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Date Created: 08/12/14
Method 4400 Determination of Carbon and Nitrogen in Sediments and Particulates of EstuarineCoastal Waters Using Elemental Analysis Carl F Zimmermann Carolyn W Keefe University of Maryland System Center for Environmental Estuarine Studies Chesapeake Biological Laboratory Solomns MD 206880038 and Jerry Bashe Technology Applications Inc 26 W Martin Luther King Drive Cincinnati OH 45219 Revision 14 September 1997 Work Assignment Manager Elizabeth J Arar National Exposure Research Laboratory Office of Research and Development US Environmental Protection Agency Cincinnati Ohio 45268 44001 Method 4400 Determination of Carbon and Nitrogen in Sediments and Particulates of EstuarineCoastal Waters Using Elemental Analysis 10 Scope and Application 11 Elemental analysis is used to determine particu late carbon PC and particulate nitrogen PN in estua rine and coastal waters and sediment The method measures the total carbon and nitrogen irrespective of source inorganic or organic Chemical Abstracts Service Analyte Registry Numbers CASRN Carbon 7440440 Nitrogen 1333740 12 The need to qualitatively or quantitatively deter mine the particulate organic fraction from the total particulate carbon and nitrogen depends on the data quality objectives of the study Section 114 outlines procedures to ascertain the organicinorganic particulate ratio The method performance presented in the method was obtained on particulate samples with greater than 80 organic content Performance on samples with a greater proportion of particulate inorganic versus organic carbon and nitrogen has not been investigated 13 Method detection limits M DLs of 105 ugL and 623 ugL for PN and PC respectively were obtained for a 200mL sample volume Sediment MDLs of PN and PC are 84 mgkg and 1300 mgkg respectively for a sediment sample weight of 1000 mg The method has been determined to be linear to 4800 ug of C and 700 ug of N in a sample Multilaboratory study validation data are in Section 13 14 This method should be used by analysts experi enced in the theory and application of elemental analysis A minimum of 6 months experience with an elemental analyzer is recommended 15 Users of the method data should set the data quality objectives prior to analysis Users of the method must document and have on file the required initial demonstration of performance data described in Section 92 prior to using the method for analysis 20 Summary of Method 21 An accurately measured amount of particulate matter from an estuarine water sample or an accurately weighed dried sediment sample is combusted at 975 C using an elemental analyzer The combustion products are passed over a copper reduction tube to convert the Revision 14 September 1997 oxides of N into molecular N Carbon dioxide water vapor and N are homogeneously mixed at a known volume temperature and pressure The mixture is released to a series of thermal conductivity detectorstraps measuring in turn by difference hydrogen as water vapor C as carbon dioxide and N as N2 Inorganic and organic C may be determined by two methods which are also presented 30 Definitions 31 Sediment Sample A fluvial sand or humic sample matrix exposed to a marine brackish or fresh water environment It is limited to that portion which may be passed through a number 10 sieve or a 2mm mesh sieve 32 Material Safety Data Sheet MSDS Written information provided by vendors concerning a chemica s toxicity health hazards physical properties fire and reactivity data including storage spill and handling pre cau ons 33 Instrument Detection Limit IDL The mini mum quantity of analyte or the concentration equivalent which gives an analyte signal equal to three times the standard deviation of the background signal at the se lected wavelength mass retention time absorbance line etc 34 Method Detection Limit MDL The minimum concentration of an analyte that can be identified mea sured and reported with 99 confidence that the analyte concentration is greater than zero 35 Linear Dynamic Range LDR The absolute quantity over which the instrument response to an analyte is nean 36 Calibration Standard CAL An accurately weighed amount of a certified chemical used to calibrate the instrument response with respect to analyte mass 37 Conditioner A standard chemical which is not necessarily accurately weighed that is used to coat the surfaces of the instrument with the analytes water vapor carbon dioxide and nitrogen 38 External Standards ES A pure anaytes that is measured in an experiment separate from the experiment used to measure the anaytes in the sample The signal observed for a known quantity of the pure external standards is used to calibrate the instrument 44002 response for