vxEPA
United States
Environmental Protection
Agency
     Sample Holding Time
          Reevaluation
       RESEARCH AND DEVELOPMENT

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                                                 EPA/600/R-05/124
                                                    October 2005
                                                    www.epa.gov
 Sample  Holding  Time
          Reevaluation
                Contract No. 68-D-99-011
              Task Order No. 18 (ORD-01-005)
                    Prepared for

                Brian A. Schumacher, Ph.D.
            U.S. Environmental Protection Agency
            National Exposure Research Laboratory
              Environmental Sciences Division
                944 East Harmon Avenue
                Las Vegas, Nevada 89119
                    Prepared by

                Battelle Memorial Institute
                Pacific Northwest Division
                  Post Office Box 999
                   Battelle Boulevard
               Richland, Washington 99352

C.C. Ainsworth, V.I. Cullinan, E.A. Crecelius, K.B. Wagnon, and L.A. Niewolny
           U.S. Environmental Protection Agency
           Office of Research and Development
                Washington, DC 20460
                                               033CMB06.RPT * 1/3/2006

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                                      Notice
The information in this document has been funded wholly by the United States Environmental
Protection Agency under contract number 68-D-99-011 to Battelle Memorial Institute. It has
been subjected to the Agency's peer and administrative review and has been approved for
publication as an EPA document. Mention of trade names or commercial products does not
constitute endorsement or recommendation by EPA for use.
                                                                                  in

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IV

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                              Executive Summary
The project's overall objective was to investigate the stability of selected contaminants in
soil/sediment samples as a function of holding time prior to extraction. Contaminants of interest
centered on SVOCs; particularly polyaromatic hydrocarbons (PAHs), polychlorinated biphenyls
(PCBs), and pesticides, Cr(VI), and several heavy metals. Contaminant specific objectives were:

   1.  Determine if selected S VOC contaminant concentrations in soil/sediment changed with
       time when held in storage beyond their established extraction maximum holding times
       (MHTs) under current preservation techniques and at -20°C;
   2.  Determine if Cr(VI) concentrations change when held in storage beyond their established
       MHTs under current preservation techniques and at -20°C;
   3.  Determine if extracted Cr(VI) concentrations change when held beyond the analysis
       MHT (24-h) when held in the dark at room temperature (~20°C) or 4°C;
   4.  Determine if air-drying soil samples will adversely impact hot acid extractable heavy
       metal concentrations.

Test soils/sediments from contaminated sites were identified,  collected and homogenized prior to
extraction by SW-846 methods. After homogenization, soil/sediment samples were stored under
designated conditions and extracted at multiples of the current MHT (depending on the
contaminant, multiples of MHT were between 0.5 and 12). Analyses of contaminant
concentrations were performed in accordance with SW-846 methodologies. Results of these
extractions were evaluated by a progression of four distinct analyses to  elucidate possible
decreases in concentration of an analyte (lines of evidence). First, the magnitude and variability
of the concentration was used to suggest a level of the signal to noise ratio; second, a t-test of the
Ho:overall mean equal to or greater than the Day 0 mean was used to provide a level of relevance
to observed change; third, a regression against time was used to estimate a rate of change; and
fourth, a nonparametric upper and  lower bound based on the Day 0 quartiles was used to provide
an alternative measure of relevance to the potential change through time. Ultimately; however,
linear regression analysis was utilized to estimate the time required to observe a specific percent
change in the extractable concentration.

The estimated number of days until a 5% decrease in Cr(VI) concentration from the estimated
intercept would be observed was greater than 140 days for all sediments/soils tested. The results
of this study suggest that the  recoveries of matrix spike and control extracts are key to
determining stability of Cr(VI) in the solid materials to be extracted and the extracts themselves.
In all cases, when the recovery of the matrix spike and control samples was good (within
acceptable parameters), the stability of Cr(VI) in the sediment/soil and extract solutions (stored
under proper conditions) appear to be longer than the current MHT specified in SW-486.

For the 17 PAH compounds that were quantified in three different soils/sediments, a holding
time of 100 days at either 4°C or -20°C would result in no more than a 20% decrease in
concentration. Importantly, there is considerable variability in the estimated holding times for

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different compounds and in different soils/sediments. The major consideration in sediment
holding time appears, from these studies, to be the number of aromatic rings (or molecular
weight) of the PAH of interest. Only the Eagle Harbor soil appeared to have significant loss to
PAHs for samples stored at 4°C as compared to samples stored at -20°C. The loss of up to 50%
occurred for compounds with relatively low molecular weights, including acenaphthene,
fluorene, dibenzothiophene, phenanthrene and anthracene. These results confirmed a previous
study that demonstrated freezing sediment/soil reduced the loss of low molecular weight (low
number of rings) PAHs.

For the three PCB Aroclor mixtures and the seven congeners that were quantified in three
different soils/sediments, a holding time of 260 days at 4°C and 281 days at -20°C would  result
in not more than a 20% decrease in concentration. An indication of the stability of the PCBs in
the three soil/sediments that were studied is the very small difference in the mean concentration
for all data across time at two storage temperatures. In almost every case, the concentrations for
the -20°C samples are slightly greater, about 10% or less, than for the 4°C mean. This could be
interpreted that about 10% more PCBs are lost during the  5.6 month storage time at 4°C than at -
20°C. Given the 25% coefficient of variation (CV) metric  for replicate precision; however, it is
unlikely that this 10% difference could be accurately quantified.

For the  10 pesticides that were quantified in four different soils/sediments, a holding time of 217
days at 4°C and 299 days at -20°C would result in not more than a 20% decrease in
concentration. These holding times are far greater than the current MHT specified in SW-846. In
almost every case, the mean concentrations  for the -20°C samples are within a few percent of the
4°C mean. This could be interpreted as less than 5% of the pesticides studied are lost during the
5.6 month storage time of samples at 4°C compared to storage at -20°C.

Extractable metal concentrations were not effected significantly by a holding time of up to 364
days or by the air drying treatment. All data sets exhibited fairly tight CVs across the holding
times. The CV data suggests that no chemically significant change  in concentration occurred
during the 364 day holding time and the pooled data exhibited no significant difference between
moist or dry sample handling.  These results suggest that it would take a minimum of 709  days
before the acid-extractable As, Cu, Pb, or Zn concentration would be reduced by 20%.
VI

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                                 Table of Contents


Notice	iii
Executive Summary	v
List of Tables	ix
List of Figures	xiii
Acknowledgements	xix

Section  1  Introduction	1
    1.1 Chromate [Cr(VI)]	1
    1.2 Semi-Volatile Organic Compounds	3
    1.3 Acid Extractable Heavy Metals	4
    1.4 Objectives	4

Section  2  Materials and Methods	5
    2.1 Soils/Sediments Identification, Collection and Selection	5
    2.2 Experimental Design	5
       2.2.1  Soils/Sediments Homogenization, Analysis, Storage and Extraction Schedule	7
       2.2.2  Cr(VI) Extraction and Analysis	8
       2.2.3  SVOC Extraction	8
       2.2.4  SVOC Analysis	9
       2.2.5  Metal Digestion (Acid-Leachable) and Analysis	13
    2.3 Statistical Analysis	13
    2.4 General Data Quality Objectives	16

Section  3  Results and Discussion	17
    3.1 Chromate [Cr(VI)]	17
       3.1.1  Spike Recovery Anomaly: Bedford Plot-6 Soil	17
       3.1.2  Cr(VI) Extraction	19
       3.1.3  Cr(VI) Extract Stability	24
       3.1.4  Cr(VI) Holding Time for Extraction and Extract Stability - Conclusions	29
    3.2 Semi-Volatile Organic Compounds (SVOCs)	29
       3.2.1  Polyaromatic Hydrocarbons (PAHs)	30
           3.2.1.1 Influence of PAH Outliers	32
           3.2.1.2 Statistical Analysis of PAH Extraction Data	32
           3.2.1.3 PAH Holding Time Study - Conclusions	56
       3.2.2  Polychlorinated Biphenyls (PCBs)	56
           3.2.2.1 Surrogate  Correction of SQ-1 Sediment PCB Extraction Data	57
           3.2.2.2 Statistical Analysis of PCB Extraction Data	59
           3.2.2.3 PCB Holding Time Study - Conclusions	65
                                                                                         VII

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       3.2.3 Pesticides	70
          3.2.3.1  Surrogate Correction of SQ-1 Sediment Pesticide Extraction Data	72
          3.2.3.2  Statistical Analysis of Pesticide Extraction Data	72
          3.2.3.3  Pesticide Holding Time Study - Conclusions	83
   3.3 Acid Extraction of Metals	86
       3.3.1 Statistical Analysis of Metals Extraction	86
       3.3.2 Metal Extraction Holding Time Study - Conclusions	91

Section 4 Conclusions	95

References	99

Appendix A Descriptive Statistics for All Sediment Holding Time Studies	A-l

Appendix B Plots of Concentration vs. Time for All Sediment/Soil Extraction
             Holding Time Studies	B-l

Appendix C Chromate [Cr(VI)] Soil Extraction	C-l

Appendix D Chromate [Cr(VI)] Soil Extract Holding Time	D-l

Appendix E Semi-Volatile Organic Compound Extraction Data	E-l

Appendix F  Metals Data for the Sinclair Sediment and Wilmington Soil	F-l
Vlll

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                                     List of Tables
Table
  1-1  Soil/sediment sample preservation, and holding times, and extract preservation, and
       holding times	2
  1-2  Changes made in Method 3060	2
  2-1  Available soils/sediments	6
  2-2  Comparison of analysis of variance and regression assuming six time points for chemical
       analysis, two replicate analyses at each time, and a linear relationship	6
  2-3  PAH analyte list	10
  2-4  PCB (Aroclors and Congeners) and chlorinated pesticide analyte list	11
  2-5  Summary of general data quality objectives	16
  3-1  Chromate extraction study soil/sediment properties	18
  3-2  Cr(VI) analyses of three Cr(VI) spiked Bedford-6 soil extracts	20
  3-3  Chromate [Cr(VI)] (mg/kg) one-sample t-test of the null hypothesis Ho: the sample is from
       a population with the mean equal to or greater than the Day 0 mean	20
  3-4  P-values for the significance of the lack-of-fit and the slope from the linear regression and
       the best fit simple linear model parameters on the natural log scale for Cr(VI)	23
  3-5  The estimated number of days until a given percentage decrease from the intercept for
       Cr(VI) (MHT=28  days)	24
  3-6  Average CV% over time and within replicates for the Cr(VI) extracts	28
  3-7  Simple linear regression analysis corrected for baseline only	28
  3-8  Estimated number of days to achieve a given percentage change in concentration using the
       regression model of the background corrected data	30
  3-9  SVOC extraction study soil/sediment properties	30
 3-10  Mean concentration (ng/g) and coefficient of variation (CV) for all data across time
       accepted for analysis (including statistical outliers)	31
 3-11  PAHs (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a population
       with the mean equal to or greater than the Day 0 mean from Appendix B for the Eagle
       Harbor soil  	33
 3-12  PAHs (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a
       population with the mean equal to or greater than the Day 0 mean from Appendix B for
       the SQ-1 sediment	34
 3-13  PAHs (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a
       population with the mean equal to or greater than the Day 0 mean from Appendix B for
       theBedford-1 soil	36
                                                                                             IX

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Table

 3-14  P-values for the significance of the lack-of-fit and the slope from the linear regression
       and the best fit simple linear model parameters on the natural log scale for PAHs for
       Eagle Harbor soil and each holding condition	37

 3-15  P-values for the significance of the lack-of-fit and the slope from the linear regression
       and the best fit simple linear model parameters on the natural log scale for PAHs for
       SQ-1 sediment and each holding condition	38

 3-16  P-values for the significance of the lack-of-fit and the slope from the linear regression
       and the best fit simple linear model parameters on the natural log scale for PAHs for
       Bedford-1 soil and each holding condition	39
 3-17  Summary of PAH statistical analyses for each soil/sediment and holding condition	40

 3-18  The estimated number of days until a given percentage decrease from the intercept for
       PAHs (MHT=14 days) from Eagle Harbor soil	42
 3-19  The estimated number of days until a given percentage decrease from the intercept for
       PAHs (MHT=14 days) from SQ-1 sediment	43
 3-20  The estimated number of days until a given percentage decrease from the intercept for
       PAHs (MHT= 14 days) from Bedford-1 soil	44
 3-21  Mean concentration (ng/g), coefficient of variation (CV), and significance of slope across time
       for analytes with CVs>25%	45

 3-22  Estimated number of days until a 20% decrease in concentration could be observed for
       those analytes having a significant negative slope, an overall CV>25%, and observations greater
       than2*MDL	46

 3-23  Mean PCB concentration (ng/g) and CV for all data across time accepted for analysis	57
 3-24  PCB (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a population
       with the mean equal to or greater than the Day 0 mean with statistical outliers removed	60
 3-25  P-values for the significance of the lack-of-fit and the slope from the linear regression and
       the best fit  simple linear model parameters on the natural log scale for PCBs by sediment
       and holding condition	61

 3-26  The estimated number of days until a given percentage decrease from the intercept for
       PCBs (MHT=14 days)	62
 3-27  Mean concentration (ng/g) and coefficient of variation (CV) for all pesticide data across
       time accepted for analysis	71
 3-28  Surrogates  used to correct each pesticide analyte for SQ-1 sediment and Bedford-1 soil	73
 3-29  Pesticides (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a
       population  with the mean equal to or greater than the Day 0 mean	75

 3-30  P-values for the significance of the lack-of-fit and the slope from the linear regression
       and the best fit simple linear model parameters on the natural log scale for pesticides by
       sediment/soil and holding condition	76

 3-31  The estimated number of days until a given percentage decrease from the intercept for
       pesticides (MHT=14 days) by sediment/soil and holding condition	78

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Table

 3-32  Sediment/soil properties of materials used in metal acid-extraction study	87

 3-33  Heavy metals (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a
       population with the mean equal to or greater than the Day 0 mean	87

 3-34  P-values for the significance of the lack-of-fit and the slope from the linear regression
       and the best fit simple linear model parameters on the natural log scale for heavy metals
       for each sediment and holding condition	90

 3-35  The estimated number of days until a given percentage decrease from the intercept for
       each sediment and holding condition for heavy metals (MHT=182 days) by sediment and
       holding condition	91
                                                                                             XI

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Xll

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                                   List of Figures
 3-1   UV/Vis spectra of a) Cr(VI) 1000 mg/L standard, b) Bedford plot-6 Cr(VI) extract
       solution, c) Bedford plot-6 Cr(VI) extract solution and diphenylcarbazide, and
       d) Bedford plot-6 extract solution prepared as prescribed by SW-846 Method 7196A	18
 3-2   Observed Cr(VI) concentration for Soil 125A at both the 4°C and -20°C holding
       temperature over holding time and associated Day 0 nonparametric bounds; there was not
       a significant trend through time	21
 3-3   Observed Cr(VI) concentration for Soil 126D at both the 4°C and -20°C holding
       temperature over holding time and associated Day 0 nonparametric bounds; there was not
       a significant trend through time	22
 3-4   Observed Cr(VI) concentration for Soil 123 at both the 4°C and -20°C holding
       temperature over holding time, associated Day 0 nonparametric bounds, and the
       significant decreasing trend for sediment held at 4°C	23
 3-5   Observed Cr(VI) concentration for Soil 125B at both the 4°C and -20°C holding
       temperature over holding time and associated Day 0 nonparametric bounds; there was not
       a significant trend through time	25
 3-6   Observed Cr(VI) concentration for Soil 125C at both the 4°C and -20°C holding
       temperature over holding time and associated Day 0 nonparametric bounds; there was not
       a significant trend through time	25
 3-7   Cr(VI) extract concentration stored at room temperature or 4°C as a function of time for
       the Frontier Hard Chrome site sandy soil	26
 3-8   Cr(VI) extract concentration stored at room temperature or 4°C as a function of time for
       the Boomsnub  soil at depths of 0.5, 3.0 or 5.5 feet	27
 3-9   Observed acenaphthylene concentration for Eagle Harbor soil at both the 4°C and -20°C
       holding temperature by holding time, significant regression lines, and associated Day 0
       nonparametric bounds (2*MDL is indicated by the red line)	47
3-10   Observed fluorene concentration  for Eagle Harbor soil at both the 4°C and -20°C
       holding temperature by holding time, significant regression line, and associated Day 0
       nonparametric bounds	47
3-11   Observed phenanthrene concentration for Eagle Harbor soil at both the 4°C and -20°C
       holding temperature by holding time, significant regression line, and associated Day 0
       nonparametric bounds	48
3-12   Observed pyrene concentration for Eagle Harbor soil at both the 4°C and -20°C holding
       temperature by holding time and  associated Day 0 nonparametric bounds; there were no
       significant trends	48
                                                                                          Xlll

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 3-13   Observed chrysene concentration for Eagle Harbor soil at both the 4°C and -20°C
        holding temperature by holding time, significant regression line, and associated Day 0
        nonparametric bounds	49
 3-14   Observed benzo[a]pyrene concentration for Eagle Harbor soil at both the 4°C and -20°C
        holding temperature by holding time, significant regression line, and associated Day 0
        nonparametric bounds	49
 3-15   Observed acenaphthylene concentration for SQ-1  sediment at both the 4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant trend	50
 3-16   Observed fluorene concentration for SQ-1 sediment at both the 4°C  and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	50
 3-17   Observed phenanthrene concentration for SQ-1 sediment at both the 4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant trend	51
 3-18   Observed pyrene concentration for SQ-1 sediment at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	51
 3-19   Observed chrysene concentration for SQ-1  sediment at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	52
 3-20   Observed benzo[a]pyrene concentration for SQ-1  sediment at both the 4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant trend	
 3-21   Observed acenaphthylene concentration for Bedford-1 soil at both the 4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant trend	
 3-22   Observed fluorene concentration for Bedford-1 soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend (2*MDL is indicated by the red line)	
 3-23   Observed phenanthrene concentration for Bedford-1 soil at both the  4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant trend	54
 3-24   Observed pyrene concentration for Bedford-1 soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	54
 3-25   Observed chrysene concentration for Bedford-1 soil at both the 4°C  and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	
 3-26   Observed benzo[a]pyrene concentration for Bedford-1 soil at both the 4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant negative trend	
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Figure
 3-27   SQ-1 sediment raw Aroclor 1254 data and surrogate recovery as a function of holding
        time (days to extraction)	58
 3-28   SQ-1 surrogate corrected data as a function of the age of extract	58
 3-29   Observed Aroclor 1254 concentration for SQ-1 sediment at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	63
 3-30   Observed PCB 153 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time, significant regression lines, and associated Day 0
        nonparametric bounds	64
 3-31   Observed Aroclor 1254 concentration for Housatonic River sediment at both the 4°C and
        -20°C holding temperature by holding time, significant regression lines, and associated
        Day 0 nonparametric bounds	64
 3-32   Observed Aroclor 1260 concentration for Housatonic River sediment at both the 4°C and
        -20°C holding temperature by holding time, significant regression lines, and associated
        Day 0 nonparametric bounds	65
 3-33   Observed Aroclor 1242 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	66
 3-34   Observed Aroclor 1260 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	66
 3-35   Observed PCB 8 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant negative trend	67
 3-36   Observed PCB 52 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	67
 3-37   Observed PCB 138 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	68
 3-38   Observed PCB 187 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	68
 3-39   Observed PCB 180 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	69
 3-40   Observed PCB 170 concentration for Tri-Cities soil at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant trend	69
 3-41   SQ-1 sediment raw oc-chlordane data and surrogate recovery	72

 3-42   SQ-1 sediment oc-chlordane surrogate corrected data as a function of the age of extract	73
                                                                                            xv

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 3-43   Bedford-1 soil raw 4,4'-DDD data and surrogate percent recovery	74
 3-44   Observed 4,4'-DDD concentration for Housatonic River sediment at both the 4°C and
        -20°C holding temperature by holding time and associated Day 0 nonparametric bounds;
        there was no significant trend	79
 3-45   Observed 4,4'-DDE concentration for Housatonic River sediment at both the 4°C and
        -20°C holding temperature by holding time, significant regression lines, and associated
        Day 0 nonparametric bounds	79
 3-46   Observed 2,4'-DDT concentration for Housatonic River sediment at both the 4°C and
        -20°C holding temperature by holding time, significant regression line, and associated
        Day 0 nonparametric bounds	80
 3-47   Observed 4,4'-DDT concentration for Housatonic River sediment at both the 4°C and
        -20°C holding temperature by holding time and associated Day 0 nonparametric bounds;
        there was no significant trend	80
 3-48   Observed oc-chlordane concentration for SQ-1 sediment (surrogate corrected) at both the
        4°C and -20°C holding temperature by holding time and associated Day 0 nonparametric
        bounds; there was no significant negative trend	81
 3-49   Observed trans nonachlor concentration for SQ-1 sediment (surrogate corrected) at both
        the 4°C and -20°C holding temperature by holding time and associated Day 0
        nonparametric bounds; there was no significant trend	81
 3-50   Observed 4,4'-DDE concentration for SQ-1 sediment (surrogate corrected) at both the
        4°C and -20°C holding temperature by holding time and associated Day 0 nonparametric
        bounds; there was no significant negative trend	82
 3-51   Observed 4,4'-DDD concentration for SQ-1 sediment (surrogate corrected) at both the
        4°C and -20°C holding temperature by holding time and associated Day 0 nonparametric
        bounds; there was no significant trend	82
 3-52   Observed 2,4'-DDT concentration for SQ-1 sediment (surrogate corrected) at both the
        4°C and -20°C holding temperature by holding time and associated Day 0 nonparametric
        bounds; there was no significant trend	83
 3-53   Observed oc-chlordane concentration for Tri-Cities soil  at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant negative trend	84
 3-54   Observed y-chlordane concentration for Tri-Cities soil  at both the 4°C and -20°C holding
        temperature by holding time and associated Day 0 nonparametric bounds; there was no
        significant negative trend	84
 3-55   Observed trans nonachlor concentration for Tri-Cities soil at both the 4°C and -20°C
        holding temperature by holding time and associated Day 0 nonparametric bounds; there
        was no significant negative trend	85
 3-56   Observed 4,4'-DDD concentration for Bedford-1  soil (surrogate corrected) at both the
        4°C and -20°C holding temperature by holding time, significant regression lines, and
        associated Day 0 nonparametric bounds	85
xvi

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3-57   Observed 4,4'-DDT concentration for Bedford-1 soil (surrogate corrected) at both the
       4°C and -20°C holding temperature by holding time and associated Day 0 nonparametric
       bounds; there was no significant trend	86
3-58   Observed As concentration for Sinclair River sediment for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	89
3-59   Observed Zn concentration for Sinclair River sediment for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	89
3-60   Observed Pb concentration for Sinclair River sediment for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	90
3-61   Observed As concentration for Wilmington soil for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	92
3-62   Observed Cu concentration for Sinclair River sediment for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	92
3-63   Observed Cu concentration for Wilmington soil for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	93
3-64   Observed Pb concentration for Wilmington soil for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	93
3-65   Observed Zn concentration for Wilmington soil for both the wet and dry holding
       condition over holding time and associated Day 0 nonparametric bounds	94
                                                                                          xvii

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                            Acknowledgements
The authors wish to thank all those individuals whose cooperation and participation contributed
to the development of the research data and this report. We greatly appreciate the guidance,
assistance, and technical review provided by the Task Order Project Officer Dr. Brian
Schumacher of the U.S. Environmental Protection Agency, National Exposure Research
Laboratory (NERL), Las Vegas, Nevada. Also, for their technical reviews of the draft report, we
thank Mr. Gary Robertson and Mr. John Zimmerman of Human Exposure and Atmospheric
Sciences Division and Environmental Sciences Division, respectively, US EPA, NERL, Las
Vegas, NV. We also wish to acknowledge Robert Maxfield and Joe Blazevich of US EPA
Regions 1 and 10, respectively, as the original Regional Methods Initiative requesters, which
lead to this project.

We are grateful to J. Gareth Pearson, Director of the Technical Support Center at Environmental
Sciences Division, US EPA, NERL, Las Vegas, NV, for his original call for potential
soil/sediment materials identification. We wish to thank the following individuals for their time
and effort in identification and collection of the soil/sediment materials utilized in this study: Joe
Blazevich (retired), Hahn Gold (formerly) and Gerald Dodo, US EPA, Region 10; Young Chang,
US EPA Region 2; Larry Heinis and Dave Mount, US EPA, Duluth, MN; Byron Mah, Robert
Maxfield, Cornell Rosiu, Dan Granz, Carolyn Casey, Mike Nalipinski, and Kymberlee Keckler,
US EPA, Region 1; Marilyn Jupp, and William  Sargent, US EPA, Region 5; Ken Mallory,
Debbie Colquitt, and Archie Lee, US EPA, Region 4; and Frank Van Ryn, Koch Industries.
                                                                                  XIX

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XX

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                                     Section 1

                                   Introduction
Extraction and determination of a contaminant concentration (organic and metal) in soil, water,
sediment, and other matrices is vital to estimating their impact on the environment. In an attempt
to standardize the determination of contaminant levels in various matrices, the U.S.
Environmental Protection Agency (USEPA) has established a set of procedures, protocols, and
techniques for sampling, preservation, and analysis for various matrices and contaminants: the
USEPA SW-846 Test Methods for Evaluating Solid Wastes,  Physical/Chemical Methods
(USEPA, 2000). As part of sample handling protocols, maximum holding times (MHT) have
been established to protect sample integrity and provide sufficient time for analyses. Holding
times have been defined as the length of time an environmental media (e.g., water, soil,
sediment, etc.) can be stored (under specific conditions) after collection and prior to analysis
with reasonable assurance that the analyte of interest's concentration does not change
significantly (Bayne et al., 1993).

Depending upon the matrix, analyte in question, and analytical methodology, soil/sediment
sample MHTs vary (Table 1-1). Extraction and analysis of contaminants beyond MHTs may
cause significant problems; for instance, analyses may be "flagged" or designated as estimates,
often requiring expensive resampling and analysis.

Holding times and preservation  requirements are set to assure that contaminant concentrations do
not change significantly between sampling and extraction because of intrinsic biogeochemical
reactions, such as biotic and abiotic  degradation, volatilization,  oxidation/reduction, or
irreversible sorption. The fate of contaminants in soils and  sediments have been extensively
studied and reported in the literature. With the exception of hexavalent Cr (and other redox
sensitive metals) and volatile organic compounds (VOCs);  however, only a limited number of
studies have looked at the impact of holding times and preservation techniques on the
determination of contaminant concentration in soils and sediments.

1.1  Chromate [Cr(VI)]

Chromium has been utilized in various products and manufacturing processes throughout the
world and chromium containing wastes have been discharged to the environment (Petura et al.,
1998). The two common valance states  of chromium [Cr(III) and Cr(VI)] exhibit vastly different
physical/chemical behavior and toxicological properties. Hexavalent Cr is fairly soluble in
aqueous environments compared to the  insoluble and immobile trivalent Cr, and it is more toxic
to exposed organisms (Petura et al.,  1998). Hence, there has been considerable research focusing
on development of a valance sensitive extraction technique for soils, sediments, and solid wastes
(USEPA, 1983, 1986).

In 1986, SW-846 Method 3060 was removed as  a regulatory  approved method for extraction of
Cr(VI) in solid samples primarily due to instability of the extract. Chromate determinations have

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been shown to be effected by oxidation/reduction reactions resulting from sample treatment: i.e.,
drying (Bartlett and James, 1996; James, 1994; James and Bartlett, 1983); base dissolution of
Fe(II) bearing minerals and subsequent reduction of Cr(VI) (Qafoku et al., 2003); and induction
of, or maintenance of anaerobic conditions (Vitale et al., 1997a). Fendorf (2000), in a recent
 Table 1-1. Soil/sediment sample preservation, and holding times, and extract preservation, and
          holding times1.
Analyte
Total Metals
(acid-extractable)
Chromate [Cr(VI)]
Semi-volatile organics
Soil/Sediment
Preservation
None
4°C
4°C
Holding Time
6 months
30 days
14 days
Extract
Preservation
4°C
4°C
4°C
Holding Time
Within 6 months
Within 4 days2
Within 40 days
  1 From Tables 3-1 and 4-7 of the SW-846 manual (USEPA, 2000).
   From Table 4-7 of SW-846 manual, but values of 3 days, 24 hrs, and as soon as possible are also quoted in Cr(VI) extraction method
   (3060A) and Cr(VI) detection methods (e.g., Methods 7196A, and 7199).
review of Cr(VI) reduction, concluded that biological processes are the principal means by which
Cr(VI) is converted to Cr(III) in aerobic systems. In addition, he surmised that the aeration status
of a system is of primary dependence, while pH and concentrations of reduced phases appeared
to be secondary. A modified Cr(VI) extraction method (Method 3060A; US EPA, 2000) was
adopted after extensive study of a large set (>1500) of diverse field samples ranging from anoxic
sediments to chromite ore processing residue (Table 1-2) (Vitale at al., 1994;  1997ab; 2000;
James 1994; James et al.,  1995).
              Table 1-2. Changes made in Method 3060.1
Change in Extraction Protocol
Wet sample wt. (g)
Alkaline digest solution volume (mL)
Solution to solid ratio
Digestion temperature (°C)
Digestion time (min)
Nitric acid acidification
Method 3060
100
400
4
Near boiling
30-45
pH7-8
Method 3060A
2.5
50
20
90-95
60
pH7-8,butif<7,
discard and start over
              ' After Vitale et al., 1994.
SW-846 Method 3060A delineates a MHT of 30-d prior to extraction. Vitale et al. (2000)
performed one of the few studies designed to specifically investigate the effect of sample holding
time on Cr(VI) extraction from contaminated solid matrices. They utilized soils contaminated
with low,  medium, and high levels of chromite ore processing residue (COPR) to follow Cr(VI)
extraction (Method 3 060A) concentration as a function of time (up to 30 days) from collection to
extraction. The relative percent difference (RPD) between holding times of 1-d to 30-d for low,
medium, and highly contaminated COPR soils were 7.4, 0.5, and 1.8%, respectively. Given that

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an RPD of >20% has been suggested as the maximum allowable variation between duplicates
without mandated re-extraction, the results of Vitale et al. (2000) clearly demonstrated Cr(VI)
stability in the COPR soils for at least 30 days when stored at 4°C.

Chromate analysis of solid matrix extracts may be analyzed by a number of methods (USEPA,
2000). Common methods of Cr(VI) detection are SW-846 Methods 7196A or 7199, which utilize
the reaction of Cr(VI) with diphenylcarbizide (DPC) to produce a red-violet complex whose
absorbance may be measured spectrophotometrically at 540 nm. The MHT for Cr(VI) extracts
prior to  analysis ranges from "as soon as possible" to 3 days (see footnote of Table 1-1)
depending on the method of analysis. The 24-h MHT associated with Method 7196A probably
arises from the prescribed (40 CFR, Part 136) holding time for aqueous Cr(VI) samples. Vitale et
al. (2000); however, investigated the Cr(VI) extract (Method 3060A/7196A) stability over a 7-d
period. They concluded that for the COPR soils investigated Cr(VI) extract stability over the 7-d
period was acceptable when extracts were stored in the dark at 4°C.

1.2 Semi-Volatile Organic Compounds

Reactions of pesticides and other semi-volatile organic compounds (SVOCs) in the soil
environment have been reviewed in great detail (Sawhney and Brown, 1989; Cheng, 1990 for
example). Of primary concern is that most organic compound concentrations will be reduced
with time as a result of biotic and abiotic reactions. Even at 4°C, most of these degradation
processes continue, albeit at a slower rate. For certain contaminants in a soil matrix; however, the
abiotic and biotic reactions are of limited concern up to and well beyond the MHT. For instance,
in a recent study of organochlorine pesticides in archived (air-dried) sludge-amended United
Kingdom (UK)  soils, half-lives of 8 pesticides ranged from 7 to 25 years (Meijer et al., 2001).
The authors suggested that volatilization was the major process causing pesticide concentration
depletion since microbial activity is typically minimal in air-dried soils. While these soils were
air-dried and stored in  sealed containers (unlike samples to be analyzed under SW-846), the
reported half-lives are  substantial and gives one pause regarding a 14 day until extraction, 4°C
MHT for pesticides as specified in SW-846.

In a recent study of selected polychlorinated biphenyls (PCBs) and polyaromatic hydrocarbons
(PAHs) in UK field soils (protected against leaching), slight increases in PCBs (congeners 28,
101, or 158) studied were observed (Cousins and Jones, 1998). The concentration increases were
attributed to gas phase deposition. Smith et al. (1976) and Moein (1976) studied an Aroclor 1254
spill site over a two-year time frame and observed no significant reduction. For studied PAHs,
the lighter molecular weight (MW) species (acenaphthene and phenanthrene) exhibited
statistically significant losses, while heavier MW species [fluoranthrene, and
benzo(ghi)perylene] showed no loss over a 281 day period.  In sludge-amended soils, half-lives
for naphthalene and benzo(ghi)perylene varied from 2.1 years to 9.1 years, respectively (Wild et
al., 1990; 1991).

A more recent study of historically contaminated soils investigated the impact of cold storage on
PAH extraction concentrations (Rost et al., 2002). Soil samples from two different sites exhibited
very different results. Quantitative recovery of PAHs from soil stored at 4°C in the dark was
observed throughout an 8 to 10 month holding time. Under identical storage conditions, a soil

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from a railroad sleeper preservation site exhibited significant losses of PAHs with low MW
compounds being more affected than the higher MW compounds. After only a 2 week holding
time, < 3-ring PAH concentrations had decreased by 29% to 73%; lesser but still significant
losses of up to 5-ring PAHs were also observed. Rost et al. (2002) demonstrated that PAH loss
was due to aerobic microbial metabolism as PAH loss was not observed in soil treated with
sodium azide prior to storage. In addition, stabilization against PAH loss was achieved by storing
the soil at -20°C.

1.3 Acid Extractable Heavy Metals

Acid digestion of solid matrices (e.g., soils, sediments) for the determination of heavy (trace)
metals concentrations is not a total digestion technique. According to SW-846 Method 3050B,
the extraction is designed to dissolve almost all elements that could become "environmentally
available". For non-redox sensitive trace metals (Cd, Cu, Pb, Zn, etc.), a hot acid extract will
probably be little affected in a time frame of years, which is  reflective of the 6 month MHT prior
to extraction. The aforementioned heavy metal contaminants are retained in soils by processes
(e.g., ion exchange, specific adsorption, precipitation etc.) that are extractable to the same extent
over long periods of time. The extraction method allows the  sample to be dried, but drying is not
required; however, sample homogeneity is typically more easily achieved with dried and sieved
materials.

