Extraction and estimation of the quantity of calcium oxalate crystals in the foliage of conifer and hardwood trees

Metadata:

Identification_Information:
Citation:
Citation_Information:
Originator: Minocha, Rakesh
Originator: Chamberlain, Bradley
Originator: Long, Stephanie
Originator: Turlapati, Swathi A.
Originator: Quigley, Gloria
Publication_Date: 2022
Title:
Extraction and estimation of the quantity of calcium oxalate crystals in the foliage of conifer and hardwood trees
Geospatial_Data_Presentation_Form: tabular digital data
Publication_Information:
Publication_Place: Fort Collins, CO
Publisher: Forest Service Research Data Archive
Online_Linkage: https://doi.org/10.2737/RDS-2022-0057
Description:
Abstract:
This data publication includes the results of a study to develop a method for the extraction and indirect estimation of the quantity of calcium oxalate (CaOx) in tree foliage. This study included five sites in New Hampshire, four of which were in the Seaboard Lowlands section of the New England Physiographic Province and the fifth in the White Mountain section of the New England Physiographic Province. A large pool of foliar tissue was collected from a single tree of ten different species (five conifer and five hardwoods) in 2010 (Experiment 1). This provided homogeneous samples used to make comparisons of extractions in different solvents. For ten replicates of each species, calcium and oxalate were extracted from foliage in the following sequential steps: 1) double deionized water (DDW), 2) 2N Acetic acid (CH3COOH), and lastly, 3) five of the ten replicates were extracted in 5% (0.83N) Perchloric acid (PCA, HClO4) and the other five in 2N Hydrochloric acid (HCl) by freeze-thawing (3X) in each solvent. Total calcium (Ca), and other elements, were extracted by microwave digestion and quantified with an Inductively Coupled Plasma Optical Emission Spectrophotometer (ICP-OES), oxalate (and other organic acids) using High Performance Liquid Chromatography (HPLC). This experiment was then repeated with two conifer and two hardwood species using four trees per species and two analytical replicates for each tree in June 2014 (Experiment 2).
Purpose:
Method development for the extraction and estimation of calcium oxalate in the foliage of several forest tree species.
Supplemental_Information:
For more information about this study and these data, see Minocha et al. (2015).
Time_Period_of_Content:
Time_Period_Information:
Multiple_Dates/Times:
Single_Date/Time:
Calendar_Date: 2010
Single_Date/Time:
Calendar_Date: 2014
Currentness_Reference:
Ground condition
Status:
Progress: Complete
Maintenance_and_Update_Frequency: As needed
Spatial_Domain:
Description_of_Geographic_Extent:
All sites lie within the state of New Hampshire. With the exception of Hedgehog Mountain in Albany, all sites are within Strafford County, entirely within the Piscataqua River (coastal) watershed. This part of New Hampshire is in the Seaboard Lowlands section of the New England Physiographic Province. Soils in this area are moderately deep to deep Inceptisols, formed in coarse glacial till, within the mesic temperature regime. Forests are northeastern coastal forests comprised of temperate broadleaf species with mixed conifers and northern hardwoods of the New England-Acadian variety. These sites are in hardiness zone 5b with an average growing season of approximately 149 days.

The Hedgehog Mountain site lies in Carroll County within the White Mountain section of the New England Physiographic Province. Soils consists of moderately deep Spodosols formed in coarse glacial till within the frigid temperature regime. Forest type is spruce-fir mixed with northern hardwoods. This site is in hardiness zone 5a.