the corresponding analytes The instru ment response is used to calculate the concentrations of the analytes in the sample 39 Response Factor RF The ratio of the re sponse of the instrument to a known amount of analyte 310 Laboratory Reagent Blank LRB A blank matrix ie a precombusted filter or sediment capsule that is treated exactly as a sample including exposure to all glassware equipment solvents and reagents that are used with other samples The LRB is used to determine if method analytes or other interferences are present in the laboratory environment the reagents or the appa ratus 311 Field Reagent Blank FRB An aliquot of reagent water or other blank matrix that is placed in a sample container in the laboratory and treated as a sample in all respects including shipment to the sampling site exposure to sampling site conditions storage preservation and all analytical procedures The purpose of the FRB is to determine if method analytes or other interferences are present in the field environment 3 12 Laboratory Duplicates LD1 and LD2 Two aliquots of the same sample taken in the laboratory and analyzed separately with identical procedures Analyses of LD1 and LD2 indicate precision associated with labo ratory procedures but not with sample collection preser vation or storage procedures 313 Field Duplicates FD1 and FD2 Two sepa rate samples collected at the same time and place under identical circumstances and treated exactly the same throughout field and laboratory procedures Analyses of FD1 and FD2 give a measure of the precision associated with sample collection preservation and storage as well as with laboratory procedures 3 14 Laboratory Fortified Blank LFB An aliquot of reagent water or other blank matrices to which known quantities of the method analytes are added in the laboratory The LFB is analyzed exactly like a sample and its purpose is to determine whether the method is in control and whether the laboratory is capable of making accurate and precise measurements 3 15 Laboratory Fortified Sample Matrix LFM An aliquot of an environmental sample to which known quantities of the method analytes are added in the laboratory The LFM is analyzed exactly like a sample and its purpose is to determine whether the sample matrix contributes bias to the analytical results The background concentrations of the analytes in the sample matrix must be determined in a separate aliquot and the measured values in the LFM corrected for background concentra tions 3 16 Standard Reference Material SRM Material 44003 which has been certified for specific analytes by a variety of analytical techniques andor by numerous laboratories using similar analytical techniques These may consist of pure chemicals buffers or compositional standards These materials are used as an indication of the accuracy of a specific analytical technique 317 Quality Control Sample QCS A solution of method analytes of known concentrations which is used to fortify an aliquot of LRB or sample matrix The QCS is obtained from a source external to the laboratory and different from the source of calibration standards It is used to check laboratory performance with externally prepared test materials 40 interferences 41 There are no known interferences for estua rinecoastal water or sediment samples The presence of C and N compounds on laboratory surfaces on fingers in detergents and in dust necessitates the utilization of careful techniques ie the use of forceps and gloves to avoid contamination in every portion of this procedure 50 Safety 51 The toxicity or carcinogenicity of each reagent used in this method has not been fully established Each chemical should be regarded as a potential health hazard and exposure to these compounds should be as low as reasonably achievable Each laboratory is responsible for maintaining a current awareness file of OSHA regulations regarding the safe handling of the chemicals specified in this method2 5 A reference file of material safety data sheets MSDS should also be made available to all personnel involved in the chemical analysis 52 The acidification of samples containing reactive materials may result in the release of toxic gases such as cyanides or sulfides Acidification of samples should be done in a fume hood 53 All personnel handling environmental samples known to contain or to have been in contact with human waste should be immunized against known disease causative agents 54 Although most instruments are adequately shielded it should be remembered that the oven tem peratures are extremely high and that care should be taken when working near the instrument to prevent possible burns 55 It is the responsibility of the user of this method to comply with relevant disposal and waste regulations For guidance