1.4 Objectives

The overall objective of this research effort was to investigate the stability of selected
contaminants in soil/sediment samples as a function of holding time prior to extraction and
analysis. Contaminants  of interest centered on SVOCs, particularly PAHs, PCBs, and pesticides,
Cr(VI), and several heavy metals. Contaminant specific objectives were:

1.  Determine if selected S VOC contaminant concentrations in soil/sediment changed with time
   when held in storage beyond their established extraction  MHTs under current preservation
   techniques and at -20°C;
2.  Determine if Cr(VI) concentrations change when held in storage beyond their established
   MHTs under current preservation techniques and at -20°C;
3.  Determine if extracted Cr(VI) concentrations change when held beyond the analysis MHT
   (24-h) when held in the dark at room temperature (~ 20°C) or 4°C;
4.  Determine if air-drying soil samples will adversely impact hot acid extractable  metal
   concentrations;
5.  Determine if hot acid extractable metal concentrations change when samples are held beyond
   their established MHT.

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                                     Section 2


                           Materials and Methods


2.1 Soils/Sediments Identification, Collection and Selection

A total of 19 soils/sediments were collected for this study (Table 2-1). Except for the Sinclair
Inlet and SQ-1 sediment, samples of soils/sediments were obtained from contaminated sites
throughout the United States. The Sinclair Inlet sample was obtained from an ongoing study at
the Battelle Marine Sciences Laboratory and the SQ-1 sediment was obtained from J. Blazevich
(retired), USEPA Region 10, Manchester, WA.

The SQ-1 sample was a sediment sample collected from Sequim Bay, WA in 1986, an area
relatively free of contamination by PAH, PCBs, and chlorinated pesticides. The grain size and
carbon content was similar to that of contaminated sediment in urban areas around the Puget
Sound. Originally the sediment was placed in a cement mixer, spiked with a mixture of organic
chemicals, mixed 7 hours, subsampled for chemical analysis, bottled in 2-oz glass jars with
Teflon lined lids, and stored frozen at -20°C. The results for the post-mixing chemical analyses
indicated this reference material was homogenous (coefficient of variation, CVs, usually less
than 20%) and the recovery of the analytes was usually greater than 50% of the expected
concentration. Over a period of 10 years, between 1986 and 1996, several laboratories analyzed
between 20 to 80 jars of SQ-1 and recovered about 50% of the expected concentrations of most
of the analytes. The CVs for the mean of these results were about 50%.

Sediment samples were drained of excess water by vacuum filtration. Samples of each material
were semi-quantitatively screened for contaminant type and concentration. From the 19
soil/sediment samples identified, 12 materials were utilized during the course of the project
(Table 2-1; material in bold). Selection of materials for use was based on contaminants present,
their concentration, and the amount of material. For instance, the CIC New Jersey sample was
rejected for heavy metal study because only a single contaminant, arsenic, was present in
significant quantity, and after screening the quantity of <2 mm material was insufficient for the
study.

2.2 Experimental Design

The overall objective of this project is to provide scientific data on contaminant concentration
changes through time. The expected contaminant concentration changes through time should be
generally linear and potentially, curvilinear. Regression analysis  allows the estimation of an
equation relating contaminant concentration as a function of time. Regression analysis with
replication provides greater power in testing for a particular response (e.g., a linear relationship)
than does the equivalent design analyzed with an analysis of variance (ANOVA). The increased
power for testing in the regression is directly related to the increased number of degrees of
freedom for the error term. For example, for six analysis time points with two replicates at each
time and a linear response, Table 2-2 shows that there are only six degrees of freedom for testing

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the linear (or curvilinear) response with an ANO VA compared to ten degrees of freedom (nine if
a quadratic term is needed) in the regression analysis. Regression analysis, on the other hand,
specifically tests for a consistent change through time (either linear or curvilinear).
      Table 2-1. Available soils/sediments.

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
Sample
Housatonic River
Tri-Cities NY2
Eagle Harbor
SQ-1
Bedford- 1
Bedford plot-6
Frontier Hard Chrome Site-2
Boomsnub site-0.5'
Boomsnub site-3.0'
Boomsnub site-5.5'
Stratford, CT Army engine plant
Sinclair Inlet, WA
Wilmington, NC
Eastland Woolen Mills, ME
Richland site-1
Frontier Hard Chrome Site-1
EPA-Athens
EPA-Athens
CIC New Jersey
Sample type
Freshwater sediment
Soil
Soil
Marine sediment
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Marine sediment
Soil
Soil
Soil
Soil
Soil
Soil
Soil
Suspected contaminants
PCBs/Pesticides
PCBs/Pesticides
PAHs
PAHs/PCBs/Pesticides
PAH
(XVI)
(XVI)
(XVI)
(XVI)
(XVI)
(XVI)
SVOCs/Metals
PAHs/Metals
DDT, DDE, Dieldrin
Several Pesticides
(XVI)
(XVI)
Cl-Pesticides
Metals
     Table 2-2. Comparison of analysis of variance and regression assuming six time points for chemical
               analysis, two replicate analyses at each time, and a linear relationship.
Analysis of Variance
Sources of Variation
Mean
Times (t)
Linear3
Remainder
Within Timesb
Total
Degrees of Freedom
1
(t-1) = 5
1
4
t*(r-l) = 6
t*r= 12
Regression Analysis
Sources of Variation
Mean
Slope = bi
Remainder13
Lack of Fit0
True Error
Total
Degrees of Freedom
1
1
t*r - 2 = 10
4
t*(r-l) = 6
t*r= 12
      " The indented sources of variation represent the splitting of the main source of variation (not indented) listed above.
      b Error for testing the null hypothesis that the slope equals zero.
      c The sum of the degrees of freedom from the split sources of variation equal the degrees of freedom for the main source of
       variation listed above.
Regression analysis has the added advantage of being able to estimate a spline point where the
relationship may change abruptly.

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2.2.1 Soils/Sediments Homogenization, Analysis, Storage and Extraction
      Schedule
An experimental design based on regression analysis was constructed. The design consisted of
initial (T = 0) extraction and analysis of multiple subsamples (4 SVOCs; 5 CrC>4, and metals),
which were followed by extraction and analysis of four subsamples (two per storage technique;
see below) at multiples of the analyte's MHT.

The selected soils/sediments were hand-screened (< 2mm) to remove rocks and twigs. The 12
sediment/soil samples were homogenized by hand through repeated cone and quartering and
recompositing the sieved material. Materials were then subsampled (cone and quartered) for
characterization of water content, total organic carbon content (by combustion; Nelson and
Sommers 1996), particle size analysis (hydrometer method; Gee and Bauder 1986), and  pH
determined from a 1:1 soil:water mixture with a combination glass electrode (Thomas, 1996).

The selected soils/sediments were hand cone and quartered to obtain T = 0 samples. Initial (T =
0) sample extraction and analysis was performed on 4  (SVOCs) or 5 [Cr(VI) and metals]
subsamples of a given sediment/soil. After subsampling for T = 0 samples, remaining materials
were cone and quartered until a given subsample mass, at least 12 times the mass required for a
given extraction, was obtained. This material was quartered and each quartered subsample placed
in either a glass jar with Teflon-lined lid  (SVOCs extraction) or polycarbonate centrifuge tubes
(CrO4 and metals) and stored under specific conditions (depending on contaminant type). This
procedure was performed repeatedly until four subsamples for each holding time were obtained
(the number of MHT elements depended on the contaminant(s) under study). The storage
conditions and sampling times were as follows:

• The chromate holding time study utilized soil/sediment numbers 6-11 (Table 2-1). Twelve
  samples of each soil/sediment were stored at 4°C and 12 samples at -20°C. For each holding
  time, two containers (duplicates) were analyzed for each holding condition (4°C and -20°C).
  Specifically, the MHT multiples were 0, 0.5*MHT, MHT, 2*MHT, 4*MHT, and 8*MHT.
  These MHT multiples were equivalent to 0, 14, 28, 56, 112, and 224 days, respectively.

• In addition to following the stability of CrO4 as a function holding time prior to extraction, the
  stability of the CrO4 extract concentration was followed with time. At T = 0, the CrO4
  concentration was determined in the initial 5 extracts within 24 hrs of extraction. The
  remaining extract solutions, standards, laboratory blanks, and matrix spikes were placed in
  brown glass bottles and stored room temperature. Another 5 subsamples were extracted (with  a
  new set of standards, laboratory blanks, and matrix spikes), and the T = 0 CrO4 concentration
  in each extract determined. This second set of extract solutions, standards, laboratory blanks,
  and matrix spikes were placed in brown glass bottles and stored at 4°C. The Cr(VI) extracts
  were analyzed at 1, 3, 7, 14, 28, and 56 days. Extracts from sediment/soil numbers 7-10 were
  utilized for this study  (Table 2-1).

  The SVOC holding time study utilized soil/sediment numbers  1-5 (Table 2-1). Twelve samples
  of each soil/sediment were stored at 4°C and 12 samples were  stored at -20°C. For each
  holding time, two containers (duplicates) were analyzed for each holding condition  (4°C and

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  -20°C). Specifically, the MHT multiples were 0, 0.5*MHT, MHT, 2*MHT, 3*MHT, 6*MHT,
  and 12*MHT. These MHT multiples were equivalent to 0, 7, 14, 28, 42, 84, and 168 days,
  respectively.

• The Sinclair Inlet sediment and the Wilmington, NC soil were used to study the stability of As,
  Cu, Pb, and Zn as a function of holding time and solid material drying treatment (soil/sediment
  numbers!2 and 13 in Table 2-1). Eight samples were stored at 4°C and 8 samples were air-
  dried for 5 days, crushed, sieved (<2 mm) and stored at room temperature. Duplicate samples
  of the material stored at 4°C  and air-dried samples were extracted and analyzed at multiples of
  the MHT (0, 0.5*MHT, MHT, 1.5*MHT, and 2*MHT); equivalent to 0, 90, 183, 284, and 392
  days.

2.2.2 Cr(VI) Extraction and Analysis
Chromate extraction of all soils/sediments was performed strictly according to SW-846 Method
3 060A-Alkaline Digestion for Hexavalent Chromium.  Analysis of the sediment/soil extracts was
conducted according SW-846 Method 7196A-Chromium, Hexavalent (colorimetric). The
colorimetric procedure was performed as prescribed except that in the interests of waste
minimization the colorimetric solutions (analyte solutions, standards,  laboratory standards, and
QA solutions) were produced in 10 mL volumes rather than the suggested 100 mL volume.
Colorimetric determinations were performed using a Perkin-Elmer Lambda 19 dual beam
spectrophotometer. QA reviewed data tables are provided in Appendix A.

2.2.3 SVOC Extraction
Housatonic River; Tri-Cities, NY; Eagle Harbor; SQ-1; and Bedford-1 soils/sediments were
extracted using SW-846 Method 3540C-Soxhlet Extraction, a procedure for extracting
nonvolatile and semivolatile organic compounds from  solids. A deviation from this method was
implemented for samples SQ-1 and Bedford-1 because the high moisture content of these
samples caused incomplete extraction using the Method 3540C-Soxhlet Extraction. A thumbnail
sketch of the procedure and the deviations are noted below for each of the soils/sediments.

Housatonic River, Eagle Harbor, and Tri Cities — Ten g of sample was mixed with 10 g
anhydrous Na2SO4 in a 125 mL Qorpak jar,  100 mL of methylene chloride was added; and the jar
rolled on a modified rock tumbler for 2 h. This mixture was transferred to a Soxhlet thimble and
put into the Soxhlet extractor. The jar was rinsed three times with 50 mL methylene chloride and
the rinsate added to the thimble. The soil/sediment was extracted overnight with 350 mL
methylene chloride. The following day, the extract was evaporated using a Kuderna-Danish
apparatus to <25 mL. The solvent exchanged to hexane, transferred to a 25 mL volumetric flask,
and brought to volume using hexane. Activated copper was added to 1 mL (Housatonic River
and Tri-Cities) or 2 mL (Eagle Harbor) of the resultant solution to remove the sulfur interference
as described in SW-846 Method 3660B-Sulfur Cleanup Method. Deviations to SW-846 Method
3660B were:

• 0.2 mL of the  copper treated Housatonic River extract or 0.05 mL Tri-Cities extract was
  placed on a conditioned Florisil column and eluted with 9 mL of 1:9 acetone:hexane mixture
  as described in SW-846 Method 3620-Florisil Cleanup. The eluate was evaporated to 1.0 mL
  and 100 |jL of internal standard PP-1195  was added.

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• 1.0 mL of the copper treated Eagle Harbor extract was placed on a silica column as described
  in SW-846 Method 3630C-Silica Gel Cleanup. The column was pre-eluted with 40 mL
  pentane and the pentane discarded. One mL of sample was added to the column and eluted
  with 25 mL pentane. This fraction was then discarded. 25 mL of 2:3 methylene
  chloride:pentane solution was added to the column and this fraction was collected in a Qorpak
  jar. The solution was then transferred to the Kuderna-Danish evaporator, solvent exchanged to
  cyclohexane, evaporated to 1.0 mL, and 100 (jL of internal standard PP-1195 was added.

SQ-7 — Initially, a 15 g sample was mixed with 10 g anhydrous Na2SO4 and  10 g activated
copper in a  125 mL Qorpak jar. One hundred mL of methylene chloride was added to the jar and
the jar rolled on a modified rock tumbler for 2 h With the exception of the initial step, the  SQ-1
sediment followed the protocol used for Housatonic River, Eagle Harbor and Tri Cities
soils/sediments.

Bedford-1  — Due to limited amount of soil, 5 to 6 g of soil was utilized for each subsample.
The mass of soil was placed in 250 ml Qorpak jars. Prior to extraction, 0.5 g of sample was
removed from the jars to determine percent dry weight. One hundred mL of methylene chloride,
10 g activated copper and 50 g anhydrous Na2SO4 were added. The vessel was shaken vigorously
then put on  a modified rock tumbler for two hours to homogenize the components. The
suspension  was transferred to a Soxhlet thimble and put into the Soxhlet extractor. The jar was
rinsed three times with 50 mL methylene chloride and the rinsate added to the thimble. The soil
was extracted overnight with 350 mL methylene chloride. The following day the sample was
evaporated  using a Kuderna-Danish apparatus to 25 mL, solvent exchanged to hexane, and again
treated with activated copper as described in SW-846 Method 3660B-Sulfur Cleanup. 0.5 mL of
the  extract was placed on the Florisil column as  described in SW-846 Method 3620-Florisil
Cleanup and 0.5 mL was placed on the silica column as  described in SW-846 Method 3630C-
Silica Gel Cleanup. Both eluates were evaporated using  a Kuderna-Danish apparatus to 1.0 mL,
solvent exchanged to cyclohexane, and 0.1 mL of laboratory produced internal standard was
added.

2.2.4 SVOC Analysis
All  SVOC extracts were analyzed prior to the SVOC 40 day MHT. Polyaromatic hydrocarbon
analysis of the SVOC extracts followed SW-846 Method 8270C-Gas Chromatography/Mass
Spectrometry (GC/MS) with specifications and modifications as noted. PAHs were separated via
high resolution capillary gas chromatography and identified and quantified using electron impact
mass spectrometry. A data system interfaced to the GC/MS was used to control acquisition and
to store, retrieve, and manipulate mass spectral data. The PAHs listed in Table 2-3 were
identified and measured in selected ion monitoring mode (SIM). Tuning followed the parameters
from the instrument manufacturer, which uses a compound PFTBA that is bled into the
instrument.  Inertness of the system was assessed using linearity and calibration check
compounds (CCCs). The only deviation from SW-846 protocol was for sensitivity and
compound degradation, which was addressed via other system checks, not specifically by a
system performance check compound (SPCC). QA reviewed data tables and QA narratives are
provided in the Appendix A.

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         Table 2-3. PAH Analyte List
Analyte
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo[a]anthracene
Chrysene
Benzo [b]fluoranthene
Benzo [kjfluoranthene
Benzo [e]pyrene
Benzo [a]pyrene
Perylene
Indeno [ 1,2,3 -c,d]pyrene
Dibenzo [a,h] anthracene
Benzo [g,h,i]perylene
Surrogate Standards
Naphthalene-dg
Acenaphthene-di 0
Phenanthrene-dio
Chrysene-di2
Perylene-d12
Internal Standards
Acenaphthylene-dg
Pyrene-dio
Benzo [a]pyrene-di 2
Quantitation Ion
128
152
154
166
184
178
178
202
202
228
228
252
252
252
252
252
276
278
276
Quantitation Ion
136
164
188
240
264
Quantitation Ion
160
212
264
Confirmation Ion
127
153
153
165
139
176
176
101
101
226
226
253
253
253
253
253
277
279
277
Confirmation Ion
137
162
184
236
265
Confirmation Ion
161
106
265
10

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Table 2-4. PCB (Aroclors and Congeners) and chlorinated pesticide analyte list.
PCBs - Aroclors
Aroclor 1242 (or 1016)
Aroclor 1248
Aroclor 1254
Aroclor 1260
PCB - Congeners
CB Number3
    8
    18
    28
    29
    44
    49
    50
    52
    66
    87
    101
    104
    105
    118
    126
    128
    138
    153
    154
    170
    180
    183
    184
    187
    188
    195
    200C
    206
    209
CAS Nomenclature13
2,4'-dichlorobiphenyl
2,2',5-trichlorobiphenyl
2,4,4'-trichlorobiphenyl
2,4,5-trichlorobiphenyl
2,3 ',3,5'-tetrachlorobiphenyl
2,2',4,5'-tetrachlorobiphenyl
2,2' 4,6'-tetrachlorobiphenyl
2,2',5,5'-tetrachlorobiphenyl
2,3'.4,4'-tetrachlorobiphenyl
2,2' 3,4,5'-pentachlorobiphenyl
2,2',4,5,5'-pentachlorobiphenyl
2,2',4,6,6'-pentachlorobiphenyl
2,3,3 ',4,4'-pentachlorobiphenyl
2,3',4,4',5-pentachlorobiphenyl
3,3 ',4,4',5-pentachlorobiphenyl
2,2',3,3',4,4'-hexachlorobiphenyl
2,2' 3,4,4',5'-hexachlorobiphenyl
2,2',4,4',5,5'-hexachlorobiphenyl
2,2',4,4',5,6'-hexachlorobiphenyl
2,2',3,3',4,4',5-heptachlorobiphenyl
2,2',3,4,4',5,5'-heptachlorobiphenyl
2,2',3,4,4',5',6-heptachlorobiphenyl
2,2',3,4,4, 6,6'-heptachlorobiphenyl
2,2',3,4',5,5',6-heptachlorobiphenyl
2,2' 3,4' 5,6,6'-heptachlorobiphenyl
2,2',3,3',4,4',5,6-octachlorobiphenyl
2,2',3,3',4,5',6,6'-octachlorobiphenyl
2,2'3,3',4,4',5,5',6-nonachlorobiphenyl
2,2'3,3',4,4',5,5',6,6'-decachlorobiphenyl
CAS Registry Number0
     34883-43-7
     37680-65-2
      7012-37-5
     15862-07-4
     41464-29-5
     41464-40-8
     62796-65-8
     35693-99-3
     32598-10-0
     38380-02-8
     37680-73-2
     56558-16-8
     32598-14-4
     31508-00-6
     57465-28-8
     38380-07-3
     35065-28-2
     35065-27-1
     60145-22-4
     35065-30-6
     35065-29-3
     52663-69-1
     74472-48-3
     52663-68-0
     74487-85-7
     52663-78-2
     40186-71-8
     40186-72-9
      2051-24-3
   a Ballschmiter and Zell numbering scheme.
   b Chemical Abstracts, Tenth Collective Index, Index Guide, American Chemical Society, Columbus, Ohio, 1982.
   c CB 200 in the Ballschmiter and Zell numbering scheme.
                                                                                                 11

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         Table 2-4, Continued
         Chlorinated Pesticides
         Aldrin
         alpha-BHC
         beta-BHC
         gamma-BRC (Lindane)
         delta-BKC
         4,4'-DDE
         4,4'-DDD
         4,4'-DDT
         (cis) alpha-Chlordane
         (trans) gamma-Chlordane
         Tech. Chlordane
         Dieldrin
         Endosulfan I
         Endosulfan II
         Endrin
         Endrin Aldehyde
         Endrin Ketone
         Heptachlor
         Heptachlor Epoxide
         Toxaphene
         Endosulfan Sulfate
         Hexachlorobenzene
         2,4'-DDD
         2,4'-DDE
         2,4'-DDT
         Mirex
         trans-Nonachlor
         Surrogate Standards
         PCB 103
         PCB 198
         Internal Standards
         Tetrachloro-/w-xylene (TCMX)
         Octachloronaphthalene (OCN)
         Hexabromobiphenyl (HBB)
Analysis of chlorinated pesticides followed SW-846 Method 8081 A. Analysis of poly chlorinated
biphenyls (PCBs) as Aroclors or individual congeners followed SW-846 Method 8082. Both
analyses utilized capillary gas chromatography with 63Ni electron-capture detection. The internal
standards were monitored closely indicating volume changes, system changes, injector changes,
12

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and linear condition but if outside data quality objectives (DQOs), the analytical run was allowed
to complete and then assessed with surrogates and spike recoveries. QA Reviewed data tables
and QA narratives are provided in the appendix. Table 2-4 lists the PCBs and pesticides targeted.

2.2.5 Metal Digestion (Acid-Leachable) and Analysis
The Wilmington soil and Sinclair Inlet sediment samples were digested using the acid-leachable
digestion detailed in SW-846 Method 3051-Microwave Assisted Acid Digestion of Sediments,
Sludges, Soils, and Oils. Digestates were analyzed via SW-846 Method 6020-Inductively
Coupled Plasma-Mass Spectrometry. The method measures ions produced by a radio-frequency
inductively coupled plasma. Analyte species originating in a liquid are nebulized and the
resulting aerosol transported by argon gas into the plasma torch. The ions produced are entrained
in the plasma gas and introduced, by means of an interface, into a mass spectrometer. The ions
produced in the plasma are sorted according to their mass-to-charge ratios and quantified with a
channel electron multiplier. There were no deviations from the aforementioned protocols. QA
reviewed data tables and QA narratives are provided in the Appendix A.

2.3 Statistical  Analysis

Descriptive statistics including the mean, standard deviation, minimum, maximum, median, and
data quartiles (first quartile, Ql, equals the 25th percentile and the third quartile, Q3, equals the
75th percentile) were calculated for each sampling period and holding condition. The mean,
standard deviation, and CV (equal to the standard deviation divided by the mean) were also
calculated for all data collected for a given holding condition.

Overall CVs of less than 20% for CrO4 and metals, and 25% for SVOCs  suggest that data has
remained within the data quality acceptance criteria for replicate precision (Table 2-5). Even
though trends may be statistically detected in such data, it would be suspect due to the normal
analytical  error that can be observed in chemical analysis. For analytes measured within this
level of noise, one would suggest that the concentration did not decrease more than would be
allowed between replicate measurements over the entire time period tested. For these analytes,
estimation of a holding time from this experiment could be considered impractical.

A one-sample, one sided, t-test of the null hypothesis Ho: the data are samples from a population
with a mean equal to or greater than the mean of the Day 0 concentration versus the alternative
HI: the samples are from a population with a mean less than the mean of the Day 0
concentration, was conducted to provide a  measure of relevance (chemical importance) of the
potential change. Simple linear regression of concentration against time was used to test 1) the
null hypothesis that the slope of the natural logarithm of the concentration of each contaminant
was equal to zero and 2) the null hypothesis that slopes associated with curvature (the lack-of-fit
to the simple linear model) were equal to zero. Plots were used to compare the observed
concentration to the nonparametric upper and lower boundaries of the Day 0 concentration
calculated as Q3+ 1.5(Q3-Q1) and Q1-1.5(Q3-Q1), respectively. The fitted regression line was
included in data plots if the slope was negative and statistically different  from zero.

The holding time (HT), defined as the number of days until a 5%, 10% and 20% decrease in the
natural logarithm of the concentration from the intercept  of the regression (Co), was calculated
                                                                                      13

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based on the lower 95% confidence limit of the slope estimate (PLCL). Thus, holding time for a
given percentage change (A%) was defined as HT = -A%*CO/PLCL- Using the lower 95%
confidence limit of the linear slope provides some conservatism to the holding time estimation
because as the data increasingly deviate from a simple linear response, the confidence interval
increases and the slope used for estimation becomes steeper. When the estimated PLCL was
greater than 0, the concentration was estimated to be increasing instead of decreasing and the
number of days until a given percentage lost was not applicable (NA). All of the analytes tested
were assumed to only decrease over time since none of the analytes measured were considered a
degradation product.

Chemical  concentrations tend to be log normally distributed. Thus, analysis was conducted on
the natural logarithm of the concentration to satisfy assumptions of the statistical analyses.
Further, the natural logarithm  of the concentration was used instead of the raw data scale because
sediments have varying amounts (i.e., 50 to 800 mg/kg) of a given analyte. The natural log
transformation rescales the observations to minimize the magnitude of the difference between the
Day 0 value and the value obtained at a given percentage change. A percentage change (i.e.,
10%) from a large number (say 800) has a larger magnitude difference (800-720=80) than the
same percentage change from a small number (50-45=5). Thus, on the raw data scale, analytes
with the same slope associated with the decrease in concentration over time but different
intercepts  would produce quite different estimates of the holding time. The natural log
transformation reduces this effect (i.e., ln[800]-.9*ln[800]=0.67 compared to ln[50]-
.9*ln[50]=0.39). The resulting holding times would still be different; however, the magnitude of
the difference would be much less than that achieved on the raw scale.

Observations were removed from data analysis including plots if they were potentially
contaminated (flagged with a B) or rejected for QC/QA reasons (flagged with an r). Analysis was
conducted with and without observations considered extreme outliers, defined as Q3 + 3*(Q3-
Ql) where the quartiles are derived from the Day 0 data. Extremely high outliers have a large
influence on the estimated  slope and, thus, the resulting holding time. Outliers in the Day 0 data
were removed from analysis and plots if the within replicate CV was greater than 25%.
Observations were removed from the Day 0 data only if a single value was extreme and if that
value was the furthest absolute distance from the median value. Extreme outliers observed during
all other sampling times were  removed from the analysis only if they made up less than  10% of
the total number of observations.

Residual plots were used to assess the lack of homogeneity of variance, lack-of-fit to the linear
model, potential outliers, and observations that could have exaggerated influence on the
estimated  slopes. Residuals, defined as the observed minus the fitted result, are assumed to have
a mean of zero and a constant variance. Residuals plotted against time should display a random
pattern about zero with  a constant variance across the x-axis. A consistent U-shaped pattern of
the residuals would indicate the need for curvature in the model if a significant (p < 0.05) lack-
of-fit was  detected. The need for a spline or nonlinear model could also be indicated by  a
significant lack-of-fit. However, if the concentration decreased and then increased over time, the
lack-of-fit was considered analytical noise. In these cases, the simple linear model was used for
the holding time estimation. A single observation that has a large amount of influence on the
estimated  slopes would be  indicated by a residual close to zero and far away on the x-axis from
14

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all other observations. Observations with too great an influence on the estimation of the slope
were removed from the analysis.

The intent of this analysis was to provide a progression of four distinct ways to evaluate a
possible decrease in the concentration of an analyte (lines of evidence). First, the magnitude and
variability of the concentration was used to suggest a level of the signal to noise ratio; second a li-
test of the Ho:overall mean equal to or greater than the Day 0 mean was used to provide a level of
relevance to observed change; third a regression against time was used to estimate a rate of
change; and fourth a nonparametric upper and lower bound based on the  Day 0 quartiles was
used to provide an alternative measure of relevance to the potential change through time. When
the t-test is not significant, the slope from the regression is not significant, and the data remain
within the nonparametric bounds, all three methods suggest a lack of degradation over the period
tested. However, when at least one of the methods differ in their results, the sensitivity and
assumptions of each method must be evaluated to sort out the most likely outcome.

The t-test uses the variability observed in all of the data to determine significance and does not
evaluate whether or not a trend over time is present. Thus, if the data is highly variable, the
probability of rejecting the null hypothesis is low even though a significant trend of decreasing
concentration may exist. The regression analysis is sensitive to detecting a linear degradation.
Thus, if the pattern of degradation is not linear, the regression analysis may not detect it. A
threshold point associated with different rates of degradation over time could cause a simple
linear regression to be not significant. However, the lack-of-fit to a simple linear regression
would be detected. Finally, the nonparametric bounds  are based  on the variability observed in the
Day 0 data. When the Day 0 variability is high, the boundaries will be wider than when the Day
0 variability is low.

Statistical versus Chemical Significance'. The determination  of statistical significance in
hypothesis testing means that a value greater than or equal to that observed of a specific statistic
has a small probability of occurring by chance alone. The definition of small is used to define the
level of significance and is usually set at a = 5%. The  probability of occurrence of the achieved
value or one greater of the statistic (p-value) is calculated based  on specific assumptions about
the distribution of the statistic assuming the null hypothesis is true. The decision to reject a null
hypothesis (reject if the achieved p-value is less than a) for a defined  alternative is based on the
level of significance chosen before analysis. However, presenting the  achieved p-value allows
one to assess the potential biological or chemical significance of the result as well.

The chemical significance of a result is a function of the minimum detection limit (MDL) in
comparison to the observed concentration and the analytical variability associated with the type
of analyte being measured (metals versus organics, for example). Concentrations close to the
MDL (defined as 2 times the MDL = 2*MDL) may exhibit a greater analytical variability than
concentrations further away from the MDL. A chemically significant  result requires that the
observed variability is greater than the analytical variability alone. For metals and organic
analytes replicate results must have a CV of less than 20% and 25%, respectively, to meet quality
control criteria for extraction variability. If all observed concentrations for a given analyte across
time display a CV of less than or equal to the analytical criteria of replicates, then any detected
statistical significance is within the noise of analytical variability and  could be spurious. If the
                                                                                        15

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achieved p-value for the test of a significant slope is close to 0.05, then the estimated slope may
be considered a curious trend. However, if the achieved p-value is very small (< 0.01), then the
observed trend should be considered chemically relevant even though all observations were
within the allowable analytical noise.

2.4 General  Data Quality Objectives

The data quality objectives are discussed in detail in the project's Quality Assurance Project Plan
(QAPP). This plan was developed based on the QA/QC requirements associated with the
different SW-846 methods utilized in this study. Of particular importance was the matrix spike
recovery and replicate precision for the individual methods (Table 2-5).

Matrix spike recovery was essential in detecting potential problems during extraction and
analysis. The concentration of the matrix spike was targeted at four times an analyte's estimated
indigenous concentration; the initial estimate of the indigenous concentration was determined
from preliminary semi-quantitative extraction and analysis. If the initial matrix spike was below
a factor of four of the extracted analyte's concentration the matrix spike was increased for the
next extraction time. As will be seen in the case of Cr(VI) extraction and analysis, the matrix
spike recovery was essential to problem identification of Cr(VI) extraction and detection.

Replicate precision was measured as the percent coefficient of variation (CV; the standard
deviation divided by the mean). Replicates are typically defined as extraction of multiple
samples of the same soil/sediment during the course of an extraction process. As discussed in
section 2.3; however, extractions data across the life of the study (e.g.,  168 days for SVOCs)
were pooled and an overall CV calculated as a method of comparison to the SW-846 prescribed
replicate precision metric listed in Table 2-5. This comparison was utilized in this study as the
initial measure of variability across time.
   Table 2-5. Summary of general data quality objectives.
Method
GC-MS (SIM) 8270C
8081/8082
90601
6010/6020
3060A/7196
Analytes
SVOC (PAHs)
Chlorinated Pesticides/PCBs
Total Organic Carbon
Metals
Cr(VI)
Spike Recovery
40-120%
40-120%
NA
75-125%
85-115%
Replicate Precision
<25%
<25%
<20%2
<20%
<20%
    1 EPA Method 9060 for TOC in water samples was adapted to soil and sediment TOC extract determination.
    2 Based on TOC by difference; RPD is the E of the RPD for TC and TIC; the RPD is typically much smaller than 20% but is
     dependent on homogeneous nature of sample and the amount of TOC.
16

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                                     Section 3

                           Results and Discussion
3.1  Chromate [Cr(VI)]

Based on preliminary qualitative extraction and analysis (no blanks, matrix spikes etc.), six soils
were chosen for the Cr(VI) extraction holding time study. The general physical and chemical
characteristics of the soils are presented in Table 3-1. The dissolved organic carbon (DOC)
values were determined after filtration and pH adjustment to 7.5 ± 0.5 of the extract solutions.
The soils exhibited circum neutral pH, fairly oxidized, and limited in clay content. The DOC
extracted from the Bedford plot-6  soil was exceptionally high and proved to be a confounding
factor in Cr(VI) extraction and analysis (discussed below). The Boomsnub site soils (125A,
125B, and 125C) and the Frontier  Hard Chrome site (126D) T = 0 extracts were utilized in the
extract stability  study.

3.1.1  Spike Recovery Anomaly: Bedford Plot-6 Soil
Determination of the T = 0 Cr(VI) extract concentration and necessary blanks and matrix spikes
for each of the extracted materials was acceptable (i.e., blanks and spikes fell within the
prescribed range) except for the Bedford plot-6  soil. Recovery of the matrix soluble and
insoluble spike for the Bedford plot-6 T = 0 extractions was very low (1 to 5%). According to the
SW-846 Method 3060A QA/QC procedures, the soil was rehomogenized  and the extraction
repeated. Similar results were obtained. As per SW-846 Method 3060A, the soil's total  organic
carbon (TOC), Fe(II), and sulfide  concentrations were determined. The TOC content was
16.24% and the  extract DOC was  393 ±16.8 mg/L. No evidence of sulfide was found. The soil's
ferrous iron content was estimated to be 14.52 ± 0.29 mg Fe(II)/g sediment following ASTM
Method D 3872-86, Standard Test Method for Ferrous Iron in Iron Oxides (ASTM, 1986).

The ASTM method uses an HC1 acid extraction of the soil under a constant stream of N2(g)
followed by a titration of the extract with a standard solution of K2Cr2Oy.  The amount of Cr(VI)
reductive power in the Bedford plot-6 sample estimated by the ASTM titration was more than
enough to reduce the Cr(VI) added to the soil in the matrix spike. It did not;  however, explain the
apparent presence  of Cr(VI) in the colorimetric extract determinations where, if all the Cr(VI)
was reduced, no Cr(VI) should have been detected. The approximate 0.20 to 0.30 absorbance
units (au), which translated to 15.9 ±4.1 mg Cr(VI)/kg soil, appeared to be the result of the high
DOC content of the extracts. This  hypothesis was supported by the fact that measurement of
absorbance at 540  nm yielded the  same response (-0.25 au) whether the extract absorbance was
measured directly without pH adjustment and addition of diphenylcarbazide, with pH adjustment
only, or as prescribed in SW-846 Method 7169A (Fig. 3-1). Further, the UV/Vis spectrum of the
extract exhibited the classic broad, slowly decreasing spectrum common to extracted organic
carbon. The absorbance spectra of humic substances are seen as generally featureless, smooth
curve whose absorbance decreases from about 400 nm to about 900 nm (Swift, 1996). At 540
nm; however, the DOC  concentration of this extract was high enough that its absorbance was
                                                                                    17

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significantly above background (-0.02 au). As a result of these data, DOC was determined for
each of other five extracts (Table 3-1).
       Table 3-1. Chromate [Cr(VI)] extraction study soil/sediment properties.