Site Locations:
Hedgehog Mountain, Albany, NH, USA (43.9742, -71.3672)
USDA Forest Service, Louis C. Wyman Forestry Sciences Laboratory, Durham, NH, USA (43.1423,
-70.9492)
University of New Hampshire-Woodman Horticultural Farm, Durham, NH, USA (43.1477, -70.9407)
University of New Hampshire-Kingman Farm, Madbury, NH, USA (43.1726, -70.9294)
University of New Hampshire-East Foss Farm, Durham, NH, USA (43.1189, -70.9368)
Bounding_Coordinates:
West_Bounding_Coordinate: -71.3672
East_Bounding_Coordinate: -70.9294
North_Bounding_Coordinate: 43.9742
South_Bounding_Coordinate: 43.1189
Bounding_Altitudes:
Altitude_Minimum: 50
Altitude_Maximum: 2500
Altitude_Distance_Units: feet
Keywords:
Theme:
Theme_Keyword_Thesaurus: ISO 19115 Topic Category
Theme_Keyword: biota
Theme_Keyword: environment
Theme:
Theme_Keyword_Thesaurus: National Research & Development Taxonomy
Theme_Keyword: Ecology, Ecosystems, & Environment
Theme_Keyword: Ecology
Theme_Keyword: Plant ecology
Theme_Keyword: Forest & Plant Health
Theme_Keyword: Botany
Theme:
Theme_Keyword_Thesaurus: None
Theme_Keyword: calcium oxalate
Theme_Keyword: calcium
Theme_Keyword: oxalic acid
Theme_Keyword: foliar physiology
Theme_Keyword: sequential extraction
Theme_Keyword: direct extraction
Theme_Keyword: red spruce
Theme_Keyword: eastern hemlock
Theme_Keyword: white pine
Theme_Keyword: Norway spruce
Theme_Keyword: balsam fir
Theme_Keyword: red oak
Theme_Keyword: black oak
Theme_Keyword: trembling aspen
Theme_Keyword: American beech
Theme_Keyword: yellow birch
Theme_Keyword: sugar maple
Place:
Place_Keyword_Thesaurus: None
Place_Keyword: New Hampshire
Place_Keyword: Hedgehog Mountain
Place_Keyword: Strafford County
Place_Keyword: Carroll County
Place_Keyword: Durham
Place_Keyword: Madbury
Place_Keyword: Albany
Place_Keyword: University of New Hampshire-Durham campus
Place_Keyword: Woodman Horticultural Farm
Place_Keyword: Kingman Farm
Place_Keyword: East Foss Farm
Place_Keyword: Louis C. Wyman Forest Sciences Laboratory
Taxonomy:
Keywords/Taxon:
Taxonomic_Keyword_Thesaurus:
None
Taxonomic_Keywords: multiple species
Taxonomic_Keywords: plants
Taxonomic_Keywords: vegetation
Taxonomic_System:
Classification_System/Authority:
Classification_System_Citation:
Citation_Information:
Originator: ITIS
Publication_Date: 2022
Title:
Integrated Taxonomic Information System
Geospatial_Data_Presentation_Form: on-line database
Other_Citation_Details:
Retrieved [May, 11, 2022]; CC0
Online_Linkage: https://doi.org/10.5066/F7KH0KBK
Online_Linkage: https://www.itis.gov
Taxonomic_Procedures:
Taxonomic_Classification:
Taxon_Rank_Name: Kingdom
Taxon_Rank_Value: Plantae
Applicable_Common_Name: plantes
Applicable_Common_Name: Planta
Applicable_Common_Name: Vegetal
Applicable_Common_Name: plants
Taxonomic_Classification:
Taxon_Rank_Name: Subkingdom
Taxon_Rank_Value: Viridiplantae
Applicable_Common_Name: green plants
Taxonomic_Classification:
Taxon_Rank_Name: Infrakingdom
Taxon_Rank_Value: Streptophyta
Applicable_Common_Name: land plants
Taxonomic_Classification:
Taxon_Rank_Name: Superdivision
Taxon_Rank_Value: Embryophyta
Taxonomic_Classification:
Taxon_Rank_Name: Division
Taxon_Rank_Value: Tracheophyta
Applicable_Common_Name: vascular plants
Applicable_Common_Name: tracheophytes
Taxonomic_Classification:
Taxon_Rank_Name: Subdivision
Taxon_Rank_Value: Spermatophytina
Applicable_Common_Name: spermatophytes
Applicable_Common_Name: seed plants
Applicable_Common_Name: phanérogames
Taxonomic_Classification:
Taxon_Rank_Name: Class
Taxon_Rank_Value: Magnoliopsida
Taxonomic_Classification:
Taxon_Rank_Name: Superorder
Taxon_Rank_Value: Rosanae
Taxonomic_Classification:
Taxon_Rank_Name: Order
Taxon_Rank_Value: Fagales
Taxonomic_Classification:
Taxon_Rank_Name: Family
Taxon_Rank_Value: Fagaceae
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Quercus
Applicable_Common_Name: chêne
Applicable_Common_Name: oak
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Quercus rubra
Applicable_Common_Name: northern red oak
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Quercus velutina
Applicable_Common_Name: black oak
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Fagus
Applicable_Common_Name: beech
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Fagus grandifolia
Applicable_Common_Name: American beech
Taxonomic_Classification:
Taxon_Rank_Name: Family
Taxon_Rank_Value: Betulaceae
Applicable_Common_Name: alder
Applicable_Common_Name: birch
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Betula
Applicable_Common_Name: birch
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Betula alleghaniensis
Applicable_Common_Name: yellow birch
Taxonomic_Classification:
Taxon_Rank_Name: Order
Taxon_Rank_Value: Sapindales
Taxonomic_Classification:
Taxon_Rank_Name: Family
Taxon_Rank_Value: Sapindaceae
Applicable_Common_Name: soapberries
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Acer
Applicable_Common_Name: maples
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Acer saccharum
Applicable_Common_Name: sugar maple
Taxonomic_Classification:
Taxon_Rank_Name: Order
Taxon_Rank_Value: Malpighiales
Taxonomic_Classification:
Taxon_Rank_Name: Family
Taxon_Rank_Value: Salicaceae
Applicable_Common_Name: willows
Applicable_Common_Name: saules
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Populus
Applicable_Common_Name: cottonwood
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Populus tremuloides
Applicable_Common_Name: quaking aspen
Taxonomic_Classification:
Taxon_Rank_Name: Class
Taxon_Rank_Value: Pinopsida
Applicable_Common_Name: conifers
Taxonomic_Classification:
Taxon_Rank_Name: Subclass
Taxon_Rank_Value: Pinidae
Taxonomic_Classification:
Taxon_Rank_Name: Order
Taxon_Rank_Value: Pinales
Applicable_Common_Name: pines
Taxonomic_Classification:
Taxon_Rank_Name: Family
Taxon_Rank_Value: Pinaceae
Applicable_Common_Name: pines
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Abies
Applicable_Common_Name: fir
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Abies balsamea
Applicable_Common_Name: balsam fir
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Picea
Applicable_Common_Name: spruce
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Picea rubens
Applicable_Common_Name: red spruce
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Picea abies
Applicable_Common_Name: Norway spruce
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Pinus
Applicable_Common_Name: pine
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Pinus strobus
Applicable_Common_Name: eastern white pine
Applicable_Common_Name: white pine
Applicable_Common_Name: northern white pine
Applicable_Common_Name: soft pine
Applicable_Common_Name: Weymouth pine
Taxonomic_Classification:
Taxon_Rank_Name: Genus
Taxon_Rank_Value: Tsuga
Applicable_Common_Name: hemlock
Taxonomic_Classification:
Taxon_Rank_Name: Species
Taxon_Rank_Value: Tsuga canadensis
Applicable_Common_Name: Canada hemlock
Applicable_Common_Name: hemlock spruce
Applicable_Common_Name: eastern hemlock
Access_Constraints: None
Use_Constraints:
These data were collected using funding from the U.S. Government and can be used without additional permissions or fees. If you use these data in a publication, presentation, or other research product please use the following citation:

Minocha, Rakesh; Chamberlain, Bradley; Long, Stephanie; Turlapati, Swathi A.; Quigley, Gloria. 2022. Extraction and estimation of the quantity of calcium oxalate crystals in the foliage of conifer and hardwood trees. Fort Collins, CO: Forest Service Research Data Archive. https://doi.org/10.2737/RDS-2022-0057
Point_of_Contact:
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA Forest Service, Northern Research Station
Contact_Person: Rakesh Minocha, Ph.D
Contact_Position: Research Plant Physiologist
Contact_Address:
Address_Type: mailing and physical
Address: 271 Mast Road
City: Durham
State_or_Province: NH
Postal_Code: 03824
Country: USA
Contact_Voice_Telephone: 603-868-7622
Contact_Electronic_Mail_Address: rakesh.minocha@usda.gov
Data_Set_Credit:
Funding support for this project was provided by the USDA Forest Service, Northern Research Station.


