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Dataset Title:  [TP metals sediments with no pretreatment] - Total phosphorus and metal
concentrations from sediment extracts from samples collected during cruises in
the Arctic Ocean, California Margin, and Equatorial Pacific from 1992-1998 (A
new marine sediment sample preparation scheme for solution 31P NMR analysis)
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Institution:  BCO-DMO   (Dataset ID: bcodmo_dataset_805216)
Information:  Summary ? | License ? | ISO 19115 | Metadata | Background (external link) | Files | Make a graph
 
Variable ?   Optional
Constraint #1 ?
Optional
Constraint #2 ?
   Minimum ?
 
   Maximum ?
 
 Type (unitless) ?          "NMR extract"    "Residue"
 Extract (unitless) ?          "H2SO4"    "NaOH-EDTA"
 Dilution (unitless) ?          "1:10"    "None"
 Sample_ID (unitless) ?          "1 ppm standard"    "blank"
 Analyte_Name (unitless) ?          "Al 308.215"    "Zn 206.200"
 Int_Corr (unknown) ?          -483.6220124    2.858785422E7
 RSD_Corr_Int (unknown) ?          0.1423364373    104133.066
 Conc_Calib (parts per million (ppm)) ?          -0.1235444804    205.1316777
 
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The Dataset Attribute Structure (.das) for this Dataset

Attributes {
 s {
  Type {
    String bcodmo_name "sample_descrip";
    String description "Type (NMR extract or Residue)";
    String long_name "Type";
    String units "unitless";
  }
  Extract {
    String bcodmo_name "sample_descrip";
    String description "Extraction solution";
    String long_name "Extract";
    String units "unitless";
  }
  Dilution {
    String bcodmo_name "treatment";
    String description "Sample dilution or \"None\"";
    String long_name "Dilution";
    String units "unitless";
  }
  Sample_ID {
    String bcodmo_name "sample";
    String description "Unique sample identifier";
    String long_name "Sample ID";
    String nerc_identifier "https://vocab.nerc.ac.uk/collection/P02/current/ACYC/";
    String units "unitless";
  }
  Analyte_Name {
    String bcodmo_name "sample_descrip";
    String description "Element analyzed";
    String long_name "Analyte Name";
    String units "unitless";
  }
  Int_Corr {
    Float64 _FillValue NaN;
    Float64 actual_range -483.6220124, 2.858785422e+7;
    String bcodmo_name "unknown";
    String description "Intensity (corrected)";
    String long_name "Int Corr";
    String units "unknown";
  }
  RSD_Corr_Int {
    Float64 _FillValue NaN;
    Float64 actual_range 0.1423364373, 104133.066;
    String bcodmo_name "standard deviation";
    String description "Relative standard deviation";
    String long_name "RSD Corr Int";
    String units "unknown";
  }
  Conc_Calib {
    Float64 _FillValue NaN;
    Float64 actual_range -0.1235444804, 205.1316777;
    String bcodmo_name "P";
    String description "Calibrated concentration of total phosphorous";
    String long_name "Conc Calib";
    String units "parts per million (ppm)";
  }
 }
  NC_GLOBAL {
    String access_formats ".htmlTable,.csv,.json,.mat,.nc,.tsv";
    String acquisition_description 
"Location:
 
Arctic Ocean: P-1-94-AR P21, 84o5' N, 174o58' W  
 California margin: W-2-98-NC TF1, 41o5' N, 125o1' W  
 Equatorial Pacific: TT013-06MC, 12o00' S, 134o56' W
 
Methodology:
 
