detectors using the advanced analytical procedure were received the ''Accepted'' statuses following the proficiency test. Copyright © 2018 Elsevier Ltd. All rights reserved.

An analytical method for 14C in environmental water based on a wet-oxidation process.

PubMed

Huang, Yan-Jun; Guo, Gui-Yin; Wu, Lian-Sheng; Zhang, Bing; Chen, Chao-Feng; Zhang, Hai-Ying; Qin, Hong-Juan; Shang-Guan, Zhi-Hong

2015-04-01

An analytical method for (14)C in environmental water based on a wet-oxidation process was developed. The method can be used to determine the activity concentrations of organic and inorganic (14)C in environmental water, or total (14)C, including in drinking water, surface water, rainwater and seawater. The wet-oxidation of the organic component allows the conversion of organic carbon to an inorganic form, and the extraction of the inorganic (14)C can be achieved by acidification and nitrogen purging. Environmental water with a volume of 20 L can be used for the wet-oxidation and extraction, and a detection limit of about 0.02 Bq/g(C) can be achieved for water with carbon content above 15 mg(C)/L, obviously lower than the natural level of (14)C in the environment. The collected carbon is sufficient for measurement with a low level liquid scintillation counter (LSC) for typical samples. Extraction or recovery experiments for inorganic carbon and organic carbon from typical materials, including analytical reagents of organic benzoquinone, sucrose, glutamic acid, nicotinic acid, humic acid, ethane diol, et cetera., were conducted with excellent results based on measurement on a total organic carbon analyzer and LSC. The recovery rate for inorganic carbon ranged tween 98.7%-99.0% with a mean of 98.9(± 0.1)%, for organic carbon recovery ranged between 93.8% and 100.0% with a mean of 97.1(± 2.6)%. Verification and an uncertainty budget of the method are also presented for a representative environmental water. The method is appropriate for (14)C analysis in environmental water, and can be applied also to the analysis of liquid effluent from nuclear facilities. Copyright © 2015 Elsevier Ltd. All rights reserved.

Solid-phase nano-extraction and laser-excited time-resolved Shpol'skii spectroscopy for the analysis of polycyclic aromatic hydrocarbons in drinking water samples.

PubMed

Wang, Huiyong; Yu, Shenjiang; Campiglia, Andres D

2009-02-15

A unique method for screening polycyclic aromatic hydrocarbons in drinking water samples is reported. Water samples (500 microl) are mixed and centrifuged with 950 microl of a commercial solution of 20 nm gold nanoparticles for pollutants extraction. The precipitate is treated with 2 microl of 1-pentanethiol and 48 microl of n-octane, and the supernatant is then analyzed via laser-excited time-resolved Shpol'skii spectroscopy. Fifteen priority pollutants are directly determined at liquid helium temperature (4.2 K) with the aid of a cryogenic fiber-optic probe. Unambiguous pollutant determination is carried out via spectral and lifetime analysis. Limits of detection are at the parts-per-trillion level. Analytical recoveries are similar to those obtained via high-performance liquid chromatography. The simplicity of the experimental procedure, use of microliters of organic solvent, short analysis time, selectivity, and excellent analytical figures of merit demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.

Concentrations of tritium and strontium-90 in water from selected wells at the Idaho National Engineering Laboratory after purging one, two, and three borehole volumes

USGS Publications Warehouse

Bartholomay, R.C.

1993-01-01

Water from 11 wells completed in the Snake River Plain aquifer at the Idaho National Engineering Laboratory was sampled as part of the U.S. Geological Survey's quality assurance program to determine the effect of purging different borehole volumes on tritium and strontium-90 concentrations. Wells were selected for sampling on the basis of the length of time it took to purge a borehole volume of water. Samples were collected after purging one, two, and three borehole volumes. The U.S. Department of Energy's Radiological and Environmental Sciences Laboratory provided analytical services. Statistics were used to determine the reproducibility of analytical results. The comparison between tritium and strontium-90 concentrations after purging one and three borehole volumes and two and three borehole volumes showed that all but two sample pairs with defined numbers were in statistical agreement. Results indicate that concentrations of tritium and strontium-90 are not affected measurably by the number of borehole volumes purged.

[Antibiotic Residue in Environmental Water in Vietnam].

PubMed

Harada, Kazuo

2018-01-01

　The increasing prevalence of antimicrobial resistance (AMR) has caused intractable infections worldwide. Nearly 50% of the healthy population of Southeast Asia carries extended-spectrum β-lactamase (ESBL)-producing Escherichia coli. The overuse of antimicrobial agents in the agriculture, aquaculture, and medical care sectors causes environmental pollution, facilitating the spread of AMR. However, there is a lack of data pertaining to antimicrobial residues in environmental water in such regions. We investigated a total of 49 chemicals, including β-lactams, sulfonamides, quinolones, and tetracyclines. Water samples were collected from rivers in city centers, and ponds in livestock and aquaculture farms, in Ha Noi, Thai Binh, and Can Tho in Vietnam. We detected antimicrobial agents at 87 of 111 sampling sites (78.4%). Among the target analytes, sulfamethoxazole, sulfamethazine, trimethoprim, cephalexin, and ofloxacin were detected frequently. The residual levels of each antimicrobial agent ranged from 0.1 to 10000 ng/L. Moreover, we detected multi-drug resistant E. coli in fishes sampled from these rivers, suggesting unwanted effects of antimicrobial residues in the environment.

Genus-specific PCR Primers Targeting Intracellular Parasite Euduboscquella (Dinoflagellata: Syndinea)

NASA Astrophysics Data System (ADS)

Jung, Jae-Ho; Choi, Jung Min; Kim, Young-Ok

2018-03-01

We designed a genus-specific primer pair targeting the intracellular parasite Euduboscquella. To increase target specificity and inhibit untargeted PCR, two nucleotides were added at the 3' end of the reverse primer, one being a complementary nucleotide to the Euduboscquella-specific SNP (single-nucleotide polymorphism) and the other a deliberately mismatched nucleotide. Target specificity of the primer set was verified experimentally using PCR of two Euduboscquella species (positive controls) and 15 related species (negative controls composed of ciliates, diatoms and dinoflagellates), and analytical comparison with SILVA SSU rRNA gene database (release 119) in silico. In addition, we applied the Euduboscquella-specific primer set to four environmental samples previously determined by cytological staining to be either positive or negative for Euduboscquella. As expected, only positive controls and environmental samples known to contain Euduboscquella were successfully amplified by the primer set. An inferred SSU rRNA gene phylogeny placed environmental samples containing aloricate ciliates infected by Euduboscquella in a cluster discrete from Euduboscquella groups a-d previously reported from loricate, tintinnid ciliates.

Do complex matrices modify the sorptive properties of polydimethylsiloxane (PDMS) for non-polar organic chemicals?

PubMed

Jahnke, Annika; Mayer, Philipp

2010-07-16

The partitioning of non-polar analytes into the silicone polydimethylsiloxane (PDMS) is the basis for many analytical approaches such as solid phase microextraction (SPME), stir bar sorptive extraction (SBSE) and environmental passive sampling. Recently, the methods have been applied to increasingly complex sample matrices. The present work investigated the possible effect of complex matrices on the sorptive properties of PDMS. First, SPME fibers with a 30 microm PDMS coating were immersed in 15 different matrices, including sediment, suspensions of soil and humic substances, mayonnaise, meat, fish, olive oil and fish oil. Second, the surface of the fibers was wiped clean, and together with matrix-free control fibers, they were exposed via headspace to 7 non-polar halogenated organic chemicals in spiked olive oil. The fibers were then solvent-extracted, analyzed, and the ratios of the mean concentrations in the matrix-immersed fibers to the control fibers were determined for all matrices. These ratios ranged from 92% to 112% for the four analytes with the highest analytical precision (i.e. polychlorinated biphenyls (PCBs) 3, 28, 52 and brominated diphenyl ether (BDE) 3), and they ranged from 74% to 133% for the other three compounds (i.e. PCBs 101, 105 and gamma-hexachlorocyclohexane (HCH)). We conclude that, for non-polar, hydrophobic chemicals, the sorptive properties of the PDMS were not modified by the diverse investigated media and consequently that PDMS is suited for sampling of these analytes even in highly complex matrices. 2010 Elsevier B.V. All rights reserved.

Coupling of multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction with pulse glow discharge-ion mobility spectrometry for analysis of triazine herbicides in water and soil samples.

PubMed

Zou, Nan; Yuan, Chunhao; Liu, Shaowen; Han, Yongtao; Li, Yanjie; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

2016-07-29

An analytical method based on stir bar sorptive extraction (SBSE) coupled with pulse glow discharge-ion mobility spectrometry (PGD-IMS) was developed for analysis of three triazine pesticide residues in water and soil samples. An injection port with sealing device and stir bars hold device were designed and constructed to directly position the SBSE fiber including the extracted samples into the heating device, making desorption and detection of analytes proceeded simultaneously. The extraction conditions such as SBSE solid phase material, extraction time, extraction temperature, pH value and salt concentration were optimized. Mixture of MWCNTs-COOH and PDMS were shown to be effective in enriching the triazines. The LODs and LOQs of three triazines were found to be 0.006-0.015μgkg(-1) and 0.02-0.05μgkg(-1), and the linear range was 0.05-10μgL(-1) with determination coefficients from 0.9987 to 0.9993. The SBSE-PGD-IMS method was environmentally friendly without organic solvent consumption in the entire experimental procedures, and it was demonstrated to be a commendable rapid analysis technique for analysis of triazine pesticide residues in environmental samples on site. The proposed method was applied for the analysis of real ground water, surface water and soil samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Identification of microplastics by FTIR and Raman microscopy: a novel silicon filter substrate opens the important spectral range below 1300 cm(-1) for FTIR transmission measurements.

PubMed

Käppler, Andrea; Windrich, Frank; Löder, Martin G J; Malanin, Mikhail; Fischer, Dieter; Labrenz, Matthias; Eichhorn, Klaus-Jochen; Voit, Brigitte

2015-09-01

The presence of microplastics in aquatic ecosystems is a topical problem and leads to the need of appropriate and reliable analytical methods to distinctly identify and to quantify these particles in environmental samples. As an example transmission, Fourier transform infrared (FTIR) imaging can be used to analyze samples directly on filters without any visual presorting, when the environmental sample was afore extracted, purified, and filtered. However, this analytical approach is strongly restricted by the limited IR transparency of conventional filter materials. Within this study, we describe a novel silicon (Si) filter substrate produced by photolithographic microstructuring, which guarantees sufficient transparency for the broad mid-infrared region of 4000-600 cm(-1). This filter type features holes with a diameter of 10 μm and exhibits adequate mechanical stability. Furthermore, it will be shown that our Si filter substrate allows a distinct identification of the most common microplastics, polyethylene (PE), and polypropylene (PP), in the characteristic fingerprint region (1400-600 cm(-1)). Moreover, using the Si filter substrate, a differentiation of microparticles of polyesters having quite similar chemical structure, like polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), is now possible, which facilitates a visualization of their distribution within a microplastic sample by FTIR imaging. Finally, this Si filter can also be used as substrate for Raman microscopy-a second complementary spectroscopic technique-to identify microplastic samples.

Hydrophilic interaction liquid chromatography coupled to high-resolution mass spectrometry to determine artificial sweeteners in environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2015-06-01

Artificial sweeteners are food additives employed as sugar substitutes which are now considered to be emerging organic contaminants. In the present study, a method is developed for the determination of a group of artificial sweeteners in environmental waters. Considering the polar and hydrophilic character of these compounds, hydrophilic interaction liquid chromatography is proposed for their separation as an alternative to traditional reversed-phase liquid chromatography. Two stationary phases with different chemistry were compared for this purpose. For the detection of the analytes, high-resolution mass spectrometry (Orbitrap) was employed to take advantage of its benefits in terms of reliable quantification and confirmation for the measurement of accurate masses. Solid-phase extraction was chosen as the sample treatment, in which the extract in a mixture of NH4OH:MeOH:ACN (1:4:15) was directly injected into the chromatographic system, simplifying the analytical procedure. The optimized method was validated on river and waste water samples. For example, in the case of effluent water samples, limits of detection ranged from 0.002 to 0.7 μg/L and limits of quantification ranged from 0.004 to 1.5 μg/L. Apparent (whole method) recoveries ranged from 57 to 74% with intra-day precision (%RSD, n = 5) ranging from 6 to 25%. The method was successfully applied to water samples from different rivers in Catalonia and different waste water treatment plants in Tarragona. Acesulfame, cyclamate, saccharine and sucralose were found in several samples.

Evaluation of polyethersulfone performance for the microextraction of polar chlorinated herbicides from environmental water samples.

PubMed

Prieto, Ailette; Rodil, Rosario; Quintana, José Benito; Cela, Rafael; Möder, Monika; Rodríguez, Isaac

2014-05-01

In this work, the suitability of bulk polyethersulfone (PES) for sorptive microextraction of eight polar, chlorinated phenoxy acids and dicamba from environmental water samples is assessed and the analytical features of the optimized method are compared to those reported for other microextraction techniques. Under optimized conditions, extractions were performed with samples (18 mL) adjusted at pH 2 and containing a 30% (w/v) of sodium chloride, using a tubular PES sorbent (1 cm length × 0.7 mm o.d., sorbent volume 8 µL). Equilibrium conditions were achieved after 3h of direct sampling, with absolute extraction efficiencies ranging from 39 to 66%, depending on the compound. Analytes were recovered soaking the polymer with 0.1 mL of ethyl acetate, derivatized and determined by gas chromatography-mass spectrometry (GC-MS). Achieved quantification limits (LOQs) varied between 0.005 and 0.073 ng mL(-1). After normalization with the internal surrogate (IS), the efficiency of the extraction was only moderately affected by the particular characteristics of different water samples (surface and sewage water); thus, pseudo-external calibration, using spiked ultrapure water solutions, can be used as quantification technique. The reduced cost of the PES polymer allowed considering it as a disposable sorbent, avoiding variations in the performance of the extraction due to cross-contamination problems and/or surface modification with usage. Copyright © 2014 Elsevier B.V. All rights reserved.

External Quality Assurance Programs Managed by the U.S. Geological Survey in Support of the National Atmospheric Deposition Program/Mercury Deposition Network

USGS Publications Warehouse

Latysh, Natalie E.; Wetherbee, Gregory A.

2007-01-01

The U.S. Geological Survey (USGS) Branch of Quality Systems operates external quality assurance programs for the National Atmospheric Deposition Program/Mercury Deposition Network (NADP/MDN). Beginning in 2004, three programs have been implemented: the system blank program, the interlaboratory comparison program, and the blind audit program. Each program was designed to measure error contributed by specific components in the data-collection process. The system blank program assesses contamination that may result from sampling equipment, field exposure, and routine handling and processing of the wet-deposition samples. The interlaboratory comparison program evaluates bias and precision of analytical results produced by the Mercury Analytical Laboratory (HAL) for the NADP/MDN, operated by Frontier GeoSciences, Inc. The HAL's performance is compared with the performance of five other laboratories. The blind audit program assesses bias and variability of MDN data produced by the HAL using solutions disguised as environmental samples to ascertain true laboratory performance. This report documents the implementation of quality assurance procedures for the NADP/MDN and the operating procedures for each of the external quality assurance programs conducted by the USGS. The USGS quality assurance information provides a measure of confidence to NADP/MDN data users that measurement variability is distinguished from environmental signals.

A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

PubMed

Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

2013-01-01

A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

Contemporary sample stacking in analytical electrophoresis.

PubMed

Malá, Zdena; Gebauer, Petr; Boček, Petr

2011-01-01

Sample stacking is of vital importance for analytical CE since it may bring the required sensitivity of analyses. A lot of new relevant papers are published every year and regular surveys seem to be very helpful for experts and practitioners. The contribution presented here is a continuation of a series of regularly published reviews on the topic and covers the last two years. It brings a survey of related literature organized, in accord with the main principle used in the procedure published, in the following mainstream sections: Kohlrausch adjustment of concentrations, pH step, micellar systems and combined techniques. Each part covers literature sorted according to the field of application as, e.g. clinical, pharmaceutical, food, environmental, etc. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Applicability of TaqMan-Based Quantitative Real-Time PCR Assays for Detecting and Enumerating Cryptosporidium spp. Oocysts in the Environment

PubMed Central

Staggs, Sarah E.; Beckman, Erin M.; Keely, Scott P.; Mackwan, Reena; Ware, Michael W.; Moyer, Alan P.; Ferretti, James A.; Sayed, Abu; Xiao, Lihua; Villegas, Eric N.

2013-01-01

Quantitative real-time polymerase chain reaction (qPCR) assays to detect Cryptosporidium oocysts in clinical samples are increasingly being used to diagnose human cryptosporidiosis, but a parallel approach for detecting and identifying Cryptosporidium oocyst contamination in surface water sources has yet to be established for current drinking water quality monitoring practices. It has been proposed that Cryptosporidium qPCR-based assays could be used as viable alternatives to current microscopic-based detection methods to quantify levels of oocysts in drinking water sources; however, data on specificity, analytical sensitivity, and the ability to accurately quantify low levels of oocysts are limited. The purpose of this study was to provide a comprehensive evaluation of TaqMan-based qPCR assays, which were developed for either clinical or environmental investigations, for detecting Cryptosporidium oocyst contamination in water. Ten different qPCR assays, six previously published and four developed in this study were analyzed for specificity and analytical sensitivity. Specificity varied between all ten assays, and in one particular assay, which targeted the Cryptosporidium 18S rRNA gene, successfully detected all Cryptosporidium spp. tested, but also cross-amplified T. gondii, fungi, algae, and dinoflagellates. When evaluating the analytical sensitivity of these qPCR assays, results showed that eight of the assays could reliably detect ten flow-sorted oocysts in reagent water or environmental matrix. This study revealed that while a qPCR-based detection assay can be useful for detecting and differentiating different Cryptosporidium species in environmental samples, it cannot accurately measure low levels of oocysts that are typically found in drinking water sources. PMID:23805235

Data Validation Package - July 2016 Groundwater Sampling at the Gunnison, Colorado, Disposal Site

DOE Office of Scientific and Technical Information (OSTI.GOV)

Linard, Joshua; Campbell, Sam

Groundwater sampling at the Gunnison, Colorado, Disposal Site is conducted every 5 years to monitor disposal cell performance. During this event, samples were collected from eight monitoring wells as specified in the 1997 Long-Term Surveillance Plan for the Gunnison, Colorado, Disposal Site. Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for US Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated, http://energy.gov/lm/downloads/sampling-and­ analysis-plan-us-department-energy-office-legacy-management-sites). Planned monitoring locations are shown in Attachment 1, Sampling and Analysis Work Order. A duplicate sample was collected from location 0723. Water levels were measured at all monitoring wells thatmore » were sampled and seven additional wells. The analytical data and associated qualifiers can be viewed in environmental database reports and are also available for viewing with dynamic mapping via the GEMS (Geospatial Environmental Mapping System) website at http://gems.lm.doe.gov/#. No issues were identified during the data validation process that require additional action or follow-up.« less

Comparison of procedures for correction of matrix interferences in the analysis of soils by ICP-OES with CCD detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sadler, D.A.; Sun, F.; Littlejohn, D.

1995-12-31

ICP-OES is a useful technique for multi-element analysis of soils. However, as a number of elements are present in relatively high concentrations, matrix interferences can occur and examples have been widely reported. The availability of CCD detectors has increased the opportunities for rapid multi-element, multi-wave-length determination of elemental concentrations in soils and other environmental samples. As the composition of soils from industrial sites can vary considerably, especially when taken from different pit horizons, procedures are required to assess the extent of interferences and correct the effects, on a simultaneous multi-element basis. In single element analysis, plasma operating conditions can sometimesmore » be varied to minimize or even remove multiplicative interferences. In simultaneous multi-element analysis, the scope for this approach may be limited, depending on the spectrochemical characteristics of the emitting analyte species. Matrix matching, by addition of major sample components to the analyte calibrant solutions, can be used to minimize inaccuracies. However, there are also limitations to this procedure, when the sample composition varies significantly. Multiplicative interference effects can also be assessed by a {open_quotes}single standard addition{close_quotes} of each analyte to the sample solution and the information obtained may be used to correct the analyte concentrations determined directly. Each of these approaches has been evaluated to ascertain the best procedure for multi-element analysis of industrial soils by ICP-OES with CCD detection at multiple wavelengths. Standard reference materials and field samples have been analyzed to illustrate the efficacy of each procedure.« less

Collection methods and quality assessment for Esche-richia coli, water quality, and microbial source tracking data within Tumacácori National Historical Park and the upper Santa Cruz River, Arizona, 2015-16

USGS Publications Warehouse

Paretti, Nicholas; Coes, Alissa L.; Kephart, Christopher M.; Mayo, Justine

2018-03-05

Tumacácori National Historical Park protects the culturally important Mission, San José de Tumacácori, while also managing a portion of the ecologically diverse riparian corridor of the Santa Cruz River. This report describes the methods and quality assurance procedures used in the collection of water samples for the analysis of Escherichia coli (E. coli), microbial source tracking markers, suspended sediment, water-quality parameters, turbidity, and the data collection for discharge and stage; the process for data review and approval is also described. Finally, this report provides a quantitative assessment of the quality of the E. coli, microbial source tracking, and suspended sediment data.The data-quality assessment revealed that bias attributed to field and laboratory contamination was minimal, with E. coli detections in only 3 out of 33 field blank samples analyzed. Concentrations in the field blanks were several orders of magnitude lower than environmental concentrations. The microbial source tracking (MST) field blank was below the detection limit for all MST markers analyzed. Laboratory blanks for E. coli at the USGS Arizona Water Science Center and laboratory blanks for MST markers at the USGS Ohio Water Microbiology Laboratory were all below the detection limit. Irreplicate data for E. coli and suspended sediment indicated that bias was not introduced to the data by combining samples collected using discrete sampling methods with samples collected using automatic sampling methods.The split and sequential E. coli replicate data showed consistent analytical variability and a single equation was developed to explain the variability of E. coli concentrations. An additional analysis of analytical variability for E. coli indicated analytical variability around 18 percent relative standard deviation and no trend was observed in the concentration during the processing and analysis of multiple split-replicates. Two replicate samples were collected for MST and individual markers were compared for a base flow and flood sample. For the markers found in common between the two types of samples, the relative standard deviation for the base flow sample was more than 3 times greater than the markers in the flood sample. Sequential suspended sediment replicates had a relative standard deviation of about 1.3 percent, indicating that environmental and analytical variability was minimal.A holding time review and laboratory study analysis supported the extended holding times required for this investigation. Most concentrations for flood and base-flow samples were within the theoretical variability specified in the most probable number approach suggesting that extended hold times did not overly influence the final concentrations reported.