Author Information:

Rakesh Minocha
USDA Forest Service, Northern Research Station
http://orcid.org/0000-0002-4055-5137

Bradley Chamberlain
USDA Forest Service, Northern Research Station

Stephanie Long
USDA Forest Service, Northern Research Station
https://orcid.org/0000-0001-6515-2126

Swathi A. Turlapati
USDA Forest Service, Northern Research Station

Gloria Quigley
USDA Forest Service, Northern Research Station
Cross_Reference:
Citation_Information:
Originator: Minocha, Rakesh
Originator: Chamberlain, Bradley
Originator: Long, Stephanie
Originator: Turlapati, Swathi A.
Originator: Quigley, Gloria
Publication_Date: 2015
Title:
Extraction and estimation of the quantity of calcium oxalate crystals in the foliage of conifer and hardwood trees
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: Tree Physiology
Issue_Identification: 35(5): 574-580
Online_Linkage: https://doi.org/10.1093/treephys/tpv031
Online_Linkage: https://www.fs.usda.gov/treesearch/pubs/48697
Analytical_Tool:
Analytical_Tool_Description:
TotalChrom (version 6.2.1) (PerkinElmer Inc., Waltham, MA, USA). Liquid chromatography (HPLC) control and data processing software.

Exclusive to PerkinElmer Inc., Life and Analytical Sciences, Shelton, CT, USA; 2002
Tool_Access_Information:
Online_Linkage: https://www.perkinelmer.com/content/relatedmaterials/brochures/bro_totalchromworkstation.pdf
Online_Linkage: https://www.perkinelmer.com/CMSResources/Images/46-74577MAN_TotalChromWorkstationVolume1.pdf
Tool_Access_Instructions:
see website
Tool_Citation:
Citation_Information:
Originator: PerkinElmer Inc.
Publication_Date: 2002
Title:
TotalChrom: Liquid chromatography (HPLC) control and data processing software
Edition: version 6.2.1
Geospatial_Data_Presentation_Form: software
Publication_Information:
Publication_Place: Shelton, CT
Publisher: PerkinElmer Inc., Life and Analytical Sciences
Online_Linkage: https://www.perkinelmer.com/content/relatedmaterials/brochures/bro_totalchromworkstation.pdf
Online_Linkage: https://www.perkinelmer.com/CMSResources/Images/46-74577MAN_TotalChromWorkstationVolume1.pdf
Analytical_Tool:
Analytical_Tool_Description:
ICP Expert-VistaPro Software - Life Sciences and Chemical Analysis Software for Inductively Coupled Plasma Optical Emission Spectrophotometer
Tool_Access_Information:
Online_Linkage: https://www.agilent.com/en/products/software-informatics/atomic-spectroscopy-data-systems/icp-expert-software-for-icp-oes
Tool_Access_Instructions:
see website
Tool_Citation:
Citation_Information:
Originator: Agilent Technologies Inc.
Publication_Date: 2010
Title:
ICP Expert-VistaPro software: life sciences and chemical analysis software for inductively coupled plasma optical emission spectrophotometer
Edition: version 4.0
Geospatial_Data_Presentation_Form: software
Publication_Information:
Publication_Place: Palo Alto, CA
Publisher: Vista CCD
Other_Citation_Details:
In May 2010 Varian Inc. was acquired by Agilent Technologies Inc., Santa Clara, CA, USA). ICP-OES control and data processing software is exclusive to Agilent Technologies Inc., Santa Clara, CA, USA.
Online_Linkage: https://www.agilent.com/en/products/software-informatics/atomic-spectroscopy-data-systems/icp-expert-software-for-icp-oes
Back to Top
Data_Quality_Information:
Attribute_Accuracy:
Attribute_Accuracy_Report:
For total and soluble elemental analyses, a standard calibration was repeated after every 20 samples, and check standards were run after every recalibration and again after every 10 samples. For total elements, National Institute of Standards and Technology (NIST, Gaithersburg, MD, USA) standards 1575A (Pine foliage), 1515 (Apple foliage) and 1547 (Peach foliage) were used for procedural verification. Total foliar extractions were done in accordance with EPA SW-846 Test Method 3052. Since there are no NIST standards available for fresh tissue, we used an in-house ground wood reference for quality control and assurance for elements in sequential and direct foliar extracts. ICP analysis was conducted following EPA SW-846 Test Method 6010.

For samples analyzed by HPLC for organic acids, we ran a large number of biological replicates as well as multiple analytical replicates on a randomly selected subset. HPLC analysis followed guidance within EPA SW-846 Test Method 8000D.

Appropriate method detection limits are tested for all analytical methods.
Logical_Consistency_Report:
For all analyses, standards were repeated to ensure accuracy and precision; for biological samples, many analytical replicates were run for assurance. Proper statistical analyses were applied to the raw data to check distribution and remove outliers.
Completeness_Report:
These data contain blanks where data were not available due to human error, missing samples, data outliers, etc.; -888.88 denotes data not available (na); and -999.99 denotes no analysis for that sample.
Lineage:
Methodology:
Methodology_Type: Field
Methodology_Description:
BACKGROUND

Sites for sampling were chosen mainly for proximity to our laboratory as well as the type of trees present and accessibility of the foliage. One healthy looking tree of ten different species, 5 broadleaf and 5 conifers, was randomly chosen for sampling. The goal was to choose a wide range of species to demonstrate the effectiveness of this method.

The first part of this study (Experiment 1) included foliar samples collected from June through September, 2010. The second part of this study (Experiment 2), where part of experiment 1 was repeated, included foliage collected in June 2014.