Sediment

Boomsnub site-0.5' (125A)
Boomsnub site-3.0' (125B)
Boomsnub site-5.5' (125C)
Frontier Hard Chrome Site-2 (126D)
Stratford CT, engine plant (123)
Bedford plot-6

pH

6.2
6.4
5.4
5.3
7.1
6.8
Eh


286
284
340
442
436
570
oca


1.27
1.49
0.30
0.13
0.09
16.2
Sand
	 o/

56.9
55.8
52.6
94.6
82.0
NDb
Silt


33.8
35.4
38.8
4.56
16.7
ND
Clay


9.3
8.8
8.6
0.84
1.3
ND
DOCa

mg/ij
75.7
76.3
17.6
10.7
6.0
393
        a Reported values are extract dissolved organic carbon performed after filtration and are the mean of triplicate
         measurements.
        b ND = nodata.
               1.5
          \\        \        \        \        \
          — Cr(VI) extract analysis - Method 7196A

                	   extract + diphenylcarbazide

                            1000 ng/L Cr(VI) standard
                                  	  extract only
            4*
            u
            a
            o
            VI
1  -
               0.5  -
                 0  -
                 350    400    450
                         500     550
                              nm
600     650
700
     Figure 3-1. UV/Vis spectra of (a) Cr(VI) 1000 mg/L standard, (b) Bedford-6 Cr(VI) extract
               solution, (c) Bedford-6 Cr(VI) extract solution and diphenylcarbazide, and (d) Bedford-
               6 extract solution prepared as prescribed by SW-846 Method 7196A.
None of the other soils extracted in this study exhibited significant background absorbance.
18

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To further investigate the Bedford plot-6 extract matrix spike anomalies, three Bedford plot-6
soil samples were extracted, filtered and pH adjusted (according to the extraction technique
prescribed by SW-846 Method 3060A) and then four subsamples of each extract were spiked
with increasing concentrations of Cr(VI); approximately 0, 2000,  6000, or 10,000 (ig/L (Table
3-2). After approximately two hr, these solutions were analyzed according to SW-846 Method
7196A and SW-846 Method 601 OB-Inductively Coupled Plasma-Atomic Emission Spectroscopy
(ICP-AES). The absorbance of the spiked samples through 6000 ng/L Cr(VI) exhibited no trend
of increasing absorbance with increasing Cr(VI) addition. However, there was a consistent, albeit
small increase in absorbance with the 10,000 [ig/L spike (Table 3-2). Based on the standard
additions, the absorbance of the extracts should have increased from approximately 0.33 au to
well over 1.3 au. and required dilution at the higher two spiking concentrations. Comparison of
the  spiked Cr(VI) concentration (calculated, Table 3-2), the colorimetric concentration, and ICP-
AES determined Crtotai showed that Cr(VI) was being reduced by the extracts. The slight increase
in Cr(VI) concentration (absorbance) at the highest Cr(VI) spiking suggested that the extract
solution's reductive potential was approaching exhaustion. The discrepancy between the
calculated Cr(VI) additions and that determined by ICP-AES was probably related to formation
and subsequent settling of Cr(OH)3 as the Cr(VI) additions increased.

Hence, we concluded that the Cr(VI) reductive ability of this sediment was extractable. While
the  Cr(VI) reduction could have been the result of Fe2+ present in the mineral phases or
complexed with the DOC, it could also have been present as reduced quinone moieties
associated with the DOC (Scott et al. 1998). In addition, the positive initial semi-quantitative
screening for Cr(VI) in the Bedford plot-6 soil was probably the result of extracted DOC. Any Cr
in this soil was probably in the reduced Cr(III) state, and based on the ICP analysis of the zero
spike addition the Cr(III) concentration was extremely low (Table 3-2). While a number of
interesting questions remain (i,e, the nature of the Cr(VI) reducing agent(s), and the reducing
capacity of the soil), addressing these issues was beyond the scope of this study.

3.1.2 Cr(VI)  Extraction
Extractable concentrations of Cr(VI) were characterized through time for each of the remaining 5
soils and holding temperatures (Appendix A-Table A-l). Soil  125C had the lowest concentration
of Cr(VI) averaging 64 mg/kg while soil 126D had the highest concentration averaging 830
mg/kg (dry weight) for all treatments and holding times. The CV for the day 0 replicates ranged
from 2% to 13%, which were within the <20% CV for replicate precision (Table 3-3). In fact,
only one soil (125A at 4°C) exhibited a CV greater than the 20% CV necessary for replicate
precision for all data across time (Table 3-3). For the 125 A soil at 4°C, the overall CV of 34%
was the result of two time period duplicates were widely variant at Days 28 and 224 (Fig. 3-2).
Based solely on SW-846 Method 3060A requirement for replicate precision (CV<20%), the
overall CV values suggest that all extraction results for a given soil had acceptable precision
between replicates regardless of extraction time.
                                                                                      19

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           Table 3-2. Cr(VI) analyses of three Cr(VI) spiked Bedford-6 soil extracts.
Sample1
Calculated spiked
Cr(VI) Cone.
Hg/L
Colorimetric analysis of Cr(VI)
spiked solutions2
Absorbance (au3)
Hg/L
ICP-AES Cr
analysis
Hg/L
1A
IB
1C
ID
0
1965
5871
9914
0.360
0.331
0.346
0.399
446
426
447
521
75.9
1623
4732
7999
2A
2B
2C
2D
0
2016
5880
9593
0.326
0.320
0.359
0.369
418
410
466
479
178.1
1713
4675
7914
3A
3B
3C
3D
0
1957
6011
10065
0.357
0.357
0.382
0.426
461
462
497
560
79.6
1599
4764
8489
             Three separate Bedford plot-6 soil samples were extracted, four subsamples of each extract received either (A)
             500 nL H2O, (B) 400 \iL H2O and 100 \]L of 100 |xg/mL Cr(VI), (C) 200 \iL H2O and 300 \iL of 100 |xg/mL
             Cr(VI), or (D) 500 \iL of 100 |xg/mL Cr(VI).
             Colorimetric analyses followed SW-846 Method 7196A.
             Absorbance (au) = arbitrary units.
     Table 3-3. Chromate [Cr(VI)] (mg/kg) one-sample t-test of the null hypothesis Ho: the sample is
                from a population with the mean equal to or greater than the Day 0 mean.
Sediment
125A
125A
125B
125B
125C
125C
126D
126D
123
123
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
Day 0 Mean
andCV
(N = 5)
91.6 (13%)
91.6 (13%)
328 (12%)
329 (12%)
62.5(11%)
62.5(11%)
815 (4%)
816 (4%)
330 (2%)
331 (2%)
Overall
Mean
93.0
96.5
339
343
64.3
63.5
828
829
325
350
Standard
Deviation
31.9
17.7
34.5
48.2
7.37
5.83
46.2
31.5
42.0
18.4
CV
34%
18%
10%
14%
11%
9%
6%
4%
13%
5%
95% Confidence
Limits
Lower
75.3
86.7
320
317
60.2
60.3
801
812
302
339
Upper
111
106
358
370
68.4
66.7
854
847
348
360
P-value
0.55
0.83
0.88
0.88
0.75
0.63
0.67
0.95
0.33
1.00
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
N
15
15
15
15
15
15
14
15
15
15
     NS = Not significant at a = 0.05
20

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200-,
-ion
ifin -
35 140

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3 50 100 150 200 2,
Days Held Until Extraction




• 125A4°C
• 125A-20°C
• • • • Upper Bound
	 Lower Bound





50
    Figure 3-2. Observed Cr(VI) concentration for Soil 125A at both the 4°C and -20°C holding
              temperature over holding time and associated Day 0 nonparametric bounds; there was
              not a significant trend through time.
The various holding time extract means were compared to the T = 0 mean by a one-tailed, t-test
whose null hypothesis Ho: the sample is from a population with the mean equal to or greater than
the Day 0 mean was not rejected for any of the soils at either holding temperature (Table 3-3).
Importantly, soil 125A held at 4°C that exhibited an overall CV>20% was not rejected. That is,
even though several of the timed extracts were widely variable (Fig. 3-2), their means were not
statistically different from the T = 0 mean. One high observation taken during the 224 day
sampling period from soil 126D held at 4°C was removed from the analysis because of its large
influence on the estimation of the slope (Fig. 3-3). The 95% confidence limits about the mean
concentration of Cr(VI) were widest for soil 125B held at -20°C and 126D held at 4°C. The
results of the t-test and the overall CV determinations suggest that there was no significant
change in Cr(VI) concentration during the 224 days of the study.

The lack-of-fit to the linear model was significant for soils 126D held at 4°C and soil 123 held at
4°C and -20°C (Table 3-4). In all cases, the residuals did  not show a consistent U-shaped pattern
through time suggesting that a parameter for curvature was not needed in the model. Therefore,
the simple linear model was used for all sediments and holding temperatures. The slope
associated with the holding time prior to extraction was not significantly different from zero (p >
0.08; Table 3-4) for any  soil except 123 (p < 0.05; Table 3-4). The estimated slopes for the 123
soil at 4°C and -20°C were negative  (-0.00119) and positive (0.000371), respectively. Figure 3-4
shows that the T = 0 data was very tightly centered on an average  of 331 mg/kg with a CV=2%
(Table 3-3). The positive slope for the  123 samples held at -20°C is probably the result of the
tight t = 0 data and the variability of the remaining timed  data; that is, the positive slope can be
attributed to analytical noise. The 123 samples held at 4°C exhibited a significant but only
                                                                                       21

-------
slightly negative slope. However, given the previous statistical analyses (CV<20% and a non-
significant t-test), the significant slope for soil 123 (4°C) is a trend rather than a verifiable
decrease in Cr(VI) concentration with holding time.
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3 50 100 150 200 2<
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• 126D4°C
• 126D-20°C
• • • • Upper Bound
	 Lower Bound




50
    Figure 3-3. Observed Cr(VI) concentration for Soil 126D at both the 4°C and -20°C holding
              temperature over holding time and associated Day 0 nonparametric bounds; there was
              not a significant trend through time.
The statistical analyses discussed previously (CV, t-test, and linear regression) showed no
significant change in Cr(VI) concentration over the life of the 224 day study (with the exception
of the linear regression for soil 123 at 4°C). However, based on the estimated slopes from the
linear regression analysis and the lower confidence limit of that slope (PLCL), the estimated
numbers of days until a 5%, 10%, and 20% decrease in natural log concentration was calculated.
A 5% decrease in Cr(VI) was estimated to require at least 140 days regardless of soil or holding
temperature (Table 3-5), which is  5 times longer than the SW-846 prescribed MHT of 28 days.
Soil 123 held at -20°C had a positive estimated PLCL and thus, the number of days until a given
percentage decrease in concentration could not be calculated. Except for Soil 125C, it appears
that the holding times for sediment held at 4°C were longer than the holding time for sediment
held at -20°C. However, because these time estimates were based on slopes that were not
significantly different from zero (and the other statistical  analyses suggest that no change
occurred during the life of the study) any differences noted as a function of holding temperature
should not be considered definitive.
22

-------
  Table 3-4. P-values for the significance of the lack-of-fit and the slope from the linear regression
            and the best fit simple linear model parameters on the natural log scale for Cr(VI).
Sediment and
Holding
Temperature
125A4°C
125A -20°C
125B 4°C
125B -20°C
125C4°C
125C -20°C
126D 4°C
126D -20°C
123 4°C
123 -20°C
P-value for
Lack of Fit
0.243
0.118
0.469
0.46
0.223
0.138
0.036
0.085
0.013
< 0.001
NS
NS
NS
NS
NS
NS
*
NS
*
**
Intercept
4.388
4.565
5.830
5.850
4.175
4.153
6.698
6.716
5.845
5.834
Slope
0.00173
-0.00018
-0.00014
-0.00034
-0.0003
-0.0001
0.000197
6.22E-05
-0.00119
0.000371
Standard
Error
0.00094
0.00063
0.00038
0.00047
0.00037
0.00032
0.00018
0.00014
0.00035
0.00016
P-value for
Slope
0.089
0.775
0.706
0.481
0.439
0.759
0.297
0.654
0.005
0.036
NS
NS
NS
NS
NS
NS
NS
NS
**
*
Df
13
13
13
13
13
13
12
13
13
13
  df = degrees of freedom
  NS = Not significant at a = 0.05
* = Significant with 0.01< p < 0.05
** = Highly significant with p < 0.01
     500
     200
                                                                        •    123   4°C
                                                                        •    123  -20°C
                                                                       ....  Upper Bound
                                                                       	Lower Bound
                                                                      	Linear (123 4°C)
                    50         100        150        200
                         Days Held Until Extraction
                 250
Figure 3-4. Observed Cr(VI) concentration for Soil 123 at both the 4°C and -20°C holding
           temperature over holding time, associated Day 0 nonparametric bounds, and the
           significant decreasing trend for sediment held at 4°C.
                                                                                              23

-------
       Table 3-5. The estimated number of days until a given percentage decrease from the
                intercept for Cr(VI) (MHT=28 days).
Sample
125A
125A
125B
125B
125C
125C
126D
126D
123
123
Holding Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
5% Decrease
729
148
305
213
189
259
1700
1455
149
NA
10% Decrease
1458
296
610
427
378
519
3400
2910
298
NA
20% Decrease
2916
592
1220
855
757
1038
6801
5821
596
NA
                  NA = not applicable because the slope and lower 95% confidence limit were positive.
Plots of the observed concentrations through time were compared to the nonparametric upper
and lower boundaries of the Day 0 concentration (Figures 3-2 to 3-6). As with the CV, t-test, and
linear regression (slope) analyses, the visual comparison showed that with except for Soil 123
held at 4°C (Fig. 3-4) the concentrations of Cr(VI) did not decline significantly over the 224 days
tested. Soil 123 held at 4°C was seen to have a significant Cr(VI) decrease through time (with
respect to the nonparametric lower boundary; Fig. 3-4) and exhibited a 5% decrease in the log
concentration by 149 days; yet the 149 day estimate was still at least 5 times longer than the SW-
846 mandated MHT. The data for soils 125B and 125C are plotted below (Figs. 3-5 and 3-6,
respectively). Both of these soils exhibit stable extracted Cr(VT) concentrations.

3.1.3  Cr(VI) Extract Stability
Inspection of the Cr(VI) extract concentration data as a function of time revealed substantial
variability between the five replicates of a given soil (Fig. 3-7 and 3-8). It was also noted that for
those extracts held at room temperature over the 56 day study period,  several soil extracts
displayed a convex curve in the data (soils 125B and 125C; Fig. 3-8) or tended to appear more
variable over time compared to those extracts stored at 4°C. Some of the noted variability
resulted from indeterminate and determinate errors as well as analysis error.  However, only the
analyses performed  at day 7 for soil 126D held at room temperature could definitively be
associated with analysis error (i.e., distinctly higher Cr(VI) concentrations) because of its  almost
uniform increase across all replicates (Fig. 3-7).

The coefficient of variation (CV) between replicates was greatest for the 125A (Boomsnub, 0.5')
soil (Table 3-6). This variability probably arose from incomplete homogenization of the soil
prior to subsampling and variations in analytical measurement over time. The Cr(VI) extraction
procedure requires that the sample remain in its original moist condition, while this is important
to the stability of Cr(VI), it makes it difficult to obtain a thoroughly mixed soil sample.
Analytical variability for given replicates across time; however, was very low regardless of
extract holding temperature (Table 3-6).  The highest CV for within replicate determinations was
8% (extract from soil 125C stored at room temperature). The extracts  stored at 4°C exhibiting a
maximum CV of 3%. Simply put, these data demonstrate that for the soil extracts investigated
there was no, or only very limited change in Cr(VI) extract concentrations over the 56-day time
24

-------
frame. When stored at 4°C, the CV across time for a given replicate was about what would be
expected from analytical variability. Investigation of room temperature storage was solely for
data comparison to the 4°C storage regime, not as a legitimate alternative. While we can not
definitively demonstrate or delineate the cause of observed differences between the two storage
regimes, it is well known that lower temperatures slow both microbial and chemical processes.
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Days Held Until Extraction






• 125B4°C
• 125B-20°C
• • • • Upper Bound
	 Lower Bound




50
           Figure 3-5. Observed Cr(VI) concentration for Soil 125B at both the 4°C and -20°C
                    holding temperature over holding time and associated Day 0
                    nonparametric bounds; there was not a significant trend through time.
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• 125C-20°C
• • • • Upper Bound
	 Lower Bound





50
           Figure 3-6. Observed Cr(VI) concentration for Soil 125C at both the 4°C and -20°C
                    holding temperature over holding time and associated Day 0
                    nonparametric bounds; there was not a significant trend through time.
                                                                                         25

-------
126D - Room Temp
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60
 Figure 3-7. Chromate [Cr(VI)] extract concentration stored at room temperature or 4°C as a
           function of time for the Frontier Hard Chrome site sandy soil; the different
           symbols refer to the five replicates.
To examine the change in Cr(IV) concentration as a function of holding time of the extract for
each sediment and storage condition, a regression analysis was conducted on the data corrected
for baseline. The lack-of-fit of the simple linear regression was significant (p > 0.05; Table 3-7)
for five of the eight sediment samples (125A, room temperature; 125B, 4°C; and 125C, room
temperature and 4°C; and 126D, room temperature). In all cases; however, the residuals plotted
against storage time did not display a consistent pattern that could be associated with holding
time. Instead, the residuals appeared to show that for specific time points, either all residuals
were high or the residuals were all low; hence, no spline analysis was necessary (see section 2.3).
The behavior of the residuals was ultimately linked to the analytical requirement of producing a
new calibrating dilution series and calibration curve for each batch of analyses. While a
calibration curve was specific to a given extraction time period, small differences between time
period curves would increase or decrease the determined extraction concentration for all soils
extracted at that time period. Hence, comparison to other time periods (particularly those extracts
that required substantial dilution) reflected those concentration differences as would the residual
plots.

Despite the lack-of-fit to a simple regression equation noted above in the baseline corrected data,
the slopes in all samples, except the 126D soil, were not significant (p > 0.1; Table 3-7); that is,
not significantly different from zero. This result compared well with the low CV% discussed
previously (particularly with the 4°C stored extracts). The variance between replicates remained
fairly constant across time (i.e., slopes not significantly different from zero, p > 0.1; Table 3-7).
26

-------



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                                                             125A-4°C
                                                 200
                                                              20        40

                                                               Time (days)
125B-4°C
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yc _
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0 20 40 60
Time (days)
Figure 3-8. Chromate [Cr(VI)] extract concentration stored at room temperature or 4°C as
           a function of time for the Boomsnub soil at depths of 0.5,3.0 or 5.5 feet; the
           different symbols refer to the five replicates.
                                                                                                27

-------
           Table 3-6. Average CV% over time and within replicates for the Cr(VI) extracts.
Soil type
125A
125B
125C
126D
Storage
room temp
4°C
room temp
4°C
room temp
4°C
room temp
4°C
Across Time
CV%(a) Averaged
over Replicates
4%
2%
2%
2%
8%
3%
3%
1%
Between Replicate
CV% Averaged
Over Time
30%
40%
4%
11%
11%
10%
4%
5%
           " CV = Coefficient of variation.
   Table 3-7. Simple linear regression analysis corrected for baseline only.
Soil
125A

125B

125C

126D

Storage
room temp
4°C
room temp
4°C
room temp
4°C
room temp
4°C
Slope
Coefficient
-0.03675
0.00785
-0.01108
-0.11826
0.04526
-0.00389
-0.9601
-0.3043
DFa
for
Error
23
23
23
23
23
23
23
23
P-value
for
Slope
0.395
0.778
0.908
0.12
0.286
0.878
0.002
0.007
DFfor
Lack-of-fit
3
3
3
3
3
o
J
o
J
3
P-value
for
Lack-of-fit
0.005
0.203
0.239
0.019
p< 0.001
0.009
0.007
0.131
95% CIb Regression
Equation
Y=-0.0132x+ 1.6422
Y= -0.0002x + 0.4089
Y=7E-05x + 0.0384
Y=5E-05x + 0.1075
Y=0.0001x + 0.1111
Y=-0.0001x + 0.1019
Y= -O.OOOSx + 0.03
Y= -9E-05x + 0.0496
   a DF - degrees of freedom.
   b CI - confidence interval.
Based on the estimated lower 95% confidence limit of the slope (PLCL), the estimated number of
days until a 5%, 10%, and 20% change in extract Cr(VI) concentration was calculated (Table
3-8). A decrease of 5% in the extract Cr(VI) concentration was estimated to occur between 20
and 81 days after extraction, which is substantially longer than the 24 h SW-846 prescribed
MHT. With the exception of soil 125B, the extract solution holding condition of 4°C yielded a
slightly greater stability (i.e., longer time to a 5% change). Regardless of holding condition or
soil, the estimated time for an observed 20% change in the Cr(VI) concentration was
approximately 3 months. The 5% change increment, while somewhat arbitrary, was seen as a
reasonable metric because determination of Cr(VI) in an extract is an analytical procedure, as
opposed  to the extraction of Cr(VI) from a  soil. From the statistical analyses of these extract
solution data, it was clear that the extract Cr(VI) concentrations were fairly stable across the time
frame of this study.
28

-------
3.1.4 Cr(VI) Holding Time for Extraction and Extract Stability - Conclusions
The purpose of this study was to investigate if the extractable Cr(VI) concentration in
soils/sediments was effected by the holding time prior to extraction according to SW-846
Method 3060A procedures. Of the six soils studied, five exhibited no or limited influence of
holding time prior to extraction for the 224 days of this study regardless of the holding condition
(4°C or -20°). The time required for the Cr(VI) concentration extracted from the five soils to
change by 20% was estimated to be > 592 days; the 20% value was based on the SW-846
prescribed replicate precision for Cr(VI) extraction from soils. The estimate of 592 days is about
21 times greater than the currently prescribed SW-846 MHT; even a 5% decrease in extractable
Cr(VI) from these five soils was estimated to be about 5 times greater than the MHT. While the
sixth soil, Bedford plot-6, exhibited a significant under recovery of the  sample spike (only 1-
5%), the method protocols (SW-846 Method 3060A) clearly indicated a problem. Further
investigation showed that the high level of extracted organic carbon yielded a false measure of
Cr(VI) and the DOC may have acted as the reductant of the Cr(VI) spike. Hence, if the method
QA/QC protocols are followed, laboratory control samples and spikes (standard additions) would
have identified the erroneous results regardless of holding time prior to extraction.

The Cr(VI) extract solutions from this study exhibited a chemical stability far beyond the
prescribed SW-846 Method 7169A MHT (24 h), when extracts were  stored in the dark at 4°C.
No one would argue that Cr(VI) extract solutions be held longer than necessary or for the length
of time required by this study to estimate a 5% decrease (20 d), but if the standards, spikes, and
laboratory control samples exhibit appropriate stability and recovery then holding times beyond
24 h seem reasonable.

3.2  Semi-Volatile Organic Compounds (SVOCs)

Five soils/sediments were utilized for the SVOC extraction study (Table 3-9). Samples were
selected to yield at least 3 PAH extractable, 3 PCB extractable, and 3 pesticide extractable
soils/sediments. The three soils (Bedford-1, Eagle Harbor,  and Tri Cities) and two sediments
(Housatonic River and SQ-1) exhibited wide ranges in TOC and particle size distributions. All
soils/sediments exhibited circum-neutral pH levels, and the Eh-pH values suggested that the
redox status of the samples were oxic. Soils/sediments were sampled and  semi-quantitative
SVOC screening performed to identify the likely samples and contaminants that would be
utilized in this part of the study. Until the screening was completed the  samples were stored at
4°C. The samples were homogenized, split, and stored as described in section 2.2.1 once the
extraction study was initiated.
                                                                                     29

-------
             Table 3-8. Estimated number of days to achieve a given percentage change in
                     concentration using the regression model of the background
                     corrected data.

Sample
125A

125B

125C

126D

Holding condition
Room temp
4°C
Room temp
4°C
Room temp
4°C
room temp
4°C
Estimated Number of Days
5% Change
36
81
81
59
20
54
26
78
10% Change
73
162
163
119
41
109
52
157
20% Change
147
325
327
238
83
219
104
315
     Table 3-9. SVOC extraction study soil/sediment properties.

Sample

Housatonic River
Tri-Cities
Eagle Harbor
SQ-1
Bedford-1
SVOC
Analysis

PCB/Pesticides
PCB/Pesticides
PAHs
PAHs/PCB/Pesticides
PAH/Pesticides

pH

7.7
NDb
9.1
7.1
8.5
Eh


510
ND
386
446
509
oca


3.57
5.60
0.55
0.97
5.80
Sand
	 0,

5.8
54.4
10.2
13.5
13.7
Silt
/

75.4
34.6
67.3
68.8
47.0
Clay


18.8
11.0
22.5
17.7
39.3
     "Reported values are the mean of duplicate measurements. OC = organic carbon.
     b ND = no data.
3.2.1 Polyaromatic Hydrocarbons (PAHs)
Concentrations of PAHs were characterized through time for each of the three sediments/soils
(Eagle Harbor, SQ-1 and Bedford-1) and holding temperatures of 4°C and -20°C (Appendix A,
Descriptive Statistics Tables A-2 to A-7). Seventeen PAHs were analyzed for in each of the
soils/sediments (Table 3-10). The Eagle Harbor soil was analyzed for three additional PAHs, 1-
methyl naphthalene, 2-methyl naphthalene, and 1-methyl phenanthrene. For the Eagle Harbor
soil, all of the observed concentrations were above 2*MDL (see section 2.3) except for 2-methyl
naphthalene and acenaphthylene. For the Bedford-1 soil, all of the observed concentrations were
above 2*MDL except for acenaphthene, fluorene, and dibenzothiophene. For the SQ-1 sediment,
benzo[k]fluoranthene was below detection limits for all observations and dibenzothiophene had
observations less than 2*MDL.
30

-------
   Table 3-10. Mean concentration (ng/g) and coefficient of variation (CV) for all data across time
               accepted for analysis (including statistical outliers)3.
Analyte
Naphthalene
1 Methyl naphthalene
2 Methyl naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
1 Methyl phenanthrene
Fluoranthene
Pyrene
Benzo[a] anthracene
Chrysene
Benzo [b] fluoranthene
Benzo [k] fluoranthene
Benzo [a]pyrene
Indeno [l,2,3-c,d] pyrene
Dibenzo [a,h] anthracene
Benzo [g,h,i] perylene
Eagle Harbor
DayO
489
19.9%
490
18.5%
144
36.3%
133
53.9%
1,501
64.8%
1,846
63.4%
728
87.8%
8,199
89.8%
1,962
42.7%
645
70.2%
9,277
60.2%
6,723
57.4%
1,901
31.6%
2,350
28.4%
2,469
14.1%
2,433
14.1%
965
15.1%
672
0.0%
330
0.0%
651
0.0%
4°C
435
36.0%
275
31.2%
74
33.5%
66
26.3%
754
40.5%
818
44.7%
214
53.7%
2,418
52.9%
1,265
32.9%
385
16.1%
5,849
27.4%
4,672
8.0%
1,409
10.8%
1,841
11.8%
1,888
16.7%
1,579
39.0%
741
10.4%
442
23.5%
157
39.8%
432
24.6%
-20°C
545
52.9%
439
52.8%
124
34.2%
71
36.0%
1,034
23.5%
1,302
19.2%
396
20.7%
4,623
18.0%
1,708
58.7%
399
16.0%
6,207
11.2%
4,457
11.9%
1,353
10.4%
1,746
9.0%
1,781
14.6%
1,443
39.7%
703
8.1%
435
24.1%
134
13.1%
432
20.5%
SQ-1
DayO
81.2
8.6%


8.14
13.0%
97.0
4.6%
90.0
8.9%

162
6.6%
71.6
16.9%

156
6.1%
139
2.7%
93.9
13.0%
111
10.7%
91.2
8.1%

70.5
2.5%
3.87
10.9%
64.2
15.0%
76.8
8.5%
4°C
72.0
15.9%


8.76
12.7%
92.5
9.8%
92.0
12.2%

147
10.4%
87.3
12.2%

187
10.7%
159
10.3%
135
14.4%
139
13.1%
125
26.5%

97.9
18.9%
5.06
38.9%
84.9
22.7%
77.4
25.7%
-20°C
73.2
21.7%


10.4
18.5%
91.6
12.4%
92.6
12.2%

149
10.7%
91.1
13.9%

185
10.7%
158
10.1%
138
13.5%
142
13.8%
122
24.1%

100
16.4%
4.91
28.3%
89.1
21.3%
81.4
18.8%
Bedford-1
DayO
283
25.5%


346
14.0%
74.6
7.6%
78.6
23.4%
108
16.0%
1,435
24.1%
343
18.2%

6,639
20.7%
6,851
19.8%
4,837
16.4%
5,278
16.4%
6,903
16.7%
2,762
16.7%
5,793
16.2%
4,454
15.4%
949
13.7%
4,088
15.6%
4°C
366
37.6%


402
24.7%
85.2
12.6%
72.7
28.4%
118
51.0%
1,782
28.5%
401
29.0%

7,371
20.9%
7,732
19.9%
5,603
20.7%
6,173
21.0%
7,236
18.7%
4,733
58.7%
7,478
30.4%
6,762
47.8%
1,160
26.8%
5,500
34.7%
-20°C
427
21.5%


444
18.1%
91.3
14.2%
91.8
30.6%
142
24.4%
1,912
22.2%
446
26.5%

7,771
17.7%
8,194
16.6%
6,002
19.3%
6,515
19.3%
7,623
16.2%
4,964
59.6%
7,862
30.6%
7,196
50.1%
1,273
29.9%
5,728
34.1%
    1 Cells highlighted with light yellow have CVs greater than 25% and cells highlighted with orange and bold text have observations less
     than 2 times the minimum detection limit and blank cells indicate too few observations above detection or accepted for analysis.
Thus, all three sediments had 12 PAHs in common that were measured in concentrations greater
than 2*MDL.
                                                                                                         31

-------
Sequim Bay-1 (SQ-1) sediments had the lowest concentration of all PAHs except acenaphthene
and fluorene (Table 3-10). Total PAH concentrations for SQ-1 averaged 1,520 ng/g (dry weight).
The Eagle Harbor soil had the highest concentration of low- and mid-molecular weight PAHs
with total PAH concentration averaging 26,500 ng/g. The Bedford-1 soil had the highest
concentrations of high molecular weight PAHs with total PAH concentrations averaging 33,200
ng/g.

3.2.1.1 Influence of PAH Outliers'. Table 3-10 shows the mean concentration and CV of all
"Day 0" data accepted for statistical analysis and the across time CV for the data at 4°C and
-20°C (i.e., all data across a time sequence except for "Day 0"). The Eagle Harbor data exhibited
a large number of Day 0 CVs>25%, but in all cases, removal of statistical outliers reduced the
CV substantially (Table 3-11). For the Eagle Harbor analysis, replicate number 3  of the Day 0
data was removed from the analysis and plots for all but five of the PAHs. This replicate was
generally 2 to 4 times greater than the median concentration for the Day 0 data. In the case of
dibenzothiophene and phenanthrene, for example, removing the outlier reduced the CV from
87.9% and 89.8%, respectively to 17% for both compounds. Four other Eagle Harbor extract
observations from Day 28 held at -20°C were identified as extreme outliers (observations greater
than the 75th percentile plus 3 times the interquartile distance of the Day 0 data) out of a total of
468 observations (1%) and were removed from the analysis (but not the plots). Likewise, for the
SQ-1 analysis, replicate 1 of the Day 0 data was removed from the analysis and plots of all of the
PAHs. This replicate result was generally less than half the concentration of the median
concentration for the Day 0 data. There were a total of 38 observations out of 367 (10%)
considered extreme outliers from all PAHs measured in the SQ-1 sediment; thus, they were not
removed from the analysis because this percentage was greater than our criteria (Section 2.3).
For the Bedford-1 analysis, replicate number 3 of the Day 0 data for fluorene was removed from
the analysis and plots because it was nearly half of the median concentration of the Day 0 data.
Twenty-four observations out of 271 (9%) were considered extreme outliers which is less than
the preset criteria of 10% so these observations were removed from the analysis but not the plots.

3.2.1.2 Statistical Analysis of PAH Extraction Data: The value of CV<25% is the SW-846
prescribed upper bound for allowable variability between replicates for SVOC extraction. Hence,
the results shown in Table 3-10  for means and CVs of across time data (excluding Day 0 data)
for samples held  at 4°C and -20°C, can be viewed as an estimate of data variability. The
variability arising for the across time CV analysis is a combination of sample heterogeneity,
analytical precision, and variability with time.