Detection of low-concentration host mRNA transcripts in Malawian children at risk for environmental enteropathy

USDA-ARS?s Scientific Manuscript database

Transcriptomic analysis of fecal samples is an emerging method for the diagnosis of gastrointestinal pathology because it is noninvasive and requires minute volumes of analyte; however, detection of mRNA in low copy numbers in human stool is challenging. Our objective was to develop a method for det...

Quantitative Digital Autoradiography for Environmental Swipe Sample Prioritization: System design, Characterization, and Initial Measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

McDonald, Benjamin S.; Zalavadia, Mital A.; Miller, Brian W.

Environmental sampling and sample analyses by the International Atomic Energy Agency’s (IAEA) Network of Analytical Laboratories (NWAL) is a critical technical tool used to detect facility misuse under a Comprehensive Safeguards Agreement and to verify the absence of undeclared nuclear material activities under an Additional Protocol. Currently all environmental swipe samples (ESS) are screened using gamma spectrometry and x-ray fluorescence to estimate the amount of U and/or Pu in the ESS, to guide further analysis, and to assist in the shipment of ESS to the NWAL. Quantitative Digital Autoradiography for Environmental Samples (QDARES) is being developed to complement existing techniquesmore » through the use of a portable, real-time, high-spatial-resolution camera called the Ionizing-radiation Quantum Imaging Detector (iQID). The iQID constructs a spatial map of radionuclides within a sample or surface in real-time as charged particles (betas) and photons (gamma/x-rays) are detected and localized on an event-by-event basis. Knowledge of the location and nature of radioactive hot spots on the ESS could provide information for subsequent laboratory analysis. As a nondestructive technique, QDARES does not compromise the ESS chain of custody or subsequent laboratory analysis. In this paper we will present the system design and construction, characterization measurements with calibration sources, and initial measurements of ESS.« less

Condensed Phase Membrane Introduction Mass Spectrometry with Direct Electron Ionization: On-line Measurement of PAHs in Complex Aqueous Samples

NASA Astrophysics Data System (ADS)

Termopoli, Veronica; Famiglini, Giorgio; Palma, Pierangela; Cappiello, Achille; Vandergrift, Gregory W.; Krogh, Erik T.; Gill, Chris G.

2016-02-01

Polycyclic aromatic hydrocarbons (PAHs) are USEPA regulated priority pollutants. Their low aqueous solubility requires very sensitive analytical methods for their detection, typically involving preconcentration steps. Presented is the first demonstrated `proof of concept' use of condensed phase membrane introduction mass spectrometry (CP-MIMS) coupled with direct liquid electron ionization (DEI) for the direct, on-line measurement of PAHs in aqueous samples. DEI is very well suited for the ionization of PAHs and other nonpolar compounds, and is not significantly influenced by the co-elution of matrix components. Linear calibration data for low ppb levels of aqueous naphthalene, anthracene, and pyrene is demonstrated, with measured detection limits of 4 ppb. Analytical response times (t10%-90% signal rise) ranged from 2.8 min for naphthalene to 4.7 min for pyrene. Both intra- and interday reproducibility has been assessed (<3% and 5% RSD, respectively). Direct measurements of ppb level PAHs spiked in a variety of real, complex environmental sample matrices is examined, including natural waters, sea waters, and a hydrocarbon extraction production waste water sample. For these spiked, complex samples, direct PAH measurement by CP-MIMS-DEI yielded minimal signal suppression from sample matrix effects (81%-104%). We demonstrate the use of this analytical approach to directly monitor real-time changes in aqueous PAH concentrations with potential applications for continuous on-line monitoring strategies and binding/adsorption studies in heterogeneous samples.

Novel capsule phase microextraction in combination with liquid chromatography-tandem mass spectrometry for determining personal care products in environmental water.

PubMed

Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Marcé, Rosa Maria; Fontanals, Núria

2018-05-01

A novel sample preparation technique named capsule phase microextraction (CPME) is presented here. The technique utilizes a miniaturized microextraction capsule (MEC) as the extraction medium. The MEC consists of two conjoined porous tubular polypropylene membranes, one of which encapsulates the sorbent through sol-gel technology, while the other encapsulates a magnetic metal rod. As such, MEC integrates both the extraction and stirring mechanisms into a single device. The aim of this article is to demonstrate the application potential of CPME as sample preparation technique for the extraction of a group of personal care products (PCPs) from water matrices. Among the different sol-gel sorbent materials (UCON ® , poly(caprolactone-dimethylsiloxane-caprolactone) (PCAP-DMS-CAP) and Carbowax 20M (CW-20M)) evaluated, CW-20M MEC demonstrated the best extraction performance for the selected PCPs. The extraction conditions for sol-gel CW-20M MEC were optimized, including sample pH, stirring speed, addition of salt, extraction time, sample volume, liquid desorption solvent, and time. Under the optimal conditions, sol-gel CW-20M MEC provided recoveries, ranging between 47 and 90% for all analytes, except for ethylparaben, which showed a recovery of 26%. The method based on CPME with sol-gel CW-20M followed by liquid chromatography-tandem mass spectrometry was developed and validated for the extraction of PCPs from river water and effluent wastewater samples. When analyzing different environmental samples, some analytes such as 2,4-dihydroxybenzophenone, 2,2-dihydroxy-4-4 methoxybenzophenone and 3-benzophenone were found at low ng L -1 .

Impact of urine preservation methods and duration of storage on measured levels of environmental contaminants.

PubMed

Hoppin, Jane A; Ulmer, Ross; Calafat, Antonia M; Barr, Dana B; Baker, Susan V; Meltzer, Helle M; Rønningen, Kjersti S

2006-01-01

Collection of urine samples in human studies involves choices regarding shipping, sample preservation, and storage that may ultimately influence future analysis. As more studies collect and archive urine samples to evaluate environmental exposures in the future, we were interested in assessing the impact of urine preservative, storage temperature, and time since collection on nonpersistent contaminants in urine samples. In spiked urine samples stored in three types of urine vacutainers (no preservative, boric acid, and chlorhexidine), we measured five groups of contaminants to assess the levels of these analytes at five time points (0, 24, 48, and 72 h, and 1 week) and at two temperatures (room temperature and 4 degrees C). The target chemicals were bisphenol A (BPA), metabolites of organophosphate (OP), carbamate, and pyrethroid insecticides, chlorinated phenols, and phthalate monoesters, and were measured using five different mass spectrometry-based methods. Three samples were analyzed at each time point, with the exception of BPA. Repeated measures analysis of variance was used to evaluate effects of storage time, temperature, and preservative. Stability was summarized with percent change in mean concentration from time 0. In general, most analytes were stable under all conditions with changes in mean concentration over time, temperature, and preservative being generally less than 20%, with the exception of the OP metabolites in the presence of boric acid. The effect of storage temperature was less important than time since collection. The precision of the laboratory measurements was high allowing us to observe small differences, which may not be important when categorizing individuals into broader exposure groups.

Sequim Marine Research Laboratory routine environmental measurements during CY-1976

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fix, J.J.; Blumer, P.J.

1977-05-01

Beginning in 1976, a routine environmental program was established at the Marine Research Laboratory (MRL) at Sequim, Washington. The program is designed, primarily, to determine levels of radioactivity present in selected biota in Sequim Bay. The biota were selected because of their presence near the laboratory and their capacity to concentrate trace elements. Other samples were obtained to determine the radionuclides in Sequim Bay and laboratory drinking water, as well as the ambient radiation exposure levels and surface deposition of fallout radionuclides for the laboratory area. A summary of the analytical methods used is included. The present document includes datamore » obtained during CY 1976, the first year of the program. Radionuclides present in samples are attributed to fallout. Data are included on content of oil and Cu in seawater samples.« less

Sensor Analytics: Radioactive gas Concentration Estimation and Error Propagation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Dale N.; Fagan, Deborah K.; Suarez, Reynold

2007-04-15

This paper develops the mathematical statistics of a radioactive gas quantity measurement and associated error propagation. The probabilistic development is a different approach to deriving attenuation equations and offers easy extensions to more complex gas analysis components through simulation. The mathematical development assumes a sequential process of three components; I) the collection of an environmental sample, II) component gas extraction from the sample through the application of gas separation chemistry, and III) the estimation of radioactivity of component gases.

A field study of selected U.S. Geological Survey analytical methods for measuring pesticides in filtered stream water, June - September 2012

USGS Publications Warehouse

Martin, Jeffrey D.; Norman, Julia E.; Sandstrom, Mark W.; Rose, Claire E.

2017-09-06

U.S. Geological Survey monitoring programs extensively used two analytical methods, gas chromatography/mass spectrometry and liquid chromatography/mass spectrometry, to measure pesticides in filtered water samples during 1992–2012. In October 2012, the monitoring programs began using direct aqueous-injection liquid chromatography tandem mass spectrometry as a new analytical method for pesticides. The change in analytical methods, however, has the potential to inadvertently introduce bias in analysis of datasets that span the change.A field study was designed to document performance of the new method in a variety of stream-water matrices and to quantify any potential changes in measurement bias or variability that could be attributed to changes in analytical methods. The goals of the field study were to (1) summarize performance (bias and variability of pesticide recovery) of the new method in a variety of stream-water matrices; (2) compare performance of the new method in laboratory blank water (laboratory reagent spikes) to that in a variety of stream-water matrices; (3) compare performance (analytical recovery) of the new method to that of the old methods in a variety of stream-water matrices; (4) compare pesticide detections and concentrations measured by the new method to those of the old methods in a variety of stream-water matrices; (5) compare contamination measured by field blank water samples in old and new methods; (6) summarize the variability of pesticide detections and concentrations measured by the new method in field duplicate water samples; and (7) identify matrix characteristics of environmental water samples that adversely influence the performance of the new method. Stream-water samples and a variety of field quality-control samples were collected at 48 sites in the U.S. Geological Survey monitoring networks during June–September 2012. Stream sites were located across the United States and included sites in agricultural and urban land-use settings, as well as sites on major rivers.The results of the field study identified several challenges for the analysis and interpretation of data analyzed by both old and new methods, particularly when data span the change in methods and are combined for analysis of temporal trends in water quality. The main challenges identified are large (greater than 30 percent), statistically significant differences in analytical recovery, detection capability, and (or) measured concentrations for selected pesticides. These challenges are documented and discussed, but specific guidance or statistical methods to resolve these differences in methods are beyond the scope of the report. The results of the field study indicate that the implications of the change in analytical methods must be assessed individually for each pesticide and method.Understanding the possible causes of the systematic differences in concentrations between methods that remain after recovery adjustment might be necessary to determine how to account for the differences in data analysis. Because recoveries for each method are independently determined from separate reference standards and spiking solutions, the differences might be due to an error in one of the reference standards or solutions or some other basic aspect of standard procedure in the analytical process. Further investigation of the possible causes is needed, which will lead to specific decisions on how to compensate for these differences in concentrations in data analysis. In the event that further investigations do not provide insight into the causes of systematic differences in concentrations between methods, the authors recommend continuing to collect and analyze paired environmental water samples by both old and new methods. This effort should be targeted to seasons, sites, and expected concentrations to supplement those concentrations already assessed and to compare the ongoing analytical recovery of old and new methods to those observed in the summer and fall of 2012.

Optimization and evaluation of multi-bed adsorbent tube method in collection of volatile organic compounds

NASA Astrophysics Data System (ADS)

Ho, Steven Sai Hang; Wang, Liqin; Chow, Judith C.; Watson, John G.; Xue, Yonggang; Huang, Yu; Qu, Linli; Li, Bowei; Dai, Wenting; Li, Lijuan; Cao, Junji

2018-04-01

The feasibility of using adsorbent tubes to collect volatile organic compounds (VOCs) has been demonstrated since the 1990's and standardized as Compendium Method TO-17 by the U.S. Environmental Protection Agency (U.S EPA). This paper investigates sampling and analytical variables on concentrations of 57 ozone (O3) precursors (C2-C12 aliphatic and aromatic VOCs) specified for the Photochemical Assessment Monitoring Station (PAMS). Laboratory and field tests examined multi-bed adsorbent tubes containing a sorbate combination of Tenax TA, Carbograph 1 TD, and Carboxen 1003. Analyte stabilities were influenced by both collection tube temperature and ambient O3 concentrations. Analytes degraded during storage, while blank levels were elevated by passive adsorption. Adsorbent tube storage under cold temperatures (- 10 °C) in a preservation container filled with solid silica gel and anhydrous calcium sulfate (CaSO4) ensured sample integrity. A high efficiency (> 99%) O3 scrubber (i.e., copper coil tube filled with saturated potassium iodide [KI]) removed O3 (i.e., < 200 ppbv) from the air stream with a sampling capacity of 30 h. Water vapor scrubbers interfered with VOC measurements. The optimal thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) desorption time of 8 min was found at 330 °C. Good linearity (R2 > 0.995) was achieved for individual analyte calibrations (with the exception of acetylene) for mixing ratios of 0.08-1.96 ppbv. The method detection limits (MDLs) were below 0.055 ppbv for a 3 L sample volume. Replicate analyses showed relative standard deviations (RSDs) of < 10%, with the majority of the analytes within < 5%.

A wall-free climate unit for acoustic levitators.

PubMed

Schlegel, M C; Wenzel, K-J; Sarfraz, A; Panne, U; Emmerling, F

2012-05-01

Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses.

A wall-free climate unit for acoustic levitators

NASA Astrophysics Data System (ADS)

Schlegel, M. C.; Wenzel, K.-J.; Sarfraz, A.; Panne, U.; Emmerling, F.

2012-05-01

Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses.

MS-Based Analytical Techniques: Advances in Spray-Based Methods and EI-LC-MS Applications

PubMed Central

Medina, Isabel; Cappiello, Achille; Careri, Maria

2018-01-01

Mass spectrometry is the most powerful technique for the detection and identification of organic compounds. It can provide molecular weight information and a wealth of structural details that give a unique fingerprint for each analyte. Due to these characteristics, mass spectrometry-based analytical methods are showing an increasing interest in the scientific community, especially in food safety, environmental, and forensic investigation areas where the simultaneous detection of targeted and nontargeted compounds represents a key factor. In addition, safety risks can be identified at the early stage through online and real-time analytical methodologies. In this context, several efforts have been made to achieve analytical instrumentation able to perform real-time analysis in the native environment of samples and to generate highly informative spectra. This review article provides a survey of some instrumental innovations and their applications with particular attention to spray-based MS methods and food analysis issues. The survey will attempt to cover the state of the art from 2012 up to 2017. PMID:29850370

Analytic Complexity and Challenges in Identifying Mixtures of Exposures Associated with Phenotypes in the Exposome Era.

PubMed

Patel, Chirag J

2017-01-01

Mixtures, or combinations and interactions between multiple environmental exposures, are hypothesized to be causally linked with disease and health-related phenotypes. Established and emerging molecular measurement technologies to assay the exposome , the comprehensive battery of exposures encountered from birth to death, promise a new way of identifying mixtures in disease in the epidemiological setting. In this opinion, we describe the analytic complexity and challenges in identifying mixtures associated with phenotype and disease. Existing and emerging machine-learning methods and data analytic approaches (e.g., "environment-wide association studies" [EWASs]), as well as large cohorts may enhance possibilities to identify mixtures of correlated exposures associated with phenotypes; however, the analytic complexity of identifying mixtures is immense. If the exposome concept is realized, new analytical methods and large sample sizes will be required to ascertain how mixtures are associated with disease. The author recommends documenting prevalent correlated exposures and replicated main effects prior to identifying mixtures.

Development of liquid chromatography high resolution mass spectrometry strategies for the screening of complex organic matter: Application to astrophysical simulated materials.

PubMed

Eddhif, Balkis; Allavena, Audrey; Liu, Sylvie; Ribette, Thomas; Abou Mrad, Ninette; Chiavassa, Thierry; d'Hendecourt, Louis Le Sergeant; Sternberg, Robert; Danger, Gregoire; Geffroy-Rodier, Claude; Poinot, Pauline

2018-03-01

The present work aims at developing two LC-HRMS setups for the screening of organic matter in astrophysical samples. Their analytical development has been demonstrated on a 100-µg residue coming from the photo-thermo chemical processing of a cometary ice analog produced in laboratory. The first 1D-LC-HRMS setup combines a serially coupled columns configuration with HRMS detection. It has allowed to discriminate among different chemical families (amino acids, sugars, nucleobases and oligopeptides) in only one chromatographic run without neither a priori acid hydrolysis nor chemical derivatisation. The second setup is a dual-LC configuration which connects a series of trapping columns with analytical reverse-phase columns. By coupling on-line these two distinct LC units with a HRMS detection, high mass compounds (350

Green analytical determination of emerging pollutants in environmental waters using excitation-emission photoinduced fluorescence data and multivariate calibration.

PubMed

Hurtado-Sánchez, María Del Carmen; Lozano, Valeria A; Rodríguez-Cáceres, María Isabel; Durán-Merás, Isabel; Escandar, Graciela M

2015-03-01

An eco-friendly strategy for the simultaneous quantification of three emerging pharmaceutical contaminants is presented. The proposed analytical method, which involves photochemically induced fluorescence matrix data combined with second-order chemometric analysis, was used for the determination of carbamazepine, ofloxacin and piroxicam in water samples of different complexity without the need of chromatographic separation. Excitation-emission photoinduced fluorescence matrices were obtained after UV irradiation, and processed with second-order algorithms. Only one of the tested algorithms was able to overcome the strong spectral overlapping among the studied pollutants and allowed their successful quantitation in very interferent media. The method sensitivity in superficial and underground water samples was enhanced by a simple solid-phase extraction with C18 membranes, which was successful for the extraction/preconcentration of the pollutants at trace levels. Detection limits in preconcentrated (1:125) real water samples ranged from 0.04 to 0.3 ng mL(-1). Relative prediction errors around 10% were achieved. The proposed strategy is significantly simpler and greener than liquid chromatography-mass spectrometry methods, without compromising the analytical quality of the results. Copyright © 2014 Elsevier B.V. All rights reserved.

"EMERGING" POLLUTANTS, MASS SPECTROMETRY, AND ...

EPA Pesticide Factsheets

A foundation for Environmental Science - Mass Spectrometry: Historically fundamental to amassing our understanding of environmental processes and chemical pollution is the realm of mass spectrometry - the mainstay of analytical chemistry - the workhorse that supplies much of the definitive data that environmental scientists rely upon for identifying the molecular compositions (and ultimately the structures) of chemicals. This is not to ignore the complementary, critical roles played by the adjunct practices of sample enrichment (via any of various means of selective extraction) and analyte separation (via the myriad forms of chromatography and electrophoresis).While the power of mass spectrometry has long been highly visible to the practicing environmental chemist, it borders on continued obscurity to the lay public and most non-chemists. Even though mass spectrometry has played a long, historic (and largely invisible) role in establishing or undergirdidng our existing knowledge about environmental processes and pollution, what recognition it does enjoy is usually relegated to that of a tool. It is ususally the relevance of ssignificance of the knowledge acquired from the application of the tool that has ultimate meaning to the public and science at large - not how the knowledge was acquired. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in

Determination of polycyclic aromatic hydrocarbons in drinking water samples by solid-phase nanoextraction and high-performance liquid chromatography.

PubMed

Wang, Huiyong; Campiglia, Andres D

2008-11-01

A novel alternative is presented for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAH) from water samples. The new approachwhich we have named solid-phase nanoextraction (SPNE)takes advantage of the strong affinity that exists between PAH and gold nanoparticles. Carefully optimization of experimental parameters has led to a high-performance liquid chromatography method with excellent analytical figures of merit. Its most striking feature correlates to the small volume of water sample (500 microL) for complete PAH analyses. The limits of detection ranged from 0.9 (anthracene) to 58 ng.L (-1) (fluorene). The relative standard deviations at medium calibration concentrations vary from 3.2 (acenaphthene) to 9.1% (naphthalene). The analytical recoveries from tap water samples of the six regulated PAH varied from 83.3 +/- 2.4 (benzo[ k]fluoranthene) to 95.7 +/- 4.1% (benzo[ g,h,i]perylene). The entire extraction procedure consumes less than 100 microL of organic solvents per sample, which makes it environmentally friendly. The small volume of extracting solution makes SPNE a relatively inexpensive extraction approach.

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

PubMed

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

VALIDATION OF STANDARD ANALYTICAL PROTOCOL FOR ...

EPA Pesticide Factsheets

There is a growing concern with the potential for terrorist use of chemical weapons to cause civilian harm. In the event of an actual or suspected outdoor release of chemically hazardous material in a large area, the extent of contamination must be determined. This requires a system with the ability to prepare and quickly analyze a large number of contaminated samples for the traditional chemical agents, as well as numerous toxic industrial chemicals. Liquid samples (both aqueous and organic), solid samples (e.g., soil), vapor samples (e.g., air) and mixed state samples, all ranging from household items to deceased animals, may require some level of analyses. To meet this challenge, the U.S. Environmental Protection Agency (U.S. EPA) National Homeland Security Research Center, in collaboration with experts from across U.S. EPA and other Federal Agencies, initiated an effort to identify analytical methods for the chemical and biological agents that could be used to respond to a terrorist attack or a homeland security incident. U.S. EPA began development of standard analytical protocols (SAPs) for laboratory identification and measurement of target agents in case of a contamination threat. These methods will be used to help assist in the identification of existing contamination, the effectiveness of decontamination, as well as clearance for the affected population to reoccupy previously contaminated areas. One of the first SAPs developed was for the determin

Nonylphenol: Properties, legislation, toxicity and determination.