see Sections 140 and 150 Revision 14 September 1997 60 Apparatus and Equipment 6 1 Elemental Analyzer 611 An elemental analyzer capable of maintaining a combustion temperature of 975 C and analyzing particu late samples and sediment samples for elemental C and N The Leeman Labs Model 240 XA Elemental Analyzer was used to produce the data presented in this method 62 A gravity convection drying oven Capable of maintaining 103105 C for extended periods of time 63 Muffle furnace Capable of maintaining 875 C Jr 15 C 64 Ultramicro balance Capable of accurately weighing to 01 pg Desiccant should be kept in the weighing chamber to prevent hygroscopic effects 65 Vacuum pump or source capable of maintaining up to 10 in Hg of vacuum 66 Mortar and pestle 67 Desiccator glass 68 Freezer capable of maintaining 20 C 1 5 C 69 47mm or 25mm vacuum filter apparatus made up of a glass filter tower fritted glass disk base and 2L vacuum flask 610 13mm Swinlok filter holder 6 1 1 Teflontipped flat blade forceps 612 Labware All reusable labware glass quartz polyethylene PTFE FEP etc should be sufficiently clean for the task objectives Several procedures found to provide clean labware include washing with a detergent solution rinsing with tap water soaking for 4 hr or more in 20 vv HCI rinsing with reagent water and storing clean All traces of organic material must be removed to prevent CN contamination 6121 Glassware Volumetric flasks graduated cylinders vials and beakers 6122 Vacuum filter flasks 250 mL and 2 L glass 6123 Funnel 64 mm id polyethylene 6124 Syringes 60mL glass 70 Reagents and Standards 71 Reagents may contain elemental impurities which affect analytical data Highpurity reagents that conform Revision 14 September 1997 to the American Chemical Society specifications should be used whenever possible If the purity of a reagent is in question analyze for contamination The acid used for this method must be of reagent grade purity or equivalent A suitable acid is available from a number of manu facturers 72 Hydrochloric acid concentrated sp gr 119 HCI 73 Acetanilide 999 purity C8H9NO CASRN 103844 74 Blanks Three blanks are used for the analysis Two blanks are instrument related The instrument zero response ZN is the background response of the instru ment without sample holding devices such as capsules and sleeves The instrument blank response BN is the response of the instrument when the sample capsule sleeve and ladle are inserted for analysis without standard or sample The BN is also the laboratory reagent blank LRB for sediment samples The LRB for water samples includes the capsule sleeve ladle and a precombusted filter without standard or sample These blanks are subtracted from the uncorrected instrument response used to calculate concentration in Sections 123 and 124 741 Laboratory fortified blank LFB The third blank is the laboratory fortified blank For sediment analysis add a weighed amount of acetanilide in an aluminum capsule and analyze for PC and PN Section 932 For aqueous samples place a weighed amount of acetanilide on a glass fiber filter the same size as used for the sample filtration Analyze the fortified filter for PC and PN Section 932 75 Quality Control Sample QCS For this meth od the QCS can be any assayed and certified sediment or particulate sample which is obtained from an external source The Canadian Reference Material BCSS1 is just such a material and was used in this capacity for the data presented in this method The percent PC has been certified in this material but percent PN has not 80 Sample Collection Preservation and Storage 8 1 Water Sample Collection Samples collected for PC and PN analyses from estuarinecoastal waters are normally collected from a ship using one of two methods hydrocast or submersible pump systems Fol low the recommended sampling protocols associated with the method used Whenever possible immediately filter the samples as described in Section 1111 Store the filtered sample pads by freezing at 20 C or storing in a desiccator after drying at 103105 C for 24 hr No significant difference has been noted in comparing the two storage procedures for a time period of up to 100 days If storage of the water sample is necessary place 44004 the sample into a clean amber bottle and store at 4 C until filtration is done 811 The volume of water sample collected will vary with the type of sample being analyzed Table 1 provides a guide for a number of matrices of interest If the matrix cannot be classified by this guide collect 2 x 1L of water from each site A minimum filtration volume of 200 mL is recommended 82 Sediment Sample Collection Estua rinecoastal sediment samples are collected with benthic samplers The type of sampler used will depend on the type of sample needed