Organic Contaminant Analytical Methods of the National Status and Trends Program: 2000-2006

This document describes the analytical methods used to quantify core organic chemicals in tissue and sediment collected as part of NOAA’s National Status and Trends Program (NS&T) for the years 2000-2006. Organic contaminat analytical methods used during the early years of the program are described in NOAA Technical Memoranda NOS ORCA 71 and 130 (Lauenstein and Cantillo, 1993; Lauenstein and Cantillo, 1998) for the years 1984-1992 and 1993-1996, respectively. These reports are available from our website (http://www.ccma.nos.gov) The methods detailed in this document were utilized by the Mussel Watch Project and Bioeffects Project, which are both part of the NS&T program. The Mussel Watch Project has been monitoring contaminants in bivalves and sediments since 1986 and is the longest active national contaminant monitoring program operating in U.S. costal waters. Approximately 280 Mussel Watch sites are sampled on a biennial and decadal timescale for bivalve tissue and sediment respectively. Similarly, the Bioeffects Assessment Project began in 1986 to characterize estuaries and near coastal environs. Using the sediment quality triad approach that measures; (1) levels of contaminants in sediments, (2) incidence and severity of toxicity, and (3) benthic macrofaunal conmmunities, the Bioeffects Project describes the spatial extent of sediment toxicity. Contaminant assessment is a core function of both projects. These methods, while discussed here in the context of sediment and bivalve tissue, were also used with other matricies including: fish fillet, fish liver, nepheloid layer, and suspended particulate matter. The methods described herein are for the core organic contaminants monitored in the NS&T Program and include polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), butyltins, and organochlorines that have been analyzed consistently over the past 15-20 years. Organic contaminants such as dioxins, perfluoro compounds and polybrominated biphenyl ethers (PBDEs) were analyzed periodically in special studies of the NS&T Program and will be described in another document. All of the analytical techniques described in this document were used by B&B Laboratories, Inc, an affiliate of TDI-Brook International, Inc. in College Station, Texas under contract to NOAA. The NS&T Program uses a performance-based system approach to obtain the best possible data quality and comparability, and requires laboratories to demonstrate precision, accuracy, and sensitivity to ensure results-based performance goals and measures. (PDF contains 75 pages)

Sediment Quality in Puget Sound Year 3 - Southern Puget Sound

As a component of a three-year cooperative effort of the Washington State Department of Ecology and the National Oceanic and Atmospheric Administration, surficial sediment samples from 100 locations in southern Puget Sound were collected in 1999 to determine their relative quality based on measures of toxicity, chemical contamination, and benthic infaunal assemblage structure. The survey encompassed an area of approximately 858 km2, ranging from East and Colvos Passages south to Oakland Bay, and including Hood Canal. Toxic responses were most severe in some of the industrialized waterways of Tacoma’s Commencement Bay. Other industrialized harbors in which sediments induced toxic responses on smaller scales included the Port of Olympia, Oakland Bay at Shelton, Gig Harbor, Port Ludlow, and Port Gamble. Based on the methods selected for this survey, the spatial extent of toxicity for the southern Puget Sound survey area was 0% of the total survey area for amphipod survival, 5.7% for urchin fertilization, 0.2% for microbial bioluminescence, and 5- 38% with the cytochrome P450 HRGS assay. Measurements of trace metals, PAHs, PCBs, chlorinated pesticides, other organic chemicals, and other characteristics of the sediments, indicated that 20 of the 100 samples collected had one or more chemical concentrations that exceeded applicable, effects-based sediment guidelines and/or Washington State standards. Chemical contamination was highest in eight samples collected in or near the industrialized waterways of Commencement Bay. Samples from the Thea Foss and Middle Waterways were primarily contaminated with a mixture of PAHs and trace metals, whereas those from Hylebos Waterway were contaminated with chlorinated organic hydrocarbons. The remaining 12 samples with elevated chemical concentrations primarily had high levels of other chemicals, including bis(2-ethylhexyl) phthalate, benzoic acid, benzyl alcohol, and phenol. The characteristics of benthic infaunal assemblages in south Puget Sound differed considerably among locations and habitat types throughout the study area. In general, many of the small embayments and inlets throughout the study area had infaunal assemblages with relatively low total abundance, taxa richness, evenness, and dominance values, although total abundance values were very high in some cases, typically due to high abundance of one organism such as the polychaete Aphelochaeta sp. N1. The majority of the samples collected from passages, outer embayments, and larger bodies of water tended to have infaunal assemblages with higher total abundance, taxa richness, evenness, and dominance values. Two samples collected in the Port of Olympia near a superfund cleanup site had no living organisms in them. A weight-of-evidence approach used to simultaneously examine all three “sediment quality triad” parameters, identified 11 stations (representing 4.4 km2, 0.5% of the total study area) with sediment toxicity, chemical contamination, and altered benthos (i.e., degraded sediment quality), 36 stations (493.5 km2, 57.5% total study area) with no toxicity or chemical contamination (i.e., high sediment quality), 35 stations (274.1 km2, 32.0% total study area) with one impaired sediment triad parameter (i.e., intermediate/high sediment quality), and 18 stations (85.7km2, 10.0% total study area) with two impaired sediment parameters (i.e., intermediate/degraded quality sediments). Generally, upon comparison, the number of stations with degraded sediments based upon the sediment quality triad of data was slightly greater in the central Puget Sound than in the northern and southern Puget Sound study areas, with the percent of the total study area degraded in each region decreasing from central to north to south (2.8, 1.3 and 0.5%, respectively). Overall, the sediments collected in Puget Sound during the combined 1997-1999 surveys were among the least contaminated relative to other marine bays and estuaries studied by NOAA using equivalent methods. (PDF contains 351 pages)