FIELD COLLECTION OF FOLIAR SAMPLES

Using a pole pruner, small branches were abscised from sun-lit positions in the mid-canopy of (Experiment 1) one tree of each of 10 different species (all locations within NH, USA: red spruce from Hedgehog mountain, eastern hemlock and red oak from Woodman Horticultural farm, and white pine, Norway spruce, balsam fir, American beech, trembling aspen, yellow birch and sugar maple from the grounds at the USFS) that varied in age and diameter at breast height (dbh). For Experiment 2, foliage was collected in the same manner from four trees each of 4 species (red spruce from Kingman farm plantation, white pine from Woodman Horticultural farm, and sugar maple and black oak from East Foss farm). Individual branches were tagged and recorded at the time of sampling. Foliage remained intact on the woody stems and were placed in a cooler for transport back to the U.S. Forest Service, Louis C. Wyman Forestry Sciences Laboratory for processing. Other than red spruce foliage from Hedgehog mountain, all samples were processed within 4 hours of collection.


LABORATORY PROCESSING OF SAMPLES

Visually healthy leaves from several branchlets were chosen from each bough. A pool of approximately 10 grams (g) of leaf disks were collected from the broadleaf species using a paper punch (6.4 millimeter (mm) in diameter, major veins and areas of necrosis were excluded) and needles from the conifers were finely chopped (1-2 mm) using scissors. Each sample was thoroughly mixed to create a homogeneous pool. From the pooled tissue from each individual tree, 10 sub-samples of ~300 milligrams (mg) fresh weight (FW) each were weighed using a digital scale and placed into clean labeled 20 milliliter (ml) plastic scintillation vials. Ten ml of DDW (double deionized water) was added; these 10 replicates were extracted in a sequential series. Direct extractions with the same solvents and samples as the sequential extractions were done for comparison using 20 more sub-samples. Of those 20 sub-samples for direct extractions, 5 each received 10 ml of DDW, 2N Acetic Acid, 5% PCA, or 2N HCl. In the repeat experiment (Experiment 2), two analytical replicates (“a, b”) from 4 trees each of 2 coniferous and 2 broadleaf species were collected, weighed, and processed as described above except for HCl extractions which were not repeated.

The remainder of each sample was placed in a separate labeled vial to be used for total calcium (Ca), and other elements, analysis. Current-year and past-year needles were collected from the same branchlet but were processed separately. Corresponding sample information of exact weights, vial labels and tree information were all logged into a field notebook and recorded in a Microsoft Excel spreadsheet. All samples were stored at -20 °Celsius (C) until further analysis.
Methodology_Citation:
Citation_Information:
Originator: Minocha, Rakesh
Originator: Shortle, Walter C.
Originator: Long, Stephanie
Originator: Minocha, Subhash C.
Publication_Date: 1994
Title:
A rapid and reliable procedure for extraction of cellular polyamines and inorganic ions from plant tissues
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: Journal of Plant Growth Regulation
Issue_Identification: 13: 187-193
Online_Linkage: https://doi.org/10.1007/bf00226036
Methodology:
Methodology_Type: Lab
Methodology_Description:
LABORATORY PROCESSING OF SAMPLES (continued)

All direct extracts were frozen/thawed for 3 cycles according to Minocha et al. (1994) and then kept frozen at -20 °C. All sequential extracts in DDW, on the third thaw, were vortexed at top speed for 30 seconds, the foliage allowed to settle, and the supernatant was carefully transferred to a clean scintillation vial using a pipette. The pellets were then washed with 40 ml DDW and dried overnight at 50 °C. The dried tissue was reconstituted with 10 ml of 2N acetic acid (second extraction in the sequence of 3), and the freeze-thawing, washing and drying steps were repeated. Again, that entire process was repeated for the final extraction where the pellets of 5 replicates were reconstituted in 10 ml 5% PCA and 5 in 2N HCl. Upon the fourth thaw, extracts were centrifuged at 13,000 x g for 8 minutes. The resulting supernatants were analyzed for soluble elements and organic acids.

The remaining foliar sub-samples (~800-1200 mg) stored at -20 °C were later thawed, dried at 60 °C for 7 days, and ground for 1 minute using a SPEX SamplePrep shatterbox (SPEX, Metuchen, NJ, USA) to produce a fine homogeneous powder. The dried, ground foliage was stored in a desiccator at room temperature until analysis for total Ca (and other elements).


ANALYTICAL LABORATORY METHODOLOGIES

Processing and Quantification of Total and Soluble Calcium (and other elements) in Foliage by Inductively Coupled Plasma Optical Emission Spectrophotometer (ICP-OES):

The extraction of total Ca (and other elements) was done in accordance with EPA SW-846 Test Method 3052; 0.2 g of each ground sample was digested in 9 ml of concentrated nitric acid in Teflon vessels using a MARS™ Xpress microwave (CEM Corporation, Matthews, NC, USA). Before analysis, concentrated nitric acid digests were diluted to 50 ml volume with DDW, and all previously frozen/thawed direct and sequential extracts were diluted 2.5 times (conifers) and 5 times (hardwoods) with the appropriate matrix (DDW, 2N Acetic acid, 5% PCA or 2N HCl). Total and soluble elemental analyses were quantified using a simultaneous axial ICP-OES (Vista CCD, Varian Inc., Palo Alto, CA) and Vista Pro software (v. 4.0) in accordance with EPA SW-846 Test Method 6010D. Raw data were expressed as parts per million (ppm) and were converted to micromoles (µmol) per g FW.