by the dataquality objectives7 Store the wet sediment in a clean jar and freeze at 20 C until ready for analysis 821 The amount of sediment collected will depend on the sample matrix and the elemental analyzer used A minimum of 10 g is recommended 90 Quality Control 91 Each laboratory using this method is required to operate a formal quality control QC program The minimum requirements of this program consist of an initial demonstration of laboratory capability and the continued analysis of laboratory reagent blanks laboratory dupli cates field duplicates and calibration standards analyzed as samples as a continuing check on performance The laboratory is required to maintain performance records that define the quality of data thus generated 92 Initial Demonstration of Performance Mandatory 921 The initial demonstration of performance is used to characterize instrument performance MDLs linear dy namic range and laboratory performance analysis of QC samples prior to the analyses conducted by this method 922 Linear dynamic range LDFI The upper limit of the LDR must be established by determining the signal responses from a minimum of three different concentra tion standards across the range one of which is close to the upper limit of the LDR Determined LDRs must be documented and kept on file The LDR which may be used for the analysis of samples should be judged by the analyst from the resulting data The upper LDR limit should be an observed signal no more than 10 below the level extrapolated from the lower standards Deter mined sample analyte concentrations that are 90 and above the upper LDR must be reduced in mass and reanalyzed New LDRs should be determined whenever there is a significant change in instrument response and for those analytes that periodically approach the upper LDR limit every 6 months or whenever there is a change in instrument analytical hardware or operating conditions 44005 923 Quality control sample 208 Section 75 When beginning the use of this method on a quarterly basis or as required to meet data quality needs verify the calibration standards and acceptable instrument perfor mance with the analyses of a QCS If the determined concentrations are not within 1 5 of the stated values performance of the determinative step of the method is unacceptable The source of the problem must be iden tified and corrected before either proceeding with the initial determination of MDLs or continuing with analyses 924 Method detection limits MDLs MDLs should be established for PC and PN using a low level estuarine water sample typically three to five times higher than the estimated MDL The same procedure should be followed for sediments To determine MDL values analyze seven replicate aliquots of water or sediment and process through the entire analytical procedure Section 11 These replicates should be randomly distributed through out a group of typical analyses Perform all calculations defined in the method Section 12 and report the con centration values in the appropriate units Calculate the MDL as follows MDL t x s Standard deviation of the repli cate analyses where S Student s tvalue for n1 degrees of freedom at the 99 confidence limit t 3143 for six degrees of freedom MDLs should be determined whenever a significant change in instrumental response change of operator or a new matrix is encountered 93 Assessing Laboratory Performance Mandatory 93 1 Laboratory reagent blank LRB The laboratory must analyze at least one LRB Section 310 with each batch of 20 or fewer samples of the same matrix LRB data are used to assess contamination from the labora tory environment LRB values that exceed the MDL indicate laboratory or reagent contamination When LRB values constitute 10 or more of the analyte level deter mined for a sample fresh samples or field duplicates of the samples must be prepared and analyzed again after the source of contamination has been corrected and acceptable LRB values have been obtained For aque ous samples the LRB is a precombusted filter of the same type and size used for samples Revision 14 September 1997 932 Laboratory fortified blank LFB The laboratory must analyze at least one LFB Section 741 with each batch of samples Calculate accuracy as percent recov ery If the recovery of any analyte falls outside the required control limits of 85115 that analyte is judged out of control and the source of the problem should be identified and resolved before continuing analyses 933 The laboratory must use LFB analyses data to assess laboratory performance against the required con trol limits of 85115 Section 932 When sufficient internal performance data become available usually a minimum of 2030 analyses optional control limits can be developed from the percent mean recovery x and