Boron isotope data from bivalves from 2022 tank experiment in the Gulf of Maine, USA

Website: https://www.bco-dmo.org/dataset/995690
Data Type: experimental
Version: 1
Version Date: 2026-03-30

Project
» Collaborative Research: Using multi-proxy paleo data to constrain natural and anthropogenic hydrographic variability in the Gulf of Maine System over the last 250 years (GoM Paleo and Tank Experiment)
ContributorsAffiliationRole
Thatcher, Diana LynnIowa State UniversityPrincipal Investigator
LaVigne, MicheleBowdoin College (Bowdoin-Schiller)Co-Principal Investigator
Wanamaker, AlanIowa State UniversityCo-Principal Investigator, Scientist
Williams, BranwenClaremont McKenna College (CMC)Co-Principal Investigator
Jellison, BrittanyUniversity of New Hampshire (UNH)Scientist
McMahon, TeaganClaremont McKenna College (CMC)Scientist
Nina, WhitneyWestern Washington University (WWU)Scientist
Stewart, JosephUniversity of Bristol, UKScientist
Giss, MayaWestern Washington University (WWU)Student
Franklin, HeidiBowdoin College (Bowdoin-Schiller)Technician
Guay, KatherineBowdoin College (Bowdoin-Schiller)Technician
Newman, SawyerWoods Hole Oceanographic Institution (WHOI BCO-DMO)BCO-DMO Data Manager

Abstract
The boron isotopic composition (δ11Bc) of many marine carbonates provides insight into the pH at the site of calcification within biocalcifiers and, by extension, the pH of ambient seawater when the carbonate formed. A 20.5-week flowthrough tank experiment was conducted in which four species of commercially important bivalves from the northwest Atlantic Ocean were grown in tanks with controlled pHT (pH 7.4 to 8.0) and temperature conditions (6 to 12 °C). A total of 106 shell samples from 99 individuals of adult and juvenile Arctica islandica (ocean quahog), juvenile Mercenaria mercenaria (northern quahog or hard clam), juvenile Mya arenaria (soft-shell clam), and juvenile Placopecten magellanicus (Atlantic sea scallop) were analyzed from this controlled experiment to assess the seawater pH, temperature, and growth rate controls on shell δ11Bc. Juvenile P. magellanicus and juvenile M. mercenaria demonstrated significant relationships (R≥0.60; p-value <0.006) between tank pHT and δ11Bc, suggesting potential utility as proxies for past ambient seawater pH. Conversely, the δ11Bc of juvenile A. islandica and juvenile M. arenaria did not yield a strong relationship with seawater pHT but instead yielded significant relationships with shell growth rate (linear extension), with a positive relationship for M. arenaria and a negative relationship for juvenile A. islandica. The δ11B results from the few (n=9) adult A. islandica shells measured show the most variability across the range of pH and temperatures (range of 16‰), and no significant relationship was found with seawater pH or growth rate. Despite rigorous oxidative cleaning of samples, the data suggest that adult A. islandica shells contain boron-rich organic phases resistant to traditional cleaning techniques. The data on this site (summary file) include the average temperature, pH, and salinity used for the boron isotope analysis, in addition to the δ11B of the borate in water calculations, δ11B measured in the shells, the B/Ca ratio measured in the shells, and the delta pH values calculated using the above values. Additional data include (temperature file) all temperature measurements from the tank experiment (every minute measurements) and daily averages. pH (pH file) and salinity (salinity file) data from weekly measurements are included. Data needed to perform the delta pH calculations are included (delta pH file). The specimens grown in each tank that were used for boron isotope measurements are also included (boron specimens by tank file). This file specifies the number and species that were grown under the various tank conditions.


Coverage

Location: Schiller Coastal Studies Center at Bowdoin College, Orr's Island, ME, USA
Temporal Extent: 2022-01-14 - 2022-06-08

Dataset Description

The data files that makeup this dataset were generated from a flow-through tank experiment conducted at the Schiller Coastal Studies Center. The experiment was designed to examine physiological or environmental responses of multiple bivalve species under controlled conditions using continuously supplied seawater.