Processing and Quantification of Oxalic acid (and other organic acids) in Foliage by High Performance Liquid Chromatography (HPLC):

Oxalic acid (and other organic acids) content was determined by HPLC based on other methods (Bai et al. 2006; Castellari et al. 2000; Pereira et al. 2010) that were optimized in our laboratory. Previously frozen samples were thawed and then vortexed at top speed. After the samples settled, they were filtered through a 0.45 micron (µm) nylon syringe filter (Pall Corporation, Port Washington, NY, USA) and placed into 2 ml autosampler vials. The samples were then run on a Series 200 PerkinElmer HPLC system including pump, auto-sampler fitted with a 200 microliter (µl) sample injection loop (20 µl injection volume), and UV/VIS detector set at a range of 0.2 and response of 0.02 (PerkinElmer Corporation, Norwalk, CT, USA). Absorbance was measured at 215 nanometers (nm). The organic acids were separated on a Phenomenex Synergi-Hydro-RP™, 4 µm, 100 x 4.6 mm I.D. C18 analytical column fitted with a Phenomenex SecurityGuard™, 5µm, 4 x 3 mm I.D. C18 cartridge guard column (Phenomenex, Torrance, CA, USA) that was heated to 25 °C, using 25 millimolar (mM) phosphate buffer (KH2PO4 + H3PO4) with 0.5 mM tetrabutylammonium hydrogensulfate and 1% methanol at pH 2.5 at a flow rate of 1.0 ml per minute. Oxalic acid typically eluted at 1.5 minutes. PerkinElmer TotalChrom HPLC software (v. 6.2.1) was used to integrate data. Calibration curves based on the elution profiles of the organic acid standards (made in the same matrix as the samples) were used to estimate concentration in sample extracts. Raw data were expressed as ppm and were then converted to µmol per g FW. HPLC analysis follows guidance within EPA SW-846, Test Method 8000D. Raw data were collected and integrated using TotalChrom HPLC software (v. 6.2.1) as nmoles (nmol) per ml and were converted to nmoles (nmol) per g FW.
Methodology_Citation:
Citation_Information:
Originator: Bai, Cheng
Originator: Reilly, Charles C.
Originator: Wood, Bruce W.
Publication_Date: 2006
Title:
Nickle deficiency disrupts metabolism of ureides, amino acids, and organic acids of young pecan foliage
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: Plant Physiology
Issue_Identification: 140: 433-443
Online_Linkage: https://doi.org/10.1104/pp.105.072983
Methodology_Citation:
Citation_Information:
Originator: Castellari, Massimo
Originator: Versari, Andrea
Originator: Spinabelli, Umberto
Originator: Galassi, Sergio
Originator: Amati, Aureliano
Publication_Date: 2000
Title:
An improved HPLC method for the analysis of organic acids, carbohydrates and alcohols in grape musts and wines
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: Journal of Liquid Chromatography and Related Technologies
Issue_Identification: 23(13): 2047-2056
Online_Linkage: https://doi.org/10.1081/JLC-100100472
Methodology_Citation:
Citation_Information:
Originator: Minocha, Rakesh
Originator: Long, Stephanie
Originator: Thangavel, Palaniswamy
Originator: Minocha, Subhash C.
Originator: Eagar, Christopher
Originator: Driscoll, Charles T.
Publication_Date: 2010
Title:
Elevation dependent sensitivity of northern hardwoods to Ca additions at Hubbard Brook Experimental Forest, NH, USA
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: Forest Ecology and Management
Issue_Identification: 260(12): 2115-2124
Online_Linkage: https://doi.org/10.1016/j.foreco.2010.09.002
Online_Linkage: https://www.fs.usda.gov/treesearch/pubs/43605
Methodology_Citation:
Citation_Information:
Originator: Pereira, Vanda
Originator: Câmara, José S.
Originator: Cacho, Juan
Originator: Marques, José C.
Publication_Date: 2010
Title:
HPLC-DAD methodology for the quantification of organic acids, furans and polyphenols by direct injection of wine samples
Geospatial_Data_Presentation_Form: journal article
Series_Information:
Series_Name: Journal of Separation Science
Issue_Identification: 33(9): 1204-1215
Online_Linkage: https://doi.org/10.1002/jssc.200900784
Methodology_Citation:
Citation_Information:
Originator: U.S. EPA
Publication_Date: 1996
Title:
SW-846, Test Method 3052: Microwave assisted acid digestion of siliceous and organically based matrices
Geospatial_Data_Presentation_Form: online document
Publication_Information:
Publication_Place: Washington, DC
Publisher: United States Environmental Protection Agency
Online_Linkage: https://www.epa.gov/hw-sw846/sw-846-test-method-3052-microwave-assisted-acid-digestion-siliceous-and-organically-based
Methodology_Citation:
Citation_Information:
Originator: U.S. EPA
Publication_Date: 2014
Title:
SW-846 Test Method 6010D: Inductively Coupled Plasma-Atomic Emission Spectrometry
Geospatial_Data_Presentation_Form: document
Series_Information:
Series_Name: SW-846 Compendium
Issue_Identification: Revision 4
Publication_Information:
Publication_Place: Washington, D.C.
Publisher: United States Environmental Protection Agency
Online_Linkage: https://www.epa.gov/hw-sw846/sw-846-compendium
Online_Linkage: https://www.epa.gov/hw-sw846/sw-846-test-method-6010d-inductively-coupled-plasma-optical-emission-spectrometry-icp-oes
Methodology_Citation:
Citation_Information:
Originator: U.S. EPA
Publication_Date: 2014
Title:
The SW-846 Compendium
Edition: Revision 8
Geospatial_Data_Presentation_Form: online document
Publication_Information:
Publication_Place: Washington, DC
Publisher: United States Environmental Protection Agency
Online_Linkage: https://www.epa.gov/hw-sw846/sw-846-compendium
Methodology_Citation:
Citation_Information:
Originator: U.S. EPA
Publication_Date: 2018
Title:
SW-846 Test Method 8000D: Determinative Chromatographic Separations
Geospatial_Data_Presentation_Form: document
Series_Information:
Series_Name: SW-846 Compendium
Issue_Identification: Revision 5
Publication_Information:
Publication_Place: Washington D.C.
Publisher: United States Environmental Protection Agency
Online_Linkage: https://www.epa.gov/hw-sw846/sw-846-compendium
Online_Linkage: https://www.epa.gov/hw-sw846/sw-846-test-method-8000d-determinative-chromatographic-separations
Process_Step:
Process_Description:
see methodology section
Process_Date: Unknown
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Entity_and_Attribute_Information:
Overview_Description:
Entity_and_Attribute_Overview:
Below you will find a list and description of the files included in this data publication.