the standard deviation S of the mean recovery These data can be used to establish the upper and lower control limits as follows Upper Control Limit x 3S Lower Control Limit x 3S The optional control limits must be equal to or better than the required control limits of 851 15 After each five to ten new recovery measurements new control limits can be calculated using only the most recent 2030 data points Also the standard deviation S data should be used to establish an ongoing precision statement for the level of concentrations included in the LFB These data must be kept on file and be available for review 94 Assessing Analyte Recovery and Data Quality 941 Percent recoveries cannot be readily obtained from particulate samples Consequently accuracy can only be assessed by analyzing check standards as samples and quality control samples QCS The use of laboratory fortified matrix samples has not been as sessed 100 Calibration and Standardization 101 Calibration After following manufacturer s installation and temperature stabilization procedures daily calibration procedures must be performed and evaluated before sample analysis may begin Single point or standard curve calibrations are possible de pending on instrumentation 1011 Establish single response factors RF for each element CH and N by analyzing three weighed portions of calibration standard acetanilide The mass of calibration standard should provide a response within 20 of the response expected for the samples being analyzed Calculate the RF for each element using the following formula Revision 14 September 1997 Response factor uvug RNZNBN WTN where RN Average instrument response to standard uv ZN Instrument zero response uv BN Instrument blank response uv and WTN MNaAWMW where M The mass of standard material in 119 Na Number of atoms of C N or H in a molecule of standard material AW Atomic weight of C 1201 N 1401 or H 101 MW Molecular weight of standard material 1352 for acetanilide If instrument response is in units other than uv then change the formula accordingly 1012 For standard curve preparation the range of calibration standard masses used should be such that the low concentration approaches but is above the MDL and the high concentration is above the level of the highest sample but no more than 90 of the linear dynamic range A minimum of three concentrations should be used in constructing the curve Measure response versus mass of element in the standard and perform a regression on the data to obtain the calibration curve 110 Procedure 1 1 1 Aqueous Sample Preparation 1111 Water Sample Filtration Precombust GFF glass fiber filters at 500 C for 15 hr The diameter of filter used will depend on the sample composition and instru ment capabilities Section 811 Store filters covered if not immediately used Place a precombusted filter on fritted filter base of the filtration apparatus and attach the filtration tower Thoroughly shake the sample container to suspend the particulate matter Measure and record the required sample volume using a graduated cylinder Pour the measured sample into the filtration tower no more than 50 mL at a time Filter the sample using a vacuum no greater than 10 in of Hg Vacuum levels greater than 10 in of Hg can cause filter rupture If less than the measured volume of sample can be practically filtered due to clogging measure and record the actual volume filtered Do not rinse the filter following filtration It has been demonstrated that sample loss occurs when the filter is rinsed with an isotonic solution or the filtrate8 Air dry the filter after the sample has passed through by continuing the vacuum for 30 sec Using Tefloncoated flattipped forceps fold the filters in half while still on the fritted glass base of the filter apparatus Store filters as described in Section 8 44006 1112 If the sample has been stored frozen place the sample in a drying oven at 103105 C for 24 hr before analysis and dry to a constant weight Precombust one nickel sleeve at 875 C for 1 hr for each sample 1113 Remove the filter pads containing the particulate material from the drying oven and insert into a pre combusted nickel sleeve using Tefloncoated flattipped forceps Tap the filter pad using a stainless steel rod The sample is ready for analysis 1 12 Sediment Samples Preparation 1121 Thaw the frozen sediment sample in a 102 105 C drying oven for at least 24 hr before analysis and dry to a constant weight After drying homogenize the dry sediment with a mortar and pestle Store in a desic cator until analysis Precombust aluminum capsules at 550 C in a muffle furnace for 15 hr for each sediment sample being analyzed Precombust one nickel sleeve at 875 C for 1 hr for each sediment sample 1122 Weigh 10 mg of the homogenized sediment to the