Survey of sediment quality in Sabine Lake, Texas and vicinity

The toxicity of sediments in Sabine Lake, Texas, and adjoining Intracoastal Waterway canals was determined as part of bioeffects assessment studies managed by NOAA’s National Status and Trends Program. The objectives of the survey were to determine: (1) the incidence and degree of toxicity of sediments throughout the study area; (2) the spatial patterns (or gradients) in chemical contamination and toxicity, if any, throughout the study area; (3) the spatial extent of chemical contamination and toxicity; and (4) the statistical relationships between measures of toxicity and concentrations of chemicals in the sediments. Surficial sediment samples were collected during August, 1995 from 66 randomly-chosen locations. Laboratory toxicity tests were performed as indicators of potential ecotoxicological effects in sediments. A battery of tests was performed to generate information from different phases (components) of the sediments. Tests were selected to represent a range in toxicological endpoints from acute to chronic sublethal responses. Toxicological tests were conducted to measure: reduced survival of adult amphipods exposed to solid-phase sediments; impaired fertilization success and abnormal morphological development in gametes and embryos, respectively, of sea urchins exposed to pore waters; reduced metabolic activity of a marine bioluminescent bacteria exposed to organic solvent extracts; and induction of a cytochrome P-450 reporter gene system in exposures to solvent extracts of the sediments. Chemical analyses were performed on portions of each sample to quantify the concentrations of trace metals, polynuclear aromatic hydrocarbons, and chlorinated organic compounds. Correlation analyses were conducted to determine the relationships between measures of toxicity and concentrations of potentially toxic substances in the samples. Based upon the compilation of results from chemical analyses and toxicity tests, the quality of sediments in Sabine Lake and vicinity did not appear to be severely degraded. Chemical concentrations rarely exceeded effects-based numerical guidelines, suggesting that toxicant-induced effects would not be expected in most areas. None of the samples was highly toxic in acute amphipod survival tests and a minority (23%) of samples were highly toxic in sublethal urchin fertilization tests. Although toxic responses occurred frequently (94% of samples) in urchin embryo development tests performed with 100% pore waters, toxicity diminished markedly in tests done with diluted pore waters. Microbial bioluminescent activity was not reduced to a great degree (no EC50 <0.06 mg/ml) and cytochrome P-450 activity was not highly induced (6 samples exceeded 37.1 ug/g benzo[a]pyrene equivalents) in tests done with organic solvent extracts. Urchin embryological development was highly correlated with concentrations of ammonia and many trace metals. Cytochrome P450 induction was highly correlated with concentrations of a number of classes of organic compounds (including the polynuclear aromatic hydrocarbons and chlorinated compounds). (PDF contains 51 pages)

Effects of macrobenthos on sediment-water oxygen and ammonium fluxes. Final Report.

