Methods

Chloride, SulfateSamples for chloride and sulfate are collected together with a peristaltic pump and tubing and in-line filtered (through a 0.40 micron polycarbonate filter) into new, 20 ml HDPE plastic containers with conical caps. The samples are stored refrigerated at 4 degrees Celsius until analysis, which should occur within 6 months. The samples are analyzed for chloride (and sulfate) simultaneously by Ion Chromatography, using a hydroxide eluent.The detection limit for chloride is approximately 0.01 ppm and the analytical range for the method extends to 100 ppm.The detection limit for sulfate is approximately 0.01 ppm and the analytical range for the method extends to 60 ppm.Method Log: Prior to January 1998 samples, chloride was determined on a Dionex DX10 Ion Chromatograph, using a chemical fiber suppressor. From 1998 to 2011, chloride was determined by a Dionex model DX500, using an electro-chemical suppressor. From January 2011 until present, chloride is determined by a Dionex model ICS 2100 using an electro-chemical suppressor.Calcium, silicon, magnesium, sodium, potassium, iron, and manganeseSamples for calcium analysis (as well as dissolved nitrogen and phosphorus, silicon, magnesium, sodium, potassium, iron, and manganese) are collected together with a peristaltic pump and tubing and in-line filtered (through a 40 micron polycarbonate filter) into 120 ml LDPE bottles and acidified to a 1percent HCl matrix by adding 1 ml of ultra pure concentrated HCl to 100 mls of sample. For every sample acidification event, three acid blanks are created by adding the same acid used on the samples to 100 mls of ultra pure water supplied from the lab. Once acidified, the samples are stable at room temperature until analysis, which should occur within one year. Until acidification, the samples should be refrigerated at 4 degrees Celsius.Calcium, as well as magnesium, sodium, potassium, iron, and manganese are analyzed simultaneously on an optical inductively-coupled plasma emission spectrophotometer (ICP-OES). The acidified samples are directly aspirated into the instrument without a digestion. Calcium is analyzed at 317.933 nm and at 315.887 nm and viewed axially for low-level analysis and radially for high level analysis.The detection limit for calcium is 0.06 ppm with an analytical range of the method extends to 50 ppm.The detection limit for iron is 0.02 ppm with an analytical range of the method extends to 20 ppm.The detection limit for magnesium is 0.03 ppm with an analytical range of the method extends to 50 ppm.The detection limit for manganese is 0.01 ppm with an analytical range of the method extends to 2 ppm.The detection limit for potassium is 0.06 ppm with an analytical range of the method extends to 10 ppm.The detection limit for sodium is 0.06 ppm with an analytical range of the method extends to 50 ppm.Method Log: Prior to January 2002, Calcium, magnesium, sodium, potassium, iron, and manganese were determined on a Perkin-Elmer model 503 Atomic Absorption Spectrophotometer. Lanthanum at a 0.8percent concentration was added as a matrix modifier to suppress chemical interferences. From January 2002 to present, samples are analyzed for calcium on a Perkin-Elmer model 4300 DV ICP.Dissolved reactive silica is determined by the Heteropoly Blue Method and the absorption is measured at 820 nm.The detection limit for silicon is 6 ppb and the analytical range is 15000 ppb.Method Log These determinations were performed manually using a Bausch and Lomb Spectrophotometer from the beginning of the project until April 1984. From 1984 through 2005, dissolved reactive silicon was determined on a Technicon Auto Analyzer II. From January 2006 to present, samples are run on an Astoria-Pacific Astoria II Autoanalyzer.

Methods

The 1991-1995 chemistry data obtained from the Lachat auto-analyzer. Like the process data, there are up to seven samples per sampling date due to Van Dorn collections across a depth interval according to percent irradiance. Voichick and LeBouton (1994) describe the autoanalyzer procedures in detail.Methods for 1984-1990 were described by Carpenter and Kitchell (1993) and methods for 1991-1997 were described by Carpenter et al. (2001).Carpenter, S.R. and J.F. Kitchell (eds.). 1993. The Trophic Cascade in Lakes. Cambridge University Press, Cambridge, England.Carpenter, S.R., J.J. Cole, J.R. Hodgson, J.F. Kitchell, M.L. Pace,D. Bade, K.L. Cottingham, T.E. Essington, J.N. Houser and D.E. Schindler. 2001. Trophic cascades, nutrients and lake productivity: whole-lake experiments. Ecological Monographs 71: 163-186.Number of sites: 8

Methods

Environmental Sampling and Analysis: Physical, chemical and biological samples were taken above the deepest point in each lake during the summer stratification period (June, July, or August). Water samples were collected from one half meter depth using a peristaltic pump, and were analyzed for pH, alkalinity, specific conductance, water color, chlorophyll-a, dissolved organic and inorganic carbon, total phosphorus, and total nitrogen (Appendix Table 1). Secchi depth, temperature and dissolved oxygen profiles, and vertical plankton tows were also taken at the deepest point. Temperature and dissolved oxygen concentrations (DO) were measured through the water column at 1 meter increments.. Conductivity, TP-TN, alkalinity and pH water samples were collected unfiltered while water for DIC-DOC and color water samples was filtered through nucleopore polycarbonate filters. Alkalinity, pH, and DIC-DOC samples were filled to the top and sealed quickly to prevent CO2 loss or invasion. Samples containing air bubbles were recollected. Chlorophyll samples were collected on glass fiber filters in the field. Water chemistry and chlorophyll a analyses were done at the Trout Lake Biological Station, Boulder Junction, WI except for TP, TN, DIC and DOC samples, which were analyzed at the Center for Limnology-Lake Mendota Laboratory, Madison, WI.

Methods

Environmental Sampling and Analysis: Physical, chemical and biological samples were taken above the deepest point in each lake during the summer stratification period (June, July, or August). Water samples were collected from one half meter depth using a peristaltic pump, and were analyzed for pH, alkalinity, specific conductance, water color, chlorophyll-a, dissolved organic and inorganic carbon, total phosphorus, and total nitrogen (Appendix Table 1). Secchi depth, temperature and dissolved oxygen profiles, and vertical plankton tows were also taken at the deepest point. Temperature and dissolved oxygen concentrations (DO) were measured through the water column at 1 meter increments.. Conductivity, TP-TN, alkalinity and pH water samples were collected unfiltered while water for DIC-DOC and color water samples was filtered through nucleopore polycarbonate filters. Alkalinity, pH, and DIC-DOC samples were filled to the top and sealed quickly to prevent CO2 loss or invasion. Samples containing air bubbles were recollected. Chlorophyll samples were collected on glass fiber filters in the field. Water chemistry and chlorophyll a analyses were done at the Trout Lake Biological Station, Boulder Junction, WI except for TP, TN, DIC and DOC samples, which were analyzed at the Center for Limnology-Lake Mendota Laboratory, Madison, WI.