The calculated overall CVs (after removal of the extreme outliers)  showed that most of the PAH
concentrations (excluding those whose concentrations were below 2*MDL) across all time
periods varied less than the SW-846 prescribed replicate precision (CV<25%; Tables 3-11, 3-12,
and 3-13). Eagle Harbor PAH concentration data (Table 3-11) showed the most variability with
15 overall CVs>25% out of a total of 36 holding time analyses (PAH and holding condition). For
the lower molecular weight PAHs (anthracene and below), except for 1 methyl naphthalene, the
Eagle Harbor soil held at 4°C exhibited a CV>25%, and CVs<25% for those held at -20°C.
Higher molecular weight PAHs, such as benzo[k]fluoranthene, benzo[a]pyrene, indeno[l,2,3,-
c,d]pyrene, dibenzo[a,h]anthracene, and benzo[g,h,i]perylene exhibited CVs>25% at 4°C and
-20°C holding conditions. Only  one PAH, indeno[l,2,3,-c,d]pyrene held at 4°C and -20°C, from
32

-------
the SQ-1 sediment exhibited a CV>25% out of a total of 31 holding time analyses (Table 3-12).
Of the 19 holding time analyses for the Bedford-1 soil, only naphthalene (4°C and -20°C),
phenanthrene (4°C and -20°C), and anthracene (4°C) exhibited overall CVs>25% (Table 3-13).
 Table 3-11. PAHs (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a population with
            the mean equal to or greater than the Day 0 mean from Appendix B for the Eagle Harbor soil".
Analyte
Naphthalene
IMethyl Naphthalene
2 Methyl Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
1 Methyl phenanthrene
Fluoranthene
Pyrene
Benzo[a]Anthracene
Chrysene
Benzo[b]Fluoranthene
Benzo[k] Fluoranthene
Benzo[a]Pyrene
Indenofl ,2,3-c,d]Pyrene
Dibenzo[a,h] Anthracene
Benzo[g,h,i]Perylene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
Day 0 Mean
andCV
(N = 4)
489 (20%)
489 (20%)
490(19%)
490(19%)
119(17%)
119(17%)
97.3(11%)
97.3(11%)
1021 (18%)
1021 (18%)
1270(19%)
1270 (19%)
410 (17%)
410 (17%)
4530 (17%)
4530 (17%)
1559 (18%)
1559(18%)
420 (13%)
420 (13%)
6504 (12%)
6504 (12%)
4807(11%)
4807(11%)
1605 (8%)
1605 (8%)
2026 (10%)
2026 (10%)
2469 (14%)
2469 (14%)
2433 (14%)
2433 (14%)
965(15%)
965 (15%)
672 (NC)
672 (NC)
330 (NC)
330 (NC)
651 (NC)
651 (NC)
Overall
Mean
450
472
334
404
84
116
72.7
76.8
811
1031
915
1295
256
399
2871
4604
1328
1450
392
404
5989
6271
4701
4532
1451
1407
1881
1806
2054
1993
1823
1747
805
784
465
462
174
156
454
456
Standard
Deviation
142
111
130
121
30.1
26
20.7
25.4
300
225
386
240
133
76.9
1469
792
402
292
60.3
60.4
1464
695
394
531
164
170
219
197
413
429
670
688
142
153
122
126
80.5
67.5
122
110
CV
32%
24%
39%
30%
36%
22%
28%
33%
37%
22%
42%
19%
52%
19%
51%
17%
30%
20%
15%
15%
24%
11%
8%
12%
11%
12%
12%
11%
20%
22%
37%
39%
18%
20%
26%
27%
46%
43%
27%
24%
95%
Confidence Limits
Lower
371
408
246
318
66.6
100
60.7
62.1
638
901
692
1157
179
354
2023
4147
1096
1274
357
369
5144
5870
4474
4225
1356
1309
1754
1692
1816
1734
1436
1331
723
691
378
365
117
104
367
371
Upper
528
536
421
490
101
131
84.6
91.5
984
1161
1138
1434
333
443
3719
5061
1560
1627
427
438
6834
6672
4928
4839
1546
1506
2007
1920
2292
2252
2210
2163
887
876
552
558
232
208
541
541
P-value
0.15
0.29
<0.01
0.03
<0.01
0.32
<0.01
<0.01
0.01
0.56
<0.01
0.65
<0.01
0.3
<0.01
0.63
0.03
0.1
0.054
0.16
0.11
0.12
0.17
0.04
<0.01
<0.01
0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
NS
NS
**
*
**
NS
**
**
*
NS
**
NS
**
NS
**
NS
*
NS
NS
NS
NS
NS
NS
*
**
**
*
**
**
**
**
**
**
**
**
**
**
**
**
**
N
15
14
11
10
14
13
14
14
14
14
14
14
14
14
14
14
14
13
14
14
14
14
14
14
14
14
14
14
14
13
14
13
14
13
10
9
10
9
10
9
     Table B2.1 and B2.2 for Eagle Harbor soil with statistical outliers removed (PAHs highlighted in yellow had concentrations < 2*MDL).

  NS = Not significant at a = 0.05
    * = Significant with O.OK p < 0.05.
   ** = Highly significant with p < 0.01.
  NC = Not calculable, too few observations.
                                                                                                33

-------
 Table 3-12. PAHs (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a population with
           the mean equal to or greater than the Day 0 mean from Appendix B for the SQ-1 sediment".
Analyte
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo [a] Anthracene
Chrysene
Benzo [bJFluoranthene
Benzo [aJPyrene
Indeno[l,2,3-c,d] Pyrene
Dibenzo[a,h] Anthracene
Benzo[g,h,i]Perylene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
Day 0 Mean
andCV
94.1 (9%)
94.1 (9%)
9.43 (13%)
9.43 (13%)
114(5%)
1 14 (5%)
105 (9%)
105 (9%)
6.7 (7%)
6.7 (7%)
189 (7%)
189(7%)
82.1(17%)
82.1(17%)
174 (6%)
174 (6%)
157(3%)
157(3%)
105 (13%)
105(13%)
126(11%)
126(11%)
108 (8%)
108 (8%)
82 (2%)
82 (2%)
4.45(11%)
4.45(11%)
74.2(15%)
74.2(15%)
91 (8%)
91 (8%)
Overall
Mean
77.1
78.4
8.91
10.2
97.5
96.7
95.1
95.6
5.85
5.94
157
158
86.1
89.0
184
183
159
157
129
131
136
138
121
119
94.3
96.1
4.92
4.81
82.4
85.7
80.5
83.6
Standard
Deviation
14.3
16.9
1.13
1.78
12.5
14.1
12.0
11.9
0.799
0.779
23.2
22.9
11.1
12.9
18.7
18.5
14.3
13.8
22.2
22.5
17.7
19.2
29.9
26.5
17.5
16.4
1.74
1.24
17.9
18.3
18.5
14.3
CV
19%
22%
13%
17%
13%
15%
13%
12%
14%
13%
15%
14%
13%
14%
10%
10%
9%
9%
17%
17%
13%
14%
25%
22%
19%
17%
35%
26%
22%
21%
23%
17%
95%
Confidence Limits
Lower
68.5
67.7
8.23
9.09
89.9
88.2
87.8
88.4
5.37
5.47
143
144
79.4
81.2
172
172
150
149
115
117
125
126
103
103
83.7
86.2
3.87
4.06
71.6
74.6
69.4
75.0
Upper
85.7
89.1
9.60
11.2
105
105
102
103
6.33
6.41
171
172
92.8
96.8
195
194
167
166
142
144
147
150
139
135
104.8
105.9
5.97
5.55
93.2
96.7
91.7
92.2
P-value
0.001
0.004
0.062
0.918
O.001
0.001
0.005
0.006
0.001
0.002
0.001
O.001
0.889
0.961
0.963
0.949
0.664
0.548
0.999
0.999
0.972
0.981
0.930
0.918
0.987
0.995
0.826
0.839
0.938
0.979
0.033
0.044
**
**
NS
NS
**
**
**
**
**
**
**
**
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
*
*
N
13
12
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
13
   a Tables B3.1 and B3.2 for SQ-1 sediment with statistical outliers removed (PAHs highlighted in yellow had concentrations < 2*MDL).
 NS = Not significant at a = 0.05
   * = Significant with 0.01 < p < 0.05
  ** = Highly significant with p < 0.01
Twenty-two holding time analyses out of a total of 86 exhibited C Vs>25%. The reason(s) for
PAH holding time variability regardless of holding conditions (4°C and -20°C) was not
determined, but likely candidates include sample heterogeneity across time, analytical variability
across time, and loss of concentration through degradation or volatilization. The latter rationale;
however, is considered most likely for those holding time analyses that exhibited  a dependence
on holding condition; that is, where the 4°C and -20°C holding condition differed. The Eagle
Harbor soil was the only material that exhibited a consistent dependence on holding condition
and then only for the lower molecular weight PAHs. The dependence on holding temperature
(4°C versus -20°C) for the loss of Eagle Harbor soil PAHs is in line with those reported by Rost
34

-------
et al. (2002) where they found low molecular weight PAHs were degraded over time when soils
were held at 4°C (see section 1.1).

A one-sample t-test of the null hypothesis Ho: the sample is from a population with the mean
equal to or greater than the Day 0 mean was rejected for 15 of the PAHs found in the Eagle
Harbor soil (with concentrations >2*MDL) for at least one holding condition (Table 3-11).
Rejection of the null hypothesis provides a measure of validity to a potential decrease in
concentration. In the Eagle Harbor soil, all of the high molecular weight PAHs [228 mw
(benz[a]anthracene) and higher] had mean concentrations that were significantly less than the
Day 0 mean for both the 4°C and -20°C holding conditions. Except for pyrene and 1 methyl
naphthalene, all the remaining lighter molecular weight PAHs that had means significantly less
than the Day 0 mean were those stored at 4°C (Table 3-11). For SQ-1 sediments, the one-sample
t-test was not significant for PAHs in Table 3-12 below phenanthrene except benzo[g,h,i]
perylene. With the exception of acenaphthylene, the lighter molecular weight PAHs had mean
concentrations that were significantly less than the Day 0 mean at both holding conditions (Table
3-12). For the Bedford-1 soil, no PAH exhibited a mean concentration that was significantly less
than its Day 0 mean (Table 3-13).

The overall CV and one sample t-test assess data variability, but in slightly different ways. The
overall CV compares variability across the entire holding time analysis sequence to the SW-846
prescribed replicate variability (CV<25%), while the t-test is a statistical evaluation of the overall
mean response compared to a single timed value using the overall variability. Comparison of
these two evaluations is most interesting for the lower molecular weight PAHs (lighter than
anthracene; Table 3-11) extracted from the Eagle Harbor soil. These PAHs, except 1 methyl
naphthalene, showed  a clear distinct difference between holding conditions; that is,  soils held at
4°C exhibited overall CVs>25% and a highly significant (p < 0.1) t-test. Eagle Harbor soil held
at -20°; however, exhibit PAH concentrations whose overall CVs<25% and t-tests that are not
significant. Even 1 methyl naphthalene, with an overall CV for both holding temperatures greater
than 25%, exhibits a difference in the significance of the t-test with the lower temperature. The
Eagle Harbor soil results clearly show the potential effect of holding temperature  on extraction
holding time for the lower molecular weight PAHs. However, the holding temperature effect
evidenced in the Eagle Harbor soil is not universal, as neither of the other soils in this study
exhibited such a clear cut distinction between holding temperatures.

The lack-of-fit to the  linear model was significant for five of the PAHs measured  in Eagle
Harbor soil regardless of storage temperature and four others at one storage temperature (Table
3-14). Thirteen of the PAHs measured in SQ-1 sediments exhibited a lack-of-fit to the linear
model at one storage temperature (Table 3-15). None of the PAHs measured in Bedford-1 soil
exhibited a lack-of-fit to the linear model (Table 3-16). The residuals for these analytes did not
show a consistent U-shaped pattern through time, nor was there a pattern observed between
storage temperatures, and; hence, the lack-of-fit was assumed to be noise. Therefore, the simple
linear model was used for all analytes, sediments, and holding temperatures. The slope
associated with the number of days held was negative and significantly different from zero for 16
of the PAHs measured (with concentrations >2*MDL) in the Eagle Harbor soil (Table 3-14). All
16 of these  PAHs exhibited significantly decreasing slopes in sediment held at 4°C while only
three of these were significantly decreasing in sediment held at -20°C. None of the slopes
                                                                                      35

-------
associated with the number of days held were both negative and significantly different from zero
for PAHs measured in either SQ-1 sediment or Bedford-1 soil (Tables 3-15 and 3-16). There
were some PAHs that had significant positive slopes; however,  these were considered to be
analytical noise.
    Table 3-13. PAHs (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a population
              with the mean equal to or greater than the Day 0 mean from Appendix B for the
              Bedford-1 soil3.
Analyte
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo[a] Anthracene
Chrysene
Benzo[b]Fluoranthene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
DayO
Mean and CV
(N = 4)
283 (25%)
283 (25%)
346 (14%)
346 (14%)
74.6 (8%)
74.6 (8%)
78.6 (23%)
78.6 (23%)
108 (16%)
108 (16%)
1435 (24%)
1435 (24%)
343 (18%)
343 (18%)
6639(21%)
6639 (21%)
6851 (20%)
6851(20%)
4837 (16%)
4837 (16%)
5278 (16%)
5278 (16%)
6903 (17%)
6903 (17%)
Overall
Mean
333
369
380
391
79.2
81.2
74.7
87.4
114
115
1643
1721
378
383
7078
7318
7380
7657
5297
5536
5815
6020
7103
7335
Standard
Deviation
119
109
84.1
74.5
9.1
8.6
19.0
24.9
46.1
19.3
464
448
98.4
90.2
1446
1421
1464
1456
1054
1148
1182
1240
1219
1194
CV
36%
30%
22%
19%
11%
11%
25%
28%
40%
17%
28%
26%
26%
24%
20%
19%
20%
19%
20%
21%
20%
21%
17%
16%
95% Confidence
Limits
Lower Upper
248
291
319
334
72.2
74.6
60.1
68.2
80.7
98.9
1311
1401
307
313
6044
6301
6333
6615
4543
4715
4969
5133
6231
6481
418
447
440
448
86
88
89
107
147
131
1975
2041
448
452
8112
8335
8427
8699
6051
6357
6661
6907
7975
8189
P-value
0.892
0.983
0.878
0.945
0.916
0.976
0.273
0.839
0.651
0.838
0.905
0.963
0.854
0.891
0.819
0.918
0.858
0.943
0.899
0.957
0.908
0.955
0.691
0.859
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
N
10
10
10
9
9
9
9
9
10
8
10
10
10
9
10
10
10
10
10
10
10
10
10
10
    " Tables B4.1 and B4.2 for Bedford-1 soil with statistical outliers removed (PAHs highlighted in yellow had concentrations
     < 2*MDL). NS = Not significant at a = 0.05.
36

-------
Table 3-14. P-values for the significance of the lack-of-fit and the slope from the linear
            regression and the best fit simple linear model parameters on the natural log
            scale for PAHs for Eagle Harbor soil and each holding condition"
Analyte
Naphthalene
1 Methyl Naphthalene
2 Methyl Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
1 Methyl Phenanthrene
Fluoranthene
Pyrene
Benzo[a] Anthracene
Chrysene
Benzo [b] Fluoranthene
Benzo [k] Fluoranthene
Benzo[a]pyrene
Indeno [l,2,3-c,d] Pyrene
Dibenzo [a,h] Anthracene
Benzo[g,h,i] Perylene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
P-value for
Lack-of-Fit
0.028
0.008
0.004
0.004
0.014
0.003
0.018
0.007
0.245
0.026
0.643
0.316
0.186
0.104
0.366
0.308
0.069
0.193
0.738
0.282
0.038
0.442
0.979
0.295
0.773
0.272
0.585
0.127
0.360
0.251
0.002
0.004
0.084
0.044
0.054
0.111
0.074
0.043
0.154
0.332
*
**
**
**
*
**
*
**
NS
*
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
*
NS
NS
NS
NS
NS
NS
NS
NS
NS
**
**
NS
*
NS
NS
NS
*
NS
NS
Intercept
6.171
6.165
5.974
6.030
4.576
4.757
4.430
4.496
7.018
6.948
7.172
7.181
5.872
6.027
8.279
8.447
7.416
7.281
6.063
6.013
8.894
8.762
8.486
8.440
7.343
7.299
7.588
7.525
7.751
7.719
7.807
7.781
6.749
6.702
6.193
6.009
5.440
5.226
6.294
6.110
Slope
-0.00264
-0.00086
-0.00415
-0.00132
-0.00441
-0.00073
-0.00391
-0.00431
-0.00887
-0.00072
-0.01004
-0.00060
-0.01022
-0.00115
-0.00973
-0.00052
-0.00595
-0.00040
-0.00213
-0.00047
-0.00493
-0.00050
-0.00071
-0.00058
-0.00145
-0.00117
-0.00115
-0.00066
-0.00305
-0.00285
-0.00870
-0.00857
-0.00153
-0.00107
-0.00120
0.00134
-0.00558
-0.00328
-0.00319
-0.00016
Standard Error
0.0016
0.0013
0.0019
0.0019
0.0015
0.0014
0.0011
0.0012
0.0009
0.0012
0.0008
0.0009
0.0011
0.0009
0.0011
0.0008
0.0010
0.0010
0.0005
0.0007
0.0007
0.0005
0.0004
0.0006
0.0004
0.0005
0.0005
0.0005
0.0006
0.0006
0.0012
0.0012
0.0007
0.0008
0.0013
0.0015
0.0014
0.0016
0.0010
0.0014
P-value for Slope
0.127
0.535
0.057
0.517
0.013
0.603
0.004
0.003
< 0.001
0.552
< 0.001
0.507
< 0.001
0.229
< 0.001
0.543
< 0.001
0.700
0.001
0.538
< 0.001
0.373
0.074
0.340
0.004
0.039
0.043
0.227
< 0.001
0.001
< 0.001
< 0.001
0.047
0.232
0.389
0.407
0.004
0.084
0.014
0.914
NS
NS
NS
NS
*
NS
**
**
**
NS
**
NS
**
NS
**
NS
**
NS
**
NS
**
NS
NS
NS
**
*
*
NS
**
**
**
**
*
NS
NS
NS
**
NS
*
NS
df
13
12
9
8
12
11
12
12
12
12
12
12
12
12
12
12
12
11
12
12
12
12
12
12
12
12
12
12
12
11
12
11
12
11
8
7
8
7
8
7
". PAHs highlighted in yellow had concentrations
* = Significant with O.OK p < 0.05. ** = Highly
< 2*MDL. df = degrees of freedom.
significant with p < 0.01.
NS = Not significant at a = 0.05.
                                                                                                  37

-------
        Table 3-15. P-values for the significance of the lack-of-fit and the slope from the linear
                    regression and the best fit simple linear model parameters on the natural log
                    scale for PAHs for SQ-1 sediment and each holding condition".
Analyte
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo[a]
Anthracene
Chrysene
Benzo[b]
Fluoranthene
Benzo[a]pyrene
Indeno[l,2,3-c,d]
Pyrene
Dibenzo [a,h]
Anthracene
Benzo[g,h,i] Perylene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
P-value for
Lack-of-Fit
0.150
0.237
0.622
0.058
0.235
0.007
0.372
0.019
0.221
0.002
0.231
0.004
0.843
0.062
0.834
0.019
0.911
0.014
0.253
0.010
0.563
0.013
0.106
0.005
0.302
0.003
0.156
0.015
0.249
0.010
0.102
0.011
NS
NS
NS
NS
NS
**
NS
*
NS
**
NS
**
NS
NS
NS
*
NS
*
NS
**
NS
*
NS
**
NS
**
NS
*
NS
**
NS
*
Intercept
4.392
4.460
2.221
2.329
4.611
4.610
4.545
4.554
1.764
1.786
5.109
5.120
4.468
4.503
5.176
5.171
5.065
5.060
4.768
4.779
4.919
4.931
4.651
4.659
4.456
4.502
1.365
1.401
4.339
4.413
4.358
4.449
Slope
-0.00232
-0.00427
-0.00151
-0.00085
-0.00146
-0.00177
0.00007
-0.00007
-0.00024
-0.00047
-0.00228
-0.00244
-0.00074
-0.00088
0.00121
0.00121
-0.00009
-0.00018
0.00273
0.00298
-0.00055
-0.00045
0.00459
0.00378
0.00275
0.00185
0.00664
0.00525
0.00185
0.00062
0.00011
-0.00149
Standard
Error
0.0018
0.0021
0.0013
0.0017
0.0012
0.0014
0.0013
0.0013
0.0014
0.0014
0.0013
0.0013
0.0013
0.0015
0.0010
0.0010
0.0010
0.0009
0.0017
0.0016
0.0014
0.0014
0.0019
0.0018
0.0018
0.0016
0.0026
0.0019
0.0023
0.0022
0.0026
0.0020
P-value for
Slope
0.214
0.072
0.262
0.629
0.263
0.247
0.957
0.960
0.867
0.749
0.110
0.089
0.578
0.564
0.263
0.236
0.928
0.844
0.133
0.087
0.693
0.752
0.034
0.055
0.147
0.270
0.026
0.018
0.435
0.786
0.966
0.474
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
*
NS
NS
NS
*
*
NS
NS
NS
NS
df
11
10
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
        a PAHs highlighted in yellow had con'

        Significant with 0.01 < p < 0.05. **
icentrations < 2*MDL. df = degrees of freedom. NS = Not significant at a = 0.05. * =

 Highly significant with p < 0.01.
38

-------
       Table 3-16. P-values for the significance of the lack-of-fit and the slope from the linear
                 regression and the best fit simple linear model parameters on the natural log
                 scale for PAHs for Bedford-1 soil and each holding condition".
Analyte
Naphthalene

Acenaphthylene

Acenaphthene

Fluorene

Dibenzothiophene

Phenanthrene

Anthracene

Fluoranthene

Pyrene

Benzo[a] Anthracene

Chrysene

Benzo[b]
Fluoranthene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
p-value for
Lack-of-Fit
0.215
0.184
0.355
0.769
0.089
0.184
0.336
0.996
0.063
0.502
0.233
0.474
0.132
0.555
0.199
0.458
0.179
0.386
0.147
0.370
0.174
0.402
0.176
0.434
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
Intercept
5.60
5.75
5.84
5.87
4.34
4.35
4.20
4.35
4.45
4.70
7.26
7.32
5.80
5.87
8.80
8.83
8.85
8.88
8.49
8.53
8.58
8.61
8.85
8.87
Slope
0.0037
0.0032
0.0019
0.0022
0.0012
0.0011
0.0021
0.0019
0.0036
0.0015
0.0028
0.0025
0.0027
0.0025
0.0013
0.0012
0.0011
0.0012
0.0016
0.0018
0.0018
0.0019
0.0002
0.0004
Standard
Error
0.0014
0.0011
0.0008
0.0005
0.0006
0.0004
0.0012
0.0014
0.0035
0.0011
0.0011
0.0011
0.0009
0.0013
0.0010
0.0010
0.0010
0.0009
0.0009
0.0009
0.0009
0.0009
0.0009
0.0008
p-value for
Slope
0.033
0.021
0.050
0.004
0.096
0.025
0.118
0.226
0.341
0.206
0.032
0.051
0.019
0.092
0.233
0.246
0.264
0.250
0.094
0.069
0.070
0.059
0.867
0.636
*
*
*
**
NS
*
NS
NS
NS
NS
*
NS
*
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
df
8
8
8
7
7
7
7
7
8
6
8
8
8
7
8
8
8
8
8
8
8
8
8
8
       " PAHs highlighted in yellow
       * = Significant with 0.01 < p
had concentrations -
< 0.05. ** = Highly
c 2*MDL. df = degrees of freedom.
significant with p < 0.01.
NS = Not significant at a = 0.05.
Table 3-17 summarizes the statistical analyses (CV, t-test, and linear regression) of the PAH
concentrations extracted from the three soils/sediments under both holding conditions (4°C and
-20°C). Three major conclusions can be drawn from these data. First, the only sediment that
exhibited a clear distinction between holding temperature and PAH concentrations was the Eagle
Harbor soil, and only then for the lower molecular weight PAHs (anthracene, phenanthrene,
dibenzothiophene, fluorene, and acenaphthene).
                                                                                             39

-------
Table 3-17. Summary of PAH statistical analyses for each soil/sediment and holding condition."
Analyte
Naphthalene
IMethyl Naphthalene
2 Methyl Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
1 Methyl Phenanthrene
Fluoranthene
Pyrene
Benzo[a] Anthracene
Chrysene
Benzo[b]Fluoranthene
Benzo [k] Fluoranthene
Benzo [a] Pyrene
Indeno[l,2,3-c,d]
Pyrene
Dibenzo[a,h] Anthracene
Benzo[g,h,i]Perylene
Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
Eagle Harbor
Significantly
Less than Day
0 Mean
NS
NS
**
*
**
NS
**
**
*
NS
**
NS
**
NS
**
NS
*
NS
NS
NS
NS
NS
NS
*
**
**
*
**
**
**
**
**
**
**
**
**
**
**
**
**
Significant
Negative
Slope
NS
NS
NS
NS
*
NS
**
**
**
NS
**
NS
**
NS
**
NS
**
NS
**
NS
**
NS
NS
NS
**
*
*
NS
**
**
**
**
*
NS
NS
NS
**
NS
*
NS
SQ-1
Significantly
Less than Day
0 Mean
**
**
NA
NA
NA
NA
NS
NS
**
**
**
**
**
**
**
**
NS
NS
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NS
NS
NS
NS
NS
NS
*
*
Significant
Negative
Slope
NS
NS
NA
NA
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
Bedford-1
Significantly
Less than Day
0 Mean
NS
NS
NA
NA
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Significant
Negative
Slope
NS
NS
NA
NA
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
a Cells highlighted in light yellow had overall
than 2*MDL. NS=Not significant (a=0.05);
NA = not applicable.
coefficients of variation greater than 25%; and cells highlighted
=Significant (O.OK p<0.05); ** = Highly significant (p< 0.01);
in orange had observations less
and
40

-------
These PAHs extracted from the soil held at 4°C exhibited CVs>25%, a statistically significant t-
test, and a statistically significant negative slope. Fluoranthene data was seen as borderline
because it's CV=24, its t-test was not significant, but it did yield a slope significantly different
from zero. These same PAHs (including fluoranthene), extracted from the same soil but held at
-20°C exhibited no significant statistics (CVs<25%, a non-significant t-test, and a non-significant
negative slope). Second, for those soils/sediments and PAHs that exhibited no significant
statistics (Table 3-17) or mixed statistical outcomes (e.g., phenanthrene, dibenzothiophene,
fluorene, and acenaphthene extracted from SQ-1 sediment),  the CV<25% indicates that the entire
holding time analyses can be considered replicates of one another; hence, there is no significant
change over the life of this study (168 days). Finally, there was no consistent pattern among the
three soils/sediments and the behavior of PAHs either between holding conditions or by
molecular weight.

The linear regression model's estimated lower confidence limit of the slope (PLCL) was utilized
to calculate a conservative holding time estimate (prior to extraction) for a 5%, 10% or 20%
decrease in concentration to occur for each PAH at each  storage temperature. The estimated days
until a 10% and 20% decrease in concentration would be observed were all greater than 42 days
regardless of storage temperature (Tables 3-18 through 3-20). Seven of the mid to light weight
PAHs held at 4°C and two of the higher molecular weight PAHs at both holding conditions from
the  Eagle Harbor soil decreased by 5% in less than 40 days and by 10% in as little as 46 days
(Table 3-18). Three of the mid to light weight PAHs held at both holding temperatures from the
SQ-1 sediment decreased by 5% in less than 40 days and by 10% in as little as 49 days (Table
3-19). None of the PAHs from the Bedford-1 soil decreased by  5% in less than 48 days and by
10% in less than 97 days (Table 3-20).

Generally, the -20°C holding temperature would be expected to yield a longer potential holding
time than samples held at 4°C because both chemical processes (e.g., volatilization) and
biological processes (e.g., degradation) tend to decrease with decreasing temperature. In order to
delineate potential holding temperature differences as a function of time, the statistical data
should exhibit an overall CV>25, a significant t-test, and a linear regression slope significantly
different from zero. Anthracene, phenanthrene, dibenzothiophene, fluorene, and acenaphthene
extracted from the Eagle Harbor soil exemplify this behavior (Table 3-18). Many of the
estimated holding times listed in Tables 3-18 thru 3-20; however, were calculated from data that
exhibited limited variability and; hence, no statistical change in concentration with time
(CV<25%). In these cases, the magnitude of estimated holding times depended solely on the
linear regression model's estimated lower confidence limit of the slope (PLCL) rather than a
discernable (statistically significant) loss of PAH concentration. Hence, the estimated holding
time for a given decrease in concentration could be shorter than the 168 day study period and/or
exhibit a longer holding time at 4°C than at -20°C.

For the Eagle Harbor soil (Table 3-18), except for two PAHs (pyrene and benzo[k]fluoranthene),
the  holding times for soils held at -20°C were considerably longer than the holding times for
sediment held at 4°C. For the SQ-1 sediment (Table 3-19), which had only small  concentrations
                                                                                      41

-------
               Table 3-18. The estimated number of days until a given percentage decrease
                           from the intercept for PAHs (MHT=14 days) from Eagle Harbor
                           soil3.
Analyte
Naphthalene
1 Methyl Naphthalene
2 Methyl Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
1 Methyl Phenanthrene
Fluoranthene
Pyrene
Benzo[a] Anthracene
Chrysene
Benzo[b]Fluoranthene
Benzo[k]Fluoranthene
Benzo[a]Pyrene
Indeno[l,2,3-c,d]Pyrene
Dibenzo[a,h] Anthracene
Benzo[g,h,i]Perylene
Holding Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
5% Decrease
50
82
35
52
64

32
106
31
143
23
96
34
181
45
139
94
143
68
261
283
229
158
161
168
211
90
91
34
34
112
114
73
134
31
37
57
86
10% Decrease
100
163
71
104
127

64
212
61
285
46
193
68
362
90
278
189
286
136
522
565
459
315
321
337
422
179
181
69
69
223
229
146
268
62
73
114
172
20% Decrease
201
326
141
208
255

129
424
123
571
92
385
136
725
181
556
378
572
272
1044
1131
917
631
642
673
843
359
362
137
138
446
458
292
536
124
147
228
344
               a cells highlighted in light yellow had overall coefficients of variation greater than 25%; and cells
               highlighted in orange had observations less than 2*MDL.
42

-------
Table 3-19. The estimated number of days until a given percentage decrease
            from the intercept for PAHs (MHT=14 days) from SQ-1 sediment."
Analyte
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo[a] Anthracene
Chrysene
Benzo [bJFluoranthene
Benzo[a]Pyrene
Indeno[l,2,3-c,d]Pyrene
Dibenzo[a,h] Anthracene
Benzo[g,h,i]Perylene
Holding Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
5% Decrease
35
24
25
25
54
46
80
75
26
49
48
61
54
247
283
114
116
244
468
69
70
NA
2643
196
135
NA
NA
68
51
38
37
10% Decrease
71
49
51
50
109
93
161
151
52
98
96
123
109
495
566
228
233
489
937
138
140
NA
5286
393
271
NA
NA
136
103
77
75
20% Decrease
142
99
102
101
219
186
322
302
105
197
192
247
219
991
1132
456
467
979
1874
276
281
NA
10572
787
543
NA
NA
273
207
154
151
a Cells highlighted in light yellow had overall coefficients of variation greater than 25% and a negative
estimated slope; and cells highlighted in orange had observations less than 2*MDL. NA = not applicable
because the slope and lower 95% confidence limit were positive.
                                                                                                43

-------
             Table 3-20. The estimated number of days until a given percentage decrease
                      from the intercept for PAHs (MHT=14 days) from Bedford-1 soil3.
Analyte
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo[a] Anthracene
Chrysene
Benzo[b]Fluoranthene
Holding Condition
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
5% Decrease
NA
NA
66209
NA


48
215
NA
22983
NA
565
443
437
420
442
1211
2358
2288
4595
239
292
10% Decrease
NA
NA
132419
NA


97
431
NA
45966
NA
1130
886
874
840
885
2423
4717
4576
9191
478
584
20% Decrease
NA
NA
264839
NA

195
863
NA
91933
NA
2260
1773
1749
1681
1771
4847
9434
9153
18382
956
1169
             " Cells highlighted in light yellow had overall coefficients of variation greater than 25% and a negative
             estimated slope; and cells highlighted in orange had observations less than 2*MDL. NA = not applicable
             because the slope and lower 95% confidence limit were positive.
of PAHs, the reverse was true with the predicted holding time generally being longer for the 4°C
storage temperature than the -20°C storage temperature. For the Bedford-1 soil (Table 3-20),
three of the PAHs had holding times held at 4°C than at -20°C. The only analytes which had a
potential for a significant decrease in concentration over the study's holding time sequence
exhibited an overall CV>25% and concentrations >2*MDL. Of these analytes, only eight had a
statistically significant negative slope of which seven were extracted from soil held at 4°C (Table
3-21) while benzo[k]fluoranthene significantly changed at the -20°C storage temperature. Based
on the  linear regression model, dibenzothiophene exhibited the shortest minimum holding time
(92 days) for a 20% decrease in concentration (Table 3-22) which is 6.6 times longer than the
current MHT (14 days).