Solid sediment samples were transferred to two 50 mL centrifuge tubes (2
sample replicates combined per tube). We added 20 mL of 0.25 M NaOH + 0.05 M
Na2EDTA solution to each tube, vortexed until all sediment was resuspended and
then shook samples for 6 h at room temperature (Cade-Menun et al. 2005). We
used a solid to solution ratio of 1:5 for this step to minimize the amount of
freeze-dried material that will need to be dissolved for the 31P NMR
experiments. Large amounts of salts from the NaOH-EDTA concentrated in NMR
samples lead to higher viscosity and increase line broadening on NMR spectra
(Cade-Menun and Liu 2013). We chose an extraction time of 6 h to improve total
P recovery while limiting the degradation of natural P compounds in the
sample. At the end of the extraction, samples were centrifuged at 3,700 rpm
for 15 min and supernatants decanted into 50 mL centrifuge tubes. We collected
a 500 \\u03bcL aliquot from each sample, which we diluted with 4.5 mL of
ultrapure water. These were refrigerated until analysis for total P content on
the ICP-OES. The sample residues and supernatants were frozen on a slant to
maximize the exposed surface area during the lyophilization step; this was
done immediately after the removal of the 500 \\u03bcL aliquot. Once completely
frozen, the uncapped tubes containing supernatants and residues were freeze-
dried over the course of 48 h. Each tube was covered with parafilm with small
holes from a tack to minimize contamination. Freeze-dried supernatants from
identical sample splits were combined and dissolved in 500 \\u03bcL each of
ultrapure water, D2O, NaOH-EDTA and 10 M NaOH prior to 31P NMR analysis. The
D2O is required as signal lock in the spectrometer (Cade-Menun and Liu 2013).
Sample pH was maintained at a pH > 12 to optimize peak separation (Cade-Menun
2005; Cade-Menun and Liu 2013). Sample pH was assessed with a glass electrode,
and verified with pH paper to account for the alkaline error caused by the
high salt content of our samples (Covington 1985).
 
Total P and metal concentrations in sediment extracts were measured using
inductively coupled plasma optical emission spectroscopy (ICP-OES). Standards
were prepared with the same solutions as those used for the extraction
procedure in order to minimize matrix effects on P measurements. Sediment
extracts and standards (0 \\u03bcM, 3.2 \\u03bcM, 32 \\u03bcM and 320 \\u03bcM)
were diluted to lower salt content to prevent salt buildup on the nebulizer.
Concentration data from both wavelengths (213 nm and 214 nm) were averaged to
obtain extract concentrations for each sample. The detection limit for P on
this instrument for both wavelengths is 0.4 \\u03bcM.
 
