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     data   graph     files  public [TP sediments with pretreatment] - Total phosphorus concentrations in NMR sediment
pretreatment 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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The Dataset's Variables and Attributes

Row Type Variable Name Attribute Name Data Type Value
attribute NC_GLOBAL access_formats String .htmlTable,.csv,.json,.mat,.nc,.tsv
attribute NC_GLOBAL acquisition_description String 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:

Prior to the extraction, we freeze-dried, ground and sieved sediment samples
to less than 125 \u03bcm (Ruttenberg 1992). For a given sample, we weighed
four sample replicates (2 g) and placed each in 250 mL HDPE bottles. Sodium
dithionite (F.W. 147.12 g/mol; 7.4 g) was added to each sample split, followed
by 200 mL of citrate-bicarbonate solution (pH 7.6). This step produces
effervescence, so the solution should be added slowly to the sample. We shook
samples for 8 h and then centrifuged them at 3,700 rpm for 15 min. We filtered
the supernatants with a 0.4 \u03bcm polycarbonate filter. We took 20 mL
aliquots from the filtrate for each sample split for MRP and total P analyses,
and kept them refrigerated until analysis within 24 h. We added 200 mL of
ultrapure water to the solid residue for each sample split as a wash step
after the above reductive step, shook samples for 2 h, and then centrifuged
them at 3,700 rpm for 15 min. We filtered the supernatants with 0.4 \u03bcm
polycarbonate filters and set aside 20 mL of filtrate from each sample split
for MRP and total P analyses. We then extracted the solid sample residues in
200 mL of sodium acetate buffer (pH 4.0) for 6 h. At the end of this
extraction step, we centrifuged the bottles at 3,700 rpm for 15 min, filtered
the supernatants with 0.4 \u03bcm polycarbonate filters and took a 20 mL
aliquot of filtrate from each sample split for MRP and total P analyses. We
added 200 mL of ultrapure water to the solid residue for each sample split as
a wash step, shook samples for 2 h, and then centrifuged them at 3,700 rpm for
15 min. We filtered the supernatants with 0.4 \u03bcm polycarbonate filters
and set aside 20 mL of filtrate from each sample split for MRP and total P
analyses. We repeated the water rinse step, and collected aliquots for MRP and
total P analyses as in the previous steps. The concentrations of TP were
determined as described below.

Solid sediment sample residues following the pretreatment described above 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).

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.