The behavior of six PAHs as a function of time and storage temperature have been plotted below
for each  soil/sediment (Figures 3-9 to 3-26; see Appendix B for all other PAH data plots). Plots
of the observed concentrations through time were compared to the nonparametric upper and
lower boundaries of the Day 0 concentration. The PAH concentrations plotted represent low
(acenapthylene, fluorene), mid (phenanthrene, pyrene) and high (chrysene, and benzo[a]pyrene)
ring number or molecular weight PAHs and are representative of the findings of this study.
44

-------
Table 3-21. Mean concentration (ng/g), coefficient of variation (CV), and significance of slope across time for
             analytes with CVs>25%a.
Analyte
Naphthalene
1 Methyl naphthalene
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Benzo [b]
fluoranthene
Benzo [k]
fluoranthene
Benzo [ajpyrene
Indeno [l,2,3-c,d]
pyrene
Dibenzo [a,h]
anthracene
Benzo [g,h,i] perylene
Eagle Harbor
Day 0
489
19.9%
490
18.5%
1,501
64.8%
1,846
63.4%
728
87.8%
8,199
89.8%
1,962
42.7%
9,277
60.2%

2,433
14.1%


330
0.0%

4°C
435
36.0%
NS
275
31.2%
NS
754
40.5%
**
818
44.7%
**
214
53.7%
**
2,418
52.9%
**
1,265
32.9%
**
5,849
27.4%
**

1,579
39.0%
**


157
39.8%
**

-20°C
545
52.9%
NS
439
52.8%
NS




1,708
58.7%
NS


1,443
39.7%
**




Sequim Bay
Day 0








91.2
8.1%


3.87
10.9%

76.8
8.5%
4°C








125
26.5%
NS


5.06
38.9%
NS

77.4
25.7%
NS
-20°C











4.91
28.3%
NS


Bedford-1
Day 0
283
25.5%




1,435
24.1%
343
18.2%


2,762
16.7%
5,793
16.2%
4,454
15.4%
949
13.7%
4,088
15.6%
4°C
366
37.6%
NS




1,782
28.5%
NS
401
29.0%
NS


4,733
58.7%
NS
7,478
30.4%
NS
6,762
47.8%
NS
1,160
26.8%
NS
5,500
34.7%
NS
-20°C






446
26.5%
NS


4,964
59.6%
NS
7,862
30.6%
NS
7,196
50.1%
NS
1,273
29.9%
NS
5,728
34.1%
NS
a Cells highlighted with light yellow have significant negative slopes. Blank cells indicate analytes with overall CVs less than 25%, observations
less than 2*MDL, or analytes that were not measured. NS=Not significant (a=0.05); ** = Highly significant (p < 0.01).
                                                                                                                    45

-------
         Table 3-22. Estimated number of days until a 20% decrease in concentration could be
                     observed for those analytes having a significant negative slope, an overall CV>
                     25%, and observations greater than 2*MDLa.
Analyte
Acenaphthene
Fluorene
Dibenzothiophene
Phenanthrene
Anthracene
Fluoranthene
Benzo[k]fluoranthene
Dibenzo[a,hlanthracene
Eagle Harbor
Day 0
1,501 64.8%
1,846 63.4%
728
87.8%
8,199 89.8%
1,962 42.7%
9,277 60.2%
2,433 14.1%
330
0.0%
4°C
754
40.5%
**
818
44.7%
**
214
53.7%
**
2,418 52.9%
**
1,265 32.9%
**
5,849 27.4%
**
1,579 39.0%
**
157
39.8%
**
-20°C






1,443 39.7%
**

Estimated Number of Days until a
20% Decrease in Concentration
Could Be Observed
4°C
129
123
92
136
181
272
137
124
-20°C






138

          " Cells highlighted with light yellow have significant negative slopes. Blank cells indicate analytes with overall CVs
          less than 25%, observations less than 2*MDL, or analytes that were not measured. ** = Highly significant (p < 0.01).
46

-------
'i 'in
19D
1
1 nn
5 '
°> sn
centration (n
i. O3 C
3 O C
0
O
9n


i •
i
«•• *
i^x^^^ *
• ^"W^^ 2*MDL
' • ^*^
•



» Acenaphthylene 4°C
• Acenaphthylene -20°C
• • • • Upper Bound
	 Lower Bound
4°C)
	 Linear (Acenaphthylene
-20°C)

0 50 100 150 200
Days to Extraction
Figure 3-9. Observed acenaphthylene concentration for Eagle Harbor soil at both the 4°C and
           -20°C holding temperature by holding time, significant regression lines, and
           associated Day 0 nonparametric bounds (2*MDL is indicated by the red line).
?nno
1800 -

ifinn
—~ 1400 -
.0) IHUU
"3)
c -| pnn -
c 1
o
.:; -inon
S
+-
= snn
0
O ROO
o
Ann
?no -
n
c

•


>
. •
• •
•
^x^:
* *^^
^^^

» ^^^
^

) 50 100 150 2
Days to Extraction





• Fluorene 4°C
• Fluorene -20°C
	 Lower Bound
	 Linear (Fluorene 4°C)




DO
Figure 3-10. Observed fluorene concentration for Eagle Harbor soil at both the 4°C and -20°C
           holding temperature by holding time, significant regression line, and associated Day
           0 nonparametric bounds.
                                                                                           47

-------
7000
6000-
i
cnnn -

"3)
c
1 — ' 4onn I
g
"+J
^ onnn
0)
O
c
/9 9OOO
1OOO
n
<

•
•
»•
> . • •
t •
V^
^x.
^^^^
* * ^""""v.
»"N>>s>>>^
^Xu. »
^x. t
) 50 100 150 2(
Days to Extraction




• phenanthrene 4°C
• nhananthreno 9H°P
• • • • Upper Bound





)0
     Figure 3-11. Observed phenanthrene concentration for Eagle Harbor soil at both the 4°C and
                -20°C holding temperature by holding time, significant regression line, and
                associated Day 0 nonparametric bounds.
vnnn
ROOD
i
cnnn ,
O)
"3>
C 1
^" 4nnn
o
'-P
TO
*- "^nnn
8
Oonnn
•innn


*, »
• •
»' » » *
:
•
•




» pyrene 4°C
• pyrene -20°C
• • • • Upper Bound
	 Lower Bound

0 50 100 150 200
Days to Extraction
     Figure 3-12. Observed pyrene concentration for Eagle Harbor soil at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there were no significant trends.
48

-------
3000 -
2500
i
5* 2000 !
0)

o
w
4-»
0)
y moo -
o
o
cnn -
0




/*
^p-*----»________A^
• _J I J — _
•
•






i



» chrysene 4°C
• chrysene -20°C
• • • • Upper Bound
	 Lower Bound
	 Linear (chrysene 4°C)




0 50 100 150 200
Days to Extraction
Figure 3-13. Observed chrysene concentration for Eagle Harbor soil at both the 4°C and -20°C
           holding temperature by holding time, significant regression line, and associated Day
           0 nonparametric bounds.
1/inn

1?00

innn
G) I
=* '
*^ pnn _

O
re
"c

-------
          14
       o>
       o
       'IS
       O
       o
       o
           2
                 » Acenaphthylene 4°C
                 • Acenaphthylene -20°C
                •• • Upper Bound
               	Lower Bound
                      20        40        60
                              Days to Extraction
80
100
     Figure 3-15. Observed acenaphthylene concentration for SQ-1 sediment at both the 4°C and
                -20°C holding temperature by holding time and associated Day 0 nonparametric
                bounds; there was no significant trend.
"\AC\
-I on
120 ,
•? 100 1
TO uu '
c
c an
O
^ 60 -
c.
<0
o
c 40
o
O
on -
n
(


.
i
i * * :
r •*
:




) 20 40 60 80 1(
Days to Extraction



* Fluorene 4°C

• Fluorene -20°C
• • • • Upper Bound
	 Lower Bound



DO
     Figure 3-16. Observed fluorene concentration for SQ-1 sediment at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was no significant trend.
50

-------
ocn

9nn i
3
"^ i
G)
_C_
O
5
** inn
0)
o
c
o
O 50
n
(




•

ft • 5

•





3 20 40 60 80 1(
Days to Extraction





• phenanthrene 4°C
• phenanthrene -20°C
• • • • Upper Bound
	 Lower Bound




30

Figure 3-17. Observed phenanthrene concentration for SQ-1 sediment at both the 4°C and -20°C
           holding temperature by holding time and associated Day 0 nonparametric bounds;
           there was no significant trend.
?no
isn

1RO 1
"^ i
-? -IAD _
O) '^u
c
1 — ' 190
c '^u
o
.:z -i|-vfi
Co
•p an
0)
0 fin
o
O an
Of)
f)
(


* •
. » »
I » 1 • f
•: •
•






) 20 40 60 80 1(
Days to Extraction






» pyrene 4°C
• pyrene -20°C
• • • • Upper Bound
	 Lower Bound



DO
Figure 3-18. Observed pyrene concentration for SQ-1 sediment at both the 4°C and -20°C holding
           temperature by holding time and associated Day 0 nonparametric bounds; there was
           no significant trend.
                                                                                         51

-------
9no
180
1RO

•S1 140 I
ra 14U
— 190 i
•- 100
2
*; RO
0
O en
O
O 4f)
9n
n
(


•
A
f *
k * *
* : i
•
^_





) 20 40 60 80 1
Days to Extraction





» chrysene 4°C
• chrysene -20°C
• • • • Upper Bound
	 Lower Bound



DO
     Figure 3-19. Observed chrysene concentration for SQ-1 sediment at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was no significant trend.
^A^\
i9n
*3 mn

i5
c 80 I
o
2 60 _
c

-------
cnn
OUU
O> cnn
0) 50°
_c_
c /inn '
O 4-UU
1
•£ onn 1

-------
^nnn
2500
3>
ra onnn
3 1 ^nn
1
o 1000 '
o
o
c;nn
n
(


: s

«•
*
1


3 50 100 150 2(
Days to Extraction




» phenanthrene 4°C
• phenanthrene -20°C
• • • • Upper Bound
	 Lower Bound


DO
     Figure 3-23. Observed phenanthrene concentration for Bedford-1 soil at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was no significant trend.
i?oon

moon
"3
n) ftnnn
c
.2 fjoOO '
1
o 4000
c
o
onnn
n
(


^
-
»
J
I
»



3 50 100 150 2(
Days to Extraction




• pyrene 4°C
• pyrene -20°C
• • • • Upper Bound
	 Lower Bound



DO
     Figure 3-24. Observed pyrene concentration for Bedford-1 soil at both the 4°C and -20°C holding
                temperature by holding time and associated Day 0 nonparametric bounds; there was
                no significant trend.
54

-------
Qnnn
soon

?nnn
•5*
o> ROOD 1
c cjOOO i
£ 4000 '
^
c
Q *5nnn

c
O 9000
1000 -
n
(



••* 	 ;


! »
, *
,*





) 50 100 150 2(
Days to Extraction






• chrysene 4°C
• • • • UppGr Bound
	 Lower Bound




DO
     Figure 3-25. Observed chrysene concentration for Bedford-1 soil at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was no significant trend.
         12000
       o) 10000
       O)
       ~  8000
       o
       2  6000
       03
       O
       o
       O
                                           D

                                          ^
4000
 »  benzo[a]pyrene 4°C
 •  benzo[a]pyrene -20°C
 o  4°C Outliers
 n  -20°C Outliers
• • •• Upper Bound
	Lower Bound
                          50          100         150
                               Days to Extraction
                                                  200
     Figure 3-26. Observed benzo[a]pyrene concentration for Bedford-1 soil at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was no significant negative trend.
For the Eagle Harbor soil's fluorene, and phenathrene data, storage at -20°C limited the loss of
these PAHs as well as the other five (Figs. 3-10, 3-11 and Table 3-22). While the loss of
chrysene and benzo[a]pyrene, regardless of storage temperature, was limited, most of the data
are still within the 95% confidence interval (Fig. 3-13, 3-14). For the most part, the six
representative PAHs exhibited stability for a length of time at least double that of the
recommended MHT in all 3 soils/sediments and both storage conditions.

All of the Eagle Harbor and SQ-1 PAHs and all but six of the Bedford-1 PAHs had observations
that fell outside of the Day 0 nonparametric boundaries (Figs. 3-21 to 3-26). For the Bedford-1
                                                                                          55

-------
soil, the higher molecular weight PAHs (benzo[k]fluoranthene and heavier) had only extreme
outliers for observations on day 168. No observations that could be used for the analysis after
day 14 (Fig. 3-24). Thus, only these PAHs were plotted and a holding time was not calculated.

3.2.1.3 PAH Holding Time Study - Conclusions: The objective of this study was to
determine if significant loses of PAHs occurred when sediment/soil samples were stored at either
4°C or -20°C  for a period of 168 days (12*MHT). Samples from three field sites were examined.
Of the 20 compounds that were quantified, there were only significant differences in the mean
concentration between samples stored at the two temperatures for about half of the PAHS in the
Eagle Harbor soil (Tables 3-10 and 3-21). The estimated number of days for eight PAH
compounds to decrease by 20% in Eagle Harbor soil ranged from 92 to 272 days for storage at
4°C and 138 days for one PAH stored at -20°C (Table 3-22). These data indicate that the stability
of PAHs varies with both sediment/soil type and storage conditions. The instability of the lower
molecular weight PAHs in the Eagle Harbor soil stored at 4°C is consistent with results of other
studies and probably is the result of both volatilization and biodegradation. Storage of the Eagle
Harbor soil at -20°C prior to extraction was observed to ameliorate the problem of low molecular
weight PAH concentration loss.

3.2.2 Polychlorinated Biphenyls (PCBs)
Concentrations of PCB congeners and Aroclors were characterized through time in three
sediments/soils; Housatonic River sediment, SQ-1 sediment, and Tri-Cities soil, and for two
holding temperatures (4°C and -20°C) (Appendix A, Descriptive Statistics Tables A-8 to A-10).
None of the analytes were analyzed in all three of the sediments/soils (Table 3-23). Housatonic
River sediments were analyzed for Aroclors 1254 and 1260. The SQ-1 sediment was analyzed
for Aroclor 1254, and Tri-Cities soil was analyzed for Aroclors 1242 and 1260 and seven PCB
congeners. All of the observed concentrations for the specific congeners and aroclors tested were
above 2*MDL. The SQ-1 sediment (after correction) had the lowest concentration of Aroclor
1254 averaging  125 ng/g (dry weight). The Housatonic River sediment had the highest
concentration of Aroclor 1260 averaging 23,400 ng/g. The Tri-Cities soil had the highest
concentration of Aroclor 1242 averaging 26,800 ng/g.

The value of CV<25% was considered the allowable variability between replicates for SVOC
extraction. Table 3-23 shows the mean concentration and CV of all Day 0 data accepted for
statistical analysis (including potential statistical outliers), and the across time CV for the data at
4°C and -20°C (i.e., all data across a time sequence except for Day 0). For the Aroclor analyses,
only the SQ-1 sediment exhibited Day 0 CVs>25%, but once the data was surrogate corrected
(discussed below), the CV was reduced to 0.6%. No other Day 0 CVs exceeded 25% although
congener PCB-8 extracted from the Tri-Cities  soil came close with a CV=24.7%.
56

-------
     Table 3-23. Mean PCB concentration (ng/g) and CV for all data across time accepted for
              analysis3.
Analyte
Aroclor 1242
Aroclor 1254
Aroclor 1260
PCB 8
PCB 52
PCB 153
PCB 138
PCB 187
PCB 180
PCB 170
Housatonic River
DayO

6,955
4.91%
24,880
3.92%







4°C

5,590
11.8%
22,580
13.4%







-20°C

5,804
13.9%
22,816
11.2%







Sequlm Bay
DayO

46.8
33.7%








4°C

104
47.6%








-20°C

104
41.5%








Tri-Cities
DayO
26,239
9.90%

10,653
18.4%
418
24.7%
717
14.7%
1,463
14.8%
927
16.1%
425
14.3%
857
16.3%
544
15.3%
4°C
27,053
18.8%

12,198
24.5%
607
26.2%
785
14.5%
1,406
29.5%
1,067
20.0%
507
32.5%
982
28.5%
585
25.1%
-20°C
28,408
17.3%

12,803
19.5%
605
28.4%
916
17.8%
1,614
31.2%
1,179
18.4%
561
21.5%
1,054
16.9%
666
23.5%
     a Cells highlighted with light yellow have CVs greater than 25%, and blank cells indicate analytes for which a sediment was not
     characterized.
The results shown in Table 3-23 for the mean and CV of across time data (excluding Day 0 data)
for sediment held at 4°C and -20°C, can be viewed as an estimate of data variability. The
variability arising for the across time CV analysis is a combination of sample heterogeneity,
analytical precision, and the variability with time. Given the metric of CV<25%, much of the
data for a given time sequence (excluding Day 0), soil or sediment, and storage temperature
could be considered valid replicates regardless of holding time.

For the SQ-1 Aroclor 1254 analyses, 1 observation from the -20°C sediments and two from the
4°C sediments were identified as extreme outliers (observations greater than the 75th percentile
plus 3 times the interquartile distance of the Day 0 data). These observations (3 out of 20 = 15%)
were identified in the plot (Fig. 3-29; discussed below) but they were not removed from the
analysis since the number of extreme outliers was greater than 10%. For the Tri-Cities soil,
analysis of individual PCB congeners, eight observations from the -20°C sediments and seven
from the 4°C sediments (15 out of 257 = 6%) were considered extreme outliers and were
removed from the analysis but not the plots (Fig. 3-34 to 3-40; discussed below).

3.2.2.1  Surrogate Correction of SQ-1 Sediment PCB Extraction Data: The SQ-1 sediment
was this project's first PCB extraction study. Over the life of the timed study with this sediment,
it was observed that surrogate recovery (concentration and %  recovery) increased with holding
time (days to extraction; Figure 3-27). Thus, the SQ-1 results  for Aroclor 1254 were surrogate
corrected using the surrogate PCB-198 per procedure (see section 2.2.4). However, even though
extracts were not held greater than 40 days (the MHT based on the analytical method), it was
noticed that extracts older than 30 days and surrogate corrected had a reduced Aroclor 1254
concentration (Figure 3-28). The age of the extract appeared to be a confounding factor.
                                                                                       57

-------
                     2507
                                                                      120%
                                   50
                                             100
                                                        150
                                                                   200
                                       Days to Extraction
                     Arochlor12544°C
                     Upper Bound    —
•  Arochlor1254-20°C O  4 C Extreme Outliers
	Lower Bound    —i—PCB-198 Surr4°C —
 -20°C Extreme Outliers
— PCB-198Surr-20"C
                Figure 3-27. SQ-1 sediment raw Aroclor 1254 data and surrogate
                           recovery as a function of holding time (days to extraction).
Concentration (ng/g)
D


160.0
120.0 -
oU.U
40.0
f
. . •» — : — i 	 \ 	
"* * »
•
3 *


0.0 i i i i
0 10 20 30 40 50
Age of Extract
Aroclor 1254 4°C • Aroclor 1254 -20°C O 4°C Extreme Outliers
-20°C Extreme Outliers • • • Upper Bound 	 Lower Bound
                Figure 3-28. SQ-1 surrogate corrected data as a function of the age of
                           extract.
Extracts older than 30 days were from the early sampling periods (Day 0-Day 7). While the
reason for the apparent time dependence was not determined, for the statistical analysis, only
extracts held for less than 30 days were used and the starting time of the experiment (Day 0) was
moved to the original Day 14. Interestingly, the same extract of SQ-1 for PCB analysis was
utilized in the PAH study (section 3.3.1) and no evidence of this type of behavior was noted in
those analyses. Regardless of organic contaminant of interest, all remaining extracts (except for
Bedford-1 pesticide) where analyzed prior to 30 days.
58

-------
3.2.2.2 Statistical Analysis of PCS Extraction Data: Once analyte extraction data for all
soils, storage temperatures, and holding time sequence were surrogate corrected (SQ-1  sediment)
and statistical outliers removed, data for a given soil and storage temperature were pooled across
time (0 to 168 days).  The mean, standard deviation and CV were calculated for the pooled data
(Table 3-24). Strictly based on the metric CV<25% as a measure of acceptable replicate
precision, the overall CV showed that all measurements for a given soil and analyte could be
considered valid replicates despite holding times prior to extraction stretching over 168 days.
The exceptions to this observation were congeners PCB 8 (at 4°C and -20°C), PCB 153 (at 4°C
and -20°C), and PCB 180 (at 4°C), which exhibited CVs slightly greater than 25. These data
confirm the general perception that PCBs in soils and sediments tend to have a long half-life.
These findings do not preclude the possibility that PCB concentrations change over the time
studied; rather, by the aforementioned metric data falls within the acceptance criterion  for
replicate precision.

A one-sample t-test of the null hypothesis Ho: the sample is from a population with the mean
equal to or greater than the Day 0 mean, was rejected for both Aroclors found in the Housatonic
River sediments at both holding temperatures (Table 3-24). For the SQ-1 sediment and the Tri-
Cities soil, none of the PCBs had mean concentrations that were significantly less than the Day 0
mean. With an overall CV<25%, rejection of the null hypothesis provides a measure of data
variability and validity to any potential decrease in concentration suggested by linear regression
(discussed below). Unlike the analysis of the PAH data, no PCB data exhibited a holding time
analysis with an overall CV>25% and a significant test. In fact, only the Housatonic River
sediment Aroclors and 5 Tri-Cities soil PCB congeners [8, 153 (at 4°C and -20°C) and 180 (at
4°C)] exhibited holding time analyses with mixed statistical analyses (CV<25% but a significant
t-test, or a CV>25% but a non-significant t-test). The other holding time analyses yielded data
that exhibited both an overall CV<25% and a non-significant t-test (Table 3-24) and; therefore,
these PCB concentrations must be considered stable over the 168 day period of the study.

The lack-of-fit to the linear model was significant for seven of the PCBs measured in all three
sediments (Table 3-25). The residuals for these analytes did not show a consistent U-shaped
pattern through time, and therefore, the lack-of-fit was assumed to be noise. Hence, the simple
linear model was used for all analytes, sediments, and holding temperatures. The slope
associated with the number of days held was negative and significantly different from zero for
both Aroclors measured in the Housatonic River sediment and for both holding conditions (Table
3-25). Neither of the  slopes associated with the number of days held were significantly different
from zero for Aroclor 1254 measured in SQ-1 sediment. For the Tri-Cities soil, only PCB 153 (at
both holding temperatures) had a significant, negative slope while PCB 8 (at 4°C) exhibited a
significant positive slope. There was no consistent pattern between the three samples and the
behavior of the aroclors or PCB congeners.
                                                                                      59

-------
 Table 3-24.  PCB (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a population
            the mean equal to or greater than the Day 0 mean with statistical outliers removed.
with
Analyte
Condition
Day 0
Mean and CV
(N = 5)
Overall
Mean
Standard
Deviation
CV
95% Confidence
Limits
Lower Upper
P-value"
N
                                       Housatonic River
Aroclor 1254
Aroclor 1260
4°C
-20°C
4°C
-20°C
6955 (5%)
6955 (5%)
24880 (4%)
24880 (4%)
5931
6111
23155
23366
845
875
2820
2400
14%
14%
12%
10%
5481
5626
21652
22037
6381
6596
24658
24695
<0.001
0.001
0.014
0.014
**
**
*
*
16
15
16
15
                                    SQ-l (Surrogate Corrected)
Aroclor 1254
4°C
-20°C
135 (1%)
135 (1%)
124
128
27.4
18.1
22%
10%
104
115
144
141
0.115
0.116
NS
NS
10
10
                                         Tri-Cities
Aroclor 1242
Aroclor 1260
PCB 8
PCB 52
PCB 153
PCB 138
PCB 187
PCB 180
PCB 170
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
26239 (10%)
26239 (10%)
10653 (18%)
10653 (18%)
418(25%)
418(25%)
717(15%)
717(15%)
1463 (15%)
1463 (15%)
927 (16%)
927 (16%)
425 (14%)
425 (14%)
857 (16%)
857 (16%)
544(15%)
544(15%)
26848
27270
12370
12266
569
528
800
848
1417
1577
1080
1116
427
463
991
1005
594
617
3817
3922
2511
2498
175
165
103
143
398
448
189
227
68
89
261
187
138
134
14%
14%
20%
20%
31%
31%
13%
17%
28%
28%
18%
20%
16%
19%
26%
19%
23%
22%
24541
25098
10920
10935
457
432
735
762
1176
1338
966
995
375
403
833
905
510
543
29155
29442
13820
13597
680
623
866
935
1658
1816
1194
1237
479
523
1149
1104
677
691
0.712
0.837
0.988
0.990
0.994
0.986
0.991
0.997
0.341
0.836
0.994
0.998
0.545
0.907
0.956
0.997
0.890
0.973
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
NS
13
15
14
16
12
14
12
13
13
16
13
16
9
11
13
16
13
15
1 NS = Not significant at a = 0.05; * = Significant with O.OK p < 0.05; ** = Highly significant with p < 0.01.
The linear regression model's estimated lower confidence limit of the slope (£LCL) was utilized
to calculate a conservative holding time estimate (prior to extraction) for a 5%, 10% or 20%
decrease in concentration to occur for each Aroclor or PCB congener and storage temperature.
Based on the linear regression analysis, the PCBs sampled from the Housatonic River sediment
(aroclors) and the Tri-Cities soil (aroclors and congeners) had a minimum holding time of 65
days until a 5% decrease in the natural log concentration would be  expected (Table 3-26). PCB
52 and 153 had the shortest holding times for both holding conditions. Only one of the PCBs
(PCB 8) had a positive estimated lower confidence limit on the slope (PLCL) and; thus, the
number of days until a given percentage decrease in concentration could not be calculated for the
4°C holding condition. For all but PCB 52, the holding time for the -20°C holding condition was
greater than the 4°C holding condition with the minimum holding time for a 5% decrease being
65 days for PCB 52. Given the prescribed SW-846 metric of CV<25% for replicate samples, the
shortest holding time for a 20% decrease in concentration was estimated to be 260 days, which is
18.5 times longer than the current SW-846 prescribed 14 days.
60

-------
          Table 3-25. P-values for the significance of the lack-of-fit and the slope from the linear
                    regression and the best fit simple linear model parameters on the natural
                    log scale for PCBs by sediment and holding condition.
Analyte and Holding
Temperature
P-value for
Lack of Fit
Intercept
Slope
Standard
Error
P-value for
Slope
df
                                        Housatonic River
Aroclor 1254 4°C
Aroclor 1254 -20°C
Aroclor 1260 4°C
Aroclor 1260 -20°C
0.009
0.005
0.043
0.057
**
**
*
NS
8.750
8.769
10.10
10.12
-0.00167
-0.00140
-0.00138
-0.00143
0.00051
0.00056
0.00047
0.00032
0.006
0.026
0.011
0.001
**
*
*
**
14
13
14
13
                                   Sequim Bay (Surrogate corrected)
Aroclor 1254 4°C
Aroclor 1254 -20°C
0.108
0.065
NS
NS
4.689
4.787
0.00200
0.00103
0.00127
0.00076
0.152
0.210
NS
NS
8
8
                                           Tri-Cities
Aroclor 1242 4°C
Aroclor 1242 -20°C
Aroclor 1260 4°C
Aroclor 1260 -20°C
PCB 8 4°C
PCB 8 -20°C
PCB 52 4°C
PCB 52 -20°C
PCB 153 4°C
PCB 153 -20°C
PCB 138 4°C
PCB 138 -20°C
PCB 187 4°C
PCB 187 -20°C
PCB 180 4°C
PCB 180 -20°C
PCB 170 4°C
PCB 170 -20°C
0.040
0.112
0.349
0.093
0.196
0.309
0.204
0.015
0.140
0.007
0.667
0.188
0.286
0.419
0.785
0.127
0.162
0.037
*
NS
NS
NS
NS
NS
NS
*
NS
**
NS
NS
NS
NS
NS
NS
NS
*
10.227
10.229
9.375
9.343
6.122
6.082
6.668
6.722
7.369
7.443
6.916
6.927
6.038
6.065
6.803
6.862
6.306
6.375
-0.00082
-0.00058
0.00060
0.00117
0.00693
0.00548
0.00035
0.00032
-0.00314
-0.00277
0.00113
0.00159
0.00026
0.00203
0.00142
0.00078
0.00118
0.00078
0.00065
0.00071
0.00102
0.00102
0.00222
0.00294
0.00133
0.00173
0.00114
0.00117
0.00079
0.00099
0.00114
0.00123
0.00106
0.00091
0.00104
0.00130
0.229
0.428
0.565
0.273
0.011
0.087
0.797
0.857
0.019
0.033
0.177
0.130
0.829
0.134
0.209
0.409
0.281
0.559
NS
NS
NS
NS
*
NS
NS
NS
*
*
NS
NS
NS
NS
NS
NS
NS
NS
11
13
12
14
10
12
10
11
11
14
11
14
7
9
11
14
11
13
          a df = degrees of freedom; NS = Not significant at a = 0.05; * = Significant with 0.01 < p < 0.05;
          ** = Highly significant with p < 0.01.
As a result of the wide variability in the slope estimate for Aroclor 1254 measured in the SQ-1
sediment (Table 3-25), the estimated numbers of days until a 10% decrease in natural log
concentration from the best-fit intercept was estimated as zero to one day. Confounding this wide
variability was the previously discussed concerns associated with SQ-1 Day 0 and Day 7
measurements that required surrogate correction. Even with surrogate correction; however, the
analyte's concentration appeared to be linked to extract age (Fig. 3-28). While it is believed that
data manipulation may have inserted bias into the values, it clearly reduced the variability of the
Day 0 data (prior to surrogate correction CV=33.7%, but after correction CV=0.6%). The
resulting tight data  set placed inordinate dependence on Day 0 data that can be clearly seen in the
plotted data (Fig. 3-29). Because of these concerns the data for SQ-1 sediments were not
presented in Table 3-26. Even with these concerns; however, the overall CV (Table 3-24) for the
SQ-1  sediment aroclor data suggests that there is no substantive change in the aroclor
concentration over the life of the study  (168 days).
                                                                                          61

-------
           Table 3-26. The estimated number of days until a given percentage decrease from the
           	intercept for PCBs (MHT=14 days)3.	
            Sediment
Holding Condition |  5% Decrease  | 10% Decrease  | 20% Decrease
                                               Housatonic River
Aroclor 1254
Aroclor 1260
4°C
-20°C
4°C
-20°C
157
168
211
239
315
337
422
478
630
674
844
956
                                                  Tri-Cities
Aroclor 1242
Aroclor 1260
PCBS
PCB52
PCB 153
PCB 138
PCB 187
PCB 180
PCB 170
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
227
243
289
454
NA
331
127
96
65
70
579
649
124
402
370
291
284
157
455
486
579
908
NA
663
255
192
130
140
1159
1298
248
805
740
583
569
314
911
972
1158
1817
NA
1326
511
385
260
281
2318
2597
496
1610
1481
1166
1139
628
          " Cells highlighted in light yellow had overall CVs>25%, cells highlighted in orange had CVs:
          estimated slope; cells highlighted in blue had CVs<25% and a negative estimated slope. NA =
          the slope and lower 95% confidence limit were positive.
                                                     •25% and a negative
                                                     not applicable because
62

-------

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50 100 150 2C
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• Aroclor 1254 -20°C
O 4°C Extreme Outliers
n -20°C Extreme
Outliers
• • • • Upper Bound
	 Lower Bound













        Figure 3-29. Observed Aroclor 1254 concentration for SQ-1 sediment at both the 4°C and
                  -20°C holding temperature by holding time and associated Day 0
                  nonparametric bounds; there was no significant trend.
Plots of the observed concentration through time were compared to the nonparametric upper and
lower boundaries of the Day 0 concentration for the Housatonic River sediment and the Tri-
Cities soil (Fig. 3-30 to 3-40). All of the PCBs had observations that fell outside of the Day 0
nonparametric boundaries. Regression lines are shown for those holding time sequences that
exhibited a negative slope (Aroclor 1254 and 1260 - Housatonic River and PCB 153 - Tri-
Cities). The PCB 153 congener extracted from the Tri-Cities soil appears to decrease over time
(Fig. 3-30) as the data exhibited a statistically significant negative slope (Table 3-25), its CV was
slightly greater than 25% (28.1% for both holding temperatures), but the t-test was not
significant, and the plotted data remained (for the most part) within the nonparametric bounds.
Taken together, the statistical data suggests that there is a decrease in PCB 153 over the life of
the study.  The regression model estimated that a decrease in PCB  153 concentration of 20%
would require 260 days (Table 3-26) which appears to be in agreement with the plotted data
(Fig. 3-30), but was beyond the duration of this study. With the exception of the Housatonic
River sediment Aroclors (Fig. 3-31 and 3-32; discussed below), the remaining plots show the
variability of the extraction data discussed previously, but also shows the stability of PCB
congeners and Aroclors though the holding time sequence of this study regardless of holding
temperature (Figs. 3-33 to Fig. 3-40).

The Housatonic River sediment Aroclor (1254 and 1260) data exhibited significant negative
slopes at both holding temperatures (Table 3-25). However, inspection of the data plots for these
Aroclors showed an anomaly that was difficult to explain (Fig. 3-31 and 3-32). For Aroclor 1254
the initial extractions (Day 0 and Day 7) had similar concentration means and distributions, but
concentrations at Day 14 had decreased to below the Day 0  lower bound and maintained that
concentration for the remaining 154 day time sequence (Fig. 3-31). While this behavior yielded a
statistically significant linear regression (Table 3-25), the plotted data suggests an extraction
                                                                                       63

-------
                                                                    •  PCB 153  4°C
                                                                    »  PCB153-20°C
                                                                 • •  • •  Upper Bound
                                                                 	Lower Bound
                                                                 	 Linear (PCB 153 4°C)
                                                                 	 Linear (PCB 153 -20°C)
                          50         100         150
                               Days to Extraction
200
     Figure 3-30. Observed PCB 153 concentration for Tri-Cities soil at both the 4°C and -20°C
                holding temperature by holding time, significant regression lines, and associated Day
                0 nonparametric bounds.
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m Aroclor1254-20°C
• • • • Upper Bound

	 Linear (Aroclor 1254 4°C)
	 Linear (Aroclor 1254 -20°C)



0
     Figure 3-31. Observed Aroclor 1254 concentration for Housatonic River sediment at both the 4°C
                and -20°C holding temperature by holding time, significant regression lines, and
                associated Day 0 nonparametric bounds.
64

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• Aroclor 1 260 -20°C
• • • • Upper Bound
	 Lower Bound
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     Figure 3-32. Observed Aroclor 1260 concentration for Housatonic River sediment at both the 4°C
               and -20°C holding temperature by holding time, significant regression lines, and
               associated Day 0 nonparametric bounds.
or analysis error because of the sharp break between 7 and 14 days. An explanation for this
behavior; however, could not be discerned from a reevaluation of the raw data. Despite this
aberrant behavior the overall CV<25% suggests that the holding time sequence concentrations of
the Aroclor would be within replicate precision prescribed by SW-846 (Table 3-24); hence the
concentration did not change significantly during the 168 day study. This conclusion was
essentially the same as that arising from the regression analysis in that a 5% decrease in
concentration required 157 days; essentially the length of the study. The extract concentration
data for Aroclor 1260 behaved in a similar manner (Fig. 3-32) and yielded very similar
conclusions (Table 3-24 and 3-26).

3.2.2.3 PCB Holding Time  Study- Conclusions: The objective of PCB extraction study was
to determine if significant loses of PCBs occurred when sediment/soil samples were stored at
either 4°C or -20°C for a period of 168 days. Samples from three field sites were examined. Of
the three Aroclors and 7 congeners that were quantified, there was no difference in the mean
concentration between samples stored at the two temperatures (Table 3-23). The minimum
estimated number of days required for Aroclors to decrease by 20% was 630 days (Aroclor 1254;
Housatonic River sediment) and 260 days for PCB 153 stored at 4°C (Table 3-26); both of these
time estimates are well beyond the currently prescribed 14 day MHT.
                                                                                      65

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» Aroclor 1242 -20°C
a 4°C Outlier
o -20°C Outlier
• • • • Upper Bound
	 Lower Bound



     Figure 3-33. Observed Aroclor 1242 concentration for Tri-Cities soil at both the 4°C and -20°C
                 holding temperature by holding time and associated Day 0 nonparametric bounds;
                 there was no significant trend.
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» Aroclor 1 260 -20°C
• • • • Upper Bound
	 Lower Bound



)0
     Figure 3-34. Observed Aroclor 1260 concentration for Tri-Cities soil at both the 4°C and -20°C
                 holding temperature by holding time and associated Day 0 nonparametric bounds;
                 there was no significant trend.
66

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» PCB 8 -20°C
• • • • Upper Bound
Lower Bound




30
Figure 3-35. Observed PCB 8 concentration for Tri-Cities soil at both the 4°C and -20°C holding
           temperature by holding time and associated Day 0 nonparametric bounds; there was
           no significant negative trend.

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• • • • Upper Bound
Lower Bound




0
Figure 3-36. Observed PCB 52 concentration for Tri-Cities soil at both the 4°C and -20°C holding
           temperature by holding time and associated Day 0 nonparametric bounds; there was
           no significant trend.
                                                                                          67

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                  ••••  Upper Bound
                        Lower Bound
                           50           100
                                Days to Extraction
150
200
     Figure 3-37. Observed PCB 138 concentration for Tri-Cities soil at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was not a significant decrease in concentration.




"3
O)
c

o
0)
o
o



QOO
POO
700

600

cno !
400 !

oOO
900
1OO

C

D
a

D $
* *

* •
\
*



) 50 100 150 2C
Days to Extraction













)0




• PCB1874°C
• PCB187-20°C

D 4°C Outlier
o -20°C Outlier
• • • • Upper Bound
	 Lower Bound




     Figure 3-38. Observed PCB 187 concentration for Tri-Cities soil at both the 4°C and -20°C
                holding temperature by holding time and associated Day 0 nonparametric bounds;
                there was not a significant decrease in concentration.
68

-------
     1600
     1400
  5*
  ^>
     1000
  v
  c
  O
  o
600
            '*
                                                             •   PCB1804°C
                                                             •   PCB180-20°C
                                                             Q   4°C Outlier
                                                            •• • •  Upper Bound
                                                            	Lower Bound
                      50          100          150
                           Days to Extraction
                                                      200
Figure 3-39. Observed PCB 180 concentration for Tri-Cities soil at both the 4°C and -20°C
           holding temperature by holding time and associated Day 0 nonparametric bounds;
           there was no significant trend.
1 nnn
Qnn
8nn

"S 700
0) I
§


c


1 nn

c


*
•*

'»* *
*
. •
^ . •
4






) Q 100 150 2C
Days to Extraction














)0




^*\ ^ >-i
• PCB 170 4°C
• PCB170-20°C
° 4°C Outlier
o -20°C Outlier
• • • • Upper Bound
	 Lower Bound





Figure 3-40. Observed PCB 170 concentration for Tri-Cities soil at both the 4°C and -20°C
           holding temperature by holding time and associated Day 0 nonparametric bounds;
           there was no significant trend.
                                                                                        69

-------
3.2.3 Pesticides
Concentrations of pesticides were characterized through time for each of four soils/sediments;
Housatonic River sediment, Sequim Bay (SQ-1) reference sediment, Tri-Cities soil, and
Bedford-1 soil and two holding temperatures (4°C and -20°C) (Appendix A, Descriptive
Statistics Tables A-l 1 to A-14). None of the analytes were analyzed in all four of the
sediments/soils. The pesticides that were characterized across time for each soil/sediment are
listed in Table 3-27. All of the observed concentrations were above 2*MDL except for
Housatonic River sediment concentrations for 4,4-DDD and SQ-1  sediment concentrations for y-
BHC (Table 3-27).  The SQ-1 sediment had the lowest concentration of all pesticides with its
highest concentration being a-chlordane averaging 11 ng/g (dry weight). The Tri-Cities soil had
the highest a and y chloradane concentrations averaging about 6,000 ng/g while and the
Housatonic River sediments had the highest 2,4-DDT concentrations averaging 1100 ng/g.