Unit abbreviations used:

µmol g⁻¹ calc FW = micromoles per gram calculated fresh weight
µmol g⁻¹ FW = micromoles per gram fresh weight


VARIABLE DESCRIPTION FILE (1)

1. \Data\_variable_descriptions.csv: Comma-separated values (CSV) file containing a list and description of variables found in all data files. (A description of these variables is also provided in the metadata below.)

Columns include:

Filename = name of data file
Variable = name of variable
Units = units (if applicable)
Precision = precision (if applicable)
Description = description of variable
Important Notes = Additional notes to interpret that variable
References = Relevant references for some variables


DATA FILES (2)
For both files, -888.88 denotes data not available (na) and -999.99 denotes no analysis for that sample.

1. \Data\Minocha_CaOX_Method_data_Exp1.csv: CSV file containing comparative estimations of soluble and total calcium and oxalic acid sequentially extracted in solvents of increasing strength (Water, 2N Acetic acid, 5% Perchloric acid or 2N Hydrochloric acid) or directly extracted (in the same solvents) from the foliage of 10 different tree species collected in 2010. (Supplemental information includes data on other elements and organic acids analyzed from the same foliar extracts.)

2. \Data\Minocha_CaOX_Method_data_Exp2.csv: CSV file containing data from repeated experiment for the comparative estimations of soluble and total calcium and oxalic acid sequentially extracted in solvents of increasing strength (Water, 2N Acetic acid, 5% Perchloric acid) or directly extracted (in the same solvents) from the foliage of 4 different tree species collected in 2014. (Supplemental information includes data on other elements and organic acids analyzed from the same foliar extracts.)

Variables in both data files include:

ID = "In-house" sample identification (Tree type-replicate number)

tree = Assigned tree number for identification (1-4)

Replicate = Assigned replicate identification (1-10, a-b)

species = Species of tree that foliage was collected from and needle age-class (Red spruce [Picea rubens], Eastern hemlock [Tsuga canadensis], White pine [Pinus strobus], Norway spruce [Picea abies], Balsam fir [Abies balsamea], American beech [Fagus grandifolia], Red oak [Quercus rubra], Trembling aspen [Populus tremuloides], Yellow birch [Betula alleghaniensis], Black oak [Quercus velutina], Sugar maple [Acer saccharum], CY = current year growth, PY = one-year growth)

Location = Sites where foliar samples were collected (Hedgehog Mountain, Albany, NH, USA [43.9742, -71.3672]; University of New Hampshire-Woodman Horticultural Farm, Durham, NH, USA [43.1477, -70.9407]; the grounds of the USDA Forest Service, Louis C. Wyman Forestry Sciences Laboratory, Durham, NH, USA [43.1423, -70.9492]; University of New Hampshire-Kingman Farm, Madbury, NH, USA [43.1726, -70.9294]; University of New Hampshire-East Foss Farm, Durham, NH, USA [43.1189, -70.9368])

experiment = There were 2 parts to this research (Experiment "1" was done with foliage of different species collected from June through October, 2010. Experiment "2" was a replicate of the sequential extractions and direct extraction in PCA from experiment 1, and was done with foliage from different species all collected in June, 2014.)

date collected = Date foliage samples were collected by month-year (June to October, 2010 and June, 2014)

Ca-Total = Total Calcium (Ca) in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by Inductively Coupled Plasma Optical Emission Spectrophotometer (ICP-OES), µmol g⁻¹ calc FW

Ca-Seq1-DDW = The portion of total Ca in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength (1st = DDW, 2nd = 2N Acetic acid, 3rd = either 2N Hydrochloric acid OR 5% (0.83N) Perchloric acid) measured by ICP-OES, µmol g⁻¹ FW

Ox-Seq1-DDW = The portion of Oxalic acid (Ox) in foliage that is solubilized by 3 F/T cycles in double deionized water in the first of a sequence of extractions in three solvents of increasing acidic strength (1st = DDW, 2nd = 2N Acetic acid, 3rd = either 2N Hydrochloric acid OR 5% (0.83N) Perchloric acid) measured by High-Performance Liquid Chromatograph, fluorescence (HPLC), µmol g⁻¹ FW

Ca-Seq2-Acetic = The portion of total Ca in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid (Acetic) in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Ox-Seq2-Acetic = The portion of Ox in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Ca-Seq3A-PCA = The portion of total Ca in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid (PCA) in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Ox-Seq3A-PCA = The portion of Ox in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Ca-Seq3B-HCl = The portion of total Ca in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid (HCl) in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Ox-Seq3B-HCl = The portion of Ox in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Ca-Direct-DDW = The portion of total Ca in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

Ox-Direct-DDW = Oxalic acid in foliage that is directly solubilized by 3 F/T cycles in DDW by HPLC, µmol g⁻¹ FW

Ca-Direct-Acetic = The portion of total Ca in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

Ox-Direct-Acetic = Oxalic acid in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by HPLC, µmol g⁻¹ FW

Ca-Direct-PCA = The portion of total Ca in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

Ox-Direct-PCA = Oxalic acid in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by HPLC, µmol g⁻¹ FW

Ca-Direct-HCl = The portion of total Ca in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

Ox-Direct-HCl = Oxalic acid in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by HPLC, µmol g⁻¹ FW

Mg-Seq1-DDW = The portion of total Magnesium (Mg) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

Mg-Direct-DDW = The portion of total Mg in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

Mg-Seq2-Acetic = The portion of total Mg in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Mg-Direct-Acetic = The portion of total Mg in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

Mg-Seq3A-PCA = The portion of total Mg in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Mg-DirectPCA = The portion of total Mg in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

Mg-Seq3B-HCl = The portion of total Mg in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Mg-Direct-HCl = The portion of total Mg in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

Mg-Total = Total Mg in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

K-Seq1-DDW = The portion of total Potassium (K) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

K-Direct-DDW = The portion of total K in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

K-Seq2-Acetic = The portion of total K in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

K-Direct-Acetic = The portion of total K in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

K-Seq3A-PCA = The portion of total K in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

K-DirectPCA = The portion of total K in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

K-Seq3B-HCl = The portion of total K in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