PubMed

Araujo, Frederico G DE; Bauerfeldt, Glauco F; Cid, Yara Peluso

2017-08-07

This paper aims to gather and discuss important information about nonylphenol, such as physical chemistry properties, toxicity and analytical methods in various matrices. As a degradation product of ethoxylated alkylphenols, nonylphenol presents a higher degree of reactivity than its precursor. Due to its harmful effects on the environment, use and production of nonylphenol has been banned in European Union countries, alongside their precursors. The guide on quality of drinking water (USEPA) recommends a maximum concentration of 28 µg L-1 for fresh water. In Brazil, there is no clear legislation containing values ​​of maximum concentration of nonylphenol. Due to this lack of regulation, a continuous monitoring is necessary of this pollutant in environmental samples. This paper aims to encourage further studies on nonylphenol, seen as a critical environmental pollutant. For proper monitoring is necessary to have reliable analytical methods and easy to perform in routine analysis.

Fate of the chemical warfare agent O-ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX) on soil following accelerant-based fire and liquid decontamination.

PubMed

Gravett, M R; Hopkins, F B; Self, A J; Webb, A J; Timperley, C M; Riches, J R

2014-08-01

In the event of alleged use of organophosphorus nerve agents, all kinds of environmental samples can be received for analysis. These might include decontaminated and charred matter collected from the site of a suspected chemical attack. In other scenarios, such matter might be sampled to confirm the site of a chemical weapon test or clandestine laboratory decontaminated and burned to prevent discovery. To provide an analytical capability for these contingencies, we present a preliminary investigation of the effect of accelerant-based fire and liquid decontamination on soil contaminated with the nerve agent O-ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX). The objectives were (a) to determine if VX or its degradation products were detectable in soil after an accelerant-based fire promoted by aviation fuel, including following decontamination with Decontamination Solution 2 (DS2) or aqueous sodium hypochlorite, (b) to develop analytical methods to support forensic analysis of accelerant-soaked, decontaminated and charred soil and (c) to inform the design of future experiments of this type to improve analytical fidelity. Our results show for the first time that modern analytical techniques can be used to identify residual VX and its degradation products in contaminated soil after an accelerant-based fire and after chemical decontamination and then fire. Comparison of the gas chromatography-mass spectrometry (GC-MS) profiles of VX and its impurities/degradation products from contaminated burnt soil, and burnt soil spiked with VX, indicated that the fire resulted in the production of diethyl methylphosphonate and O,S-diethyl methylphosphonothiolate (by an unknown mechanism). Other products identified were indicative of chemical decontamination, and some of these provided evidence of the decontaminant used, for example, ethyl 2-methoxyethyl methylphosphonate and bis(2-methoxyethyl) methylphosphonate following decontamination with DS2. Sample preparation procedures and analytical methods suitable for investigating accelerant and decontaminant-soaked soil samples are presented. VX and its degradation products and/or impurities were detected under all the conditions studied, demonstrating that accelerant-based fire and liquid-based decontamination and then fire are unlikely to prevent the retrieval of evidence of chemical warfare agent (CWA) testing. This is the first published study of the effects of an accelerant-based fire on a CWA in environmental samples. The results will inform defence and security-based organisations worldwide and support the verification activities of the Organisation for the Prohibition of Chemical Weapons (OPCW), winner of the 2013 Nobel Peace Prize for its extensive efforts to eliminate chemical weapons.

Comparison of the Reveal 20-hour method and the BAM culture method for the detection of Escherichia coli O157:H7 in selected foods and environmental swabs: collaborative study.

PubMed

Bird, C B; Hoerner, R J; Restaino, L

2001-01-01

Four different food types along with environmental swabs were analyzed by the Reveal for E. coli O157:H7 test (Reveal) and the Bacteriological Analytical Manual (BAM) culture method for the presence of Escherichia coli O157:H7. Twenty-seven laboratories representing academia and private industry in the United States and Canada participated. Sample types were inoculated with E. coli O157:H7 at 2 different levels. Of the 1,095 samples and controls analyzed and confirmed, 459 were positive and 557 were negative by both methods. No statistical differences (p <0.05) were observed between the Reveal and BAM methods.

Multiresidue analytical method for pharmaceuticals and personal care products in sewage and sewage sludge by online direct immersion SPME on-fiber derivatization - GCMS.

PubMed

López-Serna, Rebeca; Marín-de-Jesús, David; Irusta-Mata, Rubén; García-Encina, Pedro Antonio; Lebrero, Raquel; Fdez-Polanco, María; Muñoz, Raúl

2018-08-15

The work here presented aimed at developing an analytical method for the simultaneous determination of 22 pharmaceuticals and personal care products, including 3 transformation products, in sewage and sludge. A meticulous method optimization, involving an experimental design, was carried out. The developed method was fully automated and consisted of the online extraction of 17 mL of water sample by Direct Immersion Solid Phase MicroExtraction followed by On-fiber Derivatization coupled to Gas Chromatography - Mass Spectrometry (DI-SPME - On-fiber Derivatization - GC - MS). This methodology was validated for 12 of the initial compounds as a reliable (relative recoveries above 90% for sewage and 70% for sludge; repeatability as %RSD below 10% in all cases), sensitive (LODs below 20 ng L -1 in sewage and 10 ng g -1 in sludge), versatile (sewage and sewage-sludge samples up to 15,000 ng L -1 and 900 ng g -1 , respectively) and green analytical alternative for many medium-tech routine laboratories around the world to keep up with both current and forecast environmental regulations requirements. The remaining 10 analytes initially considered showed insufficient suitability to be included in the final method. The methodology was successfully applied to real samples generated in a pilot scale sewage treatment reactor. Copyright © 2018 Elsevier B.V. All rights reserved.

Isolation and identification of Salmonella spp. in environmental water by molecular technology in Taiwan

NASA Astrophysics Data System (ADS)

Kuo, Chun Wei; Hao Huang, Kuan; Hsu, Bing Mu; Tsai, Hsien Lung; Tseng, Shao Feng; Shen, Tsung Yu; Kao, Po Min; Shen, Shu Min; Chen, Jung Sheng

2013-04-01

Salmonella spp. is one of the most important causal agents of waterborne diseases. The taxonomy of Salmonella is very complicated and its genus comprises more than 2,500 serotypes. The detection of Salmonella in environmental water samples by routines culture methods using selective media and characterization of suspicious colonies based on biochemical tests and serological assay are generally time consuming. To overcome this drawback, it is desirable to use effective method which provides a higher discrimination and more rapid identification about Salmonella in environmental water. The aim of this study is to investigate the occurrence of Salmonella using molecular technology and to identify the serovars of Salmonella isolates from 70 environmental water samples in Taiwan. The analytical procedures include membrane filtration, non-selective pre-enrichment, selective enrichment of Salmonella. After that, we isolated Salmonella strains by selective culture plates. Both selective enrichment and culture plates were detected by Polymerase Chain Reaction (PCR). Finally, the serovars of Salmonella were confirmed by using biochemical tests and serological assay. In this study, 15 water samples (21.4%) were identified as Salmonella by PCR. The positive water samples will further identify their serotypes by culture method. The presence of Salmonella in environmental water indicates the possibility of waterborne transmission in drinking watershed. Consequently, the authorities need to provide sufficient source protection and to maintain the system for disease prevention. Keywords: Salmonella spp., serological assay, PCR

Simultaneous grouping and ranking with combination of SOM and TOPSIS for selection of preferable analytical procedure for furan determination in food.

PubMed

Jędrkiewicz, Renata; Tsakovski, Stefan; Lavenu, Aurore; Namieśnik, Jacek; Tobiszewski, Marek

2018-02-01

Novel methodology for grouping and ranking with application of self-organizing maps and multicriteria decision analysis is presented. The dataset consists of 22 objects that are analytical procedures applied to furan determination in food samples. They are described by 10 variables, referred to their analytical performance, environmental and economic aspects. Multivariate statistics analysis allows to limit the amount of input data for ranking analysis. Assessment results show that the most beneficial procedures are based on microextraction techniques with GC-MS final determination. It is presented how the information obtained from both tools complement each other. The applicability of combination of grouping and ranking is also discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of potential influence factors on background urinary benzene concentration among a non-smoking, non-occupationally exposed general population sample.

PubMed

Campagna, Marcello; Satta, Giannina; Campo, Laura; Flore, Valeria; Ibba, Antonio; Meloni, Michele; Tocco, Maria Giuseppina; Avataneo, Giuseppe; Flore, Costantino; Fustinoni, Silvia; Cocco, Pierluigi

2014-01-01

Analytical difficulties and lack of a biological exposure index and reference values have prevented using unmetabolized urinary benzene (UB) excretion as a biomarker of low-level environmental exposure. To explore what environmental factors beyond active smoking may contribute to environmental exposure to benzene, we monitored UB excretion in a non-smoking, non-occupationally exposed sample of the general population. Two spot urine samples were obtained from 86 non-smoking, non-occupationally exposed subjects, selected among a random sample of the general population of the metropolitan area of Cagliari (Sardinia, Italy), at 8:00 a.m. (UBm) and 8:00 p.m. (UBe). UB was measured by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry analysis. Questionnaire information on personal and environmental exposures during the sampling day was gathered with personal interviews. Multivariate analysis of variance and multiple regression model were applied to investigate the role of such variables on the level of UB. The ninety-fifth percentile of UBe in this population was 311.5 ng/L, which is tentatively proposed as the UB guidance value for unexposed populations. UBm and urban residence were the only predictors of a significant increase in UBe excretion. Self-reported residential vehicular traffic will not account for the excess median value among urban residents; commuting time among urban residents showed a suggestive nonsignificant linear correlation with UBe, but the small sample size prevented reliable inference to be drawn. Age, environmental tobacco smoking, employment status and body mass index did not affect UB excretion. Our findings support the use of unmetabolized UB as a specific and sensitive biomarker of low-level environmental exposure to benzene.

Critical evaluation and comparison of enrichment efficiency of multi-walled carbon nanotubes, C18 silica and activated carbon towards some pesticides from environmental waters.

PubMed

El-Sheikh, Amjad H; Sweileh, Jamal A; Al-Degs, Yahya S; Insisi, Ahmad A; Al-Rabady, Nancy

2008-02-15

In this work, optimization of multi-residue solid phase extraction (SPE) procedures coupled with high-performance liquid chromatography for the determination of Propoxur, Atrazine and Methidathion from environmental waters is reported. Three different sorbents were used in this work: multi-walled carbon nanotubes (MWCNTs), C18 silica and activated carbon (AC). The three optimized SPE procedures were compared in terms of analytical performance, application to environmental waters, cartridge re-use, adsorption capacity and cost of adsorbent. Although the adsorption capacity of MWCNT was larger than AC and C18, however, the analytical performance of AC could be made close to the other sorbents by appropriate optimization of the SPE procedures. A sample of AC was then oxidized with various oxidizing agents to show that ACs of various surface properties has different enrichment efficiencies. Thus researchers are advised to try AC of various surface properties in SPE of pollutants prior to using expensive sorbents (such as MWCNT and C18 silica).

Analytical methods for the assessment of endocrine disrupting chemical exposure during human fetal and lactation stages: a review.

PubMed

Jiménez-Díaz, I; Vela-Soria, F; Rodríguez-Gómez, R; Zafra-Gómez, A; Ballesteros, O; Navalón, A

2015-09-10

In the present work, a review of the analytical methods developed in the last 15 years for the determination of endocrine disrupting chemicals (EDCs) in human samples related with children, including placenta, cord blood, amniotic fluid, maternal blood, maternal urine and breast milk, is proposed. Children are highly vulnerable to toxic chemicals in the environment. Among these environmental contaminants to which children are at risk of exposure are EDCs -substances able to alter the normal hormone function of wildlife and humans-. The work focuses mainly on sample preparation and instrumental techniques used for the detection and quantification of the analytes. The sample preparation techniques include, not only liquid-liquid extraction (LLE) and solid-phase extraction (SPE), but also modern microextraction techniques such as extraction with molecular imprinted polymers (MIPs), stir-bar sorptive extraction (SBSE), hollow-fiber liquid-phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME), matrix solid phase dispersion (MSPD) or ultrasound-assisted extraction (UAE), which are becoming alternatives in the analysis of human samples. Most studies focus on minimizing the number of steps and using the lowest solvent amounts in the sample treatment. The usual instrumental techniques employed include liquid chromatography (LC), gas chromatography (GC) mainly coupled to tandem mass spectrometry. Multiresidue methods are being developed for the determination of several families of EDCs with one extraction step and limited sample preparation. Copyright © 2015 Elsevier B.V. All rights reserved.

We Make Spirit By Walking: An Application of Kovel's Spirituality to the Life and Work of Committed Environmentalists.

ERIC Educational Resources Information Center

McDonald, Barbara

An analytical framework based on Joel Kovel's five meditations on spirit (spirit power, spirit being, spirit meaning, spirit and desire, and divine spirit) was used to explore the spirituality of committed environmental activists. A purposeful and snowball sampling method was used to interview 18 individuals with a strong commitment to…

How to Recognize Success and Failure: Practical Assessment of an Evolving, First-Semester Laboratory Program Using Simple, Outcome-Based Tools

ERIC Educational Resources Information Center

Gron, Liz U.; Bradley, Shelly B.; McKenzie, Jennifer R.; Shinn, Sara E.; Teague, M. Warfield

2013-01-01

This paper presents the use of simple, outcome-based assessment tools to design and evaluate the first semester of a new introductory laboratory program created to teach green analytical chemistry using environmental samples. This general chemistry laboratory program, like many introductory courses, has a wide array of stakeholders within and…

External quality-assurance results for the national atmospheric deposition program/national trends network, 2000-2001

USGS Publications Warehouse

Wetherbee, Gregory A.; Latysh, Natalie E.; Gordon, John D.

2004-01-01

Five external quality-assurance programs were operated by the U.S. Geological Survey for the National Atmospheric Deposition Program/National Trends Network (NADP/NTN) from 2000 through 2001 (study period): the intersite-comparison program, the blind-audit program, the field-audit program, the interlaboratory-comparison program, and the collocated-sampler program. Each program is designed to measure specific components of the total error inherent in NADP/NTN wet-deposition measurements. The intersite-comparison program assesses the variability and bias of pH and specific-conductance determinations made by NADP/NTN site operators with respect to accuracy goals. The accuracy goals are statistically based using the median of all of the measurements obtained for each of four intersite-comparison studies. The percentage of site operators responding on time that met the pH accuracy goals ranged from 84.2 to 90.5 percent. In these same four intersite-comparison studies, 88.9 to 99.0 percent of the site operators met the accuracy goals for specific conductance. The blind-audit program evaluates the effects of routine sample handling, processing, and shipping on the chemistry of weekly precipitation samples. The blind-audit data for the study period indicate that sample handling introduced a small amount of sulfate contamination and slight changes to hydrogen-ion content of the precipitation samples. The magnitudes of the paired differences are not environmentally significant to NADP/NTN data users. The field-audit program (also known as the 'field-blank program') was designed to measure the effects of field exposure, handling, and processing on the chemistry of NADP/NTN precipitation samples. The results indicate potential low-level contamination of NADP/NTN samples with calcium, ammonium, chloride, and nitrate. Less sodium contamination was detected by the field-audit data than in previous years. Statistical analysis of the paired differences shows that contaminant ions are entrained into the solutions from the field-exposed buckets, but the positive bias that results from the minor amount of contamination appears to affect the analytical results by less than 6 percent. An interlaboratory-comparison program is used to estimate the analytical variability and bias of participating laboratories, especially the NADP Central Analytical Laboratory (CAL). Statistical comparison of the analytical results of participating laboratories implies that analytical data from the various monitoring networks can be compared. Bias was identified in the CAL data for ammonium, chloride, nitrate, sulfate, hydrogen-ion, and specific-conductance measurements, but the absolute value of the bias was less than analytical minimum reporting limits for all constituents except ammonium and sulfate. Control charts show brief time periods when the CAL's analytical precision for sodium, ammonium, and chloride was not within the control limits. Data for the analysis of ultrapure deionized-water samples indicated that the laboratories are maintaining good control of laboratory contamination. Estimated analytical precision among the laboratories indicates that the magnitudes of chemical-analysis errors are not environmentally significant to NADP data users. Overall precision of the precipitation-monitoring system used by the NADP/NTN was estimated by evaluation of samples from collocated monitoring sites at CA99, CO08, and NH02. Precision defined by the median of the absolute percent difference (MAE) was estimated to be approximately 10 percent or less for calcium, magnesium, sodium, chloride, nitrate, sulfate, specific conductance, and sample volume. The MAE values for ammonium and hydrogen-ion concentrations were estimated to be less than 10 percent for CA99 and NH02 but nearly 20 percent for ammonium concentration and about 17 percent for hydrogen-ion concentration for CO08. As in past years, the variability in the collocated-site data for sam

Inositol phosphates in the environment.

PubMed Central

Turner, Benjamin L; Papházy, Michael J; Haygarth, Philip M; McKelvie, Ian D

2002-01-01

The inositol phosphates are a group of organic phosphorus compounds found widely in the natural environment, but that represent the greatest gap in our understanding of the global phosphorus cycle. They exist as inositols in various states of phosphorylation (bound to between one and six phosphate groups) and isomeric forms (e.g. myo, D-chiro, scyllo, neo), although myo-inositol hexakisphosphate is by far the most prevalent form in nature. In terrestrial environments, inositol phosphates are principally derived from plants and accumulate in soils to become the dominant class of organic phosphorus compounds. Inositol phosphates are also present in large amounts in aquatic environments, where they may contribute to eutrophication. Despite the prevalence of inositol phosphates in the environment, their cycling, mobility and bioavailability are poorly understood. This is largely related to analytical difficulties associated with the extraction, separation and detection of inositol phosphates in environmental samples. This review summarizes the current knowledge of inositol phosphates in the environment and the analytical techniques currently available for their detection in environmental samples. Recent advances in technology, such as the development of suitable chromatographic and capillary electrophoresis separation techniques, should help to elucidate some of the more pertinent questions regarding inositol phosphates in the natural environment. PMID:12028785

Basic Information for EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM)

EPA Pesticide Factsheets

Contains basic information on the role and origins of the Selected Analytical Methods including the formation of the Homeland Security Laboratory Capacity Work Group and the Environmental Evaluation Analytical Process Roadmap for Homeland Security Events

Determination of a risk management primer at petroleum-contaminated sites: developing new human health risk assessment strategy.

PubMed

Park, In-Sun; Park, Jae-Woo

2011-01-30

Total petroleum hydrocarbon (TPH) is an important environmental contaminant that is toxic to human and environmental receptors. However, human health risk assessment for petroleum, oil, and lubricant (POL)-contaminated sites is especially challenging because TPH is not a single compound, but rather a mixture of numerous substances. To address this concern, this study recommends a new human health risk assessment strategy for POL-contaminated sites. The strategy is based on a newly modified TPH fractionation method and includes an improved analytical protocol. The proposed TPH fractionation method is composed of ten fractions (e.g., aliphatic and aromatic EC8-10, EC10-12, EC12-16, EC16-22 and EC22-40). Physicochemical properties and toxicity values of each fraction were newly defined in this study. The stepwise ultrasonication-based analytical process was established to measure TPH fractions. Analytical results were compared with those from the TPH Criteria Working Group (TPHCWG) Direct Method. Better analytical efficiencies in TPH, aliphatic, and aromatic fractions were achieved when contaminated soil samples were analyzed with the new analytical protocol. Finally, a human health risk assessment was performed based on the developed tiered risk assessment framework. Results showed that a detailed quantitative risk assessment should be conducted to determine scientifically and economically appropriate cleanup target levels, although the phase II process is useful for determining the potency of human health risks posed by POL-contamination. Copyright © 2010 Elsevier B.V. All rights reserved.

Proficiency Tests for Environmental Radioactivity Measurement Organized by an Accredited Laboratory

NASA Astrophysics Data System (ADS)

Aubert, Cédric; Osmond, Mélanie

2008-08-01

For 40 years, STEME (Environmental Sample Processing and Metrology Department) organized international proficiency testing (PT) exercises formerly for WHO (World Health Organization) and EC (European Community) and currently for ASN (French Nuclear Safety Authority). Five PT exercises are organized each year for the measurement of radionuclides (alpha, beta and gamma) in different matrixes (water, soil, biological and air samples) at environmental levels. ASN can deliver a French ministerial agreement to participate on environmental radioactivity measurements French network for laboratories asking it [1]. Since 2006, November, STEME is the first French entity obtaining a COFRAC (French Committee of Accreditation) accreditation as "Interlaboratory Comparisons" for the organization of proficiency tests for environmental radioactivity measurement according to standard International Standard Organization (ISO) 17025 and guide ISO 43-1. STEME has in charge to find, as far as possible, real sample or to create, by radionuclide adding, an adapted sample. STEME realizes the sampling, the samples preparation and the dispatching. STEME is also accredited according to Standard 17025 for radioactivity measurements in environmental samples and determines homogeneity, stability and reference values. After the reception of participating laboratories results, STEME executes statistical treatments in order to verify the normal distribution, to eliminate outliers and to evaluate laboratories performance. Laboratories participate with several objectives, to obtain French agreement, to prove the quality of their analytical performance in regards to standard 17025 or to validate new methods or latest developments. For 2 years, in addition to usual PT exercises, new PT about alpha or beta measurement in air filters, radioactive iodine in carbon cartridges or measurement of environmental dosimeters are organized. These PT exercises help laboratories to improve radioactive measurements and to rectify old mistakes. The PT exercises organized by STEME are becoming essential for French and some European laboratories working in radioactive measurements. The STEME organization, in respect of accreditation references, is presented.

