Chris D. Ivey John M. Besser 2019 tabular digital data Denver, CO U.S. Geological Survey https://doi.org/10.5066/F71R6P1H John M. Besser Danielle Cleveland Chris D.Ivey Laura Blake Jon Colman 20190621 publication n/a Wiley https://doi.org/10.1002/etc.4523 Attributes regarding the influence of dissolved organic matter on chronic Al exposure and the effects on Ceriodaphnia dubia survival and reproduction. The tests were conducted to estimate chronic effect aluminum concentrations for survival and reproduction of Ceriodaphnia dubia and compare this information to the USEPA water quality criterion for Al. 20170201 20170630 ground condition Complete None planned Columbia Environmental Research Center -92.284999999998 -92.27364 38.9149 38.90806 ISO 19115 Topic Category biota USGS Biocomplexity Thesaurus Toxicity Chronic toxicity Bioavailablility Water quality standards Water chemistry Dissolved organic carbon Aluminum None Hardness Equilibrium USGS Metadata Identifier USGS:5bcdf78ae4b0f0758fc28fda None Columbia Environmental Research Center Geographic Names Information System (GNIS) Massachusetts USGS Biocomplexity Thesaurus Crustaceans Integrated Taxonomic Information System (ITIS) 2018 ONLINE_REFERENCE Washington, D.C. Integrated Taxonomic Information System (ITIS) http://itis.gov Chris D Ivey U.S. Geological Survey, Columbia Environmental Research Center Fish Biologist mailing and physical

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Columbia MO 65201 United States 573-875-5399 civey@usgs.gov expert advice The test organisms were cultured at CERC from a known source that has been positively identified to species Daphnia were identified to species Kingdom Animalia Subkingdom Bilateria Infrakingdom Protostomia Superphylum Ecdysozoa Phylum Arthropoda Subphylum Crustacea Class Branchiopoda Subclass Phyllopoda Order Diplostraca Suborder Cladocera Infraorder Anomopoda Family Daphniidae Genus Ceriodaphnia Species Ceriodaphnia dubia None. Please see 'Distribution Info' for details. None. Users are advised to read the data set's metadata thoroughly to understand appropriate use and data limitations. Chris D Ivey U.S. Geological Survey, Columbia Environmental Research Center Fish Biologist mailing and physical

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Columbia MO 65201 United States 573-875-5399 civey@usgs.gov Acceptance of data from chemical analyses was based on standard QA/QC guidelines and acceptance of toxicity data was based on test acceptability criteria described by USEPA (2002). Chronic effect concentrations for total Al (e.g., 20% effect concentration or EC20) for reproduction were determined using Toxicity Relationship Analysis Program, version 1.30a (Erickson et al. 2010). The data were checked for duplicates, omissions, and transcription errors. All values fell within expected ranges. Complete na na Lab We investigated the influence of dissolved organic matter on chronic Al toxicity to Ceriodaphnia dubia by conducting a series of 7-d toxicity tests in dilutions of soft natural waters. Water collected from sites in Massachusetts, USA, with dissolved organic carbon (DOC) concentrations of 6 to 10 mg/L, were adjusted to hardness levels of 20 and 35 mg/L and diluted with hardness-adjusted lab water (DOC less than 0.4 mg/L) to produce test waters containing 100%, 50%, and 25% site water, plus 100% lab water. Tests were conducted in a controlled CO2 atmosphere to maintain pH in the range, 6.0-6.5. Results of these tests were used to estimate chronic effect concentrations for survival and reproduction, expressed as total (unfiltered) Al concentrations. ASTM International 2015 Book Not electronically available Mount DR Mount, DI 1992 Manuscript Not electronically available USEPA (United States Environmental Protection Agency) 1988 Document https://nepis.epa.gov/Exe/ZyNET.exe/2000M5FC.TXT?ZyActionD=ZyDocument&Client=EPA&Index=1986+Thru+1990&Docs=&Query=&Time=&EndTime=&SearchMethod=1&TocRestrict=n&Toc=&TocEntry=&QField=&QFieldYear=&QFieldMonth=&QFieldDay=&IntQFieldOp=0&ExtQFieldOp=0&XmlQuery=&File=D%3A%5Czyfiles%5CIndex%20Data%5C86thru90%5CTxt%5C00000008%5C2000M5FC.txt&User=ANONYMOUS&Password=anonymous&SortMethod=h%7C-&MaximumDocuments=1&FuzzyDegree=0&ImageQuality=r75g8/r75g8/x150y150g16/i425&Display=hpfr&DefSeekPage=x&SearchBack=ZyActionL&Back=ZyActionS&BackDesc=Results%20page&MaximumPages=1&ZyEntry=1&SeekPage=x&ZyPURL USEPA (United States Environmental Protection Agency) 2002 Document https://www.epa.gov/sites/production/files/2015-08/documents/short-term-chronic-freshwater-wet-manual_2002.pdf USEPA (United States Environmental Protection Agency) 2017 Document https://www.epa.gov/sites/production/files/2017-07/documents/draft-ambient-water-quality-criteria-aluminum.pdf High-Dissolved Organic Carbon (DOC) stream waters were collected from western Massachusetts and manipulated hardness and DOC levels to produce test waters for Al toxicity tests. Two separate batches of water were collected from Beaver Brook, near Royalston, Massachusetts (Lat 42°37'10" / Long 72°08'12"). Sample 1 (DOC about 7 mg/L) was collected in December 2016, sample 2 (DOC about 10 mg/L) was collected in February 2017 and each sample was shipped on ice for testing and