K-Direct-HCl = The portion of total K in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

K-Total = Total K in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

Mn-Seq1-DDW = The portion of total Manganese (Mn) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

Mn-Direct-DDW = The portion of total Mn in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

Mn-Seq2-Acetic = The portion of total Mn in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Mn-Direct-Acetic = The portion of total Mn in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

Mn-Seq3A-PCA = The portion of total Mn in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Mn-Direct-PCA = The portion of total Mn in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

Mn-Seq3B-HCl = The portion of total Mn in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Mn-Direct-HCl = The portion of total Mn in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

Mn-Total = Total Mn in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

P-Seq1-DDW = The portion of total Phosphorous (P) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

P-Direct-DDW = The portion of total P in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

P-Seq2-Acetic = The portion of total P in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

P-Direct-Acetic = The portion of total P in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

P-Seq3A-PCA = The portion of total P in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

P-DirectPCA = The portion of total P in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

P-Seq3B-HCl = The portion of total P in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

P-Direct-HCl = The portion of total P in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

P-Total = Total P in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

Al-Seq1-DDW = The portion of total Aluminum (Al) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

Al-Direct-DDW = The portion of total Al in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

Al-Seq2-Acetic = The portion of total Al in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Al-Direct-Acetic = The portion of total Al in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

Al-Seq3A-PCA = The portion of total Al in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Al-DirectPCA = The portion of total Al in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

Al-Seq3B-HCl = The portion of total Al in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Al-Direct-HCl = The portion of total Al in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

Al-Total = Total Al in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

Fe-Seq1-DDW = The portion of total Iron (Fe) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

Fe-Direct-DDW = The portion of total Fe in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

Fe-Seq2-Acetic = The portion of total Fe in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Fe-Direct-Acetic = The portion of total Fe in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

Fe-Seq3A-PCA = The portion of total Fe in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Fe-DirectPCA = The portion of total Fe in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

Fe-Seq3B-HCl = The portion of total Fe in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Fe-Direct-HCl = The portion of total Fe in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

Fe-Total = Total Fe in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

Zn-Seq1-DDW = The portion of total Zinc (Zn) in foliage that is solubilized by 3 freeze/thaw (F/T) cycles in double deionized water (DDW) in the first of a sequence of extractions in three solvents of increasing acidic strength measured by ICP-OES, µmol g⁻¹ FW

Zn-Direct-DDW = The portion of total Zn in foliage that is directly solubilized by 3 F/T cycles in DDW by ICP-OES, µmol g⁻¹ FW

Zn-Seq2-Acetic = The portion of total Zn in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Zn-Direct-Acetic = The portion of total Zn in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by ICP-OES, µmol g⁻¹ FW

Zn-Seq3A-PCA = The portion of total Zn in foliage that is solubilized by 3 F/T cycles in 5% Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Zn-DirectPCA = The portion of total Zn in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by ICP-OES, µmol g⁻¹ FW

Zn-Seq3B-HCl = The portion of total Zn in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid (HCl) in the third/final extraction in a sequence of three solvents of increasing acidic strength by ICP-OES, µmol g⁻¹ FW

Zn-Direct-HCl = The portion of total Zn in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by ICP-OES, µmol g⁻¹ FW

Zn-Total = Total Zn in foliage extracted in 15.8N Nitric acid by Microwave Digestion measured by ICP-OES, µmol g⁻¹ calc FW

Mal-Seq1-DDW = The portion of Malic acid (Mal) in foliage that is solubilized by 3 F/T cycles in double deionized water in the first of a sequence of extractions in three solvents of increasing acidic strength measured by HPLC, µmol g⁻¹ FW

Mal-Direct-DDW = Malic acid in foliage that is directly solubilized by 3 F/T cycles in DDW by HPLC, µmol g⁻¹ FW

Mal-Seq2-Acetic = The portion of Mal in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Mal-Direct-Acetic = Malic acid in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by HPLC, µmol g⁻¹ FW

Mal-Seq3A-PCA = The portion of Mal in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Mal-Direct-PCA = Malic acid in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by HPLC, µmol g⁻¹ FW

Mal-Seq3B-HCl = The portion of Mal in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Mal-Direct-HCl = Malic acid in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by HPLC, µmol g⁻¹ FW

Asc-Seq1-DDW = The portion of Ascorbic acid (Asc) in foliage that is solubilized by 3 F/T cycles in double deionized water in the first of a sequence of extractions in three solvents of increasing acidic strength measured by HPLC, µmol g⁻¹ FW

Asc-Direct-DDW = Ascorbic acid in foliage that is directly solubilized by 3 F/T cycles in DDW by HPLC, µmol g⁻¹ FW

Asc-Seq2-Acetic = The portion of Asc in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Asc-Direct-Acetic = Ascorbic acid in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by HPLC, µmol g⁻¹ FW

Asc-Seq3A-PCA = The portion of Asc in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Asc-Direct-PCA = Ascorbic acid in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by HPLC, µmol g⁻¹ FW

Asc-Seq3B-HCl = The portion of Asc in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Asc-Direct-HCl = Ascorbic acid in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by HPLC, µmol g⁻¹ FW

α-Keto-Seq1-DDW = The portion of alpha (α)-Ketoglutaric acid (α-Keto) in foliage that is solubilized by 3 F/T cycles in double deionized water in the first of a sequence of extractions in three solvents of increasing acidic strength measured by HPLC, µmol g⁻¹ FW

α-Keto-Direct-DDW = α-Ketoglutaric acid in foliage that is directly solubilized by 3 F/T cycles in DDW by HPLC, µmol g⁻¹ FW

α-Keto-Seq2-Acetic = The portion of α-Keto in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

α-Keto-Direct-Acetic = α-Ketoglutaric acid in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by HPLC, µmol g⁻¹ FW

α-Keto-Seq3A-PCA = The portion of α-Keto in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

α-Keto-Direct-PCA = α-Ketoglutaric acid in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by HPLC, µmol g⁻¹ FW

α-Keto-Seq3B-HCl = The portion of α-Keto in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