Total P 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 (1:20 dilution for
step 1, 1:10 for steps 2 \u2013 4). 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. The MRP concentrations were measured on a QuikChem 8000 automated
ion analyzer. Standards were prepared with the same solutions used for the
extraction step to minimize matrix effects on P measurements. Sediment
extracts and standards (0 \u2013 30 \u03bcM PO4) were diluted ten-fold to
prevent matrix interference with color development. The detection limit for P
on this instrument is 0.2 \u03bcM. We derived MUP concentrations by
subtracting MRP from total P concentrations.
attribute NC_GLOBAL awards_0_award_nid String 554980
attribute NC_GLOBAL awards_0_award_number String OCE-0939564
attribute NC_GLOBAL awards_0_data_url String http://www.nsf.gov/awardsearch/showAward?AWD_ID=0939564 (external link)
attribute NC_GLOBAL awards_0_funder_name String NSF Division of Ocean Sciences
attribute NC_GLOBAL awards_0_funding_acronym String NSF OCE
attribute NC_GLOBAL awards_0_funding_source_nid String 355
attribute NC_GLOBAL awards_0_program_manager String David L. Garrison
attribute NC_GLOBAL awards_0_program_manager_nid String 50534
attribute NC_GLOBAL cdm_data_type String Other
attribute NC_GLOBAL comment String TP sediments with pretreatment
PI: A. Paytan
Data Version 1: 2020-06-23
attribute NC_GLOBAL Conventions String COARDS, CF-1.6, ACDD-1.3
attribute NC_GLOBAL creator_email String info at bco-dmo.org
attribute NC_GLOBAL creator_name String BCO-DMO
attribute NC_GLOBAL creator_type String institution
attribute NC_GLOBAL creator_url String https://www.bco-dmo.org/ (external link)
attribute NC_GLOBAL data_source String extract_data_as_tsv version 2.3 19 Dec 2019
attribute NC_GLOBAL dataset_current_state String Final and no updates
attribute NC_GLOBAL date_created String 2020-03-02T22:10:22Z
attribute NC_GLOBAL date_modified String 2020-07-02T21:01:27Z
attribute NC_GLOBAL defaultDataQuery String &time<now
attribute NC_GLOBAL doi String 10.26008/1912/bco-dmo.805226.1
attribute NC_GLOBAL infoUrl String https://www.bco-dmo.org/dataset/805226 (external link)
attribute NC_GLOBAL institution String BCO-DMO
attribute NC_GLOBAL instruments_0_acronym String FIA
attribute NC_GLOBAL instruments_0_dataset_instrument_nid String 805235
attribute NC_GLOBAL instruments_0_description String 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.
attribute NC_GLOBAL instruments_0_instrument_external_identifier String https://vocab.nerc.ac.uk/collection/L05/current/LAB36/ (external link)
attribute NC_GLOBAL instruments_0_instrument_name String Flow Injection Analyzer
attribute NC_GLOBAL instruments_0_instrument_nid String 657
attribute NC_GLOBAL instruments_0_supplied_name String QuikChem 8000 automated ion analyzer
attribute NC_GLOBAL keywords String 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, step
attribute NC_GLOBAL license String https://www.bco-dmo.org/dataset/805226/license (external link)
attribute NC_GLOBAL metadata_source String https://www.bco-dmo.org/api/dataset/805226 (external link)
attribute NC_GLOBAL param_mapping String {'805226': {}}
attribute NC_GLOBAL parameter_source String https://www.bco-dmo.org/mapserver/dataset/805226/parameters (external link)
attribute NC_GLOBAL people_0_affiliation String University of California-Santa Cruz
attribute NC_GLOBAL people_0_affiliation_acronym String UC Santa Cruz
attribute NC_GLOBAL people_0_person_name String Adina Paytan
attribute NC_GLOBAL people_0_person_nid String 50821
attribute NC_GLOBAL people_0_role String Principal Investigator
attribute NC_GLOBAL people_0_role_type String originator
attribute NC_GLOBAL people_1_affiliation String University of California-Santa Cruz
attribute NC_GLOBAL people_1_affiliation_acronym String UC Santa Cruz
attribute NC_GLOBAL people_1_person_name String Dr Delphine Defforey
attribute NC_GLOBAL people_1_person_nid String 664058
attribute NC_GLOBAL people_1_role String Co-Principal Investigator
attribute NC_GLOBAL people_1_role_type String originator
attribute NC_GLOBAL people_2_affiliation String Woods Hole Oceanographic Institution
attribute NC_GLOBAL people_2_affiliation_acronym String WHOI BCO-DMO
attribute NC_GLOBAL people_2_person_name String Amber D. York
attribute NC_GLOBAL people_2_person_nid String 643627
attribute NC_GLOBAL people_2_role String BCO-DMO Data Manager
attribute NC_GLOBAL people_2_role_type String related
attribute NC_GLOBAL project String Marine Sediment Analysis 31P NMR
attribute NC_GLOBAL projects_0_acronym String Marine Sediment Analysis 31P NMR
attribute NC_GLOBAL projects_0_description String 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
attribute NC_GLOBAL projects_0_geolocation String Equatorial Pacific, California Margin, Arctic Ocean
attribute NC_GLOBAL projects_0_name String A new marine sediment sample preparation scheme for solution 31P NMR analysis
attribute NC_GLOBAL projects_0_project_nid String 664054
attribute NC_GLOBAL publisher_name String Biological and Chemical Oceanographic Data Management Office (BCO-DMO)
attribute NC_GLOBAL publisher_type String institution
attribute NC_GLOBAL sourceUrl String (local files)
attribute NC_GLOBAL standard_name_vocabulary String CF Standard Name Table v55
attribute NC_GLOBAL summary String Total phosphorus concentrations in nuclear magnetic resonance (NMR) sediment pretreatment extracts from samples collected during cruises in the Arctic Ocean, California Margin, and Equatorial Pacific from 1992-1998.
attribute NC_GLOBAL title String [TP sediments with pretreatment] - Total phosphorus concentrations in NMR sediment pretreatment 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)
attribute NC_GLOBAL version String 1
attribute NC_GLOBAL xml_source String osprey2erddap.update_xml() v1.5
variable Extract   String  
attribute Extract bcodmo_name String sample_descrip
attribute Extract description String Extract solution
attribute Extract long_name String Extract
attribute Extract units String unitless
variable Step   String  
attribute Step bcodmo_name String sample_descrip
attribute Step description String Step in the sequential extraction scheme (1-4)
attribute Step long_name String Step
attribute Step units String unitless
variable Dilution   String  
attribute Dilution bcodmo_name String sample_descrip
attribute Dilution description String Sample dilution
attribute Dilution long_name String Dilution
attribute Dilution units String unitless
variable Sample_ID   String  
attribute Sample_ID bcodmo_name String sample
attribute Sample_ID description String Sample ID, unique sample identifier
attribute Sample_ID long_name String Sample ID
attribute Sample_ID nerc_identifier String https://vocab.nerc.ac.uk/collection/P02/current/ACYC/ (external link)
attribute Sample_ID units String unitless
variable Analyte_Name   String  
attribute Analyte_Name bcodmo_name String sample_descrip
attribute Analyte_Name description String Element analyzed
attribute Analyte_Name long_name String Analyte Name
attribute Analyte_Name units String unitless
variable Int_Corr   String  
attribute Int_Corr bcodmo_name String unknown
attribute Int_Corr description String Intensity (corrected)
attribute Int_Corr long_name String Int Corr
attribute Int_Corr units String unitless
variable RSD_Corr_Int   double  
attribute RSD_Corr_Int _FillValue double NaN
attribute RSD_Corr_Int actual_range double -0.001279317841, 1840331.376
attribute RSD_Corr_Int bcodmo_name String unknown
attribute RSD_Corr_Int description String Relative standard deviation (RSD) of corrected intensity
attribute RSD_Corr_Int long_name String RSD Corr Int
attribute RSD_Corr_Int units String unitless
variable Conc_Calib   double  
attribute Conc_Calib _FillValue double NaN
attribute Conc_Calib actual_range double -0.03697121872, 192.5176767
attribute Conc_Calib bcodmo_name String P
attribute Conc_Calib description String Calibrated concentration of total phosphorous
attribute Conc_Calib long_name String Conc Calib
attribute Conc_Calib units String parts per million (ppm)

The information in the table above is also available in other file formats (.csv, .htmlTable, .itx, .json, .jsonlCSV1, .jsonlCSV, .jsonlKVP, .mat, .nc, .nccsv, .tsv, .xhtml) via a RESTful web service.


 
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