As with the PAH and PCB extractions,  the value of CV<25% is considered the allowable
variability between replicates for pesticide extraction. Table 3-27 shows the mean concentration
and CV of all Day 0 data accepted for statistical analysis (including potential statistical outliers)
and the across time CV for the data at 4°C and -20°C (i.e., all data across a time sequence except
for Day 0). The SQ-1 sediment exhibited Day 0 CVs>25% for most of the pesticides extracted
from this sediment (Table 3-27), but once the data were  surrogate corrected (as with the PCB
Aroclor) the CV was reduced considerably (discussed below). The only other soil/sediment to
exhibit CV>25% was the Day 0 Housatonic River sediment 4,4-DDD, whose concentration was
< 2*MDL. Interestingly, the Bedford-1 soil Day 0 analyses suggested the same curious analysis
time dependence observed for the SQ-1 Aroclors (section 3.3.2.1). However, unlike the SQ-1
analyses, the Day 0 Bedford-1 pesticide data were below the CV<25% metric.

The results shown in Table 3-27 for the mean  and CV of across time data (excluding Day 0 data)
for sediment held at 4°C and -20°C, can be viewed as an estimate of data variability. The
variability arising for the across time CV analysis is a combination of sample heterogeneity,
analytical precision, and the variability with time. Given the metric of CV<25%, much of the
data for a given time sequence (excluding Day 0), soil/sediment, and storage temperature could
be considered valid replicates regardless of holding time.

For the Housatonic River sediment, five observations from the -20°C holding temperature and
three for the 4°C holding temperature (8 out of 100 = 8%) were identified as extreme outliers
(observations greater than the 75th percentile plus 3 times the interquartile distance of the Day 0
data) and were removed from the analysis. For the SQ-1 analysis, 15 observations from the
-20°C holding temperature and 21 from the 4°C holding temperature out of 183 (20%) were
identified as extreme outliers. Because 20% of the data were considered extreme outliers and this
amount was  greater than the limit of 10%, these data were not removed from the analysis. For
the Bedford-1 soil analysis, seven observations from the -20°C holding temperature and eight
from the 4°C holding temperature out of 84 (18%) were identified as extreme outliers. These
data were not removed from the analysis.
70

-------
Table 3-27. Mean concentration (ng/g) and coefficient of variation (CV) for all pesticide data across time accepted for analysis3.
Analyte
a-BHC
Y-BHC
2,4-DDE
y-Chlordane
a-Chlordane
Trans Nonachlor
4,4-DDE
2,4-DDD
4,4-DDD
2,4-DDT
4,4-DDT
MIREX
Housatonic River
Day 0






139
2.52%

36.4
35.7%
197
4.80%
1,107
4.22%

4°C






137
16.4%

23.2
22.7%
189
16.6%
1,061
14.3%

-20°C






142
17.1%

26.0
41.9%
196
16.4%
1,064
11.9%

Sequim Bay
(Surrogate corrected)
Day 0
0.661
4.02%
0.640
12.6%
1.25
26.0%

4.43
28.3%
1.04
31.4%
1.36
30.9%
0.488
21.6%
1.04
29.9%
0.408
35.6%

0.798
36.1%
4°C
1.15
33.4%
1.17
35.2%
4.26
47.9%

9.33
43.8%
1.77
33.5%
2.67
46.5%
1.88
65.8%
2.26
38.5%
0.928
40.3%

1.62
35.7%
-20°C
1.16
23.3%
1.09
30.9%
3.87
41.9%

9.03
29.7%
1.81
22.6%
2.55
33.9%
1.58
72.0%
2.44
24.5%
0.815
20.1%

1.76
22.7%
Tri-Cities
Day 0



5,326
22.4%
5,971
21.8%
3,678
23.6%






4°C



5,678
23.9%
6,131
20.8%
3,930
22.4%






-20°C



6,251
24.6%
6,821
22.5%
4,325
23.5%






Bedford-1
Day 0







93.0
8.36%
355
2.23%

64.0
10.3%

4°C







96.0
24.4%
409
10.0%

95.9
30.5%

-20°C







96.3
23.7%
412
7.96%

92.6
23.2%

a Cells highlighted with light yellow have CVs greater than 25%, and cells highlighted with orange and bold text have observations less
than 2*MDL. Blank cells indicate analytes for which a soil/sediment was not characterized.

-------
                                                                      150%
         O)
                                                                       50%
                0
50           100          150

     Days to Extraction
200
               oc-CHLORDANE 4°C
               -20°C Extreme Outliers
               PCB-103Surr4°C
          a-CHLORDANE-20°C   O   4°C Extreme Outliers
          Upper Bound         	Lower Bound
          PCB-103Surr-20°C
        Figure 3-41. SQ-1 sediment raw a-chlordane data and surrogate recovery.
3.2.3.1 Surrogate Correction of SQ-1 Sediment Pesticide Extraction Data'. As with the
SQ-1 sediment PCB analyses, surrogate recovery for the SQ-lsediment pesticide results
generally increased with holding time (days to extraction; Fig. 3-41). Thus, the SQ-1 results were
surrogate corrected using either PCB 103 or PCB 198 based on their molecular weight (Table
3-28). Even though extracts were not held for more than 40 days, extracts older than 30 days
showed a reduced concentration (Figure 3-42). Those extracts held for more than 30 days were
from Day 0 and Day 7 sampling periods. Thus, for the statistical analysis, only extracts held for
less than 30 days were used, and the starting time of the experiment (Day 0) was moved to Day
14 data. The Bedford-1 soil pesticide results also showed an increase in the surrogate recovery
with holding time (Figure 3-43) and; thus, these  data were surrogate corrected using the
surrogates listed in Table 3-28.

3.2.3.2 Statistical Analysis of Pesticide Extraction Data'. Once analyte extraction data for
all soils/sediments, storage temperatures, and holding time sequences were surrogate corrected as
necessary (SQ-1 and Bedford-1) and statistical outliers removed, data for a given soil and storage
temperature were pooled across time (0 to 168 days). The mean, standard deviation and CV were
calculated for the pooled data (Table 3-29). Strictly based on CV<25% as a measure of
acceptable replicate precision, the overall CV showed that only  12 out of the 40 holding time
sequence pooled data sets did not meet the CV metric. Two of the holding time sequences with
CV>25% exhibited concentrations at < 2MDL, namely, 4,4-DDD from the Housatonic River
sediment and y-BHC from the SQ-1 sediment. The remaining pooled data at CV>25% were
extracted from the SQ-1 sediment (5), Tri-Cities soil (2), and one from Bedford-1  sediment. The
remaining 28 holding time sequence studies all exhibit an overall CV<25% (Table 3-29), which
suggests that these data met the SW-846 prescribed criteria for replicate precision except for the
obvious fact that the data were collected over a period of 168 days.
72

-------
                         Table 3-28. Surrogates used to correct each
                                   pesticide analyte for SQ-1 sediment
                                   and Bedford-1 soil.
Analyte
a-BHC
Y-BHC
2,4-DDE
a-Chlordane
Trans Nonachlor
4,4-DDE
2,4-DDD
4,4-DDD
2,4-DDT
4,4-DDT
MIREX
Surrogate
PCB 103
PCB 103
PCB 103
PCB 103
PCB 103
PCB 103
PCB 103
PCB 198
PCB 198
PCB 198
PCB 198



55
o
c

c
o
+J
(0
tl

Q)
o
c
o
o



•
D
18.0 ^
16.0-

14.0
12.0

10.0
8.0-

6.0-
4.0 -
2.0 -
o.o -



O
|






* •*
*

+ |


t *
w



I I I I
0 10 20 30 40 50
Age of Extract
a-CHLORDANE 4°C • a-CHLORDANE -20°C O 4°C Extreme Outliers
-20°C Extreme Outliers 	 Upper Bound 	 Lower Bound
       Figure 3-42. SQ-1 sediment a-chlordane surrogate corrected data as a function of the age of
                  extract.

A one-sample t-test of the null hypothesis Ho: the sample is from a population with the mean
equal to or greater than the Day 0 mean, was rejected for a total of 8 holding time sequence
studies (Table 3-29). Interestingly, only one holding time sequence exhibiting a significant t-test
also exhibited a CV>25% (i.e., Housatonic River sediment for 4,4-DDD held at 4°C), but this
pesticide holding time sequence had concentrations <2*MDL. The remaining 7 holding time
sequences presented conflicting statistical data; that is, they exhibited statistically significant t-
tests, but their overall CV was <25%. The Tri-Cities and Bedford-1 soils did not have any
pesticides that had mean concentrations that were significantly less than the Day 0 means.
                                                                                         73

-------
         500
     "
c
o
13
      0)
      o
      c
      o
     o
                                                                     160%
                                                                           140%  q
                                                                                  O
                                                                                  CQ
                                                                                  0)
                                                                                  (D
                                                                                  0
                                                                                  0
                                                                         %
         300
                                                                     80%
                            50            100
                                   Days to Extraction
                                                    150
200
.
» 4,4'-DDD4°C
• • • Upper Bound
•
4,4- DDD-20°C
Lower Bound
o
— I—
4°C Outliers
• PCB-198 Surr 4°C
D
— h-
-20°C Outliers
• PCB-198 Surr -20°C
     Figure 3-43. Bedford-1 soil raw 4,4'-DDD data and percent recovery of the surrogate.
Overall, 18 of 40 holding time sequences exhibited conflicting CV and t-test results; the series
either had CV<25% and significant t-tests (7 series), or CV>25% and non-significant t-tests
(1 Iseries) (Table 3-29). The 21 remaining holding time sequences exhibited CVs<25% and a
non-significant t-test (Table 3-29). For these 21 holding time sequences, the pesticide
concentrations did not change significantly over the 168 day life of the study. For the 18 holding
time sequences that exhibited conflicting CV and t-test statistics the potential for a small change
in concentration cannot be ruled out. However, the series that had an overall CV<25% essentially
exhibited variability that would fall within the current SW-846 prescribed replicate precision
acceptance.

The lack-of-fit to the linear model (using the natural log scale) was significant for 12 of the 40
pesticide holding time sequences measured in all sediments/soils at both holding temperatures
(Table 3-30). As with the PAH and PCB analysis, the pesticide residuals for the analytes did not
show a consistent U-shaped pattern through time and;  therefore, the lack-of-fit was assumed to
be noise. Hence, the simple linear model was used for all analytes, sediments/soils, and holding
temperatures. The slope associated with the number of days held was negative and significantly
different from zero for 5 of the pesticide holding time  series measured. Pesticides 4,4'-DDE from
Housatonic River sediment and 4,4-DDD from Bedford-1 soil had significantly decreasing
concentrations when held at both 4°C and -20°C, while 2,4-DDT from Housatonic River
sediment had significantly decreasing concentrations when held at -20°C.  None of the slopes
associated with the number of days held were both negative and significantly different from zero
for pesticides measured in either  SQ-1 sediment or Tri-Cities soil. There was no observable,
consistent pattern between the sediments/soils, temperature, and the behavior of the pesticides.
74

-------
Table 3-29. Pe
po
Analyte
sticides (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a
pulation with the mean equal to or greater than the Day 0 mean3.
Temp
DayO
Mean and CV
(N = 5)
Overall
Mean
Standard
Deviation
CV
95% Confidence
Limits
Lower Upper
P-value
N
                                                     Housatonic River
4,4-DDE
4,4-DDE
4,4-DDD
4,4-DDD
2,4-DDT
2,4-DDT
4,4-DDT
4,4-DDT
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
139 (3%)
139 (3%)
36.4 (36%)
36.4 (36%)
197 (5%)
197 (5%)
1107(4%)
1107(4%)
132
134
26.5
30.6
187
185
1073
1069
13.5
10.1
9.42
11.9
23.5
16.7
133
98.3
10%
8%
36%
39%
13%
9%
12%
9%
124
127
21.5
23.4
174
174
1002
1007
140
140
31.5
37.7
200
196
1144
1132
0.031
0.048
<0.001
0.051
0.070
0.022
0.158
0.104
*
*
**
NS
NS
*
NS
NS
14
11
16
13
15
11
16
12
                                                SQ-1 (Surrogate Corrected)
a-BHC
a-BHC
y-BHC
y-BHC
2,4-DDE
2,4-DDE
a-Chlordane
a-Chlordane
Trans Nonachlor
Trans Nonachlor
4,4-DDE
4,4-DDE
2,4-DDD
2,4-DDD
4,4-DDD
4,4-DDD
2,4-DDT
2,4-DDT
MIREX
MIREX
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
1.37(7%)
1.37(7%)
1.34(8%)
1.34(8%)
3.98 (2%)
3.98 (2%)
10.4 (7%)
10.4 (7%)
2.3 (4%)
2.3 (4%)
3.04 (6%)
3.04 (6%)
0.735 (3%)
0.735 (3%)
2.85 (5%)
2.85 (5%)
0.915 (16%)
0.915 (16%)
2.02 (1%)
2.02 (1%)
1.32
1.33
1.32
1.26
4.87
4.66
10.88
10.58
2.05
2.12
3.18
3.03
2.12
1.85
2.58
2.61
1.01
0.877
1.84
1.88
0.203
0.151
0.343
0.285
1.80
1.47
2.97
2.02
0.291
0.192
0.811
0.584
1.01
1.09
0.583
0.373
0.231
0.095
0.333
0.201
15%
11%
26%
23%
37%
32%
27%
19%
14%
9%
26%
19%
48%
59%
23%
14%
23%
11%
18%
11%
1.15
1.22
1.03
1.06
3.36
3.61
8.40
9.14
1.81
1.98
2.50
2.61
1.27
1.08
2.17
2.32
0.841
0.803
1.60
1.73
1.49
1.44
1.60
1.47
6.38
5.71
13.4
12.0
2.30
2.25
3.86
3.44
2.96
2.63
3.00
2.89
1.17
0.950
2.07
2.04
0.265
0.201
0.429
0.205
0.898
0.991
0.679
0.624
0.024
0.007
0.681
0.473
0.997
0.995
0.091
0.043
0.866
0.105
0.057
0.038
NS
NS
NS
NS
NS
NS
NS
NS
*
**
NS
NS
NS
NS
NS
*
NS
NS
NS
*
8
10
8
10
8
10
8
10
8
10
8
10
8
10
10
9
10
9
10
9
                                                         Tri-Cities
y-Chlordane
y-Chlordane
a-Chlordane
a-Chlordane
Trans Nonachlor
Trans Nonachlor
4°C
-20°C
4°C
-20°C
4°C
-20°C
5326 (22%)
5326 (22%)
5971 (22%)
5971 (22%)
3678 (24%)
3678 (24%)
5864
6004
6421
6577
4044
4130
1129
1584
1150
1573
816
1063
19%
26%
18%
24%
20%
26%
5212
5089
5690
5669
3526
3516
6516
6919
7152
7485
4562
4744
0.951
0.933
0.899
0.913
0.925
0.932
NS
NS
NS
NS
NS
NS
14
14
12
14
12
14
                                             Bedford -1 (Surrogate Corrected)
2,4-DDD
2,4-DDD
4,4-DDD
4,4-DDD
4,4-DDT
4,4-DDT
4°C
-20°C
4°C
-20°C
4°C
-20°C
109 (8%)
109 (8%)
352 (5%)
352 (5%)
63.3 (6%)
63.3 (6%)
108
109
348
352
76.2
74.5
13.1
10.6
33.0
29.5
20.5
14.1
12%
10%
10%
8%
27%
19%
101
103
330
337
65.2
67.0
115
115
366
368
87.1
82.1
0.406
0.529
0.302
0.502
0.988
0.997
NS
NS
NS
NS
NS
NS
16
16
16
16
16
16
* Highlighted cells have overall CV>25 (statistical outliers were removed). NS = Not significant at a = 0.05; * = Significant
with 0.01 < p < 0.05; ** = Highly significant with p < 0.01.
                                                                                                                            75

-------
         Table 3-30. P-values for the significance of the lack-of-fit and the slope from the linear
                    regression and the best fit simple linear model parameters on the natural log
                    scale for pesticides by sediment/soil and holding condition.
Analyte and Holding
Temperature
P-value for
Lack of Fit
Intercept
Slope
Standard
Error
P-value for Slope
df
                                                Housatonic River
4,4-DDE 4°C
4,4-DDE -20°C
4,4-DDD 4°C
4,4-DDD -20°C
2,4-DDT 4°C
2,4-DDT -20°C
4,4-DDT 4°C
4,4-DDT -20°C
0.267
0.002
0.059
0.263
0.047
0.150
0.010
0.013
NS
**
NS
NS
*
NS
**
*
4.94
4.94
3.21
3.38
5.23
5.28
6.97
6.97
-0.00239
-0.00183
0.000379
-0.000680
-0.000215
-0.00233
-0.0000249
-0.0000023
0.00077
0.00050
0.00150
0.00184
0.00076
0.00053
0.00062
0.00058
0.009
0.005
0.803
0.719
0.783
0.002
0.968
0.997
**
**
NS
NS
NS
**
NS
NS
12
9
14
11
13
9
14
10
                                         Sequim Bay (Surrogate Corrected)
a-BHC 4°C
a-BHC -20°C
y-BHC 4°C
y-BHC -20°C
2,4-DDE 4°C
2,4-DDE -20°C
a-Chlordane 4°C
a-Chlordane -20°C
Trans Nonachlor 4°C
Trans Nonachlor -20°C
4,4-DDE 4°C
4,4-DDE -20°C
2,4-DDD 4°C
2,4-DDD -20°C
4,4-DDD 4°C
4,4-DDD -20°C
2,4-DDT 4°C
2,4-DDT -20°C
MIREX 4°C
MIREX -20°C
0.134
0.219
0.016
0.067
0.164
0.073
0.094
0.143
0.134
0.375
0.131
0.204
0.007
0.001
0.001
0.089
0.396
0.264
0.087
0.076
NS
NS
*
NS
NS
NS
NS
NS
NS
NS
NS
NS
**
**
**
NS
NS
NS
NS
NS
0.176
0.211
0.098
0.120
1.230
1.364
2.148
2.234
0.693
0.771
0.938
0.984
0.103
-0.085
0.860
0.951
-0.151
-0.143
0.528
0.610
0.00146
0.00126
0.00238
0.00167
0.00477
0.00254
0.00328
0.00209
0.00026
-0.00048
0.00304
0.00206
0.00811
0.00933
0.00117
-0.00005
0.00245
0.00011
0.00116
0.00030
0.00092
0.00053
0.00129
0.00130
0.00103
0.00149
0.00119
0.00070
0.00101
0.00052
0.00112
0.00072
0.00223
0.00286
0.00151
0.00093
0.00123
0.00067
0.00119
0.00066
0.163
0.045
0.115
0.236
0.004
0.126
0.033
0.018
0.804
0.390
0.035
0.020
0.011
0.011
0.458
0.962
0.082
0.879
0.362
0.660
NS
*
NS
NS
**
NS
*
*
NS
NS
*
*
*
*
NS
NS
NS
NS
NS
NS
6
8
6
8
6
8
6
8
6
8
6
8
6
8
8
7
8
7
8
7
                                                    Tri-Cities
y-Chlordane 4°C
y-Chlordane -20°C
a-Chlordane 4°C
a-Chlordane -20°C
Trans Nonachlor 4°C
Trans Nonachlor -20°C
0.183
0.306
0.907
0.302
0.919
0.337
NS
NS
NS
NS
NS
NS
8.61
8.50
8.65
8.63
8.17
8.14
0.00109
0.00613
0.00398
0.00511
0.00469
0.00583
0.00087
0.0027
0.0013
0.0025
0.0014
0.0026
0.235
0.044
0.011
0.065
0.006
0.047
NS
*
*
NS
**
*
12
12
10
12
10
12
                                          Bedford-1 (Surrogate Corrected)
2,4-DDD 4°C
2,4-DDD -20°C
4,4-DDD 4°C
4,4-DDD -20°C
4,4-DDT 4°C
4,4-DDT -20°C
0.581
0.290
0.006
0.030
0.001
0.002
NS
NS
**
*
**
**
4.68
4.68
5.91
5.91
4.36
4.27
-0.000223
0.000116
-0.00143
-0.00102
-0.00134
0.000628
0.00055
0.00045
0.00028
0.00031
0.0012
0.00086
0.690
0.802
<0.001
0.005
0.302
0.475
NS
NS
**
**
NS
NS
14
14
14
14
14
14
         " df = degrees of freedom; NS = Not significant at a = 0.05; * = Significant with 0.01
         significant with p < 0.01.
c 0.05; and **= Highly
76

-------
Due to the wide variability in the slope estimate for many of the pesticides measured in the SQ-1
sediment [also observed for PCB Aroclors (section 3.3.2.2)], the estimated numbers of days until
a particular percent decrease (5%, 10%. or 20%) in natural log concentration from the best-fit
intercept was estimated as 0 to 24 days. Therefore, the SQ-1 sediment data were removed from
Table 3-31 because this calculation was dependent on Day 0 concentrations, which may have
been biased as a result of surrogate correction and analysis of extracts after 30 days but before 40
days. However, it can not be ignored that 14 out of 20 pooled SQ-1 pesticide data exhibited
corrected CVs<25%, which implies no significant change occurred for these analytes over the
168 day study.

The remaining pesticides sampled from the Housatonic River, Tri-Cities, and Bedford-1
sediments/soils had an estimated minimum holding time of 108 days or 217 days until a decrease
in the concentration of 10% or 20%, respectively, would be expected  (Table 3-31). The
estimated time required for concentration decreases of 10% and 20%  were 7.7 and 15.5 times
longer than the current SW-846 prescribed MHT for pesticides (14 days).  Four of the pesticide
holding time sequences (all associated with the Tri-Cities soil; Table 3-31) exhibited positive
estimated slopes associated with the lower confidence limits (PLCL) and; thus, the number of days
until a given percentage decrease in concentration could not be calculated. However, all four of
the pesticide holding time sequences with positive slopes exhibited non-significant t-tests, two
[a-chlordane (4°C) and trans nonachlor (4°C)] had overall CVs<25%, and the other two [y-
chlordane (-20°C) and trans nonachlor (-20°C)] had overall CVs of 26.4 and 25.7, suggesting
that the concentrations associated with these four pesticide holding time sequences did not
change significantly over the 168 day life of the study.

Plots of the observed concentration through time were compared to the nonparametric upper and
lower boundaries of the Day 0 concentration (Fig. 3-44 to 3-56). The  pesticide 4,4'-DDD from
the Housatonic River sediment and all pesticides from Tri-Cities soil fell within the Day 0
nonparametric bounds. All other pesticides had observations that were either greater or less than
these boundaries. Regression lines were included in the plots only when the slope was
significantly less than zero and negative.

Some of the Housatonic River sediment 4,4'-DDD concentrations were below 2*MDL and its
overall CV was >25%  (regardless of holding temperature). An inspection  of the plot (Fig. 3-44)
shows that the pesticide's concentration, while low, is apparently stable of the life of the study.
The other pesticides extracted from  the Housatonic River sediment (4,4'-DDE, 2,4-DDT, and
4,4-DDT) exhibited greater variability, and at least several extreme outliers (Fig. 3-45, 3-46, and
3-47). The 4,4'-DDE and 2,4-DDT analyses yielded a significant and negative slope for
sediments held at -20°C for both pesticides and at 4°C for 4,4'-DDE.  However, as can be seen
from the plots of both pesticides (Fig.  3-45 and 3-46), if the extreme outliers were removed from
the analysis, allowed the regression  slope became significant and negative. Despite the outlier
data removal, the estimated time estimated for an observed 5% decrease in concentration of 4,4'-
DDE and 2,4-DDT was calculated to be a minimum of 60 days (Table 3-31); more than 4 times
the currently prescribed SW-846 MHT metric of 14 days. The impact of outlier removal to meet
the 10% criteria for inclusion/exclusion of the data (see Section 2.3) can be seen in Fig. 3-47
where only a single data point was removed from the final timed data set.  The similarity in
                                                                                     77

-------
            Table 3-31. The estimated number of days until a given percentage decrease from
                      the intercept for pesticides (MHT=14 days) by sediment/soil and
                      holding condition3.
Analyte
Holding
Condition
5% Decrease
10% Decrease
20% Decrease
                                        Housatonic River
4,4-DDE
4,4-DDE
4,4-DDD
4,4-DDD
2,4-DDT
2,4-DDT
4,4-DDT
4,4-DDT
4°C
-20°C
4°C
-20°C
4°C
-20°C
4°C
-20°C
60
83


140
74
258
270
121
167


280
149
516
541
242
334


560
299
1032
1083
                                           Tri-Cities
Y-Chlordane
Y-Chlordane
a-Chlordane
a-Chlordane
Trans Nonachlor
Trans Nonachlor
4°C
-20°C
4°C
-20°C
4°C
-20°C
533
NA
NA
1177
NA
NA
1066
NA
NA
2354
NA
NA
2133
NA
NA
4708
NA
NA
                                  Bedford-1 (Surrogate Corrected)
2,4-DDD
2,4-DDD
4,4-DDD
4,4-DDD
4,4-DDT
4,4-DDT
4°C
-20°C
4°C
-20°C
4°C
-20°C
167
273
146
176
54
176
334
546
292
352
108
353
669
1092
584
705
217
706
            a Cells highlighted with light yellow have CVs greater than 25% and a negative estimated slope and cells
            highlighted in orange had concentrations < 2*MDL.NA = not applicable because the slope and lower 95%
            confidence limit were positive.
behavior between 2,4-DDT (Fig. 3-46) and 4,4-DDT (Fig. 3-47) during the initial 84 days and
the final timed extraction at 168 days was nearly the same yet the outlier removal changed the
result from a significant regression line slope to a non-significant regression line slope. The 4,4-
DDT did not have a slope significantly different than zero. In the case of 4,4-DDT, the same 5%
decrease in concentration was estimated to require a minimum of 258 days.

Pesticides extracted from the SQ-1 sediment are presented in Figures 3-48 to 3-52 which
represent only five of the ten pesticides extracted from the SQ-1 sediment. The remaining plots
are presented in Appendix B. As previously discussed, the SQ-1 sediment pesticide data required
surrogate correction, which caused the T = 0 replicates to be very tightly centered on the mean
(note the narrow upper and lower bounds in Figs.  3-48 to 3-52). Despite the need for surrogate
correction and the low concentrations of all the SQ-1 extracted pesticides, the data are relatively
tight over the life of the study. Unlike the Housatonic River sediment data for 4,4'-DDE and 2,4-
DDT, outlier removal does not appear to have greatly effected the regression line slope of the
plotted data.
78

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Days to Extraction




• 4,4'-DDD4°C
• 4,4'-DDD -20°C
• • • • Upper Bound
	 Lower Bound




10
Figure 3-44. Observed 4,4'-DDD concentration for Housatonic River sediment at both the 4°C
            and -20°C holding temperature by holding time and associated Day 0 nonparametric
            bounds; there was no significant trend.
    200
    180
 ~  160
 o
 2
 S  140
    120
    100
  •   4,4'-DDE4°C
  •   4,4'-DDE -20°C

  o   4°C Outlier
  °   -20°C Outlier
•  • • •  Upper Bound
	Lower Bound
	Linear (4,4'-DDE 4°C)
	Linear (4,4'-DDE -20°C)
             20
                    40
                           60
                                  80
                                        100
                                               120
                                                      140
                                                            160
                                                                   180
                               Days to Extraction
Figure 3-45. Observed 4,4'-DDE concentration for Housatonic River sediment at both the 4°C
            and -20°C holding temperature by holding time, significant regression lines, and
            associated Day 0 nonparametric bounds.

-------





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3 20 40 60 80 100 120 140 160 1f
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» 2,4-DDT4°C
• 2,4 - DDT -20°C
» 4°C Outlier
• • • • Upper Bound
	 Lower Bound

Linear (2,4-DDT -20°C)



     Figure 3-46. Observed 2,4'-DDT concentration for Housatonic River sediment at both the 4°C
                 and -20°C holding temperature by holding time, significant regression line, and
                 associated Day 0 nonparametric bounds.
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Days to Extraction



• 4,4'- DDT 4°C
• 4,4'- DDT -20°C
• • • • Upper Bound
	 Lower Bound



)0
     Figure 3-47. Observed 4,4'-DDT concentration for Housatonic River sediment at both the 4°C
                 and -20°C holding temperature by holding time and associated Day 0 nonparametric
                 bounds; there was no significant trend.
80

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• a- CHLORDANE -20°C
vv /IO/*N 1 — 4 /—I 4.r
v 4 L. extreme uutners
D -20°C Extreme Outliers
• • • • Upper Bound
Lower Bound




Figure 3-48. Observed a-chlordane concentration for SQ-1 sediment (surrogate corrected)
           at both the 4°C and -20°C holding temperature by holding time and associated
           Day 0 nonparametric bounds; there was no significant negative trend.

.0
25-
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* Trans Nonachlor 4°C

• Trans Nonachlor -20°C
O 4°C Extreme Outliers
n -20°C Extreme Outliers
.... Upper Bound
	 Lower Bound



Figure 3-49. Observed trans nonachlor concentration for SQ-1 sediment (surrogate
           corrected) at both the 4°C and -20°C holding temperature by holding time
           and associated Day 0 nonparametric bounds; there was no  significant trend.
                                                                                       81

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• 4,4' -DDE -20°C
/S 4°P Fytrpmp Ontlipr^

a -20°C Extreme Outliers
• • • • Upper Bound
	 Lower Bound




        Figure 3-50. Observed 4,4'-DDE concentration for SQ-1 sediment (surrogate corrected) at
                   both the 4°C and -20°C holding temperature by holding time and associated
                   Day 0 nonparametric bounds; there was no significant negative trend.

.u
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^ 4,4' -ODD 4°C
• 4 4 -ODD -20°C

O 4°C Extreme Outliers
n -20°C Extreme Outliers
• • • • Upper Bound
	 Lower Bound




        Figure 3-51. Observed 4,4'-DDD concentration for SQ-1 sediment (surrogate corrected) at
                   both the 4°C and -20°C holding temperature by holding time and associated
                   Day 0 nonparametric bounds; there was no significant trend.
82

-------
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* 2,4-DDT4°C
• 2,4 -DDT -20°C
O 4°C Extreme Outliers

n -20°C Extreme Outliers
• • • • Upper Bound
	 Lower Bound




        Figure 3-52. Observed 2,4'-DDT concentration for SQ-1 sediment (surrogate corrected) at
                  both the 4°C and -20°C holding temperature by holding time and associated
                  Day 0 nonparametric bounds; there was no significant trend.
All the Tri-Cities soil extracted pesticides (a-, and y-chlordane, and trans nonachlor) holding
time sequences had non-significant t-tests; only y-chlordane (at -20°C) and trans nonachlor (at
-20°C) had overall CVs>25% (both pesticides CV=26%); and the regression slope was either
non-significant or positive (Table 3-30). From these statistical results it is clear why the Tri-
Cities soil extracted pesticide data fell within the Day 0 nonparametric bounds (Fig. 3-53 to
3-55) indicating no significant trends in pesticide concentrations through time.

Of the three Bedford-1  soil extracted pesticides, only 4,4-DDD, and 4,4-DDT are plotted below
(Fig. 3-56 and 3-57) while the plot for 2,4-DDD is presented in Appendix B. The 4,4-DDD
extract data did have a significant and negative slope at both holding temperatures,  its CVs<25%
and the t-test was not significant (Table 3-30). Inspection of the plotted data (Fig. 3-56) shows
the slope to be minimal, which is reflected in the minimum estimated time (146 days) required to
observe a 5% decrease in concentration (Table 3-31).  The data plotted for the Bedford-1 soil
extracted 4,4-DDT were surrogate corrected and exhibited the numerous outliers that were not
removed for analyses because of the 18% outlier percentage. Even with the  outliers accounted
for, there was essentially no change in 4,4-DDT concentration over the life of the study.

3.2.3.3 Pesticide Holding Time Study- Conclusions:  The objective of the pesticide
extraction study was to determine if significant loses of chlorinated pesticides occurred when
sediment/soil samples were stored at either 4°C or -20°C for a period of 6 months. Samples from
four field sites were examined. Of the 12 compounds that were quantified, there was no
                                                                                       83

-------
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           9000

           8000

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        5  5000
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           1000
                  • a-CHLORDANE4°C
                  » a-CHLORDANE-20°C
                •  • • •  Upper Bound
                	Lower Bound
                           50         100
                                Days to Extraction
150
200
       Figure 3-53. Observed oc-chlordane concentration for Tri-Cities soil at both the 4°C and -20°C
                  holding temperature by holding time and associated Day 0 nonparametric
                  bounds; there was no significant negative trend.

10000
9000

anno
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D 50 100 150 2(
Days to Extraction





• Y-CHLORDANE 4°C
* Y-CHLORDANE -20°C
• • • • Upper Bound
Lower Bound




DO
       Figure 3-54. Observed y-chlordane concentration for Tri-Cities soil at both the 4°C and -20°C
                  holding temperature by holding time and associated Day 0 nonparametric
                  bounds; there was no significant negative trend.
84

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• Trans Nonachlor -20°C
• • • • Upper Bound
	 Lower Bound




DO
Figure 3-55. Observed trans nonachlor concentration for Tri-Cities soil at both the 4°C and -20°C
           holding temperature by holding time and associated Day 0 nonparametric bounds;
           there was no significant negative trend.
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• 4,4-DDD -20°C
• • • • Upper Bound
	 Lower Bound
^^^— Linear ^4,4 - uuu 4 L/J
	 Linear (4,4- ODD -20°C)


Figure 3-56. Observed 4,4'-DDD concentration for Bedford-1 soil (surrogate corrected) at both
           the 4°C and -20°C holding temperature by holding time, significant regression lines,
           and associated Day 0 nonparametric bounds.
                                                                                           85

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• 4 4'-DDT -20°C
• • • • Upper Bound
I D A
o 4°C Outliers
n -20°C Outliers



      Figure 3-57. Observed 4,4'-DDT concentration for Bedford-1 soil (surrogate corrected) at
                both the 4°C and -20°C holding temperature by holding time and associated Day
                0 nonparametric bounds; there was no significant trend.
difference in the mean concentration between samples stored at the two temperatures (Table
3-27). The estimate for the number of days for pesticides to decrease by 20% is 217 days for
4,4-DDT stored at 4°C and greater than 217 days for other compounds in three sediment/soils
(Table 3-31).  The data for SQ-1 samples could not be evaluated for stability because the initial
concentrations were significantly lower than the concentrations in the stored samples.