Specimens used in the experiment included both field-collected and hatchery-sourced organisms. Juvenile and adult individuals of Arctica islandica were collected offshore of Jonesport, Maine, USA (44°33.247’N, 67°16.183’W) at depths of approximately 76–85 meters. Juvenile Placopecten magellanicus were obtained from PenBay Farmed Scallops. Juvenile Mercenaria mercenaria and Mya arenaria were provided by the Downeast Institute Hatchery.

Four bivalve species were maintained in a fully factorial design with four pH treatments (~7.4, 7.6, 7.8, ~8.0) and three temperature treatments (~6, 9, 12 °C). Environmental conditions were continuously monitored (temperature) and regularly validated (pH, salinity), with all reported values representing tank-level averages. Specimen-level measurements (size, dry weight, buoyant weight) were collected at defined time points and linked to experimental treatment conditions.


Methods & Sampling

Experimental setup:

These four species were grown in four pH treatments (~7.4, 7.6, 7.8, and ambient conditions with a pH=8.0) at three temperature treatments (~6, 9, 12° C). There was one tank at each pH for T=6 and 12° C and two tanks at each pH for T=9° C.

Specimens were randomly assigned to tank conditions with roughly equal numbers of each specimen in each tank condition.

Specimens were in the tank conditions for 20.5 weeks before removed with the following exception. Half of the P. magellanicus were removed in April 2022.

Environmental Conditions:

pH and salinity were measured weekly with a YSI probe. pH was controlled within each tank condition by the Apex control system. Tanks with lower pH conditions than ambient were obtained by bubbling CO2 from compressed cylinders into the water of a mixing chamber before leading to each of the three sets of controlled pH tanks.

Temperature was measured with two Hobo Tidbit devices in each tank throughout the experiment. Temperatures were measured every minute throughout the 20.5 weeks. Temperatures were maintained within the tanks using Inkbird controllers and two (500W/800W) heaters per tank.

All pH measurements are on the total pH scale (pHT).

The reported measurements for temperature, salinity, and pHT are measured tank averages.

Specimen measurements:

All study specimens were measured for maximum height, dry (live) weight, and buoyant weight at the start and end of the experiment. For the P. magellanicus removed in April 2022, height, dry (live) weight, buoyant were measured after removal from the tanks. Photos were taken of each specimen at the conclusion of the experiment.

After the conclusion of the experiment, all specimens were dissected, shells were rinsed with DI water and allowed to air dry prior to sampling for boron isotopes.

Shell sampling:

Organic matter was removed with burring bit (Brasseler #835.11.010) and hand milling with a Dremel tool prior to sampling of the shell. 8 mg of shell was sampled (3-4 mg for P. magellanicus) for boron isotopes with the same bit and Dremel tool.

Boron samples were collected on the shells from the portion of the shell that grew from approximately week 2 to week 10 of the experiment (prior to the spring freshening and second calcein stain line in April 2022) for all species except the adult A. islandica. Due to much slower growth in the adult A islandica, the portion of the shell that grew during the entire tank experiment was sampled. 

For most shells, one sample was collected from each shell. There were two exceptions: a comparison was done between the two halves of the shell for three juvenile A. islandica (g5, g32, g48) and a comparison of the outer shell layer (both inner and outer layers of the outer shell) and the inner shell layer on two juvenile A. islandica (g40 and g52). The samples selected for these comparisons were randomly chosen.

Sample preparation:

All powdered shell samples were subject to two 15-minute leaches in warm 10% (by volume) H2O2 (80 °C; buffered in NH4OH) and a weak acid leach (0.0005 M HNO3) before powders were dissolved in distilled 0.5 M HNO3. Dissolved samples were centrifuged (1 min at 13k rpm), and if there was any visible undissolved non-carbonate material at the bottom of the microcentrifuge tube the dissolved sample was transferred to a clean vial, rejecting the small undissolved fraction.

The burring bit was used to remove all visible organic matter from the outside of the shells. The leaching in H2O2 was performed to remove the remaining organic matter. 

Chemical Processing:

All trace element and boron isotope analyses were performed at the University of Bristol. An aliquot of the dissolved sample was analyzed by Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) using well-characterized, matrix-matched, synthetic standard solutions to give B/Ca and U/Ca ratios. Samples and standards were introduced in 0.5 M HNO3 and an acid wash solution of 0.5 M HNO3 matrix and 0.3 M HF was utilized between samples/standards to aid B wash out.