Proficiency Tests for Environmental Radioactivity Measurement Organized by an Accredited Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aubert, Cedric; Osmond, Melanie

2008-08-14

For 40 years, STEME (Environmental Sample Processing and Metrology Department) organized international proficiency testing (PT) exercises formerly for WHO (World Health Organization) and EC (European Community) and currently for ASN (French Nuclear Safety Authority). Five PT exercises are organized each year for the measurement of radionuclides (alpha, beta and gamma) in different matrixes (water, soil, biological and air samples) at environmental levels. ASN can deliver a French ministerial agreement to participate on environmental radioactivity measurements French network for laboratories asking it. Since 2006, November, STEME is the first French entity obtaining a COFRAC (French Committee of Accreditation) accreditation as 'Interlaboratorymore » Comparisons' for the organization of proficiency tests for environmental radioactivity measurement according to standard International Standard Organization (ISO) 17025 and guide ISO 43-1. STEME has in charge to find, as far as possible, real sample or to create, by radionuclide adding, an adapted sample. STEME realizes the sampling, the samples preparation and the dispatching. STEME is also accredited according to Standard 17025 for radioactivity measurements in environmental samples and determines homogeneity, stability and reference values. After the reception of participating laboratories results, STEME executes statistical treatments in order to verify the normal distribution, to eliminate outliers and to evaluate laboratories performance.Laboratories participate with several objectives, to obtain French agreement, to prove the quality of their analytical performance in regards to standard 17025 or to validate new methods or latest developments. For 2 years, in addition to usual PT exercises, new PT about alpha or beta measurement in air filters, radioactive iodine in carbon cartridges or measurement of environmental dosimeters are organized. These PT exercises help laboratories to improve radioactive measurements and to rectify old mistakes. The PT exercises organized by STEME are becoming essential for French and some European laboratories working in radioactive measurements.The STEME organization, in respect of accreditation references, is presented.« less

Automated Clean Chemistry for Bulk Analysis of Environmental Swipe Samples - FY17 Year End Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ticknor, Brian W.; Metzger, Shalina C.; McBay, Eddy H.

Sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment to shorten lengthy and costly manual chemical purification procedures. This development addresses a serious need in the International Atomic Energy Agency’s Network of Analytical Laboratories (IAEA NWAL) to increase efficiency in the Bulk Analysis of Environmental Samples for Safeguards program with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on COTS equipment. It was modified for uranium/plutonium separations using renewable columns packed with Eichrom TEVA and UTEVA resins, with a chemical separation method based on the Oakmore » Ridge National Laboratory (ORNL) NWAL chemical procedure. The newly designed prepFAST-SR has had several upgrades compared with the original prepFAST-MC2. Both systems are currently installed in the Ultra-Trace Forensics Science Center at ORNL.« less

Determination of bromine, chlorine and iodine in environmental aqueous samples by epithermal neutron activation analysis and Compton suppression

USGS Publications Warehouse

Landsberger, S.; O'Kelly, D. J.; Braisted, J.; Panno, S.

2006-01-01

Halides, particularly Br- and Cl-, have been used as indicators of potential sources of Na+ and Cl- in surface water and groundwater with limited success. Contamination of groundwater and surface water by Na+ and Cl- is a common occurrence in growing urban areas and adversely affects municipal and private water supplies in Illinois and other states, as well as vegetation in environmentally sensitive areas. Neutron activation analysis (NAA) can be effectively used to determine these halogens, but often the elevated concentrations of sodium and chlorine in water samples can give rise to very high detection limits for bromine and iodine due to elevated backgrounds from the activation process. We present a detailed analytical scheme to determine Cl, Br and I in aqueous samples with widely varying Na and Cl concentrations using epithermal NAA in conjunction with Compton suppression. ?? 2006 Akade??miai Kiado??.

Data on Mercury in Water, Bed Sediment, and Fish from Streams Across the United States, 1998-2005

USGS Publications Warehouse

Bauch, Nancy J.; Chasar, Lia C.; Scudder, Barbara C.; Moran, Patrick W.; Hitt, Kerie J.; Brigham, Mark E.; Lutz, Michelle A.; Wentz, Dennis A.

2009-01-01

The U.S. Geological Survey (USGS) National Water-Quality Assessment (NAWQA) and Toxic Substances Hydrology Programs conducted the National Mercury Pilot Study in 1998 to examine relations of mercury (Hg) in water, bed sediment and fish in streams across the United States, including Alaska and Hawaii. Water and bed-sediment samples were analyzed for total Hg (THg), methylmercury (MeHg), and other constituents; fish were analyzed for THg. Similar sampling was conducted at additional streams across the country in 2002 and 2004-05. This report summarizes sample collection and processing protocols, analytical methods, environmental data, and quality-assurance data for stream water, bed sediment, and fish for these national studies. To extend the geographic coverage of the data, this report also includes four regional USGS Hg studies conducted during 1998-2001 and 2004. The environmental data for these national and regional Hg studies are provided in an electronic format.

ENVIRONMENTAL IMMUNOCHEMISTRY RESPONDING TO A SPECTRUM OF ANALYTICAL NEEDS

EPA Science Inventory

A review, with 13 references, is given on the field of environmental immunochemistry which brings together several specalties, including analytical chemistry, biochemistry, moluclar biology, and environmental engineering. This multidisciplinary nature is both benefit and a confus...

Use of mass spectrometry coupled with a solids insertion probe to prescreen soil samples for environmental samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Check, C.E.; Bach, S.B.H.

1995-12-31

The contamination of air, water, and soils by a myriad of sources generates a large sample Currently, sample volume for hazardous constituent analyses is approximately half a million samples per year. The total analytical costs associated with this are astronomical. The analysis of these samples is vital in terms of assessing the types of contamination present and to what degree a site has been contaminated. The results of these analyses are very important for making an informed, knowledgeable decision as to the need for remediation and what type of remediation processes should be initiated based on site suitability vs non-actionmore » for the various sample sites. With an ever growing environmental consciousness in today`s society, the assessment and subsequent remediation of a site needs to be accomplished promptly despite the time constraints traditional methods place on such actions. In order to facilitate a rapid assessment, it is desirable to utilize instrumentation and equipment which afford the most information about a site allowing for optimization in environmental assessment while maintaining a realistic time schedule for the resulting remediation process. Because there are various types of environmental samples that can be taken at a site, different combinations of instrumentation and methods are required for assessing the level and type of contamination present whether it is in air, water, or soils. This study is limited to analyzing soil-like media that would normally fall under EPA Method 8270 which is used to analyze solid waste matrices, soils, and groundwater for semi-volatile organic compounds.« less

Investigation of fluorine content in PM2.5 airborne particles of Istanbul, Turkey.

PubMed

Ozbek, Nil; Baltaci, Hakki; Baysal, Asli

2016-07-01

Fluorine determination in airborne samples is important due to its spread into the air from both natural and artificial sources. It can travel by wind over large distances before depositing on the Earth's surface. Its concentration in various matrices are limited and controlled by the regulations for causing health risks associated with environmental exposures. In this work, fluorine was determined in PM2.5 airborne samples by high-resolution continuum source electrothermal atomic absorption spectrometry. For these purpose, the PM2.5 airborne particulates were collected on quartz filters using high-volume samplers (500 L/min) in Istanbul (Turkey) for 96 h during January to June in 2 years. Then, instrumental and experimental parameters were optimized for the analyte in airborne samples. The validity of the method for the analyte was tested using standard reference material, and certified values were found in the limits of 95 % confidence level. The fluorine concentrations and meteorological conditions were compared statistically.

Determination of nicotine by surface-enhanced Raman scattering (SERS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barber, T.E.; List, M.S.; Haas, J.W. III

1994-11-01

The analytical application of surface-enhanced Raman spectroscopy (SERS) to the determination of nicotine is demonstrated. A simple spectroelectrochemical method using a copper or silver electrode as the SERS substrate has been developed, consisting of three steps: polishing a working electrode to a mirror finish; roughening the electrode in an electrolyte solution; and, finally, depositing the nicotine analyte onto the roughened electrode after immersion in a sample solution. During the reduction cycle, a large enhancement in nicotine Raman scattering is observed at the electrode surface. The intensity of the SERS signal on a silver electrode is linear with concentration from 10more » to 900 ppb, with an estimated detection limit of 7 ppb. The total analysis time per sample is approximately five minutes. This procedure has been used to analyze the extract from a cigarette side-stream smoke sample (environmental tobacco smoke); the SERS results agree well with those of conventional gas chromatographic analysis.« less

Love Canal monitoring program. Volume 1. Final report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

This report summarizes the prime contractor activities during the monitoring phase of the Love Canal project. Since GCA Corporation was only responsible for data collection, no analytical results appear in this report. The program involved a multifaceted sampling and analytical effort designed to detect and quantify a variety of trace metals, volatile organics, pesticides and other compounds in soil, sediment, air, biota, and water samples. The principal purpose of these activities was to provide data with which EPA could assess the extent of environmental contamination in the Love Canal Area. Since the area declared as a National Emergency was extendedmore » from those homes directly surrounding the Love Canal dumpsite to a more general area on May 21, 1980, it had been determined that the overall exposure of residents must be established as quickly as possible. The program, therefore, was on an extremely tight schedule with field sampling activities to be completed by October 31, 1980. GCA organized its efforts into seven technical elements, each of which is discussed.« less

Preliminary analytical results for a mud sample collected from the LUSI Mud Volcano, Sidoarjo, East Java, Indonesia

USGS Publications Warehouse

Plumlee, Geoffrey S.; Casadevall, Thomas J.; Wibowo, Handoko T.; Rosenbauer, Robert J.; Johnson, Craig A.; Breit, George N.; Lowers, Heather; Wolf, Ruth E.; Hageman, Philip L.; Goldstein, Harland L.; Anthony, Michael W.; Berry, Cyrus J.; Fey, David L.; Meeker, Gregory P.; Morman, Suzette A.

2008-01-01

On May 29, 2006, mud and gases began erupting unexpectedly from a vent 150 meters away from a hydrocarbon exploration well near Sidoarjo, East Java, Indonesia. The eruption, called the LUSI (Lumpur 'mud'-Sidoarjo) mud volcano, has continued since then at rates as high as 160,000 m3 per day. At the request of the United States Department of State, the U.S. Geological Survey (USGS) has been providing technical assistance to the Indonesian Government on the geological and geochemical aspects of the mud eruption. This report presents initial characterization results of a sample of the mud collected on September 22, 2007, as well as inerpretive findings based on the analytical results. The focus is on characteristics of the mud sample (including the solid and water components of the mud) that may be of potential environmental or human health concern. Characteristics that provide insights into the possible origins of the mud and its contained solids and waters have also been evaluated.

Determination of pesticides associated with suspended sediments in the San Joaquin River, California, USA, using gas chromatography-ion trap mass spectrometry

USGS Publications Warehouse

Bergamaschi, B.A.; Baston, D.S.; Crepeau, K.L.; Kuivila, K.M.

1999-01-01

An analytical method useful for the quantification of a range of pesticides and pesticide degradation products associated with suspended sediments was developed by testing a variety of extraction and cleanup schemes. The final extraction and cleanup methods chosen for use are suitable for the quantification of the listed pesticides using gas chromatography-ion trap mass spectrometry and the removal of interfering coextractable organic material found in suspended sediments. Methylene chloride extraction followed by Florisil cleanup proved most effective for separation of coextractives from the pesticide analytes. Removal of elemental sulfur was accomplished with tetrabutylammonium hydrogen sulfite. The suitability of the method for the analysis of a variety of pesticides was evaluated, and the method detection limits (MDLs) were determined (0.1-6.0 ng/g dry weight of sediment) for 21 compounds. Recovery of pesticides dried onto natural sediments averaged 63%. Analysis of duplicate San Joaquin River suspended-sediment samples demonstrated the utility of the method for environmental samples with variability between replicate analyses lower than between environmental samples. Eight of 21 pesticides measured were observed at concentrations ranging from the MDL to more than 80 ng/g dry weight of sediment and exhibited significant temporal variability. Sediment-associated pesticides, therefore, may contribute to the transport of pesticides through aquatic systems and should be studied separately from dissolved pesticides.

Quantifying the measurement uncertainty of results from environmental analytical methods.

PubMed

Moser, J; Wegscheider, W; Sperka-Gottlieb, C

2001-07-01

The Eurachem-CITAC Guide Quantifying Uncertainty in Analytical Measurement was put into practice in a public laboratory devoted to environmental analytical measurements. In doing so due regard was given to the provisions of ISO 17025 and an attempt was made to base the entire estimation of measurement uncertainty on available data from the literature or from previously performed validation studies. Most environmental analytical procedures laid down in national or international standards are the result of cooperative efforts and put into effect as part of a compromise between all parties involved, public and private, that also encompasses environmental standards and statutory limits. Central to many procedures is the focus on the measurement of environmental effects rather than on individual chemical species. In this situation it is particularly important to understand the measurement process well enough to produce a realistic uncertainty statement. Environmental analytical methods will be examined as far as necessary, but reference will also be made to analytical methods in general and to physical measurement methods where appropriate. This paper describes ways and means of quantifying uncertainty for frequently practised methods of environmental analysis. It will be shown that operationally defined measurands are no obstacle to the estimation process as described in the Eurachem/CITAC Guide if it is accepted that the dominating component of uncertainty comes from the actual practice of the method as a reproducibility standard deviation.

UPLC-MS/MS determination of ptaquiloside and pterosin B in preserved natural water.

PubMed

Clauson-Kaas, Frederik; Hansen, Hans Christian Bruun; Strobel, Bjarne W

2016-11-01

The naturally occurring carcinogen ptaquiloside and its degradation product pterosin B are found in water leaching from bracken stands. The objective of this work is to present a new sample preservation method and a fast UPLC-MS/MS method for quantification of ptaquiloside and pterosin B in environmental water samples, employing a novel internal standard. A faster, reliable, and efficient method was developed for isolation of high purity ptaquiloside and pterosin B from plant material for use as analytical standards, with purity verified by 1 H-NMR. The chemical analysis was performed by cleanup and preconcentration of samples with solid phase extraction, before analyte quantification with UPLC-MS/MS. By including gradient elution and optimizing the liquid chromatography mobile phase buffer system, a total run cycle of 5 min was achieved, with method detection limits, including preconcentration, of 8 and 4 ng/L for ptaquiloside and pterosin B, respectively. The use of loganin as internal standard improved repeatability of the determination of both analytes, though it could not be employed for sample preparation. Buffering raw water samples in situ with ammonium acetate to pH ∼5.5 decisively increased sample integrity at realistic transportation and storing conditions prior to extraction. Groundwater samples collected in November 2015 at the shallow water table below a Danish bracken stand were preserved and analyzed using the above methods, and PTA concentrations of 3.8 ± 0.24 μg/L (±sd, n = 3) were found, much higher than previously reported. Graphical abstract Workflow overview of ptaquiloside determination.

Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

PubMed

Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

2007-03-01

In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

Analytical methods for PCBs and organochlorine pesticides in environmental monitoring and surveillance: a critical appraisal

PubMed Central

Sverko, Ed

2006-01-01

Analytical methods for the analysis of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) are widely available and are the result of a vast amount of environmental analytical method development and research on persistent organic pollutants (POPs) over the past 30–40 years. This review summarizes procedures and examines new approaches for extraction, isolation, identification and quantification of individual congeners/isomers of the PCBs and OCPs. Critical to the successful application of this methodology is the collection, preparation, and storage of samples, as well as specific quality control and reporting criteria, and therefore these are also discussed. With the signing of the Stockholm convention on POPs and the development of global monitoring programs, there is an increased need for laboratories in developing countries to determine PCBs and OCPs. Thus, while this review attempts to summarize the current best practices for analysis of PCBs and OCPs, a major focus is the need for low-cost methods that can be easily implemented in developing countries. A “performance based” process is described whereby individual laboratories can adapt methods best suited to their situations. Access to modern capillary gas chromatography (GC) equipment with either electron capture or low-resolution mass spectrometry (MS) detection to separate and quantify OCP/PCBs is essential. However, screening of samples, especially in areas of known use of OCPs or PCBs, could be accomplished with bioanalytical methods such as specific commercially available enzyme-linked immunoabsorbent assays and thus this topic is also reviewed. New analytical techniques such two-dimensional GC (2D-GC) and “fast GC” using GC–ECD may be well-suited for broader use in routine PCB/OCP analysis in the near future given their relatively low costs and ability to provide high-resolution separations of PCB/OCPs. Procedures with low environmental impact (SPME, microscale, low solvent use, etc.) are increasingly being used and may be particularly suited to developing countries. Electronic supplementary material Supplementary material is available in the online version of this article at http://dx.doi.org/10.1007/s00216-006-0765-y and is accessible for authorized users. PMID:17047943

Microvolume trace environmental analysis using peak-focusing online solid-phase extraction-nano-liquid chromatography-high-resolution mass spectrometry.

PubMed

Stravs, Michael A; Mechelke, Jonas; Ferguson, P Lee; Singer, Heinz; Hollender, Juliane

2016-03-01

Online solid-phase extraction was combined with nano-liquid chromatography coupled to high-resolution mass spectrometry (HRMS) for the analysis of micropollutants in environmental samples from small volumes. The method was validated in surface water, Microcystis aeruginosa cell lysate, and spent Microcystis growth medium. For 41 analytes, quantification limits of 0.1-28 ng/L (surface water) and 0.1-32 ng/L (growth medium) were obtained from only 88 μL of sample. In cell lysate, quantification limits ranged from 0.1-143 ng/L or 0.33-476 ng/g dry weight from a sample of 88 μL, or 26 μg dry weight, respectively. The method matches the sensitivity of established online and offline solid-phase extraction-liquid chromatography-mass spectrometry methods but requires only a fraction of the sample used by those techniques, and is among the first applications of nano-LC-MS for environmental analysis. The method was applied to the determination of bioconcentration in Microcystis aeruginosa in a laboratory experiment, and the benefit of coupling to HRMS was demonstrated in a transformation product screening.

Microextraction techniques combined with capillary electrophoresis in bioanalysis.

PubMed

Kohler, Isabelle; Schappler, Julie; Rudaz, Serge

2013-01-01

Over the past two decades, many environmentally sustainable sample-preparation techniques have been proposed, with the objective of reducing the use of toxic organic solvents or substituting these with environmentally friendly alternatives. Microextraction techniques (MEs), in which only a small amount of organic solvent is used, have several advantages, including reduced sample volume, analysis time, and operating costs. Thus, MEs are well adapted in bioanalysis, in which sample preparation is mandatory because of the complexity of a sample that is available in small quantities (mL or even μL only). Capillary electrophoresis (CE) is a powerful and efficient separation technique in which no organic solvents are required for analysis. Combination of CE with MEs is regarded as a very attractive environmentally sustainable analytical tool, and numerous applications have been reported over the last few decades for bioanalysis of low-molecular-weight compounds or for peptide analysis. In this paper we review the use of MEs combined with CE in bioanalysis. The review is divided into two sections: liquid and solid-based MEs. A brief practical and theoretical description of each ME is given, and the techniques are illustrated by relevant applications.

Mercury and gold concentrations of highly polluted environmental samples determined using prompt gamma-ray analysis and instrument neutron activation analysis

NASA Astrophysics Data System (ADS)

Osawa, Takahito; Hatsukawa, Yuichi; Appel, Peter W. U.; Matsue, Hideaki

2011-04-01

The authors have established a method of determining mercury and gold in severely polluted environmental samples using prompt gamma-ray analysis (PGA) and instrumental neutron activation analysis (INAA). Since large amounts of mercury are constantly being released into the environment by small-scale gold mining in many developing countries, the mercury concentration in tailings and water has to be determined to mitigate environmental pollution. Cold-vapor atomic absorption analysis, the most pervasive method of mercury analysis, is not suitable because tailings and water around mining facilities have extremely high mercury concentrations. On the other hand, PGA can determine high mercury concentrations in polluted samples as it has an appropriate level of sensitivity. Moreover, gold concentrations can be determined sequentially by using INAA after PGA. In conclusion, the analytical procedure established in this work using PGA and INAA is the best way to evaluate the degree of pollution and the tailing resource value. This method will significantly contribute to mitigating problems in the global environment.

Enrichment and determination of octylphenol and nonylphenol in environmental water samples by solid-phase microextraction with carboxylated carbon nano-spheres coating prior to gas chromatography-mass spectrometry.

PubMed

Gong, Sheng-Xiang; Wang, Xia; Li, Lei; Wang, Ming-Lin; Zhao, Ru-Song

2015-11-01

In this paper, a novel and simple method for the sensitive determination of endocrine disrupter compounds octylphenol (OP) and nonylphenol (NP) in environmental water samples has been developed using solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry. Carboxylated carbon nano-spheres (CNSs-COOH) are used as a novel SPME coating via physical adhesion. The CNSs-COOH fiber possessed higher adsorption efficiency than 100 μm polydimethysiloxane (PDMS) fiber and was similar to 85 μm polyacrylate (PA) fiber for the two analytes. Important parameters, such as extraction time, pH, agitation speed, ionic strength, and desorption temperature and time, were investigated and optimized in detail. Under the optimal parameters, the developed method achieved low limits of detection of 0.13~0.14 ng·L(-1) and a wide linear range of 1~1000 ng·(-1) for OP and NP. The novel method was validated with several real environmental water samples, and satisfactory results were obtained.

Geochemical data for environmental studies of mineral deposits at Nabesna, Kennecott, Orange Hill, Bond Creek, Bremner, and Gold Hill, Wrangell-St. Elias National Park and Preserve, Alaska

USGS Publications Warehouse

Eppinger, R.G.; Briggs, P.H.; Rosenkrans, D.S.; Ballestrazze, Vanessa; Aldir, Jose; Brown, Z.A.; Crock, J.G.; d'Angelo, W. M.; Doughten, M.W.; Fey, D.L.; Hageman, P.L.; Hopkins, R.T.; Knight, R.J.; Malcolm, M.J.; McHugh, J.B.; Meier, A.L.; Motooka, J.M.; O'Leary, R. M.; Roushey, B.H.; Sultley, S.J.; Theodorakos, P.M.; Wilson, S.A.