α-Keto-Direct-HCl = α-Ketoglutaric acid in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by HPLC, µmol g⁻¹ FW

Cit-Seq1-DDW = The portion of Citric acid (Cit) in foliage that is solubilized by 3 F/T cycles in double deionized water in the first of a sequence of extractions in three solvents of increasing acidic strength measured by HPLC, µmol g⁻¹ FW

Cit-Direct-DDW = Citric acid in foliage that is directly solubilized by 3 F/T cycles in DDW by HPLC, µmol g⁻¹ FW

Cit-Seq2-Acetic = The portion of Cit in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Cit-Direct-Acetic = Citric acid in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by HPLC, µmol g⁻¹ FW

Cit-Seq3A-PCA = The portion of Cit in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Cit-Direct-PCA = Citric acid in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by HPLC, µmol g⁻¹ FW

Cit-Seq3B-HCl = The portion of Cit in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Cit-Direct-HCl = Citric acid in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by HPLC, µmol g⁻¹ FW

Succ-Seq1-DDW = The portion of Succinic acid (Succ) in foliage that is solubilized by 3 F/T cycles in double deionized water in the first of a sequence of extractions in three solvents of increasing acidic strength measured by HPLC, µmol g⁻¹ FW

Succ-Direct-DDW = Succinic acid in foliage that is directly solubilized by 3 F/T cycles in DDW by HPLC, µmol g⁻¹ FW

Succ-Seq2-Acetic = The portion of Succ in foliage that is solubilized by 3 F/T cycles in 2N Acetic acid in the second of a sequence of extractions in three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Succ-Direct-Acetic = Succinic acid in foliage that is directly solubilized by 3 F/T cycles in 2N Acetic acid by HPLC, µmol g⁻¹ FW

Succ-Seq3A-PCA = The portion of Succ in foliage that is solubilized by 3 F/T cycles in 5% (0.83N) Perchloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Succ-Direct-PCA = Succinic acid in foliage that is directly solubilized by 3 F/T cycles in 5% PCA by HPLC, µmol g⁻¹ FW

Succ-Seq3B-HCl = The portion of Succ in foliage that is solubilized by 3 F/T cycles in 2N Hydrochloric acid in the third/final extraction in a sequence of three solvents of increasing acidic strength by HPLC, µmol g⁻¹ FW

Succ-Direct-HCl = Succinic acid in foliage that is directly solubilized by 3 F/T cycles in 2N HCl by HPLC, µmol g⁻¹ FW
Entity_and_Attribute_Detail_Citation:
Minocha, Rakesh; Chamberlain, Bradley; Long, Stephanie; Turlapati, Swathi A.; Quigley, Gloria. 2015. Extraction and estimation of the quantity of calcium oxalate crystals in the foliage of conifer and hardwood trees. Tree Physiology, 35(5): 574-580. https://doi.org/10.1093/treephys/tpv031

Minocha, Rakesh; Long, Stephanie; Thangavel, Palaniswamy; Minocha, Subhash C.; Eagar, Christopher; Driscoll, Charles T. 2010. Elevation dependent sensitivity of northern hardwoods to Ca addition at Hubbard Brook Experimental Forest, NH, USA. Forest Ecology and Management 260(12): 2115-2124. https://doi.org/10.1016/j.foreco.2010.09.002
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Distribution_Information:
Distributor:
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA Forest Service, Research and Development
Contact_Position: Research Data Archivist
Contact_Address:
Address_Type: mailing and physical
Address: 240 West Prospect Road
City: Fort Collins
State_or_Province: CO
Postal_Code: 80526
Country: USA
Contact_Voice_Telephone: see Contact Instructions
Contact Instructions: This contact information was current as of June 2022. For current information see Contact Us page on: https://doi.org/10.2737/RDS.
Resource_Description: RDS-2022-0057
Distribution_Liability:
Metadata documents have been reviewed for accuracy and completeness. Unless otherwise stated, all data and related materials are considered to satisfy the quality standards relative to the purpose for which the data were collected. However, neither the author, the Archive, nor any part of the federal government can assure the reliability or suitability of these data for a particular purpose. The act of distribution shall not constitute any such warranty, and no responsibility is assumed for a user's application of these data or related materials.

The metadata, data, or related materials may be updated without notification. If a user believes errors are present in the metadata, data or related materials, please use the information in (1) Identification Information: Point of Contact, (2) Metadata Reference: Metadata Contact, or (3) Distribution Information: Distributor to notify the author or the Archive of the issues.
Standard_Order_Process:
Digital_Form:
Digital_Transfer_Information:
Format_Name: CSV
Format_Version_Number: see Format Specification
Format_Specification:
Comma-separated values file
File_Decompression_Technique: Files zipped with 7-Zip 19.0
Digital_Transfer_Option:
Online_Option:
Computer_Contact_Information:
Network_Address:
Network_Resource_Name: https://doi.org/10.2737/RDS-2022-0057
Fees: None
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Metadata_Reference_Information:
Metadata_Date: 20220617
Metadata_Contact:
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA Forest Service, Northern Research Station
Contact_Person: Rakesh Minocha
Contact_Position: Plant Physiologist
Contact_Address:
Address_Type: mailing and physical
Address: 271 Mast Road
City: Durham
State_or_Province: NH
Postal_Code: 03824
Country: USA
Contact_Voice_Telephone: 603-868-7622
Contact_Electronic_Mail_Address: rakesh.minocha@usda.gov
Contact_Information:
Contact_Organization_Primary:
Contact_Organization: USDA Forest Service, Northern Research Station
Contact_Person: Stephanie Long
Contact_Position: Biological Technician
Contact_Address:
Address_Type: mailing and physical
Address: 271 Mast Road
City: Durham
State_or_Province: NH
Postal_Code: 03824
Country: USA
Contact_Voice_Telephone: 603-868-7623
Contact_Electronic_Mail_Address: stephanie.long2@usda.gov
Metadata_Standard_Name: FGDC Biological Data Profile of the Content Standard for Digital Geospatial Metadata
Metadata_Standard_Version: FGDC-STD-001.1-1999
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