The remaining sample containing between 4 and 40 ng of B was separated from the carbonate matrix using 20 μl micro-columns containing Amberlite IRA 743 boron-specific anionic exchange resin. The boron separation from the matrix was performed only on the day preceding Multi Collector-ICP-MS (MC-ICP-MS) analysis. All samples, blanks, and standard solutions were introduced to the instrument in a 0.5 M HNO3 and 0.3 M HF acid matrix again to ensure optimal B wash out.

A total of 108 samples were prepared for boron isotope analysis. There were two samples that did not produce useful results due to blocked columns (one adult A. islandica and one juvenile P. magellanicus). 

See Thatcher et al., (2026; GCA) and McMahon et al. (2024; PLOS Climate) for full details on the methods.


BCO-DMO Processing Description

- Loaded sheet 1 from "Thatcher et al_summary data.xlsx" in xlsx format, using row 1 as header, with missing values defined as empty strings, "nd", "**", "Column blocked", and "N/A". These various missing data values are retained within the dataset to differentiate between types of data flags, as they differ between columns.
- Renamed fields: "Average temperature (°C)" to Average_temperature, "Average salinity (psu)" to Average_salinity, "Average pHT" to Average_pHT, "Sample species" to Sample_species, "Sample description" to Sample_description, "δ11B Borate (‰, water)" to boron_isotope_value_borate_ion, "δ11B (‰)" to boron_isotope_value_shell, "B/Ca (µmol/mol)" to boron_calcium_ratio, "ΔpH" to delta_pH
- Set data columns to the following data types: Average_temperature, Average_salinity, Average_pHT, boron_isotope_value_borate_ion, boron_isotope_value_shell, delta_pH as number; boron_calcium_ratio as integer; SampleID, Sample_description, Sample_species as string
- Renamed resource from "thatcher_et_al_summary_data-1" to "995690_v1_bivalve_boron_isotopes"
- Output written to 995690_v1_bivalve_boron_isotopes.csv


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Data Files

File
995690_v1_bivalve_boron_isotopes.csv
(Comma Separated Values (.csv), 9.12 KB)
MD5:558a521e88870a95c10c9f495a49e538
Public Description:Primary data file for dataset ID 995690, version 1

This primary data file includes the average tank temperature, pH, and salinity used for the boron isotope analysis, in addition to the δ11B of the borate in water calculations, δ11B measured in the shells, the B/Ca ratio measured in the shells, and the delta pH values calculated using the supplemental files associated with this dataset.

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Supplemental Files

File
Boron specimens by tank
filename: Thatcher et al_boron specimens by tank.xlsx
(Microsoft Excel, 10.95 KB)
MD5:fdd68dfa9792986a7d4888275e5d4ff7
A summary of the specimens in each tank that were sampled for boron isotopes.
Delta pH calculations
filename: Thatcher et al_delta pH calculations.xlsx
(Microsoft Excel, 16.15 KB)
MD5:f536de1d9a7c40846fe99c71c036ed14
Data used to calculate delta pH values.

delta pH = pH of the calcifying fluid - pH of the seawater.
pH
filename: Thatcher et al_pH.xlsx
(Microsoft Excel, 16.40 KB)
MD5:da29e346839d88c06b32be89f0c75011
Weekly pH measurement from each tank. At the bottom of each column (tank) are the specimens sampled for boron isotopes that were grown in that tank.
Salinity
filename: Thatcher et al_salinity.xlsx
(Microsoft Excel, 12.24 KB)
MD5:b17ae92ac28533db5821d7752db11a43
Weekly salinity (psu) data from each tank. At the bottom of the column are the specimens that were sampled for boron isotopes from each tank.
Temperature (degrees Celsius)
filename: Thatcher et al_temperature.xlsx
(Microsoft Excel, 46.52 MB)
MD5:3f58b75c3736049eca7cec0ff788161e
Every minute temperature data (tab 1) and daily averages of temperature data (tab 2). At the top of tab 2 are the tank averages of temperature. Each tank had 2 loggers and the average temperature is the average of each day of the experiment from the two loggers.