analysis at CERC. At CERC, field-collected waters were mixed with small amounts of hard well water to produce two hardness levels: 20 mg/L and 35 mg/L. After hardness adjustment, each water was mixed with a low-DOC (less than 0.5 mg/L) laboratory water with the same hardness, prepared by diluting well water with deionized water. At each hardness level, a series of dilutions produced 4 test waters with varying content of site water and DOC: A, high DOC (100% site water); B, intermediate DOC (50% site water); C, low DOC (25% site water); and D (DOC ‘control’; 100% lab water. The first eight tests were conducted in batch 1 (20-hardness lab waters; tests A1-D1) and batch 2 (35-hardness hard waters; tests A2-D2). Test waters that did not produce satisfactory results in these initial tests (A1 and D2) were re-tested in batches 3 and 4 (Tests A3, A4, and D3;). Toxicity tests were conducted in temperature-controlled plant growth chambers with a controlled-CO2 atmosphere to facilitate pH control in the target range, 6.0 to 6.5. The pH of test waters was initially adjusted with HCl or NaOH, then maintained by manipulating CO2 concentrations in the range, 1.0% to 1.2% CO2; (Mount and Mount 1992). 2017 Seven-day chronic toxicity tests were conducted with the cladoceran, Ceriodaphnia dubia. Test conditions based on a standard method (USEPA 2002) were started with less than 24-hr old neonates (parthenogenic females), which were cultured at a hardness of about 20 mg/L for about 8 weeks before the start of the test. One neonate was stocked in each of ten 10 replicate 30-mL exposure cups per treatment, with 20 mL test water per cup, and each cup was fed daily with 0.1 ml portions of two diet suspensions: (1) yeast-cerophyll-trout chow (1800 mg/L stock solution) and (2) algae (Pseudokirschneriella subcapitata, 3.0 X 107 cell/mL, Aquatic Bio Systems, Fort Collins, CO). On each day of the test, stocked C. dubia were transferred to fresh test solutions and recorded as alive or dead and the number of young produced was recorded. Tests were ended after 6 to 8 days, with the end date determined by when at least 60% of stocked adults in the control group had produced at least three broods averaging 15 or more young per female. 2017 Each toxicity test consisted of 5 Al concentrations in a 50% percent dilution series of one of the test waters, plus a control without added Al. One day before the start of a test, the high-Al solution was prepared by dissolving aluminum chloride salt directly into each test water, adjusting the pH as needed, and preparing four additional Al concentrations by 50% serial dilutions of the high-Al test water and pH-adjusted lab water. Exposure cups with test water were equilibrated in the temperature-controlled (25 °C) incubator for 24 hours before animals were stocked and fed to start the test. Remaining portions of Al-spiked test waters were used to fill additional sets of 10 cups per treatment daily over the remaining days of the study and each test organism was transferred into a cup with equilibrated test water daily. Test solutions prepared one day before the start of the study were used for water replacements for the entire 7-day study period, based on stability studies that demonstrated average measured total-Al concentrations remained stable over this seven-day period. Test solutions were prepared in glass jars and stored in a walk-in cooler at 4 °C between use. 2017 Test waters were analyzed for total Al (unfiltered samples, acidified to pH 2) Al, filtered Al (less than 0.45 μm), DOC, major ions, and other water quality parameters. Total Al was used as the primary measure of Al exposure, based on recommendations of USEPA (2017) and ASTM International(2015), with both “new” (freshly equilibrated) samples and “old” (24 hr after stocking and feeding) total-Al samples collected from all Al treatments on two sampling dates during each test. Total Al samples were acidified by addition of in-house sub-boiling distilled nitric acid (J.T. Baker, Baker Analyzed ACS Reagent, Avantor Performance Materials, Center Valley, PA), to result in final acid content of 1-2 % (v/v) nitric acid. Samples for DOC analysis were collected in pre-cleaned amber glass bottles, vacuum-filtered through 0.45 μm polyethersulfone membranes, and then acidified with 9N high-purity sulfuric acid (BDH Aristar Ultra, VWR International, Radnor, PA) to pH 2 or less within 48 hours of receipt. DOC was measured as non-purgeable organic carbon (NPOC) by high temperature combustion catalytic oxidation-nondispersive infrared spectroscopy using a total organic carbon analyzer (Model TOC-L CSH, Shimadzu Scientific Instruments, Inc., Columbia, MD). Samples for analyses of chloride and sulfate were collected in pre-cleaned plastic bottles and preserved at 4°C in a laboratory refrigerator before anion analysis by an ion chromatography system (Dionex ICS-1100) equipped with a Dionex Ionpac AS22 anion exchange column and a suppressed conductivity detector. A 4.5 mM sodium carbonate/1.4 mM sodium bicarbonate mobile phase were used to elute the anions of interest. 