1999-01-01

Environmental geochemical investigations were carried out between 1994 and 1997 in Wrangell-St. Elias National Park and Preserve (WRST), Alaska. Mineralized areas studied include the historic Nabesna gold mine/mill and surrounding areas; the historic Kennecott copper mill area and nearby Bonanza, Erie, Glacier, and Jumbo mines; the historic mill and gold mines in the Bremner district; the active gold placer mines at Gold Hill; and the unmined copper-molybdenum deposits at Orange Hill and Bond Creek. The purpose of the study was to determine the extent of possible environmental hazards associated with these mineralized areas and to establish background and baseline levels for selected elements. Thus, concentrations of a large suite of trace elements were determined to assess metal loadings in the various sample media collected. This report presents the methodology, analytical results, and sample descriptions for water, leachate, sediment, heavy-mineral concentrate, rock, and vegetation (willow) samples collected during these geochemical investigations. An interpretive U.S. Geological Survey Professional Paper incorporating these geochemical data will follow.

Array biosensor for detection of toxins

NASA Technical Reports Server (NTRS)

Ligler, Frances S.; Taitt, Chris Rowe; Shriver-Lake, Lisa C.; Sapsford, Kim E.; Shubin, Yura; Golden, Joel P.

2003-01-01

The array biosensor is capable of detecting multiple targets rapidly and simultaneously on the surface of a single waveguide. Sandwich and competitive fluoroimmunoassays have been developed to detect high and low molecular weight toxins, respectively, in complex samples. Recognition molecules (usually antibodies) were first immobilized in specific locations on the waveguide and the resultant patterned array was used to interrogate up to 12 different samples for the presence of multiple different analytes. Upon binding of a fluorescent analyte or fluorescent immunocomplex, the pattern of fluorescent spots was detected using a CCD camera. Automated image analysis was used to determine a mean fluorescence value for each assay spot and to subtract the local background signal. The location of the spot and its mean fluorescence value were used to determine the toxin identity and concentration. Toxins were measured in clinical fluids, environmental samples and foods, with minimal sample preparation. Results are shown for rapid analyses of staphylococcal enterotoxin B, ricin, cholera toxin, botulinum toxoids, trinitrotoluene, and the mycotoxin fumonisin. Toxins were detected at levels as low as 0.5 ng mL(-1).

A comparative study between different alternatives to prepare gaseous standards for calibrating UV-Ion Mobility Spectrometers.

PubMed

Criado-García, Laura; Garrido-Delgado, Rocío; Arce, Lourdes; Valcárcel, Miguel

2013-07-15

An UV-Ion Mobility Spectrometer is a simple, rapid, inexpensive instrument widely used in environmental analysis among other fields. The advantageous features of its underlying technology can be of great help towards developing reliable, economical methods for determining gaseous compounds from gaseous, liquid and solid samples. Developing an effective method using UV-Ion Mobility Spectrometry (UV-IMS) to determine volatile analytes entails using appropriate gaseous standards for calibrating the spectrometer. In this work, two home-made sample introduction systems (SISs) and a commercial gas generator were used to obtain such gaseous standards. The first home-made SIS used was a static head-space to measure compounds present in liquid samples and the other home-made system was an exponential dilution set-up to measure compounds present in gaseous samples. Gaseous compounds generated by each method were determined on-line by UV-IMS. Target analytes chosen for this comparative study were ethanol, acetone, benzene, toluene, ethylbenzene and xylene isomers. The different alternatives were acceptable in terms of sensitivity, precision and selectivity. Copyright © 2013 Elsevier B.V. All rights reserved.

Concentrations of tritium and strontium-90 in water from selected wells at the Idaho National Engineering Laboratory after purging one, two, and three borehole volumes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bartholomay, R.C.

1993-12-31

Water from 11 wells completed in the Snake River Plain aquifer at the Idaho National Engineering Laboratory was sampled as Part of the US. Geological Survey`s quality assurance program to determine the effect of Purging different borehole volumes on tritium and strontium-90 concentrations. Wells were selected for sampling on the basis of the length of time it took to purge a borehole volume of water. Samples were collected after purging one, two, and three borehole volumes. The US Department of Energy`s Radiological and Environmental Sciences Laboratory provided analytical services. Statistics were used to determine the reproducibility of analytical results. Themore » comparison between tritium and strontium-90 concentrations after purging one and three borehole volumes and two and three borehole volumes showed that all but two sample pairs with defined numbers were in statistical agreement. Results indicate that concentrations of tritium and strontium-90 are not affected measurably by the number of borehole volumes purged.« less

ENVIRONMENTAL ANALYTICAL CHEMISTRY OF ...

EPA Pesticide Factsheets

Within the scope of a number of emerging contaminant issues in environmental analysis, one area that has received a great deal of public interest has been the assessment of the role of pharmaceuticals and personal care products (PPCPs) as stressors and agents of change in ecosystems as well as their role in unplanned human exposure. The relationship between personal actions and the occurrence of PPCPs in the environment is clear-cut and comprehensible to the public. In this overview, we attempt to examine the separations aspect of the analytical approach to the vast array of potential analytes among this class of compounds. We also highlight the relationship between these compounds and endocrine disrupting compounds (EDCs) and between PPCPs and EDCs and the more traditional environmental analytes such as the persistent organic pollutants (POPs). Although the spectrum of chemical behavior extends from hydrophobic to hydrophilic, the current focus has shifted to moderately and highly polar analytes. Thus, emphasis on HPLC and LC/MS has grown and MS/MS has become a detection technique of choice with either electrospray ionization or atmospheric pressure chemical ionization. This contrasts markedly with the bench mark approach of capillary GC, GC/MS and electron ionization in traditional environmental analysis. The expansion of the analyte list has fostered new vigor in the development of environmental analytical chemistry, modernized the range of tools appli

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoogheem, T.J.; Woods, L.A.

The Monsanto Analytical Testing (MAT) program was devised and implemented in order to provide analytical standards to Monsanto manufacturing plants involved in the self-monitoring of plant discharges as required by National Pollutant Discharge Elimination System (NPDES) permit conditions. Standards are prepared and supplied at concentration levels normally observed at each individual plant. These levels were established by canvassing all Monsanto plants having NPDES permits and by determining which analyses and concentrations were most appropriate. Standards are prepared by Monsanto's analyses and concentrations were most appropriate. Standards are prepared by Monsanto's Environmental Sciences Center (ESC) using Environmental Protection Agency (EPA) methods.more » Eleven standards are currently available, each in three concentrations. Standards are issued quarterly in a company internal round-robin program or on a per request basis or both. Since initiation of the MAT program in 1981, the internal round-robin program has become an integral part of Monsanto's overall Good Laboratory Practices (GLP) program. Overall, results have shown that the company's plant analytical personnel can accurately analyze and report standard test samples. More importantly, such personnel have gained increased confidence in their ability to report accurate values for compounds regulated in their respective plant NPDES permits. 3 references, 3 tables.« less

Analysis of Carbamate Pesticides: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS666

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for analysis of aldicarb, bromadiolone, carbofuran, oxamyl, and methomyl in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS666. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in MS666 for analysis of carbamatemore » pesticides in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS666 can be determined.« less

Analysis of Ethanolamines: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS888

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Vu, A; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method titled 'Analysis of Diethanolamine, Triethanolamine, n-Methyldiethanolamine, and n-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS): EPA Method MS888'. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in 'EPA Method MS888' for analysis of themore » listed ethanolamines in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of 'EPA Method MS888' can be determined.« less

Analysis of Thiodiglycol: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS777

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for the analysis of thiodiglycol, the breakdown product of the sulfur mustard HD, in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS777 (hereafter referred to as EPA CRL SOP MS777). This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to verifymore » the analytical procedures described in MS777 for analysis of thiodiglycol in aqueous samples. The gathered data from this study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS777 can be determined.« less

Advances in the analysis of steroid hormone drugs in pharmaceuticals and environmental samples (2004-2010).

PubMed

Görög, Sándor

2011-06-25

A critical review of the literature of the analysis of steroid hormone drugs is presented based on 213 publications published between 2004 and 2010. The state of the art of the assay and purity check of bulk drug materials is characterized on the basis of the principal pharmacopoeias supplemented by the literature dealing with their impurity profiling and solid state characterization. The determination of the active ingredients and impurities/degradants in pharmaceutical formulation by HPLC, other chromatographic, electrodriven, spectrophotometric and other methods is also summarized. A short section deals with the application of analytical methods in drug research. The literature of the determination of steroid hormones in environmental samples is summarized in tabulated form. Copyright © 2010 Elsevier B.V. All rights reserved.

Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

PubMed

Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

2017-12-01

In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

Elemental line scanning of an increment core using EDXRF: from fundamental research to environmental forensics applications

Treesearch

Kevin T. Smith; Jean Christophe Balouet; Gil Oudijk

2008-01-01

Environmental forensics seeks to determine the responsible parties for contamination from leaks or spills of petroleum or other toxic products. Dendrochemistry contributes to environmental forensics at the intersection of analytical chemistry, tree biology, and environmental responsibility. To be useful, dendrochemistry requires the rigorous application of analytical...

Results of Fall 1994 sampling of gunite and associated tanks at the Oak Ridge National Laboratory, Oak Ridge, Tennessee

DOE Office of Scientific and Technical Information (OSTI.GOV)

NONE

1995-06-01

This Technical Memorandum, was developed under Work Breakdown Structure 1.4.12.6.1.01.41.12.02. 11 (Activity Data Sheet 3301, ``WAG 1``). This document provides the Environmental Restoration Program with analytical results from liquid and sludge samples from the Gunite and Associated Tanks (GAAT). Information provided in this report forms part of the technical basis for criticality safety, systems safety, engineering design, and waste management as they apply to the GAAT treatability study and remediation.

Department of Defense Operational Range Sustainability through Management of Munitions Constituents

DTIC Science & Technology

2014-04-01

the MCs resulting from military training activities on ranges, to characterize the environmental deposition of MCs on military ranges, and to develop...technologies to manage or contain MCs in soil and groundwater. The results from these efforts can be found in numerous technical reports and journal...groundwater flow rate (if available), aquifer characteristics, monitoring well logs (if available), and historical sampling and analytical results

Environmental and Water Quality Operational Studies. General Guidelines for Monitoring Contaminants in Reservoirs

DTIC Science & Technology

1986-02-01

espacially trte for the topics of sampling and analytical methods, statistical considerations, and the design of general water quality monitoring networks. For...and to the establishment and habitat differentiation of biological populations within reservoirs. Reservoir operatirn, esp- cially the timing...8217 % - - % properties of bottom sediments, as well as specific habitat associations of biological populations of reservoirs. Thus, such heterogeneities

Determination of hydroxytyrosol and tyrosol by liquid chromatography for the quality control of cosmetic products based on olive extracts.

PubMed

Miralles, Pablo; Chisvert, Alberto; Salvador, Amparo

2015-01-01

An analytical method for the simultaneous determination of hydroxytyrosol and tyrosol in different types of olive extract raw materials and cosmetic cream samples has been developed. The determination was performed by liquid chromatography with UV spectrophotometric detection. Different chromatographic parameters, such as mobile phase pH and composition, oven temperature and different sample preparation variables were studied. The best chromatographic separation was obtained under the following conditions: C18 column set at 35°C and isocratic elution of a mixture ethanol: 1% acetic acid solution at pH 5 (5:95, v/v) as mobile phase pumped at 1 mL min(-1). The detection wavelength was set at 280 nm and the total run time required for the chromatographic analysis was 10 min, except for cosmetic cream samples where 20 min runtime was required (including a cleaning step). The method was satisfactorily applied to 23 samples including solid, water-soluble and fat-soluble olive extracts and cosmetic cream samples containing hydroxytyrosol and tyrosol. Good recoveries (95-107%) and repeatability (1.1-3.6%) were obtained, besides of limits of detection values below the μg mL(-1) level. These good analytical features, as well as its environmentally-friendly characteristics, make the presented method suitable to carry out both the control of the whole manufacture process of raw materials containing the target analytes and the quality control of the finished cosmetic products. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of a dual-analyte fluorescent sensor for the determination of bioactive nitrite and selenite in water samples.

PubMed

Martínez-Tomé, M J; Esquembre, R; Mallavia, R; Mateo, C R

2010-01-20

Nitrite and selenium are two bioactive compounds found in the environment which show beneficial effects for health at low levels but have toxic effects at higher doses. Consequently, quantification of both analytes in water samples results of great interest in areas such as biomedicine, food technology and environmental analysis. In a recent paper, we immobilized the inclusion complex formed between 2,3-diaminonaphthalene (DAN) and 2-hydroxypropyl-beta-cyclodextrin (HP-beta-CD) in a sol-gel matrix, in order to prepare a highly sensitive reagentless fluorescence-based sensor for the specific measurement of nitrite. Here we have explored the possibility of using the sol-gel immobilized complex to quantify selenite (Se (IV)), the more toxic form of selenium, as well as to act as a dual-analyte chemical sensor for simultaneous quantification of both nitrite and selenite in aqueous samples. Results show that (a) inclusion of DAN in HP-beta-CD and its subsequent immobilization in a sol-gel matrix do not modify the reactivity of DAN against selenite, (b) the reaction product formed (4,5-benzopiazselenol) remains into the cyclodextrin increasing considerably its fluorescence quantum yield and avoiding, therefore, its extraction into organic solvents, (c) the developed sensor can detect selenite concentrations at submicromolar level with a minimum detection limit of 13 nM, (d) the immobilized system is able to simultaneously quantify nitrite and selenite at submicromolar concentrations in natural water samples with no further sample pre-treatment.

Analytical methods of the U.S. Geological Survey's New York District Water-Analysis Laboratory

USGS Publications Warehouse

Lawrence, Gregory B.; Lincoln, Tricia A.; Horan-Ross, Debra A.; Olson, Mark L.; Waldron, Laura A.

1995-01-01

The New York District of the U.S. Geological Survey (USGS) in Troy, N.Y., operates a water-analysis laboratory for USGS watershed-research projects in the Northeast that require analyses of precipitation and of dilute surface water and soil water for major ions; it also provides analyses of certain chemical constituents in soils and soil gas samples.This report presents the methods for chemical analyses of water samples, soil-water samples, and soil-gas samples collected in wateshed-research projects. The introduction describes the general materials and technicques for each method and explains the USGS quality-assurance program and data-management procedures; it also explains the use of cross reference to the three most commonly used methods manuals for analysis of dilute waters. The body of the report describes the analytical procedures for (1) solution analysis, (2) soil analysis, and (3) soil-gas analysis. The methods are presented in alphabetical order by constituent. The method for each constituent is preceded by (1) reference codes for pertinent sections of the three manuals mentioned above, (2) a list of the method's applications, and (3) a summary of the procedure. The methods section for each constitutent contains the following categories: instrumentation and equipment, sample preservation and storage, reagents and standards, analytical procedures, quality control, maintenance, interferences, safety considerations, and references. Sufficient information is presented for each method to allow the resulting data to be appropriately used in environmental investigations.

Determination of steroid hormones and related compounds in filtered and unfiltered water by solid-phase extraction, derivatization, and gas chromatography with tandem mass spectrometry

USGS Publications Warehouse

Foreman, William T.; Gray, James L.; ReVello, Rhiannon C.; Lindley, Chris E.; Losche, Scott A.; Barber, Larry B.

2012-01-01

A new analytical method has been developed and implemented at the U.S. Geological Survey National Water Quality Laboratory that determines a suite of 20 steroid hormones and related compounds in filtered water (using laboratory schedule 2434) and in unfiltered water (using laboratory schedule 4434). This report documents the procedures and initial performance data for the method and provides guidance on application of the method and considerations of data quality in relation to data interpretation. The analytical method determines 6 natural and 3 synthetic estrogen compounds, 6 natural androgens, 1 natural and 1 synthetic progestin compound, and 2 sterols: cholesterol and 3--coprostanol. These two sterols have limited biological activity but typically are abundant in wastewater effluents and serve as useful tracers. Bisphenol A, an industrial chemical used primarily to produce polycarbonate plastic and epoxy resins and that has been shown to have estrogenic activity, also is determined by the method. A technique referred to as isotope-dilution quantification is used to improve quantitative accuracy by accounting for sample-specific procedural losses in the determined analyte concentration. Briefly, deuterium- or carbon-13-labeled isotope-dilution standards (IDSs), all of which are direct or chemically similar isotopic analogs of the method analytes, are added to all environmental and quality-control and quality-assurance samples before extraction. Method analytes and IDS compounds are isolated from filtered or unfiltered water by solid-phase extraction onto an octadecylsilyl disk, overlain with a graded glass-fiber filter to facilitate extraction of unfiltered sample matrices. The disks are eluted with methanol, and the extract is evaporated to dryness, reconstituted in solvent, passed through a Florisil solid-phase extraction column to remove polar organic interferences, and again evaporated to dryness in a reaction vial. The method compounds are reacted with activated -methyl--trimethylsilyl trifluoroacetamide at 65 degrees Celsius for 1 hour to form trimethylsilyl or trimethylsilyl-enol ether derivatives that are more amenable to gas chromatographic separation than the underivatized compounds. Analysis is carried out by gas chromatography with tandem mass spectrometry using calibration standards that are derivatized concurrently with the sample extracts. Analyte concentrations are quantified relative to specific IDS compounds in the sample, which directly compensate for procedural losses (incomplete recovery) in the determined and reported analyte concentrations. Thus, reported analyte concentrations (or analyte recoveries for spiked samples) are corrected based on recovery of the corresponding IDS compound during the quantification process. Recovery for each IDS compound is reported for each sample and represents an absolute recovery in a manner comparable to surrogate recoveries for other organic methods used by the National Water Quality Laboratory. Thus, IDS recoveries provide a useful tool for evaluating sample-specific analytical performance from an absolute mass recovery standpoint. IDS absolute recovery will differ and typically be lower than the corresponding analyte’s method recovery in spiked samples. However, additional correction of reported analyte concentrations is unnecessary and inappropriate because the analyte concentration (or recovery) already is compensated for by the isotope-dilution quantification procedure. Method analytes were spiked at 10 and 100 nanograms per liter (ng/L) for most analytes (10 times greater spike levels were used for bisphenol A and 100 times greater spike levels were used for 3--coprostanol and cholesterol) into the following validation-sample matrices: reagent water, wastewater-affected surface water, a secondary-treated wastewater effluent, and a primary (no biological treatment) wastewater effluent. Overall method recovery for all analytes in these matrices averaged 100 percent, with overall relative standard deviation of 28 percent. Mean recoveries of the 20 individual analytes for spiked reagent-water samples prepared along with field samples and analyzed in 2009–2010 ranged from 84–104 percent, with relative standard deviations of 6–36 percent. Concentrations for two analytes, equilin and progesterone, are reported as estimated because these analytes had excessive bias or variability, or both. Additional database coding is applied to other reported analyte data as needed, based on sample-specific IDS recovery performance. Detection levels were derived statistically by fortifying reagent water at six different levels (0.1 to 4 ng/L) and range from about 0.4 to 4 ng/L for 16 analytes. Interim reporting levels applied to analytes in this report range from 0.8 to 8 ng/L. Bisphenol A and the sterols (cholesterol and 3-beta-coprostanol) were consistently detected in laboratory and field blanks. The minimum reporting levels were set at 100 ng/L for bisphenol A and at 200 ng/L for the two sterols to prevent any bias associated with the presence of these compounds in the blanks. A minimum reporting level of 2 ng/L was set for 11-ketotestosterone to minimize false positive risk from an interfering siloxane compound emanating as chromatographic-column bleed, from vial septum material, or from other sources at no more than 1 ng/L.

A modeling approach to compare ΣPCB concentrations between congener-specific analyses

USGS Publications Warehouse

Gibson, Polly P.; Mills, Marc A.; Kraus, Johanna M.; Walters, David M.

2017-01-01

Changes in analytical methods over time pose problems for assessing long-term trends in environmental contamination by polychlorinated biphenyls (PCBs). Congener-specific analyses vary widely in the number and identity of the 209 distinct PCB chemical configurations (congeners) that are quantified, leading to inconsistencies among summed PCB concentrations (ΣPCB) reported by different studies. Here we present a modeling approach using linear regression to compare ΣPCB concentrations derived from different congener-specific analyses measuring different co-eluting groups. The approach can be used to develop a specific conversion model between any two sets of congener-specific analytical data from similar samples (similar matrix and geographic origin). We demonstrate the method by developing a conversion model for an example data set that includes data from two different analytical methods, a low resolution method quantifying 119 congeners and a high resolution method quantifying all 209 congeners. We used the model to show that the 119-congener set captured most (93%) of the total PCB concentration (i.e., Σ209PCB) in sediment and biological samples. ΣPCB concentrations estimated using the model closely matched measured values (mean relative percent difference = 9.6). General applications of the modeling approach include (a) generating comparable ΣPCB concentrations for samples that were analyzed for different congener sets; and (b) estimating the proportional contribution of different congener sets to ΣPCB. This approach may be especially valuable for enabling comparison of long-term remediation monitoring results even as analytical methods change over time. 

New approach on trace analysis of triclosan in personal care products, biological and environmental matrices.

PubMed

Silva, Ana Rita M; Nogueira, J M F

2008-02-15

Stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-LC-DAD) is proposed for the determination of triclosan in personal care products, biological and environmental matrices, which is included in the priority lists, set by several international regulatory organizations. Instrumental conditions and experimental parameters that affecting SBSE-LD efficiency are fully discussed. Throughout systematic assays on 25 mL water samples spiked at the 10.0 microg L(-1) level, it had been established that stir bars coated with 126 microL of polydimethylsiloxane, an equilibrium time of 1h (1000 rpm) and acetonitrile under sonification (60 min) as back-extraction solvent, allowed the best analytical performance to determine triclosan in water matrices. From the data obtained, good recovery and remarkable repeatability were attained, providing experimental average yields (78.5+/-2.2%), although slightly lower than the theoretical equilibrium (99.7%) described by the octanol-water partition coefficients (K(PDMS/W)0.9992) from 0.4 to 108.0 microg L(-1). The application of the present method to determine triclosan in real matrices such as commercial toothpaste, saliva and urban wastewater samples, allowed appropriate selectivity, high sensitivity and accuracy using the standard addition methodology. The proposed method showed to be feasible and sensitive with a low-sample volume requirement to monitor triclosan in personal care products, biological and environmental matrices at the trace level, in compliance with international regulatory directives.