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Related Publications

Douglas Bates, Martin Mächler, Ben Bolker, & Steven Walker. (2015). Fitting linear mixed-effects models using lme4. Journal of Statistical Software, 67(1), 1–48. https://doi.org/10.18637/jss.v067.i01
Software
Florian Hartig, Daniel J. Smith, & Michael Scherer. (2022). DHARMa: Residual diagnostics for hierarchical (multi-level/mixed) regression models (R package version 0.4.6). https://CRAN.R-project.org/package=DHARMa
Software
McMahon, T., Thatcher, D., Williams, B., Wanamaker, A., Jellison, B., Franklin, H., Guay, K., Whitney, N. M., Stewart, J. A., & LaVigne, M. (2024). Contrasting responses of commercially important Northwest Atlantic bivalve species to ocean acidification and temperature conditions. PLOS Climate, 3(11), e0000509. https://doi.org/10.1371/journal.pclm.0000509
Results

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Parameters

ParameterDescriptionUnits
SampleID

Name/ID of specimen in sample.

unitless
Sample_species

Species of specimen in sample.

unitless
Sample_description

Sample description.

unitless
Average_temperature

Average tank temperature of the experiment tank.

degrees Celsius
Average_pHT

Average total pH of the experiment tank.

pH units
Average_salinity

Average salinity of the experiment tank.

psu
boron_isotope_value_borate_ion

Boron isotope value of the borate ion.

per mil (‰, water)
boron_isotope_value_shell

Boron isotope value of the shell. Missing data identifier "Column blocked" within this column indicates where delta pH values were not calculated for this sample.

per mil (‰)
boron_calcium_ratio

Boron to calcium ratio.

(umol/mol)
delta_pH

Delta pH. Missing data identifier "**" ** indicates samples where the d11B values are not explainable by pH variability alone. "N/A" values indicate delta pH values were not calculated for this sample.

pH units


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Instruments

Dataset-specific Instrument Name
Inductively Coupled Plasma Mass Spectrometer (ICP-MS)
Generic Instrument Name
Inductively Coupled Plasma Mass Spectrometer
Dataset-specific Description
A Inductively Coupled Plasma Mass Spectrometer (ICP-MS) was to quantify elemental ratios (e.g., B/Ca, U/Ca) from dissolved shell samples using matrix-matched standards.
Generic Instrument Description
An ICP Mass Spec is an instrument that passes nebulized samples into an inductively-coupled gas plasma (8-10000 K) where they are atomized and ionized. Ions of specific mass-to-charge ratios are quantified in a quadrupole mass spectrometer.

Dataset-specific Instrument Name
Inductively Coupled Plasma-Mass Spectrometer (ICP-MS)
Generic Instrument Name
Multi Collector Inductively Coupled Plasma Mass Spectrometer
Dataset-specific Description
An aliquot of the dissolved sample was analyzed by Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) using well-characterized, matrix-matched, synthetic standard solutions to give B/Ca and U/Ca ratios. Samples and standards were introduced in 0.5 M HNO3 and an acid wash solution of 0.5 M HNO3 matrix and 0.3 M HF was utilized between samples/standards to aid B wash out.
Generic Instrument Description
A Multi Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICPMS) is a type of mass spectrometry where the sample is ionized in a plasma (a partially ionized gas, such as Argon, containing free electrons) that has been generated by electromagnetic induction. A series of collectors is used to detect several ion beams simultaneously. A MC-ICPMS is a hybrid mass spectrometer that combines the advantages of an inductively coupled plasma source and the precise measurements of a magnetic sector multicollector mass spectrometer. The primary advantage of the MC-ICPMS is its ability to analyze a broader range of elements, including those with high ionization potential that are difficult to analyze by Thermal Ionization Mass Spectrometry (TIMS). The ICP source also allows flexibility in how samples are introduced to the mass spectrometer and allows the analysis of samples introduced either as an aspirated solution or as an aerosol produced by laser ablation.

Dataset-specific Instrument Name
Mettler Toledo ME204E
Generic Instrument Name
scale or balance
Dataset-specific Description
Used to measure dry (live) weight of specimens at the beginning and end of the experiment. These measurements contribute to growth and condition metrics in the dataset.
Generic Instrument Description
Devices that determine the mass or weight of a sample.