3.3 Acid Extraction of Metals

The six month holding time between sample collection and extraction/analysis is a substantial
time period. The larger issue of drying a solid matrix (i.e., a soil or sediment) is often questioned.
The extraction method allows the sample to be dried, but drying is not required. However,
sample homogeneity is typically more easily achieved with dried and sieved materials.

This study utilized a soil and sediment to determine if extractable concentrations of As, Cu, Pb,
and Zn changed with time, and the impact of air drying the  sample. The soil and sediment
utilized in this study exhibited very different pHs and particle size distributions (Table 3-32).

3.3.1 Statistical Analysis of Metals Extraction
Metals (As, Cu, Pb, and Zn) were characterized through  time for Sinclair river sediment and
Wilmington soil and for holding conditions (moist and air-dried) (Appendix A Descriptive
Statistics Tables A-15, A-16). The Sinclair sediment had the highest concentrations of Cu and Zn
averaging at least 487 |j,g/g and 448 ng/g, respectively (Table 3-33).  The Wilmington soil had
the highest concentrations of As and Pb averaging at least 62 (ig/g and 5653 |j,g/g, respectively
(Table 3-33).  Within replicate (Day 0) CVs ranged from 6.4% (As) to 15.9% (Pb) for the Sinclair
River sediment.
86

-------
    Table 3-32. Sediment/soil properties of materials used in metal acid-extraction study.
Sediment/Soil
Wilmington Soil
Sinclair River Sediment
Metal Analyses
As, Cu, Pb, Zn
As, Cu, Pb, Zn
pH
1.6
7.7
Eh
mv
742
462
oca
Sand
Silt
Clay
	 o/ 	

1.84
2.79
8.5
35.4
78.1
16.4
13.4
48.2
    Table 3-33. Heavy metals (ng/g) one-sample t-test of the null hypothesis Ho: the sample is from a
              population with the mean equal to or greater than the Day 0 mean.
Metal
Condition
DayO
Mean and CV
(N = 5)
Overall
Mean
Standard
Deviation
CV
95% Confidence
Limits
Lower Upper
P-value
N
                                           Sinclair
As
As
Cu
Cu
Pb
Pb
Zn
Zn
Wet
Dry
Wet
Dry
Wet
Dry
Wet
Dry
22.5 (6%)
22.5 (6%)
504 (10%)
504 (10%)
164 (16%)
164 (16%)
470 (6%)
470 (6%)
22.5
20.7
510
487
165
180
469
448
2.18
2.51
61.8
41.8
26.1
43.7
26.1
32.6
10%
12%
12%
9%
16%
24%
6%
7%
21.1
19.2
473
462
148
152
453
429
23.8
22.2
548
512
182
207
484
468
0.469
0.013
0.642
0.083
0.548
0.880
0.427
0.017
NS
*
NS
NS
NS
NS
NS
*
13
13
13
13
12
12
13
13
                                         Wilmington
As
As
Cu
Cu
Pb
Pb
Zn
Zn
Wet
Dry
Wet
Dry
Wet
Dry
Wet
Dry
63.4 (5%)
63.4 (5%)
122 (6%)
122 (6%)
5676 (8%)
5676 (8%)
61.5 (8%)
61.5 (8%)
63.5
62.0
125
127
5653
5771
62.7
63.7
3.83
4.64
8.8
9.79
813
677
7.89
5.62
6%
8%
7%
8%
14%
12%
13%
9%
61.2
59.2
120
121
5162
5362
57.7
60.1
65.8
64.8
130
133
6144
6180
67.7
67.2
0.521
0.148
0.890
0.955
0.461
0.690
0.707
0.900
NS
NS
NS
NS
NS
NS
NS
NS
13
13
13
13
13
13
12
12
    NS = Not significant at a = 0.05; * = Significant with O.OK p < 0.05.
The CVs ranged from 4.8% (As) to 8.3% (Pb) for the Wilmington soils. Two observations from
Day 0 were removed from the analysis, one observation for Pb from the Sinclair sediment and
one observation for Zn from the Wilmington soil because of possible sample contamination.
Data for each holding time sequence were pooled (Table 3-33). Only one pooled data set
exhibited a CV>20% (i.e., Sinclair River sediment for Pb held in the dry condition). The
remaining data sets exhibited fairly tight CVs across time ranging from 5.6 to 15.8. The pooled
CV data suggests that no chemically significant change in concentration occurred during the 12
month time sequence; further, the pooled data exhibited no clear cut difference between moist or
dry sample handling techniques.  The holding time sequence pooled CV data (with the exception
of the Sinclair River sediment Pb, air-dried series) are well within the SW-846 prescribed
replicate precision metric of CV<20% for the hot acid metal extraction from soils/sediments.

A one-sample t-test of the null hypothesis Ho: the sample is from a population with the mean
equal to or greater than the Day 0 mean, was rejected for the dry Sinclair sediment for As and Zn
                                                                                        87

-------
(Table 3-33). The remaining 14 data sets failed to reject the null hypothesis. For those holding
time sequences that exhibited CV<20% and a non-significant t-test, the extractable
concentrations did not changed significantly over the 12 month period of this study. Importantly,
Pb extracted from the air-dried Sinclair sediment exhibited a non-significant t-test, but a pooled
CV>20%. In contrast, Zn and As extracted from the air-dried Sinclair River sediment exhibited a
pooled CV<20%, but a significant t-test. These apparent contradictory statistics can be
reconciled by inspection of the data plots (Figs. 3-58 to 3-60).

The Sinclair River sediment As plot (Fig. 3-58) showed As concentrations to be low and the Day
0 mean to be very tightly focused around 22.5 |j,g/g sediment. In contrast, the concentration for
the dry sediment at 217 days was the lowest value measured and was outside the Day 0
nonparametric bounds. In addition, the 392 day dry sediment As concentration was also low.
These two holding time data sets were responsible for the As significant t-test.  Likewise, the
extracted Zn concentration plot for the air-dried Sinclair River sediment (Fig. 3-58) exhibited a
similar pattern at 392 days; the mean of these data were well outside the Day 0 mean (470 |j,g/g
sediment) which was sufficient to reject the t-test null hypothesis. The Pb extraction from the air-
dried Sinclair River sediment (Fig. 3-60), on the other hand, exhibited only one data set whose
mean (253 |j,g/g sediment) that was well outside of the Day 0 mean (164 |j,g/g sediment) and
resulted in an overall CV>20%, but a non-significant t-test. It seems clear that despite the
conflicting statistics the extractable concentrations of As, Pb, and Zn from the air-dried Sinclair
sediment did not change significantly over the 392 day period of this study.

The lack-of-fit to the linear model was significant only for As from the wet Sinclair River
sediment (Table 3-34). The residuals; however, did not show a consistent U-shaped pattern
through time suggesting that a parameter for curvature was not needed in the model. Therefore,
the simple linear model was used for all sediments and holding temperatures. Except for Zn in
both dry sediments, the slope associated with the number of days held was not  significantly
different from zero for any of the remaining metals and sediments (p > 0.07; Table 3-34). For all
metals and sediments; however, the absolute value of the estimated slope was very small
(<0.001) suggesting that a significant decrease was not occurring within the 392 day time frame
of the study.

The estimated numbers of days until a 5% decrease in metal concentration from the estimated
intercept would be observed were all greater than 177 days; a 20% decrease in  concentration was
estimated to require 709 days for As (Table 3-35) which had the least amount of time required
for a 20% change to be detected. Zn from the Wilmington dry sediment had a positive estimated
lower confidence limit on the slope (PLCL) and; thus, the number of days until a given percentage
decrease in concentration could not be calculated. Except for Pb in both matrices and Cu in
Wilmington soil, it appeared that the holding times for matrices held in moist state were longer
than the holding time for sediment held in an air-dried state. However, these estimates were
made from data whose slopes were not significantly different from zero and no difference was
observed between wet and air-dried samples. Hence, the estimated time required for a given
increase was directly related to the data's variability. The conservative estimate; however, is the
smaller number of days.

-------
in

25
^o ,
.
3 !
"Si 20
i
c
•S 15
5 1b
*-
c
0)
o
c 10
c 1U
0
K.
n
(


•
: »

.
•




) 100 200 300 400 5(
Days Held Until Extraction




• As-Wet
• As-Dry
.... Upper Bound
Lower Bound



)0
  Figure 3-58. Observed As concentration for Sinclair River sediment for both the wet and dry
              holding condition over holding time and associated Day 0 nonparametric
              bounds.
600

550
i
^inn
5 i
0)
±L 4^0 -
~— ' 1
O
•— 400
5
c
® TiO

O
o
^nn
9cin
200
(



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!
_ »
: - ' :






3 100 200 300 400 5(
Days Held Until Extraction






• Zn-Wet
• Zn-Dry
.... Upper Bound
	 Lower Bound




DO
Figure 3-59. Observed Zn concentration for Sinclair River sediment for both the wet and dry
           holding condition over holding time and associated Day 0 nonparametric bounds.
                                                                                          89

-------
^nn

250
"i! 200
a.
. 	 .
c
o
.= -I en i
1
0)
o
C inn
o
o
^n
n _
(


	 • 	
•
.
> »
• • • * t
;




) 100 200 300 400 5(
Days Held Until Extraction




• Pb-Wet
• Pb-Dry
• • • • Upper Bound
	 Lower Bound




DO
     Figure 3-60. Observed Pb concentration for Sinclair River sediment for both the wet and dry
                 holding condition over holding time and associated Day 0 nonparametric bounds.
     Table 3-34. P-values for the significance of the lack-of-fit and the slope from the linear regression
               and the best fit simple linear model parameters on the natural log scale for heavy
               metals for each sediment and holding condition.
Metal
P-value for
Lack of Fit
Intercept
Slope
Standard Error
P-value for
Slope
Df
                                            Sinclair Wet
As
Cu
Pb
Zn
0.048
0.696
0.651
0.350
*
NS
NS
NS
3.100
6.254
5.093
6.159
0.000048
-0.000172
0.000014
-0.000074
0.00020
0.00023
0.00031
0.00011
0.815
0.475
0.965
0.507
NS
NS
NS
NS
11
11
10
11
                                             Sinclair Dry
As
Cu
Pb
Zn
0.114
0.798
0.114
0.594
NS
NS
NS
NS
3.082
6.230
5.052
6.150
-0.000391
-0.000303
0.000707
-0.000315
0.00022
0.00015
0.00042
0.00011
0.099
0.066
0.127
0.014
NS
NS
NS
*
11
11
10
11
                                          Wilmington Wet
As
Cu
Pb
Zn
0.576
0.128
0.191
0.161
NS
NS
NS
NS
4.156
4.823
8.694
4.177
-0.00005
0.00002
-0.00044
-0.00029
0.00012
0.00014
0.00025
0.00024
0.709
0.909
0.107
0.260
NS
NS
NS
NS
11
11
11
10
                                           Wilmington Dry
As
Cu
Pb
Zn
0.148
0.418
0.054
0.251
NS
NS
NS
NS
4.156
4.812
8.700
4.093
-0.00021
0.00019
-0.00031
0.00036
0.00013
0.00014
0.00021
0.00016
0.142
0.194
0.166
0.043
NS
NS
NS
*
11
11
11
10
   NS = Not significant at a = 0.05; * = Significant with O.OK p < 0.05.
90

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                 Table 3-35. The estimated number of days until a given percentage
                          decrease from the intercept for each sediment and
                          holding condition for heavy metals (MHT=182 days) by
                	sediment and holding condition.	
                 Metal
5% Decrease  10% Decrease  20% Decrease
                                        Sinclair Wet
As
Cu
Pb
Zn
399
458
377
990
799
916
754
1980
1598
1833
1508
3961
                                        Sinclair Dry
As
Cu
Pb
Zn
177
494
1053
556
354
989
2107
1113
709
1978
4215
2227
                                      Wilmington Wet
As
Cu
Pb
Zn
695
840
444
253
1390
1680
888
507
2781
3360
1776
1014
                                      Wilmington Dry
As
Cu
Pb
Zn
414
2190
563
NAa
828
4381
1127
NA
1656
8763
2254
NA
                 NA = not applicable because the slope and lower 95% confidence limit were positive.
Figures 3-61 to 3-65 show the observed concentration through time and the nonparametric upper
and lower boundaries of the Day 0 concentration for the Wilmington soil As, Cu, Pb, and Zn,
and the Sinclair sediment Cu. All observations fell within the Day 0 nonparametric boundaries.
Thus, the concentration of metals in the two sediments held either wet or dry did not decline
significantly over the 12 month life of the study.

3.3.2  Metal Extraction Holding Time  Study - Conclusions
The objective of the metal hot acid extraction study  was to determine if the concentrations of As,
Cu, Pb, and Zn exhibited significant decreases when stored at either 4°C in either an air-dried or
field moist state for a period of 12 months. None of the metals exhibited a statistically significant
decrease in extractable concentration over the 392 day test period. In addition, none of the metal
concentration data, as a function of time,  exhibited a slope statistically different from zero.
Hence, none of the metal concentrations,  regardless  of matrix or storage condition decreased
during the life of the study. Estimates of stability suggest that a 20% decrease in concentration
would occur most rapidly for As but would require 709 days or about 3.9 times longer than the
current MHT.
                                                                                        91

-------
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fo
70
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= 60 '
s 60
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O
0 50

40 -
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J
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) 100 200 300 400 5(
Days Held Until Extraction





• As-Wet
• As-Dry
• • • • Upper Bound
	 Lower Bound





DO
     Figure 3-61. Observed As concentration for Wilmington soil for both the wet and dry holding
                condition over holding time and associated Day 0 nonparametric bounds.
onn
700 -

~* fiOO -
_o> DUU
3)
i
^ ^nn !
o
'•&
t Ann -
0
o
c
O onn
pnn _
100
(



•
•
I * *
• B
' • •
* » »
> m





) 100 200 300 400 5(
Days Held Until Extraction





• Cu-Wet
• Cu-Dry
• • • • Upper Bound
Lower Bound




30
     Figure 3-62. Observed Cu concentration for Sinclair River sediment for both the wet and dry
                holding condition over holding time and associated Day 0 nonparametric bounds.
92

-------
1RO
1 en

140
"55 1^0 i
0)
a i?n 1
c
.2 1 1 n !
5
C inn

O QO -
0
sn -
70 -
RO -
(



	 • 	
•
•
.
! m
> * * »
•
k






) 100 200 300 400 5f
Days Held Until Extraction






• Cu-Wet
• Cu-Dry
• • • • Upper Bound
	 Lower Bound




DO
Figure 3-63. Observed Cu concentration for Wilmington soil for both the wet and dry holding
           condition over holding time and associated Day 0 nonparametric bounds.
ROflO

7000 -
"55 '
"S< fiOOO I
I ;
.2 cnnn
5
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Qfl
80
~* 7fl
O) /u
"3)
* '
^ Rn
0 I
1
•5 £n
0)
o
,9 40 -
•2(1
on
(


•
•
_
:
> •
t
^ * *
*




) 100 200 300 400 5(
Days Held Until Extraction




• Zn-Wet
• Zn-Dry
• • • • Upper Bound
	 Lower Bound



)0
     Figure 3-65. Observed Zn concentration for Wilmington soil for both the wet and dry holding
                condition over holding time and associated Day 0 nonparametric bounds.
94

-------
                                     Section 4

                                   Conclusions
The extractable concentration of Cr(VI) was investigated in six soils/sediments. Of the six soils
studied, five exhibited no or only limited influence of holding time prior to extraction for the 224
days of this study regardless of the holding condition (4°C or -20°). The estimated number of
days until a 5% decrease in natural log concentration from the estimated intercept would be
observed was greater than 140 days for all sediment/soils tested.

The sixth Cr(VI) contaminated soil exhibited poor recovery (<5%) of the matrix spikes from the
outset of the study. Standard additions of Cr(VI) added to the extract solutions after filtration and
pH adjustment were not detectable by SW-846 Method 7196A, Chromium, Hexavalent
(colorimetric). Regardless of the Cr(VI) standard addition, a constant, lowUV/Vis absorbance
(-0.25  au) was measured at the prescribed 540 nm wavelength. However, the same low
absorbance was observed whether the extract absorbance was measured directly without pH
adjustment and addition of diphenylcarbazide with pH adjustment only, or as prescribed in SW-
846 Method  7196 A. These results were directly related to the high DOC content of the extracts,
which was high enough that its absorbance was significantly above background (-0.02 au).
Reduction by the dissolved Fe2+ and/or the quinine character of the DOC reduced the Cr(VI)
added to the  system to Cr(III). It is likely that Cr(VI) was not associated with this soil and the
prescreen positive Cr(VI) results were the result of high levels of extracted DOC.

The stability of the Cr(VI) soils/sediment extracts over the 56 day holding period was far beyond
the MHT of 24 hrs specified in SW-846. Even with the noted variability between replicates, the
CV across time was low with the extracts stored at 4°C exhibiting a maximum CV of 3%. When
extracts were stored at 20°C, the maximum CV was substantially greater (8%). These data
demonstrate  that for the soil/sediment extracts investigated, there was no or only very limited
change in Cr(VI) concentration within the 56-day time frame. While we can not definitively
demonstrate  or delineate the cause of observed differences between the two storage regimes, it is
well known that lower temperatures slow both microbial and chemical processes.  While these
studies strongly demonstrate that when extract stability is present at "Day 0" (that is,  the matrix
and laboratory control samples are within the specified range), it is likely that the  stability of the
extract will last considerably longer than the SW-846 specified MHT. However, because of the
chemical nature of the extract and the analysis, it advisable that sample analysis be completed as
soon as possible.

The results of the Cr(VI) study suggest that the recoveries of the control and matrix spikes are
key to determining stability of Cr(VI) in the solid materials to be extracted and the extracts
themselves. In all cases, when the recovery of the matrix  spike and control samples was good
(within acceptable parameters), the stability of Cr(VI) in the sediment/soil and extract solutions
(stored under proper conditions)  appear to be longer than the current SW-846 specified MHT.
                                                                                     95

-------
For the 17 PAH compounds that were quantified in three different soils/sediments, a holding
time of 100 days at either 4°C or -20°C would result in not more than a 20% decrease in PAH
concentration. Importantly, there is considerable variability in the estimated holding times for
different compounds and in different soils/sediments. The major consideration in sediment
holding time appears, from these studies, to be the ring number (or molecular weight) of the
PAH of interest.

The Eagle Harbor soil was collected from a creosote treatment site and contained the greatest
number of PAHs. This was the only soil/sediment that appeared to have significant loss to PAHs
for samples stored at 4°C refrigerated compared to frozen at -20°C. Compounds with relatively
low molecular weights, acenaphthene, fluorene, dibenzothiophene, phenanthrene, and anthracene
extracted from the soil held at 4°C were estimated to lose 5% of their concentration in as little as
23 days and 20% in as few as 92 days. The minimum calculated number of days for a 5% and
20% loss in concentration of these same five PAHs was 106 days and 424 days, respectively,
when the soil was held at -20°C. Our work is supported by studies of the stability of PAHs in
contaminated soil by Rost et al. (2002) who also observed significant losses of the lower
molecular weight compounds stored refrigerated compared to no significant losses for soil stored
frozen for a six week  period. Their conclusion was that microbiological degradation was the
cause for the loss because PAH concentrations in samples treated with sodium azide (a
preservative biocide)  did not change for the entire 3 month experiment.

The PAH results for the SQ-1 sediment and Bedford-1 soil exhibited none of the holding
temperature versus molecular weight results seen in the Eagle Harbor soil. However, the
minimum holding times for a 5% and 20% decrease in PAH concentrations for the SQ-1
sediment was 24 days and 99 days, respectively. The Bedford-1 soil minimum calculated holding
times for 5% and 20% PAH concentration decreases was 48 days and 195 days, respectively.
Given the SW-846 prescribed replicate precision metric of CV<25%, the shortest number of days
estimated for a 20% decrease (92 days) is 6.6 times longer than the current SW-846 MHT (14
days). Also, the results of the Eagle Harbor soil and those of Rost et al., (2002) suggest that a
holding temperature of-20°C seems appropriate regardless of the PAH under investigation.

For the three PCB Aroclor mixtures and the seven congener concentrations that were quantified
in three different soils/sediments remained fairly stable throughout the study. The minimum
estimated number of days required for Aroclors to decrease by 20% was 630 days (Aroclor
1254) and 260 days for PCB 153 stored at 4°C (Table 3-26). Both of these time estimates are
well beyond the currently prescribed SW-846 MHT of 14 days.

An indication of the stability of the PCBs in the three soil/sediments was the very small
difference in the mean concentration for all data across time at the two different storage
temperatures. In almost every case, the mean concentrations for the -20°C samples were slightly
greater, about 10% or less, than for the 4°C mean concentrations. This could be interpreted that
about 10% more PCBs are lost during 168 day storage at 4°C than at -20°C. The difference
between the "overall means" for two different temperatures similarly showed that storage for 168
day in a refrigerator resulted in not more than about  10% loss compared to freezer storage. Given
the 25% CV precision metric prescribed in SW-846, it is unlikely that this difference could be
accurately quantified.
96

-------
The pesticides sampled from the Housatonic River, Tri-Cities, and Bedford-1 sediments/soils
had a minimum holding time of 108 days and 217 days until a 10% or 20%, respectively,
decrease in the concentration would be expected. The estimated time required for concentration
decreases of 10% and 20% were 7.7 and 15.5 times longer than the current SW-846 prescribed
MHT for pesticides (14 days).  Due to the wide variability in the slope estimate for many of the
pesticides measured in the SQ-1 sediment [also observed for PCB Aroclors], the estimated
numbers of days until a 10% decrease in natural log concentration from the best-fit intercept was
estimated as 0 to 24 days. While the SQ-1 sediment pesticide holding time estimates were not
calculated because of the Day  0 data required surrogate correction, it can not be ignored that 14
out of 20 pooled SQ-1  pesticide data exhibited corrected CVs<25%, which implies no significant
change occurred for these analytes over the 168  day study. For the 10 pesticides that were
quantified in four different soil/sediments, a holding time of 217 days at 4°C and 299 days at
-20°C would result in not more than a 20% decrease in concentration, which is far greater than
the currently prescribed SW-846 MHT (14 days). There was no observable, consistent pattern
between the sediments/soils, storage temperature, and the pesticide concentrations.

Extractable metal concentrations were not affected  significantly by a holding time of up to 392
days or by air drying of the soils. Only one pooled data set exhibited a CV>20%, which is the
current SW-846 precision metric for hot acid extraction of metals. However, CV>20% was
found to be the result of one holding time data set that was well outside the Day 0 mean. The
remaining data sets exhibited fairly tight CVs across time ranging from 5.6 to 15.8%. The CV
data suggests that no chemically significant change in concentration occurred during the holding
time sequence and the pooled data exhibited no clear cut difference between moist or dry sample
handling. These results suggest that it would take a minimum of 709 days before the acid-
extractable  As, Cu, Pb, or Zn concentration would be  reduced by 20%.
                                                                                      97

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98

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Vitale, R. J., G. R. Mussoline, K. A. Rinehimer, K. L. Moeser, and J. C. Petura. 2000. An
   evaluation of a technical holding time for the preparation and analysis of hexavalent
   chromium in soils/sediments. Soil Sediment Contamin. 9, 247-259.

Wild, S. R., J. P. Obbard, C. Munn, M. L. Berrow, and K. C. Jones. 1991. The long-term
   persistence of polynuclear aromatic hydrocarbons in an agricultural soil amended with metal-
   contaminated sewage sludge. The Science of the Total Environment 101, 235-253.

Wild, S. R., K. S. Waterhouse, S. P. McGrath, and K. C. Jones. 1990.  Organic contaminants in
   an agricultural soil with a known history of sewage sludge amendments: polynuclear
   aromatic hydrocarbons. Environ. Sci. Technol. 24, 1706-1711.

US EPA, 1983. Methods of Chemical Analysis of Water and Wastes. US EPA rep. 600/4-79-
   020. US EPA Environ. Monit. And Support Lab., Office of Res. And Dev. Cincinnati,  OH.

US EPA, 1986. Determination of Stable Valence States of Chromium in Aqueous and Solid
   Waste Matrices - Experimental Verification of Chemical Behavior. US EPA Rep. 600/4-
   86/039. US EPA, Cincinnati, OH.

US EPA. 2000. Test Methods for Evaluating Solid Wastes, Physical/Chemical Methods, SW-
   846, On-line. Office of Solid Waste and Emergency Response. Washington, D.C.
                                                                                   101

-------

-------
           Appendix A

     Descriptive Statistics for
All Sediment Holding Time Studies
               Al

-------
A2

-------
Table A-l. Chrome (VI) descriptive statistics by day for each sediment and holding
temperature
Sediment and
Holding
Temperature
125A4°C





125A-20°C





125B4°C





125B-20°C





125C4°C





125C-20°C





126D4°C





126D-20°C




Day
0
14
28
56
112
224
0
14
28
56
112
224
0
14
28
56
112
224
0
14
28
56
112
224
0
14
28
56
112
224
0
14
28
56
112
224
0
14
28
56
112
224
0
14
28
56
112
N
5
2
2
2
2
2
5
2
2
2
2
2
5
2
2
2
2
2
5
2
2
2
2
2
5
2
2
2
2
2
5
2
2
2
2
2
5
2
2
2
2
1
5
2
2
2
2
Mean
(mg/kg)
91.6
61.5
104
82.4
80.4
140
91.6
90.2
107
93.3
124
80.5
328
331
355
378
344
315
328
339
383
391
333
310
62.5
64.3
76.6
62.5
62.1
60.4
62.5
58.2
65.5
71.7
65.1
59.4
815
771
868
802
833
846
815
820
874
844
799
Median
(mg/kg)
95.7
61.5
104
82.4
80.4
140
95.7
90.2
107
93.3
124
80.5
344
331
355
378
344
315
344
339
383
391
333
310
61.4
64.3
76.6
62.5
62.1
60.4
61.4
58.2
65.5
71.7
65.1
59.4
828
771
867
802
833
846
828
820
874
844
799
Standard
Deviation
11.7
2.67
50.2
3.14
10.1
61.7
11.7
19.5
24.5
4.36
20.0
3.98
39.4
58.3
2.43
14.2
36.5
7.93
39.4
31.7
79.8
80.5
25.5
22.8
7.14
6.26
12.4
0.27
0.99
0.25
7.14
0.76
2.90
2.97
2.16
2.96
30.6
0.43
18.3
13.4
8.66
*
30.6
20.5
27.0
6.52
9.13
Minimum
(mg/kg)
74.0
59.6
68.1
80.2
73.2
96.8
74.0
76.3
89.4
90.2
110
111
272
290
353
368
318
310
272
317
327
334
315
293
56.1
59.9
67.8
62.3
61.4
60.2
56.1
57.7
63.5
69.6
63.5
57.3
770
770
855
793
827
846
770
805
855
840
792
Maximum
(mg/kg)
102
63.4
139
84.6
87.5
184
102
104
124
96.4
138
83.3
362
372
356
388
369
321
362
361
440
447
351
326
74.0
68.8
85.3
62.7
62.8
60.6
74.0
58.8
67.6
73.8
66.6
61.5
840
771
881
812
839
846
840
834
893
849
805
First
Quartile
(mg/kg)
80.0
*
*
*
*
*
80.0
*
*
*
*
*
287
*
*
*
*
*
287
*
*
*
*
*
56.7
*
*
*
*
*
56.7
*
*
*
*
*
784
*
*
*
*
*
784
*
*
*
*
Third
Quartile
(mg/kg)
101
*
*
*
*
*
101
*
*
*
*
*
361
*
*
*
*
*
361
*
*
*
*
*
69.0
*
*
*
*
*
69.0
*
*
*
*
*
840
*
*
*
*
*
840
*
*
*
*
                                       A3

-------
Sediment and
Holding
Temperature

123 4°C





123-20°C





Day
224
0
14
28
56
112
224
0
14
28
56
112
224
N
2
5
2
2
2
2
2
5
2
2
2
2
2
Mean
(mg/kg)
846
330
326
379
368
273
268
330
339
366
375
352
365
Median
(mg/kg)
846
332
326
379
368
273
268
332
339
366
375
352
365
Standard
Deviation
28.7
5.60
7.86
10.6
29.3
15.4
42.4
5.60
5.86
8.81
3.20
6.57
8.60
Minimum
(mg/kg)
825
322
321
372
347
262
238
322
335
360
372
347
359
Maximum
(mg/kg)
866
336
332
387
388
284
298
336
344
373
377
357
371
First
Quartile
(mg/kg)
*
325
*
*
*
*
*
325
*
*
*
*
*
Third
Quartile
(mg/kg)
*
335
*
*
*
*
*
335
*
*
*
*
*
* = Not calculable
                                                  A4

-------
Table A-2. PAH descriptive statistics for Eagle Harbor sediment held at 4°C
Analyte
Naphthalene






1 Methyl Naphthalene




2 Methyl Naphthalene






Acenaphthalene






Acenaphthene






Fluorene






Dibenzothiophene






Day
0
7
14
28
42
84
168
0
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
4
2
1
2
2
2
2
3
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
Mean
(ng/g)
489
467
507
624
442
206
401
490
359
319
152
269
119
105
99.1
81.8
70.0
39.2
63.7
97.3
66.1
92.1
58.4
70.0
82.1
39.9
1021
913
977
1010
866
649
220
1270
1162
1185
1054
797
671
224
410
380
274
257
210
112
77.8
Median
(ng/g)
478
467
507
624
442
206
401
503
359
319
152
269
110
105
99.1
81.8
70.0
39.2
63.7
96.3
66.1
92.1
58.4
70.0
82.1
39.9
944
913
977
1010
866
649
220
1133
1162
1185
1054
797
671
224
374
380
274
257
210
112
77.8
Standard
Deviation
97.4
144
*
169
0.00
51.2
85.2
90.8
13.5
0.00
33.5
44.7
20.3
25.6
*
3.58
0.00
10.0
10.8
10.5
9.48
*
6.53
0.00
8.01
9.21
186
179
*
140
0.00
175
18.8
247
250
*
145
0.00
144
30.7
67.9
80.4
*
50.9
0.00
39.1
10.1
Minimum
(ng/g)
401
365
507
505
442
170
341
394
349
319
128
238
106
86.7
99.1
79.3
70.0
32.2
56.0
87.5
59.4
92.1
53.8
70.0
76.5
33.3
885
786
977
911
866
525
206
1122
986
1185
952
797
570
203
368
324
274
221
210
84.5
70.6
Maximum
(ng/g)
601
568
507
744
442
242
461
574
368
319
176
301
143
123
99.1
84.3
70.0
46.3
71.3
108.3
72.8
92.1
63.0
70.0
87.8
46.4
1233
1039
977
1108
866
772
233
1555
1339
1185
1157
797
773
246
488
437
274
293
210
140
84.9
First
Quartile
(ng/g)
404
*
*
*
*
*
*
394
*
*
*
*
106
*
*
*
*
*
*
87.5
*
*
*
*
*
*
885
*
*
*
*
*
*
1122
*
*
*
*
*
*
368
*
*
*
*
*
*
Third
Quartile
(ng/g)
586
*
*
*
*
*
*
574
*
*
*
*
143
*
*
*
*
*
*
108.3
*
*
*
*
*
*
1233
*
*
*
*
*
*
1555
*
*
*
*
*
*
488
*
*
*
*
*
*
                                       A5

-------
Analyte
Phenanthrene






Anthracene






1 Methyl Phenanthrene






Fluoranthene






Pyrene






Benzo[a] Anthracene






Chrysene






Day
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
3
2
1
2
2
2
2
Mean
(ng/g)
4530
4217
3414
2843
2194
1430
911
1559
1525
1630
1334
1254
1520
511
420
426
472
397
374
390
292
6504
6661
6926
6744
6443
6100
2758
4807
4842
5019
4905
4601
4497
4343
1605
1489
1617
1495
1347
1367
1242
2026
2057
1918
1814
1704
1968
1623
Median
(ng/g)
4190
4217
3414
2843
2194
1430
911
1687
1525
1630
1334
1254
1520
511
412
426
472
397
374
390
292
6462
6661
6926
6744
6443
6100
2758
4887
4842
5019
4905
4601
4497
4343
1627
1489
1617
1495
1347
1367
1242
2041
2057
1918
1814
1704
1968
1623
Standard
Deviation
771
956
*
877
0.00
467
135
283
12.0
*
39.6
0.00
437
27.2
53.9
68.5
*
29.4
0.00
64.6
8.04
793
746
*
757
0.00
656
143
542
479
*
508
0.00
507
258
122
88.2
*
187
0.00
90.6
204
193
175
*
184
0.00
174
330
Minimum
(ng/g)
3988
3541
3414
2223
2194
1100
816
1234
1516
1630
1306
1254
1211
492
371
377
472
376
374
344
286
5733
6134
6926
6209
6443
5636
2657
4229
4503
5019
4546
4601
4139
4161
1473
1427
1617
1363
1347
1303
1098
1825
1934
1918
1684
1704
1845
1389
Maximum
(ng/g)
5413
4893
3414
3462
2194
1761
1006
1756
1533
1630
1362
1254
1829
531
478
474
472
418
374
436
298
7318
7189
6926
7279
6443
6564
2859
5304
5181
5019
5265
4601
4856
4525
1714
1552
1617
1628
1347
1431
1386
2211
2181
1918
1944
1704
2091
1856
First
Quartile
(ng/g)
3988
*
*
*
*
*
*
1234
*
*
*
*
*
*
371
*
*
*
*
*
*
5733
*
*
*
*
*
*
4229
*
*
*
*
*
*
1473
*
*
*
*
*
*
1825
*
*
*
*
*
*
Third
Quartile
(ng/g)
5413
*
*
*
*
*
*
1756
*
*
*
*
*
*
478
*
*
*
*
*
*
7318
*
*
*
*
*
*
5304
*
*
*
*
*
*
1714
*
*
*
*
*
*
2211
*
*
*
*
*
*
A6