Trace analysis of 61 natural and synthetic progestins in river water and sewage effluents by ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Shen, Xiaoyan; Chang, Hong; Sun, Dezhi; Wang, Linxia; Wu, Fengchang

2018-04-15

A broad number of natural and synthetic progestins are widely used in human and veterinary therapies. Although progestins exhibit adverse effects in aquatic organisms, information about environmental occurrence and fate have been limited to several compounds, hampering the accuracy of risk assessments of the compounds. In this study, a selective and sensitive analytical method was established to simultaneously determine 19 natural and 42 synthetic progestins in environmental waters, and the synthetic progestins included 19-nortestosterone, 17α-hydroxyprogesterone and progesterone derivatives. All of the target compounds were effectively separated using an HSS T3 column, and the recoveries for effluent and river samples were 80-115% and 75-105%, respectively. The detection limits for the 61 analytes were in the range of 0.05-0.60 ng/L and 0.03-0.40 ng/L for the effluent and river samples, respectively. The developed method is applied to analyze the target progestogens in sewage effluent and river water samples from Beijing. The detected concentrations of natural progesterone metabolites (3α-hydroxy-5β-tetrahydroprogesterone) were up to 63 times higher than those of the parent compound. Of the three groups of synthetic progestins, the progesterone derivatives were detected for the first time and had the highest concentrations followed by the 19-nortestosterone and 17α-hydroxyprogesterone derivatives. In contrast to previous studies, the predominant derivative compounds of 19-nortestosterone were found to be 19-nortestosterone, gestodene and mifepristone, and those of 17α-hydroxyprogesterone were 6-epi-medroxy progesterone 17-acetate and melengestrol acetate. The toxicities and environmental risk of these emerging progestins deserves more attention in the future. Copyright © 2018 Elsevier Ltd. All rights reserved.

Simultaneous analysis of perfluoroalkyl and polyfluoroalkyl substances including ultrashort-chain C2 and C3 compounds in rain and river water samples by ultra performance convergence chromatography.

PubMed

Yeung, Leo W Y; Stadey, Christopher; Mabury, Scott A

2017-11-03

An analytical method using ultra performance convergence chromatography (UPC 2 ) coupled to a tandem mass spectrometer operated in negative electrospray mode was developed to measure perfluoroalkyl and polyfluoroalkyl substances (PFASs) including the ultrashort-chain PFASs (C2-C3). Compared to the existing liquid chromatography tandem mass spectrometry method using an ion exchange column, the new method has a lower detection limit (0.4pg trifluoroacetate (TFA) on-column), narrower peak width (3-6s), and a shorter run time (8min). Using the same method, different classes of PFASs (e.g., perfluoroalkyl sulfonates (PFSAs) and perfluorinated carboxylates (PFCAs), perfluorinated phosphonates (PFPAs) and phosphinates (PFPiAs), polyfluoroalkyl phosphate diesters (diPAPs)) can be measured in a single analysis. Rain (n=2) and river water (n=2) samples collected in Toronto, ON, were used for method validation and application. Results showed that short-chain PFAS (C2-C7 PFCAs and C4 PFSA) contributed to over 80% of the detectable PFASs in rain samples and the C2-C3 PFASs alone accounted for over 40% of the total. Reports on environmental levels of these ultrashort-chain PFASs are relatively scarce. Relatively large contribution of these ultrashort-chain PFASs to the total PFASs indicate the need to include the measurement of short-chain PFASs, especially C2 and C3 PFASs, in environmental monitoring. The sources of TFA and other short-chain PFASs in the environment are not entirely clear. The newly developed analytical method may help further investigation on the sources and the environmental levels of these ultrashort-chain PFASs. Copyright © 2017 Elsevier B.V. All rights reserved.

Rainfall, Discharge, and Water-Quality Data During Stormwater Monitoring, July 1, 2007, to June 30, 2008; Halawa Stream Drainage Basin and the H-1 Storm Drain, Oahu, Hawaii

USGS Publications Warehouse

Presley, Todd K.; Jamison, Marcael T.J.; Young, Stacie T.M.

2008-01-01

Storm runoff water-quality samples were collected as part of the State of Hawaii Department of Transportation Stormwater Monitoring Program. The program is designed to assess the effects of highway runoff and urban runoff on Halawa Stream and to assess the effects from the H-1 storm drain on Manoa Stream. For this program, rainfall data were collected at three stations, continuous discharge data at four stations, and water-quality data at six stations, which include the four continuous discharge stations. This report summarizes rainfall, discharge, and water-quality data collected between July 1, 2007, and June 30, 2008. A total of 16 environmental samples were collected over two storms during July 1, 2007, to June 30, 2008, within the Halawa Stream drainage area. Samples were analyzed for total suspended solids, total dissolved solids, nutrients, chemical oxygen demand, and selected trace metals (cadmium, chromium, copper, lead, and zinc). Additionally, grab samples were analyzed for oil and grease, total petroleum hydrocarbons, fecal coliform, and biological oxygen demand. Some samples were analyzed for only a partial list of these analytes because an insufficient volume of sample was collected by the automatic samplers. Three additional quality-assurance/quality-control samples were collected concurrently with the storm samples. A total of 16 environmental samples were collected over four storms during July 1, 2007, to June 30, 2008 at the H-1 Storm Drain. All samples at this site were collected using an automatic sampler. Samples generally were analyzed for total suspended solids, nutrients, chemical oxygen demand, oil and grease, total petroleum hydrocarbons, and selected trace metals (cadmium, chromium, copper, lead, nickel, and zinc), although some samples were analyzed for only a partial list of these analytes. During the storm of January 29, 2008, 10 discrete samples were collected. Varying constituent concentrations were detected for the samples collected at different times during this storm event. Two quality-assurance/quality-control samples were collected concurrently with the storm samples. Three additional quality-assurance/quality-control samples were collected during routine sampler maintenance to check the effectiveness of equipment-cleaning procedures.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bass, D A; TenKate, L B

Graphite furnace atomic absorption spectrophotometry (GFAAS) is used for determination of ultra-trace metals in environmentally important samples. In the generation of GFAAS calibration curves for many environmental applications, low concentration calibration standards must be prepared dally, as required by the Statement of Work (SOW) for the US Environmental Protection Agency (EPA) Contract Laboratory Program (CLP). This results in significant time and work for the analyst and significant cost to the Analytical Chemistry Laboratory (ACL) for chemicals and waste management. While EPA SW 846 is less prescriptive than the CLP SOW, ACL has been following the CLP guidelines because in-house criteriamore » regarding the stability of GFAAS standards have not been established. A study was conducted to determine the stability of GFAAS standards for analytes commonly used in the ACL (single and mixed) as a function of time. Data were collected over nine months. The results show that GFAAS standards for Sb, Pb, Se, Ag, and TI are stable for a longer period of time than currently assumed by the CLP SOW. Reducing the frequency of preparing these standards will increase efficiency, decrease the handling of hazardous the quantity of hazardous waste generated, and decrease the quantity of hazardous substances to be ordered and stocked by the laboratory. These benefits will improve GFAAS analysis quality, reduce costs, enhance safety, and lower environmental concerns.« less

Sample and data processing considerations for the NIST quantitative infrared database

NASA Astrophysics Data System (ADS)

Chu, Pamela M.; Guenther, Franklin R.; Rhoderick, George C.; Lafferty, Walter J.; Phillips, William

1999-02-01

Fourier-transform infrared (FT-IR) spectrometry has become a useful real-time in situ analytical technique for quantitative gas phase measurements. In fact, the U.S. Environmental Protection Agency (EPA) has recently approved open-path FT-IR monitoring for the determination of hazardous air pollutants (HAP) identified in EPA's Clean Air Act of 1990. To support infrared based sensing technologies, the National Institute of Standards and Technology (NIST) is currently developing a standard quantitative spectral database of the HAPs based on gravimetrically prepared standard samples. The procedures developed to ensure the quantitative accuracy of the reference data are discussed, including sample preparation, residual sample contaminants, data processing considerations, and estimates of error.

FLOQSwab™: Optimisation of Procedures for the Recovery of Microbiological Samples from Surfaces

PubMed Central

Finazzi, Guido; Losio, Marina Nadia; Varisco, Giorgio

2016-01-01

The FLOQSwab™ is a specimen collection device worldwide recognised for its superior performance in the clinical diagnostics. The aim of this work was to evaluate FLOQSwab™ for the recovery of microbiological samples from surfaces compared to the traditional swab (rayon tipped swab) as per ISO 18593:2004 standard. The FLOQSwab™, thanks to its innovative manufacturing technology, allows improving the efficiency of recovery and release of analyte. The study has been divided into two experiments. In the first experiment the two swabs were evaluated for their capacity to recover and release the analyte (three different bacterial loads of Escherichia coli). In the second experiment, the two swabs were evaluated for their capacity to recover three different bacterial loads of E. coli from two different surface materials (stainless steel and polypropylene). In all experiments the flocked swab demonstrated a higher recovery rate compared to the traditional rayon tipped swab. The data obtained from this preliminary study demonstrated that the FLOQSwab™ could be a good food surfaces collection device, which improves the recovery of the analyte and thus produces accurate results. Based on the outcomes of the study, a larger field study is in progress using the FLOQSwab™ for samples collection to improve both environmental monitoring and the efficacy of the hygiene controls for food safety. PMID:27853708

Pesticide data for selected Wyoming streams, 1976-78

USGS Publications Warehouse

Butler, David L.

1987-01-01

In 1976, the U.S. Geological Survey, in cooperation with the Wyoming Department of Agriculture, started a monitoring program to determine pesticide concentrations in Wyoming streams. This program was incorporated into the water-quality data-collection system already in operation. Samples were collected at 20 sites for analysis of various insecticides, herbicides, polychlorinated biphenyls, and polychlorinated napthalenes.\\The results through 1978 revealed small concentrations of pesticides in water and bottom-material samples were DDE (39 percent of the concentrations equal to or greater than the minimum reported concentrations of the analytical methods), DDD (20 percent), dieldrin (21 percent), and polychlorinated biphenyls (29 percent). The herbicides most commonly found in water samples were 2,4-D (29 percent of the concentrations equal to or greater than the minimum reported concentrations of the analytical method) and picloram (23 percent). Most concentrations were significantly less than concentrations thought to be harmful to freshwater aquatic life based on available toxicity data. However for some pesticides, U.S. Environmental Protection Agency water-quality criteria for freshwater aquatic life are based on bioaccumulation factors that result in criteria concentrations less than the minimum reported concentrations of the analytical methods. It is not known if certain pesticides were present at concentrations less than the minimum reported concentrations that exceeded these criteria.

Advances in metabolome information retrieval: turning chemistry into biology. Part I: analytical chemistry of the metabolome.

PubMed

Tebani, Abdellah; Afonso, Carlos; Bekri, Soumeya

2018-05-01

Metabolites are small molecules produced by enzymatic reactions in a given organism. Metabolomics or metabolic phenotyping is a well-established omics aimed at comprehensively assessing metabolites in biological systems. These comprehensive analyses use analytical platforms, mainly nuclear magnetic resonance spectroscopy and mass spectrometry, along with associated separation methods to gather qualitative and quantitative data. Metabolomics holistically evaluates biological systems in an unbiased, data-driven approach that may ultimately support generation of hypotheses. The approach inherently allows the molecular characterization of a biological sample with regard to both internal (genetics) and environmental (exosome, microbiome) influences. Metabolomics workflows are based on whether the investigator knows a priori what kind of metabolites to assess. Thus, a targeted metabolomics approach is defined as a quantitative analysis (absolute concentrations are determined) or a semiquantitative analysis (relative intensities are determined) of a set of metabolites that are possibly linked to common chemical classes or a selected metabolic pathway. An untargeted metabolomics approach is a semiquantitative analysis of the largest possible number of metabolites contained in a biological sample. This is part I of a review intending to give an overview of the state of the art of major metabolic phenotyping technologies. Furthermore, their inherent analytical advantages and limits regarding experimental design, sample handling, standardization and workflow challenges are discussed.

Development of a selective and sensitive flotation method for determination of trace amounts of cobalt, nickel, copper and iron in environmental samples.

PubMed

Karimi, H; Ghaedi, M; Shokrollahi, A; Rajabi, H R; Soylak, M; Karami, B

2008-02-28

A simple, selective and rapid flotation method for the separation-preconcentration of trace amounts of cobalt, nickel, iron and copper ions using phenyl 2-pyridyl ketone oxime (PPKO) has been developed prior to their flame atomic absorption spectrometric determinations. The influence of pH, amount of PPKO as collector, type and amount of eluting agent, type and amount of surfactant as floating agent and ionic strength was evaluated on the recoveries of analytes. The influences of the concomitant ions on the recoveries of the analyte ions were also examined. The enrichment factor was 93. The detection limits based on 3 sigma for Cu, Ni, Co and Fe were 0.7, 0.7, 0.8, and 0.7 ng mL(-1), respectively. The method has been successfully applied for determination of trace amounts of ions in various real samples.

Nuclear analytical techniques in medicine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cesareo, R.

1988-01-01

This book acquaints one with the fundamental principles and the instrumentation relevant to analytical technique based on atomic and nuclear physics, as well as present and future biomedical applications. Besides providing a theoretical description of the physical phenomena, a large part of the book is devoted to applications in the medical and biological field, particularly in hematology, forensic medicine and environmental science. This volume reviews methods such as the possibility of carrying out rapid multi-element analysis of trace elements on biomedical samples, in vitro and in vivo, by XRF-analysis; the ability of the PIXE-microprobe to analyze in detail and tomore » map trace elements in fragments of biomedical samples or inside the cells; the potentiality of in vivo nuclear activation analysis for diagnostic purposes. Finally, techniques are described such as radiation scattering (elastic and inelastic scattering) and attenuation measurements which will undoubtedly see great development in the immediate future.« less

Forensic collection of trace chemicals from diverse surfaces with strippable coatings.

PubMed

Jakubowski, Michael J; Beltis, Kevin J; Drennan, Paul M; Pindzola, Bradford A

2013-11-07

Surface sampling for chemical analysis plays a vital role in environmental monitoring, industrial hygiene, homeland security and forensics. The standard surface sampling tool, a simple cotton gauze pad, is failing to meet the needs of the community as analytical techniques become more sensitive and the variety of analytes increases. In previous work, we demonstrated the efficacy of non-destructive, conformal, spray-on strippable coatings for chemical collection from simple glass surfaces. Here we expand that work by presenting chemical collection at a low spiking level (0.1 g m(-2)) from a diverse array of common surfaces - painted metal, engineering plastics, painted wallboard and concrete - using strippable coatings. The collection efficiency of the strippable coatings is compared to and far exceeds gauze pads. Collection from concrete, a particular challenge for wipes like gauze, averaged 73% over eight chemically diverse compounds for the strippable coatings whereas gauze averaged 10%.

Nanoparticle functionalised small-core suspended-core fibre - a novel platform for efficient sensing.

PubMed

Doherty, Brenda; Csáki, Andrea; Thiele, Matthias; Zeisberger, Matthias; Schwuchow, Anka; Kobelke, Jens; Fritzsche, Wolfgang; Schmidt, Markus A

2017-02-01

Detecting small quantities of specific target molecules is of major importance within bioanalytics for efficient disease diagnostics. One promising sensing approach relies on combining plasmonically-active waveguides with microfluidics yielding an easy-to-use sensing platform. Here we introduce suspended-core fibres containing immobilised plasmonic nanoparticles surrounding the guiding core as a concept for an entirely integrated optofluidic platform for efficient refractive index sensing. Due to the extremely small optical core and the large adjacent microfluidic channels, over two orders of magnitude of nanoparticle coverage densities have been accessed with millimetre-long sample lengths showing refractive index sensitivities of 170 nm/RIU for aqueous analytes where the fibre interior is functionalised by gold nanospheres. Our concept represents a fully integrated optofluidic sensing system demanding small sample volumes and allowing for real-time analyte monitoring, both of which are highly relevant within invasive bioanalytics, particularly within molecular disease diagnostics and environmental science.

SP70-alpha-benzoin oxime chelating resin for preconcentration-separation of Pb(II), Cd(II), Co(II) and Cr(III) in environmental samples.

PubMed

Narin, Ibrahim; Surme, Yavuz; Bercin, Erdogan; Soylak, Mustafa

2007-06-25

In the presented work, alpha-benzoin oxime immobilized SP70 chelating resin was synthesized for separation and preconcentration of Pb(II), Cd(II), Co(II) and Cr(III). The optimization procedure for analytical parameters including pH, eluent type, flow rate, etc. was examined in order to gain quantitative recoveries of analyte ions. The effects of foreign ions on the recoveries of studied metal ions were also investigated. The detection limits (3sigma) were found to be 16.0, 4.2, 1.3, 2.4microgL(-1) for Pb, Cd, Co and Cr, respectively. The preconcentration factor was 75 for Pb, 100 for Cd, Co and Cr. The optimized method was validated with certified reference materials and successfully applied to the waters, crops and pharmaceutical samples with good results (recoveries greater than 95%, R.S.D. lower than 10%).

Ultrasound extraction and thin layer chromatography-flame ionization detection analysis of the lipid fraction in marine mucilage samples.

PubMed

Mecozzi, M; Amici, M; Romanelli, G; Pietrantonio, E; Deluca, A

2002-07-19

This paper reports an analytical procedure based on ultrasound to extract lipids in marine mucilage samples. The experimental conditions of the ultrasound procedure (solvent and time) were identified by a FT-IR study performed on different standard samples of lipids and of a standard humic sample, before and after the sonication treatment. This study showed that diethyl ether was a more suitable solvent than methanol for the ultrasonic extraction of lipids from environmental samples because it allowed to minimize the possible oxidative modifications of lipids due to the acoustic cavitation phenomena. The optimized conditions were applied to the extraction of total lipid amount in marine mucilage samples and TLC-flame ionization detection analysis was used to identify the relevant lipid sub-fractions present in samples.

A New Project-Based Lab for Undergraduate Environmental and Analytical Chemistry

ERIC Educational Resources Information Center

Adami, Gianpiero

2006-01-01

A new project-based lab was developed for third year undergraduate chemistry students based on real world applications. The experience suggests that the total analytical procedure (TAP) project offers a stimulating alternative for delivering science skills and developing a greater interest for analytical chemistry and environmental sciences and…

Ambient Mass Spectrometry Imaging Using Direct Liquid Extraction Techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Laskin, Julia; Lanekoff, Ingela

2015-11-13

Mass spectrometry imaging (MSI) is a powerful analytical technique that enables label-free spatial localization and identification of molecules in complex samples.1-4 MSI applications range from forensics5 to clinical research6 and from understanding microbial communication7-8 to imaging biomolecules in tissues.1, 9-10 Recently, MSI protocols have been reviewed.11 Ambient ionization techniques enable direct analysis of complex samples under atmospheric pressure without special sample pretreatment.3, 12-16 In fact, in ambient ionization mass spectrometry, sample processing (e.g., extraction, dilution, preconcentration, or desorption) occurs during the analysis.17 This substantially speeds up analysis and eliminates any possible effects of sample preparation on the localization of moleculesmore » in the sample.3, 8, 12-14, 18-20 Venter and co-workers have classified ambient ionization techniques into three major categories based on the sample processing steps involved: 1) liquid extraction techniques, in which analyte molecules are removed from the sample and extracted into a solvent prior to ionization; 2) desorption techniques capable of generating free ions directly from substrates; and 3) desorption techniques that produce larger particles subsequently captured by an electrospray plume and ionized.17 This review focuses on localized analysis and ambient imaging of complex samples using a subset of ambient ionization methods broadly defined as “liquid extraction techniques” based on the classification introduced by Venter and co-workers.17 Specifically, we include techniques where analyte molecules are desorbed from solid or liquid samples using charged droplet bombardment, liquid extraction, physisorption, chemisorption, mechanical force, laser ablation, or laser capture microdissection. Analyte extraction is followed by soft ionization that generates ions corresponding to intact species. Some of the key advantages of liquid extraction techniques include the ease of operation, ability to analyze samples in their native environments, speed of analysis, and ability to tune the extraction solvent composition to a problem at hand. For example, solvent composition may be optimized for efficient extraction of different classes of analytes from the sample or for quantification or online derivatization through reactive analysis. In this review, we will: 1) introduce individual liquid extraction techniques capable of localized analysis and imaging, 2) describe approaches for quantitative MSI experiments free of matrix effects, 3) discuss advantages of reactive analysis for MSI experiments, and 4) highlight selected applications (published between 2012 and 2015) that focus on imaging and spatial profiling of molecules in complex biological and environmental samples.« less

Determination of lead and nickel in environmental samples by flame atomic absorption spectrometry after column solid-phase extraction on Ambersorb-572 with EDTA.

PubMed

Baytak, Sitki; Türker, A Rehber

2006-02-28

Lead and nickel were preconcentrated as their ethylenediaminetetraacedic acid (EDTA) complexes from aqueous sample solutions using a column containing Ambersorb-572 and determined by flame atomic absorption spectrometry (FAAS). pH values, amount of solid phase, elution solution and flow rate of sample solution have been optimized in order to obtain quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of Pb and Ni under the optimum conditions were 99 +/- 2 and 97 +/- 3%, respectively, at 95% confidence level. Seventy-five-fold (using 750 mL of sample solution and 10 mL of eluent) and 50-fold (using 500 mL of sample solution and 10 mL of eluent) preconcentration was obtained for Pb and Ni, respectively. Time of analysis is about 4.5 h (for obtaining enrichment factor of 75). By applying these enrichment factors, the analytical detection limits of Pb and Ni were found as 3.65 and 1.42 ng mL(-1), respectively. The capacity of the sorbent was found as 0.17 and 0.21 mmol g(-1) for Pb and Ni, respectively. The interferences of some cations, such as Mn2+, Co2+, Fe3+, Al3+, Zn2+, Cd2+, Ca2+, Mg2+, K+ and Na+ usually present in water samples were also studied. This procedure was applied to the determination of lead and nickel in parsley, green onion, sea water and waste water samples. The accuracy of the procedure was checked by determining Pb and Ni in standard reference tea leaves sample (GBW-07605). The results demonstrated good agreement with the certified values.