Freeze-dried sample residues were ashed in crucibles at 550oC for 2 h and then
extracted in 25 mL of 0.5 M sulfuric acid for 16 h (Olsen and Sommers 1982;
Cade-Menun and Lavkulich 1997). We centrifuged samples at 3,700 rpm for 15
min, filtered supernatants with 0.4 \\u03bcm polycarbonate filters, and
measured P content on an ICP-OES.";
    String awards_0_award_nid "554980";
    String awards_0_award_number "OCE-0939564";
    String awards_0_data_url "http://www.nsf.gov/awardsearch/showAward?AWD_ID=0939564";
    String awards_0_funder_name "NSF Division of Ocean Sciences";
    String awards_0_funding_acronym "NSF OCE";
    String awards_0_funding_source_nid "355";
    String awards_0_program_manager "David L. Garrison";
    String awards_0_program_manager_nid "50534";
    String cdm_data_type "Other";
    String comment 
"TP metals sediments with no pretreatment 
  PI: Adina Paytan 
  Data Version 1: 2020-06-23";
    String Conventions "COARDS, CF-1.6, ACDD-1.3";
    String creator_email "info@bco-dmo.org";
    String creator_name "BCO-DMO";
    String creator_type "institution";
    String creator_url "https://www.bco-dmo.org/";
    String data_source "extract_data_as_tsv version 2.3  19 Dec 2019";
    String dataset_current_state "Final and no updates";
    String date_created "2020-03-02T22:08:39Z";
    String date_modified "2020-07-02T21:01:48Z";
    String defaultDataQuery "&time<now";
    String doi "10.26008/1912/bco-dmo.805216.1";
    String history 
"2024-11-15T06:24:02Z (local files)
2024-11-15T06:24:02Z https://erddap.bco-dmo.org/erddap/tabledap/bcodmo_dataset_805216.html";
    String infoUrl "https://www.bco-dmo.org/dataset/805216";
    String institution "BCO-DMO";
    String instruments_0_acronym "FIA";
    String instruments_0_dataset_instrument_nid "805225";
    String instruments_0_description "An instrument that performs flow injection analysis. Flow injection analysis (FIA) is an approach to chemical analysis that is accomplished by injecting a plug of sample into a flowing carrier stream. FIA is an automated method in which a sample is injected into a continuous flow of a carrier solution that mixes with other continuously flowing solutions before reaching a detector. Precision is dramatically increased when FIA is used instead of manual injections and as a result very specific FIA systems have been developed for a wide array of analytical techniques.";
    String instruments_0_instrument_external_identifier "https://vocab.nerc.ac.uk/collection/L05/current/LAB36/";
    String instruments_0_instrument_name "Flow Injection Analyzer";
    String instruments_0_instrument_nid "657";
    String instruments_0_supplied_name "QuikChem 8000 automated ion analyzer";
    String keywords "analyte, Analyte_Name, bco, bco-dmo, biological, calib, chemical, conc, Conc_Calib, corr, data, dataset, dilution, dmo, erddap, extract, int, Int_Corr, management, name, oceanography, office, preliminary, rsd, RSD_Corr_Int, sample, Sample_ID, type";
    String license "https://www.bco-dmo.org/dataset/805216/license";
    String metadata_source "https://www.bco-dmo.org/api/dataset/805216";
    String param_mapping "{'805216': {}}";
    String parameter_source "https://www.bco-dmo.org/mapserver/dataset/805216/parameters";
    String people_0_affiliation "University of California-Santa Cruz";
    String people_0_affiliation_acronym "UC Santa Cruz";
    String people_0_person_name "Adina Paytan";
    String people_0_person_nid "50821";
    String people_0_role "Principal Investigator";
    String people_0_role_type "originator";
    String people_1_affiliation "University of California-Santa Cruz";
    String people_1_affiliation_acronym "UC Santa Cruz";
    String people_1_person_name "Dr Delphine Defforey";
    String people_1_person_nid "664058";
    String people_1_role "Co-Principal Investigator";
    String people_1_role_type "originator";
    String people_2_affiliation "Woods Hole Oceanographic Institution";
    String people_2_affiliation_acronym "WHOI BCO-DMO";
    String people_2_person_name "Amber D. York";
    String people_2_person_nid "643627";
    String people_2_role "BCO-DMO Data Manager";
    String people_2_role_type "related";
    String project "Marine Sediment Analysis 31P NMR";
    String projects_0_acronym "Marine Sediment Analysis 31P NMR";
    String projects_0_description 
"We developed and tested a new approach to prepare marine sediment samples for solution 31P nuclear magnetic resonance spectroscopy (31P NMR). This approach addresses the effects of sample pretreatment on sedimentary P composition and increases the signal of low abundance P species in 31P NMR spectra by removing up the majority inorganic P  from sediment samples while causing minimal alteration of the chemical structure of organic P compounds. The method was tested on natural marine sediment samples from different localities (Equatorial Pacific, California Margin and Arctic Ocean) with high inorganic P content, and allowed for the detection of low abundance P forms in samples for which only an orthophosphate signal could be resolved with an NaOH-EDTA extraction alone. This new approach will allow the use of 31P NMR on samples for which low organic P concentrations previously hindered the use of this tool, and will help answer longstanding question regarding the fate of organic P in marine sediments. We developed and tested a new approach to prepare marine sediment samples for solution 31P nuclear magnetic resonance spectroscopy (31P NMR). This approach addresses the effects of sample pretreatment on sedimentary P composition and increases the signal of low abundance P species in 31P NMR spectra by removing up the majority inorganic P  from sediment samples while causing minimal alteration of the chemical structure of organic P compounds. The method was tested on natural marine sediment samples from different localities (Equatorial Pacific, California Margin and Arctic Ocean) with high inorganic P content, and allowed for the detection of low abundance P forms in samples for which only an orthophosphate signal could be resolved with an NaOH-EDTA extraction alone. This new approach will allow the use of 31P NMR on samples for which low organic P concentrations previously hindered the use of this tool, and will help answer longstanding question regarding the fate of organic P in marine sediments. 
NSF C-DEBI Award #156246 to Dr. Adina Paytan
NSF C-DEBI Award #157598 to Dr. Delphine Defforey";
    String projects_0_geolocation "Equatorial Pacific, California Margin, Arctic Ocean";
    String projects_0_name "A new marine sediment sample preparation scheme for  solution 31P NMR analysis";
    String projects_0_project_nid "664054";
    String publisher_name "Biological and Chemical Oceanographic Data Management Office (BCO-DMO)";
    String publisher_type "institution";
    String sourceUrl "(local files)";
    String standard_name_vocabulary "CF Standard Name Table v55";
    String summary "Total phosphorus and metal concentrations from sediment extracts from samples collected during cruises in the Arctic Ocean, California Margin, and Equatorial Pacific from 1992-1998.";
    String title "[TP metals sediments with no pretreatment] - Total phosphorus and metal concentrations from sediment extracts from samples collected during cruises in the Arctic Ocean, California Margin, and Equatorial Pacific from 1992-1998 (A new marine sediment sample preparation scheme for  solution 31P NMR analysis)";
    String version "1";
    String xml_source "osprey2erddap.update_xml() v1.5";
  }
}

 

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