Chemicals of Emerging Concern in Water and Bottom Sediment in the Great Lakes Basin, 2012—Collection Methods, Analytical Methods, Quality Assurance, and Study Data

Abstract

In synoptic surveys of surface-water quality across the United States, a large group of organic chemicals associated with agricultural, household, and industrial waste have been detected. These chemicals are referred to collectively as chemicals of emerging concern (CECs) and include prescription drugs and antibiotics, over-the-counter medications, reproductive hormones, personal-care products, detergent metabolites, and flame retardants.

The U.S. Geological Survey (USGS) collaborated with the U.S. Fish and Wildlife Service and the U.S. Environmental Protection Agency on a study to identify the presence of CECs in water and bottom-sediment samples collected during 2012 at 66 sites throughout the Great Lakes Basin. The 2012 effort is part of a long-term study that was initiated in 2010.

The purposes of this report are to document the collection and analytical methods, provide the quality-assurance data and analyses, and provide the water and bottom-sediment data for this study of CECs in the Great Lakes Basin for 2012. A previous report documents data collected during 2010 and 2011. The methods used for chemical analyses were identical between the 2010–11 and 2012 studies, with the exception that a method to determine nontarget chemicals was used during 2010–11. The data from this study are published as a USGS Data Series Report to ensure adequate documentation of the original methods and provide a citable source for study data. This report contains no interpretations of the study data. The chemical data are as reported by the laboratory and have not been censored or adjusted unless otherwise noted.

Field measurements were recorded and samples were collected in April and May and in September 2012, by U.S. Geological Survey, U.S. Fish and Wildlife Service, and U.S. Environmental Protection Agency personnel. Study sites included tributaries to the Great Lakes located near Duluth, Minnesota; King, Wisconsin; Green Bay, Wis.; Detroit, Michigan; Monroe, Mich.; Toledo, Ohio, and Rochester, New York. Water and bottom-sediment samples were analyzed at the USGS National Water Quality Laboratory in Denver, Colorado, for a broad suite of CECs.

During this 2012 study, 140 environmental and 8 field duplicate samples of surface water and wastewater effluent, 1 field blank water sample, and 5 field spike water samples were collected or prepared. Water samples were analyzed at the USGS National Water Quality Laboratory using laboratory schedule 4433 for wastewater indicators, research method 8244 for pharmaceuticals, and laboratory schedule 4434 for steroid hormones, sterols, and bisphenol A. For wastewater indicators in unfiltered water, 61 of the 68 chemicals analyzed using laboratory schedule 4433 had detectable concentrations ranging from 0.002 to 64.4 micrograms per liter. Thirty-eight of the 48 chemicals analyzed using research method 8244 for pharmaceuticals in unfiltered water had detectable concentrations ranging from 0.002 to 3.32 micrograms per liter. Twelve of the 20 chemicals analyzed using laboratory schedule 4434 for steroid hormones, sterols, and bisphenol A in unfiltered water had detectable concentrations ranging from 0.43 to 120,000 nanograms per liter.

During this study, 53 environmental samples, 4 field duplicate samples, and 8 field spike samples of bottom sediment and laboratory matrix-spike samples were analyzed for a wide variety of CECs at the USGS National Water Quality Laboratory using laboratory schedule 5433 for wastewater indicators; research method 6434 for steroid hormones, sterols, and bisphenol A; and research method 9008 for human-use pharmaceuticals and antidepressants. Forty of the 57 chemicals analyzed using laboratory schedule 5433 had detectable concentrations ranging from 1 to 49,000 micrograms per kilogram. Fourteen of the 20 chemicals analyzed using research method 6434 had detectable concentrations ranging from 0.04 to 24,940 nanograms per gram. Ten of the 20 chemicals analyzed using research method 9008 had detectable concentrations ranging from 0.59 to 197.5 micrograms per kilogram. Five of the 11 chemicals analyzed using research method 9008 had detectable concentrations ranging from 1.16 to 25.0 micrograms per kilogram.

First posted March 30, 2015

Revised January 8, 2016