Online analysis of five organic ultraviolet filters in environmental water samples using magnetism-enhanced monolith-based in-tube solid phase microextraction coupled with high-performance liquid chromatography.

PubMed

Mei, Meng; Huang, Xiaojia

2017-11-24

Due to the endocrine disrupting properties, organic UV filters have been a great risk for humans and other organisms. Therefore, development of accurate and effective analytical methods is needed for the determination of UV filters in environmental waters. In this work, a fast, sensitive and environmentally friendly method combining magnetism-enhanced monolith-based in-tube solid phase microextraction with high-performance liquid chromatography with diode array detection (DAD) (ME-MB-IT/SPME-HPLC-DAD) for the online analysis of five organic UV filters in environmental water samples was developed. To extract UV filters effectively, an ionic liquid-based monolithic capillary column doped with magnetic nanoparticles was prepared by in-situ polymerization and used as extraction medium of online ME-MB-IT/SPME-HPLC-DAD system. Several extraction conditions including the intensity of magnetic field, sampling and desorption flow rate, volume of sample and desorption solvent, pH value and ionic strength of sample matrix were optimized thoroughly. Under the optimized conditions, the extraction efficiencies for five organic UV filters were in the range of 44.0-100%. The limits of detection (S/N=3) and limits of quantification (S/N=10) were 0.04-0.26μg/L and 0.12-0.87μg/L, respectively. The precisions indicated by relative standard deviations (RSDs) were less than 10% for both intra- and inter-day variabilities. Finally, the developed method was successfully applied to the determination of UV filters in three environmental water samples and satisfactory results were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

Radiochemical determination of 241Am and Pu(alpha) in environmental materials.

PubMed

Warwick, P E; Croudace, I W; Oh, J S

2001-07-15

Americium-241 and plutonium determinations will become of greater importance over the coming decades as 137Cs and 241Pu decay. The impact of 137Cs on environmental chronology has been great, but its potency is waning as it decays and diffuses. Having 241Am and Pu as unequivocal markers for the 1963 weapon fallout maximum is important for short time scale environmental work, but a fast and reliable procedure is required for their separation. The developed method described here begins by digesting samples using a lithium borate fusion although an aqua regia leachate is also effective in many instances. Isolation of the Am and Pu is then achieved using a combination of extraction chromatography and conventional anion exchange chromatography. The whole procedure has been optimized, validated, and assessed for safety. The straightforwardness of this technique permits the analysis of large numbers of samples and makes 241Am-based techniques for high-resolution sediment accumulation rate studies attractive. In addition, the technique can be employed for the sequential measurement of Pu and Am in environmental surveillance programs, potentially reducing analytical costs and turnround times.

Quality-control results for ground-water and surface-water data, Sacramento River Basin, California, National Water-Quality Assessment, 1996-1998

USGS Publications Warehouse

Munday, Cathy; Domagalski, Joseph L.

2003-01-01

Evaluating the extent that bias and variability affect the interpretation of ground- and surface-water data is necessary to meet the objectives of the National Water-Quality Assessment (NAWQA) Program. Quality-control samples used to evaluate the bias and variability include annual equipment blanks, field blanks, field matrix spikes, surrogates, and replicates. This report contains quality-control results for the constituents critical to the ground- and surface-water components of the Sacramento River Basin study unit of the NAWQA Program. A critical constituent is one that was detected frequently (more than 50 percent of the time in blank samples), was detected at amounts exceeding water-quality standards or goals, or was important for the interpretation of water-quality data. Quality-control samples were collected along with ground- and surface-water samples during the high intensity phase (cycle 1) of the Sacramento River Basin NAWQA beginning early in 1996 and ending in 1998. Ground-water field blanks indicated contamination of varying levels of significance when compared with concentrations detected in environmental ground-water samples for ammonia, dissolved organic carbon, aluminum, and copper. Concentrations of aluminum in surface-water field blanks were significant when compared with environmental samples. Field blank samples collected for pesticide and volatile organic compound analyses revealed no contamination in either ground- or surface-water samples that would effect the interpretation of environmental data, with the possible exception of the volatile organic compound trichloromethane (chloroform) in ground water. Replicate samples for ground water and surface water indicate that variability resulting from sample collection, processing, and analysis was generally low. Some of the larger maximum relative percentage differences calculated for replicate samples occurred between samples having lowest absolute concentration differences and(or) values near the reporting limit. Surrogate recoveries for pesticides analyzed by gas chromatography/mass spectrometry (GC/MS), pesticides analyzed by high performance liquid chromatography (HPLC), and volatile organic compounds in ground- and surface-water samples were within the acceptable limits of 70 to 130 percent and median recovery values between 82 and 113 percent. The recovery percentages for surrogate compounds analyzed by HPLC had the highest standard deviation, 20 percent for ground-water samples and 16 percent for surface-water samples, and the lowest median values, 82 percent for ground-water samples and 91 percent for surface-water samples. Results were consistent with the recovery results described for the analytical methods. Field matrix spike recoveries for pesticide compounds analyzed using GC/MS in ground- and surface-water samples were comparable with published recovery data. Recoveries of carbofuran, a critical constituent in ground- and surface-water studies, and desethyl atrazine, a critical constituent in the ground-water study, could not be calculated because of problems with the analytical method. Recoveries of pesticides analyzed using HPLC in ground- and surface-water samples were generally low and comparable with published recovery data. Other methodological problems for HPLC analytes included nondetection of the spike compounds and estimated values of spike concentrations. Recovery of field matrix spikes for volatile organic compounds generally were within the acceptable range, 70 and 130 percent for both ground- and surface-water samples, and median recoveries from 62 to 127 percent. High or low recoveries could be related to errors in the field, such as double spiking or using spike solution past its expiration date, rather than problems during analysis. The methodological changes in the field spike protocol during the course of the Sacramento River Basin study, which included decreasing the amount of spike solu

Aptamer based electrochemical sensors for emerging environmental pollutants

PubMed Central

Hayat, Akhtar; Marty, Jean L.

2014-01-01

Environmental contaminants monitoring is one of the key issues in understanding and managing hazards to human health and ecosystems. In this context, aptamer based electrochemical sensors have achieved intense significance because of their capability to resolve a potentially large number of problems and challenges in environmental contamination. An aptasensor is a compact analytical device incorporating an aptamer (oligonulceotide) as the sensing element either integrated within or intimately associated with a physiochemical transducer surface. Nucleic acid is well known for the function of carrying and passing genetic information, however, it has found a key role in analytical monitoring during recent years. Aptamer based sensors represent a novelty in environmental analytical science and there are great expectations for their promising performance as alternative to conventional analytical tools. This review paper focuses on the recent advances in the development of aptamer based electrochemical sensors for environmental applications with special emphasis on emerging pollutants. PMID:25019067

Aptamer based electrochemical sensors for emerging environmental pollutants

NASA Astrophysics Data System (ADS)

Hayat, Akhtar; Marty, Jean Louis

2014-06-01

Environmental contaminants monitoring is one of the key issues in understanding and managing hazards to human health and ecosystems. In this context, aptamer based electrochemical sensors have achieved intense significance because of their capability to resolve a potentially large number of problems and challenges in environmental contamination. An aptasensor is a compact analytical device incorporating an aptamer (oligonulceotide) as the sensing element either integrated within or intimately associated with a physiochemical transducer surface. Nucleic acid is well known for the function of carrying and passing genetic information, however, it has found a key role in analytical monitoring during recent years. Aptamer based sensors represent a novelty in environmental analytical science and there are great expectations for their promising performance as alternative to conventional analytical tools. This review paper focuses on the recent advances in the development of aptamer based electrochemical sensors for environmental applications with special emphasis on emerging pollutants.

Analytical techniques and method validation for the measurement of selected semivolatile and nonvolatile organofluorochemicals in air.

PubMed

Reagen, William K; Lindstrom, Kent R; Thompson, Kathy L; Flaherty, John M

2004-09-01

The widespread use of semi- and nonvolatile organofluorochemicals in industrial facilities, concern about their persistence, and relatively recent advancements in liquid chromatography/mass spectrometry (LC/MS) technology have led to the development of new analytical methods to assess potential worker exposure to airborne organofluorochemicals. Techniques were evaluated for the determination of 19 organofluorochemicals and for total fluorine in ambient air samples. Due to the potential biphasic nature of most of these fluorochemicals when airborne, Occupational Safety and Health Administration (OSHA) versatile sampler (OVS) tubes were used to simultaneously trap fluorochemical particulates and vapors from workplace air. Analytical methods were developed for OVS air samples to quantitatively analyze for total fluorine using oxygen bomb combustion/ion selective electrode and for 17 organofluorochemicals using LC/MS and gas chromatography/mass spectrometry (GC/MS). The experimental design for this validation was based on the National Institute of Occupational Safety and Health (NIOSH) Guidelines for Air Sampling and Analytical Method Development and Evaluation, with some revisions of the experimental design. The study design incorporated experiments to determine analytical recovery and stability, sampler capacity, the effect of some environmental parameters on recoveries, storage stability, limits of detection, precision, and accuracy. Fluorochemical mixtures were spiked onto each OVS tube over a range of 0.06-6 microg for each of 12 compounds analyzed by LC/MS and 0.3-30 microg for 5 compounds analyzed by GC/MS. These ranges allowed reliable quantitation at 0.001-0.1 mg/m3 in general for LC/MS analytes and 0.005-0.5 mg/m3 for GC/MS analytes when 60 L of air are sampled. The organofluorochemical exposure guideline (EG) is currently 0.1 mg/m3 for many analytes, with one exception being ammonium perfluorooctanoate (EG is 0.01 mg/m3). Total fluorine results may be used to determine if the individual compounds quantified provide a suitable mass balance of total airborne organofluorochemicals based on known fluorine content. Improvements in precision and/or recovery as well as some additional testing would be needed to meet all NIOSH validation criteria. This study provided valuable information about the accuracy of this method for organofluorochemical exposure assessment.

Ultra-high-stability, pH-resistant sol-gel titania poly(tetrahydrofuran) coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

PubMed

Segro, Scott S; Cabezas, Yaniel; Malik, Abdul

2009-05-15

A sol-gel titania poly(tetrahydrofuran) (poly-THF) coating was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). Poly-THF was covalently bonded to the sol-gel titania network which, in turn, became chemically anchored to the inner surface of a 0.25mm I.D. fused silica capillary. For sample preconcentration, a 38-cm segment of the sol-gel titania poly-THF coated capillary was installed on an HPLC injection port as a sampling loop. Aqueous samples containing a variety of analytes were passed through the capillary and, during this process, the analytes were extracted by the sol-gel titania poly-THF coating on the inner surface of the capillary. Using isocratic and gradient elution with acetonitrile/water mobile phases, the extracted analytes were desorbed into the on-line coupled HPLC column for separation and UV detection. The sol-gel titania poly-THF coating was especially efficient in extracting polar analytes, such as underivatized phenols, alcohols, amines, and aromatic carboxylic acids. In addition, this coating was capable of extracting moderately polar and nonpolar analytes, such as ketones and polycyclic aromatic hydrocarbons. The sol-gel titania poly-THF coated capillary was also able to extract polypeptides at pH values near their respective isoelectric points. Extraction of these compounds can be important for environmental and biomedical applications. The observed extraction behavior can be attributed to the polar and nonpolar moieties in the poly-THF structure. This coating was found to be stable under extremely low and high pH conditions-even after 18h of exposure to 1M HCl (pH approximately 0.0) and 1M NaOH (pH approximately 14.0).

Investigation of the persistence of nerve agent degradation analytes on surfaces through wipe sampling and detection with ultrahigh performance liquid chromatography-tandem mass spectrometry.

PubMed

Willison, Stuart A

2015-01-20

The persistence of chemical warfare nerve agent degradation analytes on surfaces is important, from indicating the presence of nerve agent on a surface to guiding environmental restoration of a site after a release. Persistence was investigated for several chemical warfare nerve agent degradation analytes on indoor surfaces and presents an approach for wipe sampling of surfaces, followed by wipe extraction and liquid chromatography-tandem mass spectrometry detection. Commercially available wipe materials were investigated to determine optimal wipe recoveries. Tested surfaces included porous/permeable (vinyl tile, painted drywall, and wood) and largely nonporous/impermeable (laminate, galvanized steel, and glass) surfaces. Wipe extracts were analyzed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). UPLC provides a separation of targeted degradation analytes in addition to being nearly four times faster than high-performance liquid chromatography, allowing for greater throughput after a large-scale contamination incident and subsequent remediation events. Percent recoveries from nonporous/impermeable surfaces were 60-103% for isopropyl methylphosphonate (IMPA), GB degradate; 61-91% for ethyl methylphosphonate (EMPA), VX degradate; and 60-98% for pinacolyl methylphosphonate (PMPA), GD degradate. Recovery efficiencies for methyl phosphonate (MPA), nerve agent degradate, and ethylhydrogen dimethylphosphonate (EHDMAP), GA degradate, were lower, perhaps due to matrix effects. Diisopropyl methylphosphonate, GB impurity, was not recovered from surfaces. The resulting detection limits for wipe extracts were 0.065 ng/cm(2) for IMPA, 0.079 ng/cm(2) for MPA, 0.040 ng/cm(2) for EMPA, 0.078 ng/cm(2) for EHDMAP, and 0.013 ng/cm(2) for PMPA. The data indicate that laboratories may hold wipe samples for up to 30 days prior to analysis. Target analytes were observed to persist on surfaces for at least 6 weeks.

Monitoring environmental risk in fibrous minerals in New Caledonia: a comparison between different analytical methods.

NASA Astrophysics Data System (ADS)

Petriglieri, Jasmine Rita; Laporte-Magoni, Christine; Salvioli-Mariani, Emma; Gunkel-Grillon, Peggy; Tribaudino, Mario; Mantovani, Luciana; Bersani, Danilo; Lottici, Pier Paolo; Tomatis, Maura

2017-04-01

The New Caledonia is covered by ultrabasic units for more than a third of its surface, and it is one of the largest world producers of nickel ore. Mining activity, focused on extraction from lateritic ore deposits formed by the alteration of ultramafic rocks, must deal with the natural occurrence of asbestos and fibrous minerals. Almost all outcrops of geological units in open mines contain serpentine and amphibole, also as asbestos varieties (Lahondère, 2007). Owing to humid tropical to sub-tropical conditions, weathering processes and supergene mineralization are one of the main responsible for fibrogenesis of asbestos minerals. The presence of fibrous minerals in mining and storage sites requires attention due to public health problems and for the safety of the operators. In this context, the evaluation of risk and health hazard to prevent the effects due to exposition is closely linked to the formation, alteration and release of fibers into the environment. It has been demonstrated that different fibrous minerals have different toxicity (Fubini & Otero-Arean, 1999; Fubini & Fenoglio, 2007). An analytical strategy to discriminate and characterize, with certainty, the different varieties of the asbestiform phases is required to the establishment of an environmental monitoring system. We have therefore analyzed by different methods a set of about fifty asbestos sampled for mapping environmental risk in fibrous minerals in New Caledonia. The samples contain serpentines (chrysotile, antigorite) and amphibole (tremolite), all fibrous and have been sorted by their different degree of alteration. Data obtained with the more traditional mineralogical and petrological analytical techniques - such as optical microscopy, X-ray diffraction, secondary electron microscopy (SEM-EDS), and transmission electron microscopy - have been completed by the employment of more specialized tools as phase contrast microscopy (PCM), Raman spectroscopy, and thermal analysis (DTA). Moreover analytical performances of a Raman portable equipment, to be used in field observation, were assessed against other laboratory methods. Portable Raman was tested first in laboratory to check its reliability, and then on fieldtrip, directly on the mining front under normal environmental conditions (sun, strong wind, high temperature, etc.). Thus, for each analytical method, ability for fibers identification was tested. This project is part of the French-Italian program "Amiantes et Bonnes Pratiques", financed by the CNRT "Nickel and its environment" of New Caledonia. Fubini, B., & Otero-Arean, C. (1999): Chemical aspects of the toxicity of inhaled mineral dusts. Chemical Society Reviews, 28(6), 373-381. Fubini, B., & Fenoglio, I. (2007): Toxic potential of mineral dusts. Elements, 3(6), 407-414. Lahondère, D. (2007): L'amiante environnemental en Nouvelle Calédonie: Expertise géologique des zones amiantifères. Evaluation des actions engagées. BRGM/RP-55894-FR, 55 p.

Sediment studies in the Assabet River, central Massachusetts, 2003

USGS Publications Warehouse

Zimmerman, Marc J.; Sorenson, Jason R.

2005-01-01

From its headwaters in Westborough, Massachusetts, to its confluence with the Sudbury River, the 53-kilometer-long Assabet River passes through a series of small towns and mixed land-use areas. Along the way, wastewater-treatment plants release nutrient-rich effluents that contribute to the eutrophic state of this waterway. This condition is most obvious where the river is impounded by a series of dams that have sequestered large amounts of sediment and support rooted and floating macrophytes and epiphytic algae. The water in parts of these impoundments may also have low concentrations of dissolved oxygen, another symptom of eutrophication. All of the impoundments had relatively shallow maximum water depths, which ranged from approximately 2.4 to 3.4 meters, and all had extensive shallow areas. Sediment volumes estimated for the six impoundments ranged from approximately 380 cubic meters in the Aluminum City impoundment to 580,000 cubic meters in the Ben Smith impoundment. The other impoundments had sediment volumes of 120,000 cubic meters (Powdermill), 67,000 cubic meters (Gleasondale), 55,000 cubic meters (Hudson), and 42,000 cubic meters (Allen Street). The principal objective of this study was the determination of sediment volume, extent, and chemistry, in particular, the characterization of toxic inorganic and organic chemicals in the sediments. To determine the bulk-sediment chemical-constituent concentrations, more than one hundred sediment cores were collected in pairs from the six impoundments. One core from each pair was sampled for inorganic constituents and the other for organic constituents. Most of the cores analyzed for inorganics were sectioned to provide information on the vertical distribution of analytes; a subset of the cores analyzed for organics was also sectioned. Approximately 200 samples were analyzed for inorganic constituents and 100 for organics; more than 10 percent were quality-control replicate or blank samples. Maximum bulk-sediment phosphorus concentrations in surface samples from the impoundments increased along a downstream gradient, with the exception of samples from the last impoundment, where the concentrations decreased. In addition, the highest phosphorus concentrations were generally in the surface samples; this finding may prove helpful if surface dredging is selected as a means to control phosphorus release from sediments. There is no known relation, however, between bulk-sediment concentration of phosphorus and the concentrations of phosphorus available to biota. Potentially toxic metals, including arsenic, cadmium, chromium, copper, nickel, lead, and zinc were frequently measured at concentrations that exceeded U.S. Environmental Protection Agency sediment-quality guidelines for the protection of aquatic life and that occasionally exceeded Massachusetts Department of Environmental Protection guidelines governing landfill disposal (reuse). Due to the effects of matrix interference and sample dilution on laboratory analyses, neither pesticides nor volatile organic compounds were detected at any sites. However, samples collected in other studies from nearby streams indicated the possibility that pesticides might have been detected in the impoundments if not for these analytical problems. Although polychlorinated biphenyl concentrations, as individual Aroclors, generally exceeded published U.S. Environmental Protection Agency guideline concentrations for potential effects on aquatic life, the U.S. Environmental Protection Agency guideline concentrations for human contact or the Massachusetts guidelines for landfill reuse were rarely exceeded. Concentrations of polycyclic aromatic hydrocarbons, both individually and total, frequently were greater than guideline concentrations. Concentrations of total extractable petroleum hydrocarbons did not exceed Massachusetts guideline concentrations in any samples. When the sediment analytes from surface samples are considered togethe

INVESTIGATING ENVIRONMENTAL SINKS OF MACROLIDE ANTIBIOTICS WITH ANALYTICAL CHEMISTRY

EPA Science Inventory

Possible environmental sinks (wastewater effluents, biosolids, sediments) of macrolide antibiotics (i.e., azithromycin, roxithromycin and clarithromycin)are investigated using state-of-the-art analytical chemistry techniques.

Environmental Response Laboratory Network (ERLN) Data Submission Requirements

EPA Pesticide Factsheets

These Environmental Response Laboratory Network specifications are essential to the mission of providing consistent analytical data of know and documented quality for each Analytical Service Request (ASR).

Egoistic, altruistic, and biospheric environmental concerns: a path analytic investigation of their determinants.

PubMed

Swami, Viren; Chamorro-Premuzic, Tomas; Snelgar, Rosemary; Furnham, Adrian

2010-04-01

Previous studies have shown that environmental concerns (ECs) can be reduced to a three-factor model - comprising altruistic, biospheric, and egoistic concerns - but there have been few studies examining individual difference predictors of ECs. In this study with 203 individuals from a British community sample, we show that biospheric concern was significantly associated with participants' age, political orientation, Machiavellianism, and the Big Five personality traits of Agreeableness, Emotional Stability, and Conscientiousness. Altruistic concern was significantly associated with sex, age, political orientation, and Machiavellianism, but not the Big Five traits, whereas egoistic concern was not significantly associated with any of these predictors except sex. These results are discussed in relation to previous work on ECs and pro-environmental behavior.