nearest 0001 mg with an ultramicro balance into a precombusted aluminum capsule Crimp the top of the aluminum capsule with the Tefloncoated flattipped for ceps and place into a precombusted nickel sleeve The sample is ready for analysis 113 Sample Analysis 1131 Measure instrument zero response Section 74 and instrument blank response Section 74 and record values Condition the instrument by analyzing a condi tioner Calibrate the instrument according to Section 10 and analyze all preliminary QC samples as required by Section 9 When satisfactory control has been estab lished analyze samples according to the instrument manufacturer s recommendations Record all response data 1132 Report data as directed in Section 12 114 Determination of Particulate Organic and Inorganic Carbon 1141 Method 1 Thermal Partitioning The difference found between replicate samples one of which has been analyzed for total PC and PN and the other which was muffled at 550 C and analyzed is the particulate organic component of that sample This method of thermally partitioning organic and inorganic PC may underestimate slightly the carbonate minerals contribution in the inorganic fraction since some carbonate minerals decompose below 500 C although CaCO3 does not9 1142 Method 2 Fuming HCI Allow samples to dry overnight at 103105 C and then place in a desiccator containing concentrated HCI cover and fume for 24 hr in a hood The fuming HCI converts inorganic carbonate in the samples to water vapor CO2 and calcium chloride 44007 Analyze the samples for particulate C The resultant data are particulate organic carbon 120 Data Analysis and Calculations 121 Sample data should be reported in units of ugL for aqueous samples and mgkg dry weight for sediment samples 122 Report analyte concentrations up to three signifi cant figures for both aqueous and sediment samples 123 For aqueous samples calculate the sample con centration using the following formula Corrected Concentration ugL sample response uv Sample volume L x RF uvug where RF Response Factor Section 1011 Corrected Sample Response Section 74 124 For sediment samples calculate the sample con centration using the following formula Corrected Concentration mgkg sample response uv Sample weight g x RF uvug where RF Response Factor Section 1011 Corrected Sample Response Section 74 Note Units of ugg mgkg 125 The QC data obtained during the analyses provide an indication of the quality of the sample data and should be provided with the sample results 130 Method Performance 131 Single Laboratory Performance 1311 Single laboratory performance data for aqueous samples from the Chesapeake Bay are provided in Table 2 1312 Single laboratory precision and accuracy data for the marine sediment reference material BCSS1 are listed in Table 3 132 Multilaboratory Performance 1321 In a multilab study 13 participants analyzed sediment and filtered estuarine water samples for particulate carbon and nitrogen The data were analyzed Revision 14 September 1997 using the statistical procedures recommended in ASTM D277786 for replicate designs See Table 4 for summary statistics 1322 Accuracy as mean recovery was estimated from the analyses of the NRC of Canada Marine Sediment Reference Material BCSS1 Mean recovery was 982 of the certified reference carbon value and 100 of the noncertified nitrogen value 1323 Overall precision for analyses of carbon and nitrogen in sediments was 111 RSD while the analyses of both particulate carbon and nitrogen in estuarine water samples was 914 RSD 1324 Single analyst precision for carbon and nitrogen in sediment samples was 18 RSD and 49 for water samples 1325 Pooled method detection limits pMDLs were calculated using the pooled single analyst standard deviations The pMDLs for particulate nitrogen and carbon in estuarine waters were 0014 mg NL and 0064 mg CL respectively The pMDLs for percent carbon and nitrogen in estuarine sediments were not estimated because the lowest concentration sediment used in the study was still 20 times higher than the estimated MDLs Estimates of pMDLs from these data would be unrealistically high 140 Pollution Prevention 141 Pollution prevention encompasses any technique that reduces or eliminates the quantity or toxicity of waste at the point of generation Numerous opportunities for pollution prevention exist in laboratory operation The EPA has established a preferred hierarchy of environ mental management techniques that places pollution prevention as the management option of first choice Whenever feasible laboratory personnel should use pollution prevention techniques to address their waste generation When wastes cannot be feasibly reduced at the source the Agency recommends recycling as the next best option 142 For information about