Sediments are an important location in determining the fate of nutrients entering the estuary. Role of sediments needs to be incorporated into water quality models. Purpose of this study was to estimate the portion of sediment oxygen consumption (SOC) and sediment ammonium (NH4+) release directly attributable to benthic invertebrates via the respiratory use of oxygen and catabolic release of ammonium. Samples were collected at 8 locations from August 1985 through November 1988. (PDF contains 45 pages)

San Francisco Bay regional sediment management strategy development

The San Francisco Bay Conservation and Development Commission (BCDC), in continued partnership with the San Francisco Bay Long Term Management Strategies (LTMS) Agencies, is undertaking the development of a Regional Sediment Management Plan for the San Francisco Bay estuary and its watershed (estuary). Regional sediment management (RSM) is the integrated management of littoral, estuarine, and riverine sediments to achieve balanced and sustainable solutions to sediment related needs. Regional sediment management recognizes sediment as a resource. Sediment processes are important components of coastal and riverine systems that are integral to environmental and economic vitality. It relies on the context of the sediment system and forecasting the long-range effects of management actions when making local project decisions. In the San Francisco Bay estuary, the sediment system includes the Sacramento and San Joaquin delta, the bay, its local tributaries and the near shore coastal littoral cell. Sediment flows from the top of the watershed, much like water, to the coast, passing through rivers, marshes, and embayments on its way to the ocean. Like water, sediment is vital to these habitats and their inhabitants, providing nutrients and the building material for the habitat itself. When sediment erodes excessively or is impounded behind structures, the sediment system becomes imbalanced, and rivers become clogged or conversely, shorelines, wetlands and subtidal habitats erode. The sediment system continues to change in response both to natural processes and human activities such as climate change and shoreline development. Human activities that influence the sediment system include flood protection programs, watershed management, navigational dredging, aggregate mining, shoreline development, terrestrial, riverine, wetland, and subtidal habitat restoration, and beach nourishment. As observed by recent scientific analysis, the San Francisco Bay estuary system is changing from one that was sediment rich to one that is erosional. Such changes, in conjunction with increasing sea level rise due to climate change, require that the estuary sediment and sediment transport system be managed as a single unit. To better manage the system, its components, and human uses of the system, additional research and knowledge of the system is needed. Fortunately, new sediment science and modeling tools provide opportunities for a vastly improved understanding of the sediment system, predictive capabilities and analysis of potential individual and cumulative impacts of projects. As science informs management decisions, human activities and management strategies may need to be modified to protect and provide for existing and future infrastructure and ecosystem needs. (PDF contains 3 pages)

A GEOPASS-NERC project on diatom deposition and sediment accumulation in Lake Baikal, Siberia

This new project is multidisciplinary, with physical and chemical palaeolimnological aspects mainly the responsibility of Swiss and Russian scientists, and the biological limnology and palaeolimnology components mainly undertaken by the British and Russian groups. The overall project aim is to improve palaeoclimate reconstructions using sedimentary diatoms by promoting better understanding of diatom ecology and sediment-forming processes. The initial work plan is divided into four main parts: To understand diatom phytoplankton ecology more fully, to assess taphonomic changes associated with the transformation of phytoplankton diatom communities into sediment assemblages, to demonstrate sediment core integrity and representativity and to calibrate modern diatom assemblages against contemporary climate records. The preliminary results from the interrelated studies of phytoplankton, sediment traps and sediment cores used in GEOPASS-NERC, demonstrate the complexity of links between the living and fossil systems. Furthermore, the nature of recent sedimentation in Lake Baikal is spatially variable and incompletely known. This poses a major challenge to palaeolimnological interpretation. Turbidite deposits and differential preservation of microfossils, combined with inadequate knowledge of the modern ecology of endemic diatoms, all conspire to obfuscate the sedimentary record of environmental change.

Procedures to prevent the occurrence of potentially dangerous situations during the operation of the Mackereth 1-metre mini or short sediment corer

During the 1950s and 1960s, F.J.H. Mackereth developed and published plans for a series of pneumatic samplers for lake sediments. Unfortunately, as the equipment was continually evolving during ensuing research, no user manuals, beyond the original publication, had been produced. Over the last few years there have been a few potentially very serious accidents with the 1-metre corer, which has prompted the authors to carry out a risk assessment. This highlighted two weaknesses in the design and its later developments. They can be corrected simply by checking for screw threads that may have been added to the exhaust port on the mini-corer, and by changing the operating procedure. An A4 nine-page user manual is now available from the authors. A small charge ( pound sterling 10 in 1998) will be made to cover handling costs and postage.