An automated baseline correction protocol for infrared spectra of atmospheric aerosols collected on polytetrafluoroethylene (Teflon) filters

NASA Astrophysics Data System (ADS)

Kuzmiakova, Adele; Dillner, Ann M.; Takahama, Satoshi

2016-06-01

A growing body of research on statistical applications for characterization of atmospheric aerosol Fourier transform infrared (FT-IR) samples collected on polytetrafluoroethylene (PTFE) filters (e.g., Russell et al., 2011; Ruthenburg et al., 2014) and a rising interest in analyzing FT-IR samples collected by air quality monitoring networks call for an automated PTFE baseline correction solution. The existing polynomial technique (Takahama et al., 2013) is not scalable to a project with a large number of aerosol samples because it contains many parameters and requires expert intervention. Therefore, the question of how to develop an automated method for baseline correcting hundreds to thousands of ambient aerosol spectra given the variability in both environmental mixture composition and PTFE baselines remains. This study approaches the question by detailing the statistical protocol, which allows for the precise definition of analyte and background subregions, applies nonparametric smoothing splines to reproduce sample-specific PTFE variations, and integrates performance metrics from atmospheric aerosol and blank samples alike in the smoothing parameter selection. Referencing 794 atmospheric aerosol samples from seven Interagency Monitoring of PROtected Visual Environment (IMPROVE) sites collected during 2011, we start by identifying key FT-IR signal characteristics, such as non-negative absorbance or analyte segment transformation, to capture sample-specific transitions between background and analyte. While referring to qualitative properties of PTFE background, the goal of smoothing splines interpolation is to learn the baseline structure in the background region to predict the baseline structure in the analyte region. We then validate the model by comparing smoothing splines baseline-corrected spectra with uncorrected and polynomial baseline (PB)-corrected equivalents via three statistical applications: (1) clustering analysis, (2) functional group quantification, and (3) thermal optical reflectance (TOR) organic carbon (OC) and elemental carbon (EC) predictions. The discrepancy rate for a four-cluster solution is 10 %. For all functional groups but carboxylic COH the discrepancy is ≤ 10 %. Performance metrics obtained from TOR OC and EC predictions (R2 ≥ 0.94 %, bias ≤ 0.01 µg m-3, and error ≤ 0.04 µg m-3) are on a par with those obtained from uncorrected and PB-corrected spectra. The proposed protocol leads to visually and analytically similar estimates as those generated by the polynomial method. More importantly, the automated solution allows us and future users to evaluate its analytical reproducibility while minimizing reducible user bias. We anticipate the protocol will enable FT-IR researchers and data analysts to quickly and reliably analyze a large amount of data and connect them to a variety of available statistical learning methods to be applied to analyte absorbances isolated in atmospheric aerosol samples.

Applying the Analytic Hierarchy Process to Oil Sands Environmental Compliance Risk Management

NASA Astrophysics Data System (ADS)

Roux, Izak Johannes, III

Oil companies in Alberta, Canada, invested $32 billion on new oil sands projects in 2013. Despite the size of this investment, there is a demonstrable deficiency in the uniformity and understanding of environmental legislation requirements that manifest into increased project compliance risks. This descriptive study developed 2 prioritized lists of environmental regulatory compliance risks and mitigation strategies and used multi-criteria decision theory for its theoretical framework. Information from compiled lists of environmental compliance risks and mitigation strategies was used to generate a specialized pairwise survey, which was piloted by 5 subject matter experts (SMEs). The survey was validated by a sample of 16 SMEs, after which the Analytic Hierarchy Process (AHP) was used to rank a total of 33 compliance risks and 12 mitigation strategy criteria. A key finding was that the AHP is a suitable tool for ranking of compliance risks and mitigation strategies. Several working hypotheses were also tested regarding how SMEs prioritized 1 compliance risk or mitigation strategy compared to another. The AHP showed that regulatory compliance, company reputation, environmental compliance, and economics ranked the highest and that a multi criteria mitigation strategy for environmental compliance ranked the highest. The study results will inform Alberta oil sands industry leaders about the ranking and utility of specific compliance risks and mitigations strategies, enabling them to focus on actions that will generate legislative and public trust. Oil sands leaders implementing a risk management program using the risks and mitigation strategies identified in this study will contribute to environmental conservation, economic growth, and positive social change.

Cross-Study Differences in the Etiology of Reading Comprehension: a Meta-Analytical Review of Twin Studies.

PubMed

Little, Callie W; Haughbrook, Rasheda; Hart, Sara A

2017-01-01

Numerous twin studies have examined the genetic and environmental etiology of reading comprehension, though it is likely that etiological estimates are influenced by unidentified sample conditions (e.g. Tucker-Drob and Bates, Psychol Sci:0956797615612727, 2015). The purpose of this meta-analysis was to average the etiological influences of reading comprehension and to explore the potential moderators influencing these estimates. Results revealed an average heritability estimate of h 2  = 0.59, with significant variation in estimates across studies, suggesting potential moderation. Moderation results indicated publication year, grade level, project, zygosity methods, and response type moderated heritability estimates. The average shared environmental estimate was c 2  = 0.16, with publication year, grade and zygosity methods acting as significant moderators. These findings support the role of genetics on reading comprehension, and a small significant role of shared environmental influences. The results suggest that our interpretation of how genes and environments influence reading comprehension should reflect aspects of study and sample.

Manual of analytical methods for the Environmental Health Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gray, C. E.

1975-06-01

This manual was compiled from techniques used In the Environmental Health Laboratory of Sandia Laboratories at Albuquerque. New Mexico, and is a revision of an earlier publication (SC-M-07-3044) edited by Lial W. Brewer. The procedures arc similar to those used in other laboratories devoted to Environmental Health practices. Some of the methods are standard and others are modified to suit our needs; others were developed at Sandia. The author has attempted to present all methods in a simple and concise manner, but in sufficient detail to make them readily usable. It is not inferred that the methods are universal formore » any type of sample, but they have been found very reliable for the types of samples mentioned. The author will welcome inquiry for clarification of any part of this manual. It is the desire of the author that this manual will be of use and service to others. New and revised procedures will be issued as supplements to this document.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Streets, W.E.

As the need for rapid and more accurate determinations of gamma-emitting radionuclides in environmental and mixed waste samples grows, there is continued interest in the development of theoretical tools to eliminate the need for some laboratory analyses and to enhance the quality of information from necessary analyses. In gamma spectrometry the use of theoretical self-absorption coefficients (SACs) can eliminate the need to determine the SAC empirically by counting a known source through each sample. This empirical approach requires extra counting time and introduces another source of counting error, which must be included in the calculation of results. The empirical determinationmore » of SACs is routinely used when the nuclides of interest are specified; theoretical determination of the SAC can enhance the information for the analysis of true unknowns, where there may be no prior knowledge about radionuclides present in a sample. Determination of an exact SAC does require knowledge about the total composition of a sample. In support of the Department of Energy`s (DOE) Environmental Survey Program, the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory developed theoretical self-absorption models to estimate SACs for the determination of non-specified radionuclides in samples of unknown, widely-varying, compositions. Subsequently, another SAC model, in a different counting geometry and for specified nuclides, was developed for another application. These two models are now used routinely for the determination of gamma-emitting radionuclides in a wide variety of environmental and mixed waste samples.« less

Background Radioactivity in River and Reservoir Sediments near Los Alamos, New Mexico

DOE Office of Scientific and Technical Information (OSTI.GOV)

S.G.McLin; D.W. Lyons

2002-05-05

As part of its continuing Environmental Surveillance Program, regional river and lake-bottom sediments have been collected annually by Los Alamos National Laboratory (the Laboratory) since 1974 and 1979, respectively. These background samples are collected from three drainage basins at ten different river stations and five reservoirs located throughout northern New Mexico and southern Colorado. Radiochemical analyses for these sediments include tritium, strontium-90, cesium-137, total uranium, plutonium-238, plutonium-239,-240, americium-241, gross alpha, gross beta, and gross gamma radioactivity. Detection-limit radioactivity originates as worldwide fallout from aboveground nuclear weapons testing and satellite reentry into Earth's atmosphere. Spatial and temporal variations in individual analytemore » levels originate from atmospheric point-source introductions and natural rate differences in airborne deposition and soil erosion. Background radioactivity values on sediments reflect this variability, and grouped river and reservoir sediment samples show a range of statistical distributions that appear to be analyte dependent. Traditionally, both river and reservoir analyte data were blended together to establish background levels. In this report, however, we group background sediment data according to two criteria. These include sediment source (either river or reservoir sediments) and station location relative to the Laboratory (either upstream or downstream). These grouped data are statistically evaluated through 1997, and background radioactivity values are established for individual analytes in upstream river and reservoir sediments. This information may be used to establish the existence and areal extent of trace-level environmental contamination resulting from historical Laboratory research activities since the early 1940s.« less

Quantitative on-line preconcentration-liquid chromatography coupled with tandem mass spectrometry method for the determination of pharmaceutical compounds in water.

PubMed

Idder, Salima; Ley, Laurent; Mazellier, Patrick; Budzinski, Hélène

2013-12-17

One of the current environmental issues concerns the presence and fate of pharmaceuticals in water bodies as these compounds may represent a potential environmental problem. The characterization of pharmaceutical contamination requires powerful analytical method able to quantify these pollutants at very low concentration (few ng L(-1)). In this work, a multi-residue analytical methodology (on-line solid phase extraction-liquid chromatography-triple quadrupole mass spectrometry using positive and negative electrospray ionization) has been developed and validated for 40 multi-class pharmaceuticals and metabolites for tap and surface waters. This on-line SPE method was very convenient and efficient compared to classical off-line SPE method because of its shorter total run time including sample preparation and smaller sample volume (1 mL vs up to 1 L). The optimized method included several therapeutic classes as lipid regulators, antibiotics, beta-blockers, non-steroidal anti-inflammatories, antineoplastic, etc., with various physicochemical properties. Quantification has been achieved with the internal standards. The limits of detection are between 0.7 and 15 ng L(-1) for drinking waters and 2-15 ng L(-1) for surface waters. The inter-day precision values are below 20% for each studied level. The improvement and strength of the analytical method has been verified along a monitoring of these 40 pharmaceuticals in Isle River, a French stream located in the South West of France. During this survey, 16 pharmaceutical compounds have been detected. Copyright © 2013 Elsevier B.V. All rights reserved.

New analytical method for the determination of styrene oligomers formed from polystyrene decomposition and its application at the coastlines of the North-West Pacific ocean.

PubMed

Saido, Katsuhiko; Koizumi, Koshiro; Sato, Hideto; Ogawa, Naoto; Kwon, Bum Gun; Chung, Seon-Yong; Kusui, Takashi; Nishimura, Masahiko; Kodera, Yoichi

2014-03-01

The pollution caused by plastic debris is an environmental problem with increasing concern in the oceans. Among the plastic polymers, polystyrene (PS) is one of the most problematic plastics due to the direct public health risk associated with their dispersion, as well as the numerous adverse environmental impacts which arise both directly from the plastics and from their degradation products. Little is known about their potential distribution characteristics throughout the oceans. For the first time, we report here on the regional distribution of styrene monomer (SM), styrene dimers (SD; 2,4-diphenyl-1-butene, SD1; 1,3-diphenyl propane, SD2), and styrene trimer (2,4,6-triphenyl-1-hexene: ST1), as products of PS decomposition determined from samples of sand and seawater from the shorelines of the North-West Pacific ocean. In order to quantitatively determine SM, SD (=SD1+SD2), and ST1, a new analytical method was developed. The detection limit was 3.3 μg L(-1), based on a signal-to-noise ratio of three, which was well-suited to quantify levels of SM, SD, and ST1 in samples. Surprisingly, the concentrations of SM, SD, and ST1 in sand samples from the shorelines were consistently greater than those in seawater samples from the same location. The results of this study suggest that SM, SD, and ST1 can be widely dispersed throughout the North-West Pacific oceans. Copyright © 2013 Elsevier B.V. All rights reserved.

Environmental Contaminants, Metabolites, Cells, Organ Tissues, and Water: All in a Day’s Work at the EPA Analytical Chemistry Research Core

EPA Science Inventory

The talk will highlight key aspects and results of analytical methods the EPA National Health and Environmental Effects Research Laboratory (NHEERL) Analytical Chemistry Research Core (ACRC) develops and uses to provide data on disposition, metabolism, and effects of environmenta...

Micelle assisted thin-film solid phase microextraction: a new approach for determination of quaternary ammonium compounds in environmental samples.

PubMed

Boyacı, Ezel; Pawliszyn, Janusz

2014-09-16

Determination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized labware. Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds. The proposed micelle assisted TF-SPME method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily acts as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating. The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2-97.3%; as such, this method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.

Fabrication of magnetic microsphere-confined graphene for the preconcentration of some phthalate esters from environmental water and soybean milk samples followed by their determination by HPLC.

PubMed

Wang, Weina; Ma, Ruiyang; Wu, Qiuhua; Wang, Chun; Wang, Zhi

2013-05-15

In this study, a magnetic microsphere-confined graphene (Fe3O4@SiO2-G) was prepared as a novel adsorbent for the preconcentration of some phthalate esters in environmental water and soybean milk samples prior to high performance liquid chromatography analysis. The properties and morphology of the Fe3O4@SiO2-G were characterized by transmission electron microscopy and X-ray diffraction. This novel graphene-based magnetic nanocomposite showed great adsorptive ability toward the analytes. The method, which takes the advantages of both the high adsorption capacity of G and easy phase separation of the magnetic adsorbent from the sample solution, could avoid the time-consuming experimental procedures related to the traditional solid phase extraction. Various experimental parameters that could affect the extraction efficiencies, such as the amount of Fe3O4@SiO2-G, the extraction time, the pH of sample solution and the desorption conditions, were investigated. Under the optimum conditions, the limits of detection (S/N=3) of the method for the compounds were between 0.07 and 0.10 ng mL(-1) in water samples, and between 0.15 and 0.30 ng mL(-1) in soybean milk samples. The relative standard deviations (RSDs) varied from 2.7% to 6.1% (n=5). The recoveries of the method were in the range between 87.2% and 109.0% for environmental water and soybean milk samples. The method is suitable to determine the five phthalate esters (diallyl phthalate, di-n-propyl-phthalate, benzyl butyl phthalate, dicyclohexyl-phthalate and diethyl-hexyl-phthalate) in environmental water and soybean milk samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Mixed hemimicelle solid-phase extraction based on magnetic halloysite nanotubes and ionic liquids for the determination and extraction of azo dyes in environmental water samples.

PubMed

Liu, Wei; Fizir, Meriem; Hu, Fan; Li, Ang; Hui, Xuanhong; Zha, Jun; He, Hua

2018-05-25

An effective and greener mixed hemimicelles magnetic solid phase extraction (MHMSPE) based on magnetic halloysite nanotubes (MHNTs) and ionic liquid (IL) is developed for the simultaneous enrichment and determination of anionic azo dyes in a spiked environmental water sample. In this MHMSPE, the formation of C 16 mimBr with mixed hemimicelles on the surface of MHNTs leads to the retention of analytes by strong hydrophobic, p-p and electrostatic interactions. This MHMSPE technique combines the advantages of MHNTs and mixed hemimicelles. Zeta potential data demonstrated that mixed hemimicelles were formed in [C 16 mimBr]/[MHNTs] ratios of the range from 0.15 to 1.33. Different important factors affecting the preconcentration of analytes were investigated and optimized by response surface methodology and one variable at a time. Under the optimum conditions, the limits of detection (LOD) for methyl red and methyl orange (MR and MO) were 0.042 and 0.050 μg L -1 in samples, respectively. The accuracy of the method was assessed by recovery measurements on a spiked sample, and good recoveries 85-87% for MR and 89-93% for MO, with preconcentration factors of 481 and 524, respectively. The low relative standard deviations from 1.6-3.1% for tap water and 2.5-5.4% for lake water was achieved. So far as we know, this is the first development of a mixed hemimicelles SPE based on MHNTs and IL for the extraction of trace anionic azo dyes in environment water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Sensitive, accurate and rapid detection of trace aliphatic amines in environmental samples with ultrasonic-assisted derivatization microextraction using a new fluorescent reagent for high performance liquid chromatography.

PubMed

Chen, Guang; Liu, Jianjun; Liu, Mengge; Li, Guoliang; Sun, Zhiwei; Zhang, Shijuan; Song, Cuihua; Wang, Hua; Suo, Yourui; You, Jinmao

2014-07-25

A new fluorescent reagent, 1-(1H-imidazol-1-yl)-2-(2-phenyl-1H-phenanthro[9,10-d]imidazol-1-yl)ethanone (IPPIE), is synthesized, and a simple pretreatment based on ultrasonic-assisted derivatization microextraction (UDME) with IPPIE is proposed for the selective derivatization of 12 aliphatic amines (C1: methylamine-C12: dodecylamine) in complex matrix samples (irrigation water, river water, waste water, cultivated soil, riverbank soil and riverbed soil). Under the optimal experimental conditions (solvent: ACN-HCl, catalyst: none, molar ratio: 4.3, time: 8 min and temperature: 80°C), micro amount of sample (40 μL; 5mg) can be pretreated in only 10 min, with no preconcentration, evaporation or other additional manual operations required. The interfering substances (aromatic amines, aliphatic alcohols and phenols) get the derivatization yields of <5%, causing insignificant matrix effects (<4%). IPPIE-analyte derivatives are separated by high performance liquid chromatography (HPLC) and quantified by fluorescence detection (FD). The very low instrumental detection limits (IDL: 0.66-4.02 ng/L) and method detection limits (MDL: 0.04-0.33 ng/g; 5.96-45.61 ng/L) are achieved. Analytes are further identified from adjacent peaks by on-line ion trap mass spectrometry (MS), thereby avoiding additional operations for impurities. With this UDME-HPLC-FD-MS method, the accuracy (-0.73-2.12%), precision (intra-day: 0.87-3.39%; inter-day: 0.16-4.12%), recovery (97.01-104.10%) and sensitivity were significantly improved. Successful applications in environmental samples demonstrate the superiority of this method in the sensitive, accurate and rapid determination of trace aliphatic amines in micro amount of complex samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Tributyltin--critical pollutant in whole water samples--development of traceable measurement methods for monitoring under the European Water Framework Directive (WFD) 2000/60/EC.

PubMed

Richter, Janine; Fettig, Ina; Philipp, Rosemarie; Jakubowski, Norbert

2015-07-01

Tributyltin is listed as one of the priority substances in the European Water Framework Directive (WFD). Despite its decreasing input in the environment, it is still present and has to be monitored. In the European Metrology Research Programme project ENV08, a sensitive and reliable analytical method according to the WFD was developed to quantify this environmental pollutant at a very low limit of quantification. With the development of such a primary reference method for tributyltin, the project helped to improve the quality and comparability of monitoring data. An overview of project aims and potential analytical tools is given.

Ultramicroelectrode Array Based Sensors: A Promising Analytical Tool for Environmental Monitoring

PubMed Central

Orozco, Jahir; Fernández-Sánchez, César; Jiménez-Jorquera, Cecilia

2010-01-01

The particular analytical performance of ultramicroelectrode arrays (UMEAs) has attracted a high interest by the research community and has led to the development of a variety of electroanalytical applications. UMEA-based approaches have demonstrated to be powerful, simple, rapid and cost-effective analytical tools for environmental analysis compared to available conventional electrodes and standardised analytical techniques. An overview of the fabrication processes of UMEAs, their characterization and applications carried out by the Spanish scientific community is presented. A brief explanation of theoretical aspects that highlight their electrochemical behavior is also given. Finally, the applications of this transducer platform in the environmental field are discussed. PMID:22315551

Development, validation, and application of a method for the GC-MS analysis of fipronil and three of its degradation products in samples of water, soil, and sediment.

PubMed

de Toffoli, Ana L; da Mata, Kamilla; Bisinoti, Márcia C; Moreira, Altair B

2015-01-01

A method for the identification and quantification of pesticide residues in water, soil, and sediment samples has been developed, validated, and applied for the analysis of real samples. The specificity was determined by the retention time and the confirmation and quantification of analyte ions. Linearity was demonstrated over the concentration range of 20 to 120 µg L(-1), and the correlation coefficients varied between 0.979 and 0.996, depending on the analytes. The recovery rates for all analytes in the studied matrix were between 86% and 112%. The intermediate precision and repeatability were determined at three concentration levels (40, 80, and 120 µg L(-1)), with the relative standard deviation for the intermediate precision between 1% and 5.3% and the repeatability varying between 2% and 13.4% for individual analytes. The limits of detection and quantification for fipronil, fipronil sulfide, fipronil-sulfone, and fipronil-desulfinyl were 6.2, 3.0, 6.6, and 4.0 ng L(-1) and 20.4, 9.0, 21.6, and 13.0 ng L(-1), respectively. The method developed was used in water, soil, and sediment samples containing 2.1 mg L(-1) and 1.2% and 5.3% of carbon, respectively. The recovery of pesticides in the environmental matrices varied from 88.26 to 109.63% for the lowest fortification level (40 and 100 µg kg(-1)), from 91.17 to 110.18% for the intermediate level (80 and 200 µg kg(-1)), and from 89.09 to 109.82% for the highest fortification level (120 and 300 µg kg(-1)). The relative standard deviation for the recovery of pesticides was under 15%.

U.S. Geological Survey external quality-assurance project report to the National Atmospheric Deposition Program / National Trends Network and Mercury Deposition Network, 2007-08

USGS Publications Warehouse

Wetherbee, Gregory A.; Latysh, Natalie E.; Chesney, Tanya A.

2010-01-01

The U.S. Geological Survey (USGS) used six distinct programs to provide external quality-assurance monitoring for the National Atmospheric Deposition Program / National Trends Network (NTN) and Mercury Deposition Network (MDN) during 2007-08. The field-audit program assessed the effects of onsite exposure, sample handling, and shipping on the chemistry of NTN samples, and a system-blank program assessed the same effects for MDN. Two interlaboratory-comparison programs assessed the bias and variability of the chemical analysis data from the Central Analytical Laboratory (CAL), Mercury (Hg) Analytical Laboratory (HAL), and 12 other participating laboratories. A blind-audit program was also implemented for the MDN to evaluate analytical bias in HAL total Hg concentration data. A co-located-sampler program was used to identify and quantify potential shifts in NADP data resulting from replacement of original network instrumentation with new electronic recording rain gages (E-gages) and prototype precipitation collectors. The results indicate that NADP data continue to be of sufficient quality for the analysis of spatial distributions and time trends of chemical constituents in wet deposition across the U.S. NADP data-quality objectives continued to be achieved during 2007-08. Results also indicate that retrofit of the NADP networks with the new E-gages is not likely to create step-function type shifts in NADP precipitation-depth records, except for sites where annual precipitation depth is dominated by snow because the E-gages tend to catch more snow than the original NADP rain gages. Evaluation of prototype precipitation collectors revealed no difference in sample volumes and analyte concentrations between the original NADP collectors and modified, deep-bucket collectors, but the Yankee Environmental Systems, Inc. (YES) collector obtained samples of significantly higher volumes and analyte concentrations than the standard NADP collector.