pollution prevention that may be applicable to laboratories and research institu tions consult Less is Better Laboratory Chemical Man agement for Waste Reduction available from the Ameri can Chemical Society s Department of Government Re lations and Science Policy 1155 16th Street NW Washington DC 20036 202 8724477 150 Waste Management 151 The Environmental Protection Agency requires that laboratory waste management practices be con ducted consistent with all applicable rules and regula tions The Agency urges laboratories to protect the air water and land by minimizing and controlling all releases from hoods and bench operations complying with the Revision 14 September 1997 letter and spirit of any sewer discharge permits and regulations and by complying with all solid and hazard ous waste regulations particularly the hazardous waste identification rules and land disposal restrictions For further information on waste management consult The Waste Management Manual for Laboratory Personnel available from the American Chemical Society at the address listed in Section 142 160 References 1 40 CFR Part 136 Appendix B Definition and Procedure for the Determination of the Method Detection Limit Revision 111 2 Carcinogens Working With Carcinogens Department of Health Education and Welfare Public Health Service Center for Disease Control National Institute for Occupational Safety and Health Publication No 77206 Aug 1977 3 OSHA Safety and Health Standards General Industry 29 CFR 1910 Occupational Safety and Health Administration OSHA 2206 Revised January 1976 4 Safety in Academic Chemistry Laboratories American Chemical Society Publication Committee on Chemical Safety 3rd Edition 1979 5 Proposed OSHA Safety and Health Standards Laboratories Occupational Safety and Health Administration Federal Register July 24 1986 6 Rohrdough WG et al Reagent Chemicals American Chemical Society Specifications 7th Edition American Chemical Society Washington DC 1986 7 Holme NA and AD Mclntyre eds 1971 Methods for the Study of Marine Benthos International Biome Program IBP Handbook 16 FA Davis Co Philadelphia PA 8 Hurd DC and DW Spencer eds 1991 Marine Particles Analysis and Characterization Geophysical Monograph 63 American Geophysical Union Washington DC 472p 9 HirotaJand JPSzyper 1975 Separation of total particulate carbon into inorganic and organic components Limnol and Oceanogr 20 896900 10 Grasshoff K M Ehrhardt and K Kremling eds 1983 Methods of Seawater Analysis Verlag Chemie 44008 170 Tables Diagrams Flowcharts and Validation Data Table 1 Filter Diameter Selection Guide Filter diameter Sample matrix 47mm 25mm 13mm Sample matrix volume Open ocean 2000 mL 500 mL 100 mL Coastal 1000 mL 400500 mL 100 mL Estuarine 500700 mL 250400 mL 50 mL low particulate Estuarine 100400 mL 75200 mL 25 mL high particulate Table 2 Performance DataChesapeake Bay Aqueous Samples Measured Measured nitrogen carbon concentration SDA concentration SDA Sample HgL HgL HgL HgL 1 147 i 4 1210 i 49 2 148 i 11 1240 i 179 3 379 1 51 3950 Jr 269 4 122 9 1010 i 63 A Standard deviation based on 7 replicates Table 3 Precision and Accuracy Data Canadian Sediment Reference Material BCSS1 Mean measured Element TVA value OORSDB Recovery Carbon 219 218 i 33 995 Nitrogen 0195 0194 i 39 995 A True value Carbon value is certified nitrogen value is listed but not certified 3 Percent relative standard deviation based on 10 replicates 0 As calculated from TV 44009 Revision 14 September 1997 Table 4 Overall and Single Analyst Precision Estimates from Collaborative Study Analyte Sample Ni Mean 2 Overall Overall Analyst Analyst Conc Std Dev RSD Std Dev RSD Particulate A 1 1 00655 00081 124 00050 76 Nitrogen as N in B 12 00730 00076 103 00057 77 Efgfggne c 12 00349 00110 129 00060 71 D 12 0126 00138 110 00071 56 E 11 0182 00245 135 00157 86 Nitrogen 1 10 0178 00190 107 00131 73 as N in Water 3 10 0436 00173 41 00104 24 4 10 0497 00183 37 00082 16 5 10 0580 00207 36 00150 26 Particulate B 12 0369 00505 137 00222 60 Carbon as C in A 12 0417 00490 113 00230 55 5jtJ e D 12 0619 00707 114 00226 36 C 12 0710 00633 89 00367 52 E 12 0896 01192 133 00569 64 Carbon 1 13 178 01517 85 01346 76 as C in Sed39me tS 3 13 318 00435 14 00343 11 4 13 492 01201 24 00779 16 5 13 592 00621 11 00547 09 1 N Number of participants whose data was used 2 Concentration in mgL or percent as indicated Revision 14 September 1997 440010 Method 4450 In Vitro Determination of Chlorophyll a and Pheophytin a in Marine and Freshwater Algae by Fluorescence Elizabeth J Arar and Gary B Collins Revision 12 September 1997 National Exposure Research Laboratory Office of Research and Development US Environmental Protection Agency Cincinnati Ohio 45268 44501
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