Factors influencing the downstream transport of sediment in the Lough Feeagh catchment, Burrishoole, Co. Mayo, Ireland

Research laboratories in the Burrishoole catchment have been the focus of salmonid research since 1955. One aspect of the research has been to monitor the number of salmon and sea trout migrating to sea as smolts and returning to the catchment as adults. In the early 1990s it became clear that the smolt output from the catchment had declined over the previous two decades. At about the same time the presence of fine particles of peat silt in the hatchery became increasingly apparent and led to a higher incidence of mortality of young fry. These observations and management difficulties led to a study of silt transport in the surface waters of the catchment, which is described in this article. The authors describe geology, soils, climate and hydrology of Burrishoole before examining the sediment deposition in Lough Feeagh.

A simple method for counting bacteria with active electron transport system in water and sediment samples [Translation from: Kiel. Meeresforsch. 31(2) 83-86, 1975]

Description of a simple method for counting bacteria with active electron transport systems in water and sediment samples. Sodium succinate, NADH and NADPH served as electron donors. It is possible to see several sites of electron transport in the larger cells. Especially impressive are the plankton-algae, protozoa, and small metazoa. This is a partial translation of the ”method” section only.

Profile soundings in lakes of the younger morainal area of Sleswick-Holstein with a sediment-echo-sounder of 30 kHz [Translation from: Wass.Boden 26, 135-138, 1974]

To be able to carry out physical, chemical and biological investigations on a lake, one needs a thorough knowledge of the volume of water and the shape of the lake basin. Little is known about the about the morphology of the lakes in Schleswig-Holstein and its ecological consequences. For this research a 30 KHz echo sounder with sediment transceiver was used to carry out profile determinations (echo soundings). This apparatus continuously records on paper the different reflexions and absorptions of the sediment and water body in the corresponding depth. By this, acoustically noticeable layers and different densities in the sediment and 'scattering layers' in the water body due to physical, chemical and biological reasons (e.g. plans and single fish) are made visible. Result are summarised here regarding the echo soundings in Blunker See.

Analysis and adsorption of phosalone on aquatic sediment

Phosalone is a non systematic, wide spectrum organophosphate pesticide which was discovered in 1961 in the laboratories of the Societe des Usines Chimique Rhone-Poulenc in France. It has been approved for commercial use since 1964 in France, in Australia since 1966, in the United Kingdom in 1967 and in many other countries including Japan, Egypt, USSR and the USA. This study provides a full literature review on all aspects of phosalone including its physical, biological and chemical characteristics, and analytical methods of analysis with particular reference to soils/sediments. Furthermore, it aims to develop a method for the determintion of phosalone in aquatic sediments and to determine the adsorption of phosalone onto kaolinite.

An annotated bibliography of aquatic sediment traps and trapping methods

This annotated bibliography is intended to give as reasonably complete a review of the existing literature as possible, and to offer some practical guidance in the selection and operation of sediment traps in future monitoring programmes.

Calcite covering of sediment as a possible way of curbing blue-green algae

Natural calcite precipitation in lakes is a well-known control mechanism of eutrophication. In hard-water lakes, calcite deposits on the flat bottoms of shallow lakes and near the shores of deeper lakes resulted from biogenic decalcification during the millenia after the last glacial period. The objective of a new restoration technology is to intensify the natural process of precipitation by utilizing the different qualities of calcareous mud layers. In a pilot experiment in Lake Rudower See, East Germany, phosphorus-poor deeper layers of the sediments were flushed out and spread over the phosphorus-rich uppermost sediments, to promote the co- precipitation of calcite with phosphorus from the water-column.

Changes of water quality and sediment phosphorus of a small productive lake following decreased phosphorus loading

Esthwaite Water is the most productive or eutrophic lake in the English Lake District. Since 1945 its water quality has been determined from weekly or biweekly measurements of temperature, oxygen, plant nutrients and phytoplankton abundance. The lake receives phosphorus from its largely lowland-pasture catchment, sewage effluent from the villages of Hawkshead and Near Sawrey, and from a cage-culture fish farm. From 1986 phosphorus has been removed from the sewage effluent of Hawkshead which was considered to contribute between 47% and 67% of the total phosphorus loading to the lake. At the commencement of phosphorus removal regular measurements of phosphorus in the superficial 0-4 cm layer of lake sediment were made from cores collected at random sites. Since 1986 the mean annual concentration of alkali-extractable sediment phosphorus has decreased by 23%. This change is not significant at the 5% level but nearly so. There has been no marked change in water quality over this period. Summer dominance of blue-green algae which arose in the early 1980s after decline of the previous summer forms, Ceratium spp., has been maintained. Improvement in water quality is unlikely to be achieved at the present phosphorus loading.