2017 Measured concentration of Al in C. dubia chronic exposures Text file containing data. Producer Defined Treatment An indicator of the test water source and/or properties Producer Defined 20 hard well CERC well water diluted to a hardness of 20 mg per liter calcium and magnesium Producer defined 25% site water Field collected stream water (Site) diluted 25% with CERC well water Producer defined 50% site water Field collected stream water (Site) diluted 50% with CERC well water Producer defined 100% site water Field collected stream water (Site) diluted 0% with CERC well water Producer defined 35 hard well CERC well water diluted to a hardness of 35 mg per liter calcium and magnesium Producer defined Test Concentration (mg/L) The target or nominal aluminum (CASRN 7784-27-2) concentration in mg/L Producer Defined 0.0 20.0 Milligrams per liter Batch Numeric identifier for a set of related tests run concurrently. Producer Defined Numeric identifier for a set of related tests run concurrently. Test Day The number of 24-hour periods (days) that have elapsed since the start of the study, upon which samples were collected. Producer Defined 1 6 Days In/Out Denotes if sample was taken from incoming or outgoing treatment water Producer Defined Out Treatment water at time 24 hour Producer defined In Treatment water at time 0 hour Producer defined Filtered/Unfiltered Denotes if sample taken was filtered or unfiltered Producer Defined Unfiltered Sample was not filtered Producer defined Filtered Sample was filtered through a 0.45 micron filter Producer defined Measured Aluminum (mg/L) Analyzed concentration of aluminum in treatment water in mg/L Producer Defined LT # The concentration of aluminium in the sample, was Less Than (LT) the specific numeric value (#), reported in milligrams per liter. The measured concentration was less than the detection limit of the analytical method. Producer defined 0.05 34.2 Milligrams per liter Dissolved organic carbon (mg/L) Analyzed concentration of dissolved orgainc carbon in treatment water in mg/L Producer Defined -- Attribute was not measured in the sample Producer defined 0.3 10.7 Milligrams per liter LT # The concentration of DOC in the sample, was Less Than (LT) the specific numeric value (#), reported in milligrams per liter. The measured concentration was less than the detection limit of the analytical method. Producer defined Measured water quality parameters for C. dubia chronic Al exposures Text file containing data. Producer Defined Treatment An indicator of the test water source and/or properties Producer Defined 20 hard well CERC well water diluted to a hardness of 20 mg per liter calcium and magnesium Producer defined 25% site water Field collected stream water (Site) diluted 25% with CERC well water Producer defined 50% site water Field collected stream water (Site) diluted 50% with CERC well water Producer defined 100% site water Field collected stream water (Site) diluted 0% with CERC well water Producer defined 35 hard well CERC well water diluted to a hardness of 35 mg per liter calcium and magnesium Producer defined Test Concentration (mg/L) The target or nominal aluminum (CASRN 7784-27-2) concentration in mg/L Producer Defined 0.0 20.0 Milligrams per liter Batch Numeric identifier for a set of related tests run concurrently. Producer Defined Numeric identifier for a set of related tests run concurrently. Test Day The number of 24-hour periods (days) that have elapsed since the start of the study, upon which samples were collected. Producer Defined 0 7 Days pH (In) pH of incoming test water at time 0 hour Producer Defined -- Attribute was not measured in the sample Producer defined 5.35 6.58 pH units pH (out) pH of outgoing test water at time 24 hour Producer Defined -- Attribute was not measured in the sample Producer defined 5.51 7.11 pH units Hardness Concentration of magnesium and calcium in mg/L Producer Defined -- Attribute was not measured in the sample Producer defined 20 40 Milligrams per liter Survival and reproduction of C. dubia in chronic Al exposures Text file containing data. Producer Defined Batch Numeric identifier for a set of related tests run concurrently. Producer Defined Numeric identifier for a set of related tests run concurrently. Treatment An indicator of the test water source and/or properties Producer Defined 20 hard well CERC well water diluted to a hardness of 20 mg per liter calcium and magnesium Producer defined 25% site water Field collected stream water (Site) diluted 25% with CERC well water Producer defined 50% site water Field collected stream water (Site) diluted 50% with CERC well water Producer defined 100% site water Field collected stream water (Site) diluted 0% with CERC well water Producer defined 35 hard well CERC well water diluted to a hardness of 35 mg per liter calcium and magnesium Producer defined Test Concentration (mg Al/L) The target or nominal aluminum (CASRN 7784-27-2) concentration in mg/L Producer Defined 0.0 20.0 Milligrams per liter Survival Number of viable test organisms at the end of the bioassay Producer Defined 0 10 Number of individuals observed Reproduction Number of young produced by a females in the treatment Producer Defined 0 408 Number of individuals observed GS ScienceBase U.S. Geological Survey mailing and physical

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