Dataset-specific Instrument Name
Ohaus Adventurer AR1140
Generic Instrument Name
scale or balance
Dataset-specific Description
Used to measure buoyant weight of specimens at the start and end of the experiment. Buoyant weight measurements are used to estimate calcification and shell growth.
Generic Instrument Description
Devices that determine the mass or weight of a sample.

Dataset-specific Instrument Name
Onset HOBO TidbiT MX2032
Generic Instrument Name
Temperature Logger
Dataset-specific Description
Deployed in duplicate within each tank to record water temperature at 1-minute intervals throughout the 20.5-week experiment. Dataset temperature values represent tank-averaged time series derived from these measurements.
Generic Instrument Description
Records temperature data over a period of time.

Dataset-specific Instrument Name
YSI Pro Plus Multiparameter Meter (Xylem Inc.)
Generic Instrument Name
YSI Professional Plus Multi-Parameter Probe
Dataset-specific Description
Used to collect weekly spot measurements of pH and salinity in each tank. These measurements provide calibration/validation for controlled pH conditions and are reported as tank averages in the dataset.
Generic Instrument Description
The YSI Professional Plus handheld multiparameter meter provides for the measurement of a variety of combinations for dissolved oxygen, conductivity, specific conductance, salinity, resistivity, total dissolved solids (TDS), pH, ORP, pH/ORP combination, ammonium (ammonia), nitrate, chloride and temperature. More information from the manufacturer.


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Project Information

Collaborative Research: Using multi-proxy paleo data to constrain natural and anthropogenic hydrographic variability in the Gulf of Maine System over the last 250 years (GoM Paleo and Tank Experiment)

Coverage: Gulf of Maine/NW Atlantic Ocean


NSF Award Abstract:

The Gulf of Maine is located in the Northwestern Atlantic Ocean. Its waters serve as home to the economically important Atlantic Cod and shellfish industry. But recent changes to this environment pose a threat to the ecosystem and the commercial fishing industry. However, only a few long-term records of the environment exist in this area making it difficult to tell exactly when these changes started and how much is related to human activities. In this project, a team of researchers from three universities will construct a 250-year history of the regional environment by measuring yearly growth bands in local clams and algae. Chemical fingerprints in these growth bands will be used to determine the water temperature, salinity, biological productivity and pH conditions. This allow scientists to study how natural changes have affected the environment and compare these to changes caused by greenhouse global warming. This information will inform policy decisions of the newly-formed Maine Climate Council on how to better manage this area. The proposed work will also support training for early career scientists, broaden participation in science programs, and support undergraduate research opportunities.

Specifically, the team will use a multi-pronged approach using geochemical proxies in two types of high-resolution marine climate archives (clams and crustose coralline algae) to reconstruct past changes in oceanographic conditions, including near surface seawater temperatures, salinity, and pH in the Gulf of Maine through the last 250 years. Geochemical fingerprints (or proxies) preserved in the annual growth bands of clam shells and skeletons of long-lived marine calcifiers have been used extensively as archives of past ocean conditions. Discrete calcium carbonate layers can be sampled from the growth bands of clams and crustose coralline algae for geochemical analysis, generating proxy archive records. These reconstructions of past environmental conditions fill data gaps prior to instrumental records. Hence, the proposed research will potentially yield several multi-centennial, annually-resolved, absolutely-dated datasets of oceanographic variability in the Northwestern Atlantic, including the Gulf of Maine, prior to the Industrial Revolution, which will be used to evaluate the role of Atlantic meridional overturning circulation, and other climate forcings, on observed changes. By combining new data derived from traditional and novel proxies with existing hydrographic records, the relative contributions of source waters into the Gulf of Maine through time will be characterized to better understand the drivers of variability within the Gulf of Maine. Understanding past oceanographic variability in the Gulf of Maine is therefore critical for predicting the likely extent and magnitude of future change, and for planning to safeguard ecosystems and fisheries. Results will be widely disseminated to science and non-science audiences through publications, conference presentations, mentoring programs, coursework, and outreach activities at area schools, museums, and science centers.

This award reflects NSF's statutory mission and has been deemed worthy of support through evaluation using the Foundation's intellectual merit and broader impacts review criteria.



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Funding

Funding SourceAward
NSF Division of Ocean Sciences (NSF OCE)

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