-------
Analyte
Benzo [b] Fluoranthene





Benzo [k] Fluoranthene





Benzo [a] Pyrene





Indeno [1 ,2,3-c,d] Pyrene





Dibenzo [a,h] Anthracene





Benzo[g,h,i] Perylene





Day
0
7
28
42
84
168
0
7
28
42
84
168
0
7
28
42
84
168
0
7
28
42
84
168
0
7
28
42
84
168
0
7
28
42
84
168
N
4
2
2
2
2
2
4
2
2
2
2
2
4
2
2
2
2
2
1
1
2
2
2
2
1
1
2
2
2
2
1
1
2
2
2
2
Mean
(ng/g)
2469
2023
2130
1929
1998
1359
2433
1995
1816
1640
1990
456
965
810
741
667
799
687
672
684
417
368
408
454
330
309
163
148
139
102
651
674
439
392
444
331
Median
(ng/g)
2381
2023
2130
1929
1998
1359
2347
1995
1816
1640
1990
456
911
810
741
667
799
687
672
684
417
368
408
454
330
309
163
148
139
102
651
674
439
392
444
331
Standard
Deviation
348
171
240
0.00
36.4
254
342
167
207
0.00
41.8
87.8
145
55.0
79.9
0.00
9.9
105
*
*
33.7
0.00
13.2
108
*
*
12.2
0.00
5.98
27.9
*
*
31.8
0.00
9.40
81.4
Minimum
(ng/g)
2180
1903
1961
1929
1973
1180
2148
1877
1670
1640
1960
394
862
771
685
667
792
612
672
684
393
368
399
378
330
309
154
148
134
81.8
651
674
417
392
438
273
Maximum
(ng/g)
2934
2144
2300
1929
2024
1539
2889
2113
1963
1640
2019
518
1177
849
798
667
806
761
672
684
441
368
417
531
330
309
171
148
143
121
651
674
462
392
451
388
First
Quartile
(ng/g)
2191
*
*
*
*
*
2159
*
*
*
*
*
867
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
Third
Quartile
(ng/g)
2835
*
*
*
*
*
2792
*
*
*
*
*
1119
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
* = Not calculable, too few observations
                                                    A7

-------
Table A-3. PAH descriptive statistics for Eagle Harbor sediment held at -20°C
Analyte
Naphthalene






1 Methyl Naphthalene




2 Methyl Naphthalene






Acenaphthalene






Acenaphthene






Fluorene






Dibenzothiophene






Day
0
7
14
28
42
84
168
0
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
4
1
2
2
2
2
2
3
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
Mean
(ng/g)
489
548
475
970
505
254
521
490
681
433
200
444
119
130
133
173
119
62.8
132
97.3
91.8
114
63.0
52.0
71.6
45.3
1021
1127
1172
1246
949
639
1115
1270
1421
1448
1528
1146
1023
1308
410
446
450
476
349
288
389
Median
(ng/g)
478
548
475
970
505
254
521
503
681
433
200
444
110
130
133
173
119
62.8
132
96.3
91.8
114
63.0
52.0
71.6
45.3
944
1127
1172
1246
949
639
1115
1133
1421
1448
1528
1146
1023
1308
374
446
450
476
349
288
389
Standard
Deviation
97.4
*
2.90
530
55.9
2.42
58.2
90.8
377
47.4
8.56
37.2
20.3
*
4.64
71.9
14.5
2.72
2.47
10.5
*
7.75
14.3
6.83
4.57
1.12
186
*
28.0
302
114
78.1
4.00
247
*
10.8
477
80.7
139
72.5
67.9
*
6.01
129
1.24
34.3
15.2
Minimum
(ng/g)
401
548
472
595
466
252
480
394
414
399
194
418
106
130
129
123
109
60.8
130
87.5
91.8
108
52.9
47.1
68.4
44.5
885
1127
1152
1032
868
584
1112
1122
1421
1440
1190
1088
925
1257
368
446
446
385
348
264
379
Maximum
(ng/g)
601
548
477
1344
545
255
562
574
948
466
206
470
143
130
136
224
130
64.7
133
108
91.8
119
73.1
56.8
74.8
46.1
1233
1127
1192
1460
1030
694
1118
1555
1421
1456
1865
1203
1121
1359
488
446
455
567
350
312
400
First
Quartile
(ng/g)
404
*
*
*
*
*
*
394
*
*
*
*
106
*
*
*
*
*
*
87.5
*
*
*
*
*
*
885
*
*
*
*
*
*
1122
*
*
*
*
*
*
368
*
*
*
*
*
*
Third
Quartile
(ng/g)
586
*
*
*
*
*
*
574
*
*
*
*
143
*
*
*
*
*
*
108
*
*
*
*
*
*
1233
*
*
*
*
*
*
1555
*
*
*
*
*
*
488
*
*
*
*
*
*
                                       A8

-------
Analyte
Phenanthrene






Anthracene






1 Methyl Phenanthrene






Fluoranthene






Pyrene






Benzo[a] Anthracene






Chrysene






Day
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
3
1
2
2
2
2
2
Mean
(ng/g)
4530
4961
5081
5360
4160
3641
4707
1559
1595
1721
2925
1219
1117
1614
420
422
461
416
360
326
422
6504
6334
6596
6802
5919
5362
6295
4807
4593
4800
4813
4278
3735
4593
1605
1357
1537
1405
1277
1249
1299
2026
1736
1907
1845
1595
1601
1788
Median
(ng/g)
4190
4961
5081
5360
4160
3641
4707
1687
1595
1721
2925
1219
1117
1614
412
422
461
416
360
326
422
6462
6334
6596
6802
5919
5362
6295
4887
4593
4800
4813
4278
3735
4593
1627
1357
1537
1405
1277
1249
1299
2041
1736
1907
1845
1595
1601
1788
Standard
Deviation
771
*
125
1540
335
501
455
283
*
16.1
2379
47.2
105
471
53.9
*
5.24
117
17.7
30.4
45.8
793
*
324
973
766
456
574
542
*
237
711
576
331
372
122
*
107
86.3
182
89.6
162
193
*
121
102
230
80.2
16.9
Minimum
(ng/g)
3988
4961
4992
4271
3923
3287
4386
1234
1595
1709
1243
1185
1043
1281
371
422
457
334
347
304
389
5733
6334
6367
6114
5377
5040
5889
4229
4593
4632
4310
3871
3501
4330
1473
1357
1461
1344
1149
1186
1184
1825
1736
1821
1773
1433
1544
1776
Maximum
(ng/g)
5413
4961
5169
6449
4397
3995
5029
1756
1595
1732
4608
1252
1191
1947
478
422
465
499
372
347
454
7318
6334
6825
7490
6460
5685
6701
5304
4593
4968
5316
4686
3970
4856
1714
1357
1612
1466
1406
1312
1413
2211
1736
1993
1917
1757
1658
1800
First
Quartile
(ng/g)
3988
*
*
*
*
*
*
1234
*
*
*
*
*
*
371
*
*
*
*
*
*
5733
*
*
*
*
*
*
4229
*
*
*
*
*
*
1473
*
*
*
*
*
*
1825
*
*
*
*
*
*
Third
Quartile
(ng/g)
5413
*
*
*
*
*
*
1756
*
*
*
*
*
*
478
*
*
*
*
*
*
7318
*
*
*
*
*
*
5304
*
*
*
*
*
*
1714
*
*
*
*
*
*
2211
*
*
*
*
*
*
A9

-------
Analyte
Benzo [b] Fluoranthene





Benzo [k] Fluoranthene





Benzo [a] Pyrene





Indeno [1,2,3-c,d] Pyrene




Dibenzo [a,h] Anthracene




Benzo[g,h,i] Perylene




Day
0
7
28
42
84
168
0
7
28
42
84
168
0
7
28
42
84
168
0
28
42
84
168
0
28
42
84
168
0
28
42
84
168
N
4
1
2
2
2
2
4
1
2
2
2
2
4
1
2
2
2
2
1
2
2
2
2
1
2
2
2
2
1
2
2
2
2
Mean
(ng/g)
2469
1776
1969
1888
1872
1400
2433
1751
1678
1608
1865
466
965
720
689
655
712
747
672
368
372
441
561
330
142
141
135
118
651
384
398
489
457
Median
(ng/g)
2381
1776
1969
1888
1872
1400
2347
1751
1678
1608
1865
466
911
720
689
655
712
747
672
368
372
441
561
330
142
141
135
118
651
384
398
489
457
Standard
Deviation
348
*
78.4
343
24.4
118
342
*
69.3
294
26.2
38.3
145
*
24.8
89.2
89.0
3.80
*
15.7
65.1
74.0
136
*
6.90
28.9
12.3
20.8
*
24.5
71.3
121
141
Minimum
(ng/g)
2180
1776
1913
1646
1855
1317
2148
1751
1629
1400
1847
439
862
720
672
592
649
744
672
357
326
389
465
330
137
120
126
104
651
366
348
404
357
Maximum
(ng/g)
2934
1776
2024
2130
1889
1484
2889
1751
1727
1816
1884
493
1177
720
707
718
775
749
672
379
418
493
657
330
147
161
144
133
651
401
449
574
557
First
Quartile
(ng/g)
2191
*
*
*
*
*
2159
*
*
*
*
*
867
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
Third
Quartile
(ng/g)
2835
*
*
*
*
*
2792
*
*
*
*
*
1119
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
' = Not calculable, too few observations
                                                   A10

-------
Table A-4. PAH descriptive statistics for SQ-1 sediment by day for sediment held at 4°C
Analyte
Naphthalene




Acenaphthalene




Acenaphthene




Fluorene





Dibenzothiophene




Phenanthrene





Anthracene





Fluoranthene





Day
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
N
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
Mean
(ng/g)
94.12
66.49
67.50
79.53
80.70
65.66
9.43
9
10
8
8
9
114.0
90.1
95.7
89.9
92.6
94.2
105
89
92
84
94
101
7
6
5
5
6
6
189.12
147
152
142
152
144
82
92
91
84
89
80
173.59
183
192
179
180
201
Median
(ng/g)
91.32
66.49
67.50
79.53
80.70
65.66
9.2
9
10
8
8
9
113.9
90.1
95.7
89.9
92.6
94.2
101
89
92
84
94
101
7
6
5
5
6
6
1 91 .49
147
152
142
152
144
79
92
91
84
89
80
171.33
183
192
179
180
201
Standard
Deviation
8.08
1.72
15.2
7.75
20.4
5.37
1.221
0.58
0.962
0.658
2.24
0.29
5.3
4.96
7.3
1.82
24.6
0.382
9.38
5.73
2.55
7.57
27
0.81
0.451
0.0071
0.163
0.1344
1.78
0.0778
12.54
4.93
3.82
2.05
43.6
2.2
13.87
4.59
4.27
2.12
27.6
0.891
10.62
5.63
0.88
8.04
52.3
5.64
Minimum
(ng/g)
87.8
65.3
56.7
74.1
66
61.86
8.34
8.92
9.03
7.54
6.55
8
109
87
91
89
75
93.94
99.2
85
90.6
78.6
74.5
100
6
6
5
5
5
6
176
144
149
141
122
142.11
70
89
88
82
70
79
164
179
191
173
143
196.88
Maximum
(ng/g)
103.2
67.7
78.3
85.0
95
69.46
10.75
9.74
10.39
8.47
9.72
9
119
94
101
91
110
94.48
116.1
93
94.2
89.3
112.6
102
7
6
6
5
7
6
200
151
155
144
183
145.22
97
95
94
85
109
81
185
187
192
184
217
204.85
First
Quartile
(ng/g)
87.8
*
*
*
*
8.34
*
*
*
*
109
*
*
*
*
99.2
*
*
*
*
*
6
*
*
*
*
176
*
*
*
*
*
70
*
*
*
*
*
164
*
*
*
*
*
Third
Quartile
(ng/g)
103.22
*
*
*
*
10.75
*
*
*
*
119.29
*
*
*
*
116.11
*
*
*
*
*
7.08
*
*
*
*
200.3
*
*
*
*
*
97.22
*
*
*
*
*
185.16
*
*
*
*
*
                                       All

-------
Analyte
Pyrene





Benzo[a] Anthracene





Chrysene





Benzo [b] Fluoranthene





Benzo [a] Pyrene





Indeno [1,2,3-c,d] Pyrene





Dibenzo [a,h] Anthracene





Benzo[g,h,i] Perylene





Day
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
N
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
Mean
(ng/g)
156.91
158
168
154.2
155.3
160
105.31
141.09
140.16
120.89
122.2
152.98
125.62
149.1
151.3
131.5
132.6
131
108.3
119.5
123.9
102.1
102.1
179.1
82
101.27
100.8
83.875
85.3
118.48
4.453
4.425
4.6
3.6
4.2
8.4
74.2
98.84
84.9
64.8
75.4
100.35
90.96
95.3
66.2
57
75.4
92.9
Median
(ng/g)
156.29
158
168
154.2
155.3
160
102.27
141.09
140.16
120.89
122.2
152.98
119.1
149.1
151.3
131.5
132.6
131
108.52
119.5
123.9
102.1
102.1
179.1
81.96
101.27
100.8
83.875
85.3
118.48
4.33
4.425
4.6
3.6
4.2
8.4
70.9
98.84
84.9
64.8
75.4
100.35
95.38
95
66.2
57
75.4
92.9
Standard
Deviation
4.26
5.55
0.48
3.2
45.7
4.73
13.7
10.57
12.98
4.37
40.3
5.23
13.49
11.62
11.93
5.29
42.8
2.87
8.72
6.79
14.9
4.51
32.3
23.9
2.02
4.26
16
1.28
32
13.51
0.487
0.375
0.608
0.424
2.03
0.933
11.16
0.396
18.8
2.79
32.1
9.19
7.69
0.269
16
6.51
32.4
5.23
Minimum
(ng/g)
153
154
167.9
152.0
123
156.57
93.4
133.61
131.0
117.8
94
149.28
116.67
140.85
142.86
127.78
102.3
128.79
99.47
115
113.4
98.9
79.3
162.2
80.0
98.3
89.5
83.0
62.6
108.92
4.04
4.16
4.18
3.33
2.79
7.75
65.08
98.56
71.6
62.87
52.7
93.85
82.08
95.06
54.9
52.64
52.6
89.21
Maximum
(ng/g)
161
162
168.6
156.5
188
163.3
120.3
148.56
149.3
124.0
151
156.67
141.14
157.29
159.73
135.26
162.9
132.9
116.91
124
134.4
105.2
124.9
196.0
84.0
104.3
112.1
84.8
107.9
128.03
4.99
4.69
5.04
3.93
5.66
9.07
86.64
99.12
98.2
66.81
98.1
106.84
95.43
95.44
77.5
61.85
98.4
96.6
First
Quartile
(ng/g)
153
*
*
*
*
*
93.4
*
*
*
*
*
116.67
*
*
*
*
*
99.47
*
*
*
*
*
80.0
*
*
*
*
*
4.04
*
*
*
*
*
65.08
*
*
*
*
*
82.08
*
*
*
*
*
Third
Quartile
(ng/g)
1 61 .45
*
*
*
*
*
120.27
*
*
*
*
*
141.14
*
*
*
*
*
116.91
*
*
*
*
*
84.04
*
*
*
*
*
4.99
*
*
*
*
*
86.64
*
*
*
*
*
95.43
*
*
*
*
*
* = Not calculable, too few observations
                                                   A12

-------
Table A-5. PAH descriptive statistics for SQ-1 sediment by day for sediment held at
-20°C
Analyte
Naphthalene




Acenaphthalene




Acenaphthene




Fluorene





Dibenzothiophene




Phenanthrene





Anthracene





Fluoranthene




Day
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
N
3
1
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
Mean
(ng/g)
94.12
71.01
90.71
58.35
79.605
65.1
9.43
10.06
13.56
8.89
9.755
9.66
113.98
91.85
103.23
74.87
93.93
94
105.31
92.44
99.24
75.1
94.22
102.15
6.697
5.84
6.23
4.535
5.62
6.34
189.12
158.7
163.42
123.97
151.22
147.6
82.12
96.96
108.09
76.08
91.71
82.66
173.59
180.09
206.35
159.98
177.52
Median
(ng/g)
91.32
71.01
90.71
58.35
79.605
65.1
9.2
10.06
13.56
8.89
9.755
9.66
113.94
91.85
103.23
74.87
93.93
94
100.68
92.44
99.24
75.1
94.22
102.15
6.81
5.84
6.23
4.535
5.62
6.34
1 91 .49
158.7
163.42
123.97
151.22
147.6
79.18
96.96
108.09
76.08
91.71
82.66
171.33
180.09
206.35
159.98
177.52
Standard
Deviation
8.08
5.83
6.46
1.096
25.9
1.221
0.198
0.735
1.287
1.322
1.56
5.3
6.12
5.51
4.28
1.97
14.5
9.38
5.73
10.82
5.65
4.48
8.05
0.451
0.594
0.17
0.318
0.0849
0.0707
12.54
16
2.09
6.65
0.85
9.81
13.87
10.01
5.64
4.96
6.2
1.77
10.62
12.45
5.16
7.87
3.21
Minimum
(ng/g)
87.81
71.01
86.59
53.78
78.83
46.8
8.34
9.92
13.04
7.98
8.82
8.56
108.7
87.52
99.33
71.84
92.54
83.7
99.15
88.39
91.59
71.1
91.05
96.46
6.2
5.42
6.11
4.31
5.56
6.29
175.56
147.4
161.94
119.27
150.62
140.67
69.96
89.88
104.1
72.57
87.32
81.4
164.29
171.29
202.7
154.41
175.25
Maximum
(ng/g)
103.22
71.01
94.83
62.91
80.38
83.4
10.75
10.2
14.08
9.8
10.69
10.77
119.29
96.18
107.12
77.89
95.32
104.3
116.11
96.49
106.89
79.09
97.39
107.84
7.08
6.26
6.35
4.76
5.68
6.39
200.3
170
164.9
128.67
151.82
154.54
97.22
104.03
112.08
79.59
96.09
83.91
185.16
188.89
210
165.54
179.79
First
Quartile
(ng/g)
87.81
*
*
*
*
8.34
*
*
*
*
108.7
*
*
*
*
99.15
*
*
*
*
*
6.2
*
*
*
*
175.56
*
*
*
*
*
69.96
*
*
*
*
*
164.29
*
*
*
*
Third
Quartile
(ng/g)
103.22
*
*
*
*
10.75
*
*
*
*
119.29
*
*
*
*
116.11
*
*
*
*
*
7.08
*
*
*
*
200.3
*
*
*
*
*
97.22
*
*
*
*
*
185.16
*
*
*
*
                                       A13

-------
Analyte

Pyrene





Benzo[a] Anthracene





Chrysene





Benzo [b] Fluoranthene





Benzo [a] Pyrene





Indeno [1,2,3-c,d] Pyrene





Dibenzo [a,h] Anthracene





Benzo[g,h,i] Perylene





Day
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
N
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
3
2
2
2
2
2
Mean
(ng/g)
203.1
156.91
155.77
180.09
137.95
153.46
160.35
105.31
136.54
157.81
113.8
127.48
156.25
125.62
145.59
173.27
120.76
135.38
133.66
108.3
110.04
138.22
98.51
98.73
166.8
82
94.82
123.77
83.56
89.68
109.48
4.453
4.185
5.14
3.56
4.405
7.265
74.19
88.9
117.15
63.26
87.66
88.65
90.96
86.45
97.18
56.54
85.24
81.49
Median
(ng/g)
203.1
156.29
155.77
180.09
137.95
153.46
160.35
102.27
136.54
157.81
113.8
127.48
156.25
119.05
145.59
173.27
120.76
135.38
133.66
108.52
110.04
138.22
98.51
98.73
166.8
81.96
94.82
123.77
83.56
89.68
109.48
4.33
4.185
5.14
3.56
4.405
7.265
70.86
88.9
117.15
63.26
87.66
88.65
95.38
86.45
97.18
56.54
85.24
81.49
Standard
Deviation
17.9
4.26
12.28
5.3
7.26
2.14
13.51
13.7
9.75
6.82
12.13
0.76
4.65
13.49
10.52
6.03
13.48
2.57
4.68
8.72
2.41
0.47
11.42
0.948
26
2.02
5.66
1.24
11.38
1.87
12.05
0.487
0.177
0.0424
0.792
0.148
0.587
11.16
2.82
9.83
12.28
2.38
8.95
7.69
3.51
7.98
12.7
1.58
7.74
Minimum
(ng/g)
190.5
152.99
147.09
176.34
132.82
151.95
150.79
93.38
129.64
152.98
105.22
126.94
152.96
116.67
138.15
169
1 1 1 .22
133.56
130.35
99.47
108.33
137.88
90.43
98.06
148.4
80
90.82
122.89
75.51
88.35
100.96
4.04
4.06
5.11
3
4.3
6.85
65.08
86.9
110.2
54.57
85.98
82.32
82.08
83.97
91.53
47.56
84.12
76.01
Maximum
(ng/g)
215.8
161.45
164.45
183.83
143.09
154.98
169.9
120.27
143.43
162.63
122.38
128.02
159.54
141.14
153.03
177.53
130.29
137.2
136.97
116.91
111.74
138.55
106.58
99.4
185.1
84.04
98.83
124.65
91.61
91
118
4.99
4.31
5.17
4.12
4.51
7.68
86.64
90.89
124.1
71.94
89.34
94.98
95.43
88.93
102.82
65.52
86.36
86.96
First
Quartile
(ng/g)
*
152.99
*
*
*
*
*
93.38
*
*
*
*
*
116.67
*
*
*
*
*
99.47
*
*
*
*
*
80
*
*
*
*
*
4.04
*
*
*
*
*
65.08
*
*
*
*
*
82.08
*
*
*
*
*
Third
Quartile
(ng/g)
*
1 61 .45
*
*
*
*
*
120.27
*
*
*
*
*
141.14
*
*
*
*
*
116.91
*
*
*
*
*
84.04
*
*
*
*
*
4.99
*
*
*
*
*
86.64
*
*
*
*
*
95.43
*
*
*
*
*
' = Not calculable, too few observations
                                                   A14

-------
Table A-6. PAH descriptive statistics for Bedford -1 sediment by day for sediment held at
4°C
Analyte
Naphthalene


Acenaphthalene


Acenaphthene


Fluorene



Dibenzothiophene


Phenanthrene



Anthracene



Fluoranthene



Pyrene


Benzo[a] Anthracene


Chrysene


Benzo [b] Fluoranthene

Day
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
N
4
2
2
2
4
2
2
2
4
2
2
1
3
2
2
2
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
Mean
(ng/g)
283
221
374
503
346
309
420
476
74.6
72.8
88.2
92.3
78.6
57.5
65.2
95.3
108
47.7
150
155
1435
1219
1860
2267
343
274
410
518
6639
5681
8330
8102
6851
6072
8809
8315
4837
4293
6135
6380
5278
4730
6661
7129
6903
6108
8521
Median
(ng/g)
282
221
374
503
336
309
420
476
73.1
72.8
88.2
92.3
79.2
57.5
65.2
95.3
109
47.7
150
155
1506
1219
1860
2267
341
274
410
518
6846
5681
8330
8102
7001
6072
8809
8315
5006
4293
6135
6380
5437
4730
6661
7129
6989
6108
8521
Standard
Deviation
72.1
90.9
76.0
24.5
48.4
0.610
137
37.0
5.67
0.997
7.87
*
18.4
14.8
16.0
7.44
17.2
47.6
30.9
8.61
345
84.4
403
74.3
62.2
14.1
80.5
35.7
1376
505
1723
17.5
1359
569
1746
71.0
794
544
1097
11.7
867
624
1235
73.2
1151
912
1555
Minimum
(ng/g)
210
157
320
486
302
308
323
450
69.7
72.1
82.6
92.3
59.9
47.0
53.9
90.1
86.5
14.0
128
149
1005
1159
1575
2215
270
264
353
493
5001
5323
7112
8090
5261
5670
7574
8265
3850
3908
5360
6371
4190
4289
5788
7077
5509
5463
7421
Maximum
(ng/g)
357
285
428
521
412
309
517
502
82.4
73.5
93.8
92.3
96.8
67.9
76.5
101
126
81.4
172
161
1724
1278
2145
2320
417
284
467
543
7863
6038
9548
8115
8143
6474
10044
8365
5488
4678
6911
6388
6047
5171
7534
7181
8124
6753
9621
First
Quartile
(ng/g)
216
*
*
306
*
*
70.1
*
*
*
59.9
*
*
*
90.6
*
*
*
1081
*
*
*
283
*
*
*
5252
*
*
*
5495
*
*
*
4022
*
*
*
4386
*
*
5751
*
Third
Quartile
(ng/g)
350
*
*
397
*
*
80.6
*
*
*
96.8
*
*
*
124
*
*
*
1719
*
*
*
403
*
*
*
7819
*
*
*
8059
*
*
*
5484
*
*
*
6010
*
*
7968
*
                                      A15

-------
Analyte

Benzo [k] Fluoranthene



Benzo [a] Pyrene



Indeno [1,2,3-c,d] Pyrene


Dibenzo [a,h] Anthracene



Benzo[g,h,i] Perylene


Day
168
0
7
14
0
7
14
168
0
7
14
0
7
14
168
0
7
14
0
N
2
4
2
2
4
2
2
1
4
2
2
4
2
2
1
4
2
2
4
Mean
(ng/g)
7078
2762
2501
3436
5793
5157
7282
9936
4454
3953
5563
949
827
1184
1444
4088
3660
5110
2762
Median
(ng/g)
7078
2819
2501
3436
5897
5157
7282
9936
4540
3953
5563
969
827
1184
1444
4154
3660
5110
2819
Standard
Deviation
27.1
460
316
555
937
761
1317
*
686
547
1067
130
110
234
*
638
507
955
460
Minimum
(ng/g)
7059
2199
2277
3044
4644
4619
6350
9936
3599
3566
4809
781
749
1018
1444
3304
3302
4435
2199
Maximum
(ng/g)
7097
3211
2725
3828
6733
5695
8214
9936
5137
4340
6317
1077
904
1350
1444
4739
4018
5786
3211
First
Quartile
(ng/g)
*
2295
*
*
4845
*
*
*
3756
*
*
815
*
*
*
3443
*
*
2295
Third
Quartile
(ng/g)
*
3172
*
*
6637
*
*
*
5067
*
*
1063
*
*
*
4667
*
*
3172
' = Not calculable, too few observations
                                                   A16

-------
Table A-7. PAH descriptive statistics for Bedford -1 sediment by day for sediment held at
-20°C
Analyte
Naphthalene


Acenaphthalene


Acenaphthene


Fluorene



Dibenzothiophene


Phenanthrene



Anthracene



Fluoranthene



Pyrene


Benzo[a] Anthracene


Chrysene


Benzo [b] Fluoranthene

Day
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
168
0
7
14
N
4
2
2
2
4
2
1
2
4
2
1
2
3
2
2
2
4
2
1
1
4
2
2
2
4
2
2
1
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
2
4
2
2
Mean
(ng/g)
283
337
418
526
346
377
367
506
74.6
84.9
78.2
92.4
78.6
78.7
90.2
106
108
107
137
139
1435
1550
1913
2274
343
342
433
524
6639
6656
8349
8309
6851
7120
8817
8643
4837
4965
6216
6824
5278
5389
6688
7468
6903
6881
8415
Median
(ng/g)
282
337
418
526
336
377
367
506
73.1
84.9
78.2
92.4
79.2
78.7
90.2
106
109
107
137
139
1506
1550
1913
2274
341
342
433
524
6846
6656
8349
8309
7001
7120
8817
8643
5006
4965
6216
6824
5437
5389
6688
7468
6989
6881
8415
Standard
Deviation
72.1
15.3
75.3
23.6
48.4
37.4
*
23.2
5.67
4.93
*
2.97
18.4
0.346
55.4
10.1
17.2
18.8
*
*
345
315
515
110
62.2
47.9
128
*
1376
1543
1802
226
1359
1658
1710
215
794
1200
1239
378
867
1287
1327
291
1151
1544
1652
Minimum
(ng/g)
210
326
365
509
302
350
367
490
69.7
81.4
78.2
90.3
59.9
78.5
51
99.2
86.5
93.7
137
139
1005
1327
1548
2196
270
309
342
524
5001
5565
7075
8149
5261
5948
7608
8491
3850
4116
5339
6558
4190
4479
5749
7262
5509
5790
7247
Maximum
(ng/g)
357
348
471
543
412
403
367
522
82.4
88.4
78.2
94.5
96.8
79.0
129
113
126
120
137
139
1724
1772
2277
2351
417
376
524
524
7863
7746
9623
8468
8143
8293
10026
8795
5488
5813
7092
7091
6047
6299
7626
7674
8124
7973
9584
First
Quartile
(ng/g)
216
*
*
306
*
*
70.1
*
*
*
59.9
*
*
*
90.6
*
*
*
1081
*
*
*
283
*
*
*
5252
*
*
*
5495
*
*
*
4022
*
*
*
4386
*
*
5751
*
Third
Quartile
(ng/g)
350
*
*
397
*
*
80.6
*
*
*
96.8
*
*
*
124
*
*
*
1719
*
*
*
403
*
*
*
7819
*
*
*
8059
*
*
*
5484
*
*
*
6010
*
*
7968
*
                                      A17

-------
Analyte

Benzo [k] Fluoranthene


Benzo [a] Pyrene


Indeno [1,2,3-c,d] Pyrene


Dibenzo [a,h] Anthracene


Benzo[g,h,i] Perylene


Day
168
0
7
14
0
7
14
0
7
14
0
7
14
0
7
14
N
2
4
2
2
4
2
2
4
2
2
4
2
2
4
2
2
Mean
(ng/g)
7571
2762
2793
3389
5793
5837
7120
4454
4465
5404
949
944
1177
4088
4133
4978
Median
(ng/g)
7571
2819
2793
3389
5897
5837
7120
4540
4465
5404
969
944
1177
4154
4133
4978
Standard
Deviation
376
460
617
734
937
1385
1387
686
988
1051
130
208
251
638
931
934
Minimum
(ng/g)
7305
2199
2357
2870
4644
4857
6140
3599
3767
4661
781
797
1000
3304
3474
4318
Maximum
(ng/g)
7837
3211
3230
3908
6733
6817
8101
5137
5164
6147
1077
1091
1355
4739
4791
5639
First
Quartile
(ng/g)
*
2295
*
*
4845
*
*
3756
*
*
815
*
*
3443
*
*
Third
Quartile
(ng/g)
*
3172
*
*
6637
*
*
5067
*
*
1063
*
*
4667
*
*
' = Not calculable, too few observations
                                                   A18

-------
Table A-8. PCB descriptive statistics for Housatonic River sediment by day and holding condition.


Analyte


Day


N

Mean
(ng/g)

Median
(ng/g)

Standard
Deviation

Minimum
(ng/g)

Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
                                       Housatonic River 4°C
Arochlor 1254






Arochlor 1260






0
7
14
28
42
84
168
0
7
14
28
42
84
168
4
2
2
2
2
2
2
4
2
2
2
2
2
2
6955
6672
5250
5864
5616
4990
5147
24880
26736
22528
23149
23659
18426
20980
7014
6672
5250
5864
5616
4990
5147
25281
26736
22528
23149
23659
18426
20980
342
121
312
63
774
103
444
976
140
202
696
4672
256
957
6510
6587
5030
5820
5069
4917
4833
23428
26637
22385
22658
20355
18245
20303
7283
6758
5471
5909
6163
5063
5461
25532
26836
22670
23641
26963
18607
21657
6602
*
*
*
*
*
*
23885
*
*
*
*
*
*
7250
*
*
*
*
*
*
25475
*
*
*
*
*
*
                                      Housatonic River -20°C
Arochlor 1254






Arochlor 1260






0
7
14
28
42
84
168
0
7
14
28
42
84
168
4
2
2
2
1
2
2
4
2
2
2
1
2
2
6955
7217
5784.3
5663.5
4882.4
5278.1
5540
24880
25896
24165
24317
21563
19728
20599
7014
7217
5784
5664
4882
5278
5540
25281
25896
24165
24317
21563
19728
20599
342
737
83.2
128.7
*
76.2
579
976
885
162
2181
*
937
1134
6510
6696
5726
5572
4882
5224
5131
23428
25270
24050
22775
21563
19066
19797
7283
7738
5843
5755
4882
5332
5949
25532
26522
24280
25860
21563
20391
21401
6602
*
*
*
*
*
*
23885
*
*
*
*
*
*
7250
*
*
*
*
*
*
25475
*
*
*
*
*
*
* = Not calculable, too few observations
                                              A19

-------
Table A-9. PCB descriptive statistics for SQ-1 sediment by day and holding condition.
Data has been surrogate corrected, and only extracts held less than 30 days were used in
the analysis.	
 Analyte
         Mean  Median
Day  N   (ng/g)   (ng/g)
                             First     Third
Standard  Minimum  Maximum   Quartile  Quartile
Deviation   (ng/g)     (ng/g)     (ng/g)    (ng/g)
SQ-1 4°C
Arochlor 1 254 0
14
28
70
154

Arochlor 1254 0
14
28
70
154
2
2
2
2
2

2
2
2
2
2
135
117
89.6
117.9
160.1

135
129
105
120
150
135
117
89.6
117.9
160.1
SQ-1
135
129
105
120
150
0.810
4.00
26.7
19.4
15.6
-20°C
0.810
1.04
6.39
9.50
24.5
135
114
70.8
104
149

135
128
101
113
132
136
120
109
132
171

136
130
110
127
167
*
*
*
*
*

*
*
*
*
*
* = Not calculable, too few observations
                                            A20

-------
Table A-10. PCB descriptive statistics for Tri-Cities NY sediment by day and holding condition.
Analyte
Day
N
Mean
(ng/g)
Median
(ng/g)
Standard
Deviation
Minimum
(ng/g)
Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
                                             Tri-Cities, NY 4°C
Arochlor 1242






Arochlor 1260






PCB 8






PCB 52






PCB 153






PCB 138






PCB 187






0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
4
2
1
1
1
2
2
4
2
1
1
2
2
2
4
2
1
1
2
2
0
4
2
1
1
2
2
0
4
2
0
1
2
2
2
4
2
0
1
2
2
2
4
1
0
1
2
0
1
26239
26619
25479
29211
28566
32565
21223
10653
12213
10839
11775
14991
15174
11599
418
497
566
519
837
699
*
717
902
860
786
883
761
*
1463
1900
*
1923
1423
918
1081
927.1
1146
*
1161
1081
1156
1206
425
450
*
524
356
*
461
25467
26619
25479
29211
28566
32565
21223
10820
12213
10839
11775
14991
15174
11599
407
497
566
519
837
699
*
683.8
902
860
786
883
761
*
1391
1900
*
1923
1423
918
1081
883.6
1146
*
1161
1081
1156
1206
403
450
*
524
356
*
461
2598
320
*
*
*
3688
427
1957
2493
*
*
1605
312
4053
103
13.0
*
*
124
86.0
*
105.4
39.0
*
*
108
41.5
*
216
340
*
*
104
108
412
150
200
*
*
25.9
137
385
60.6
*
*
*
65.8
*
*
24178
26393
25479
29211
28566
29958
20921
8208
10450
10839
11775
13856
14953
8734
320
488
566
519
749
638
*
636
875
860
786
806
731
*
1306
1660
*
1923
1349
842
790
811
1004
*
1161
1062
1059
934
379
450
*
524
309
*
461
29846
26845
25479
29211
28566
35173
21525
12763
13975
10839
11775
16126
15394
14465
536.2
507
566
519
925
760
*
864
930
860
786
959
790
*
1765
2140
*
1923
1497
994
1373
1131
1287
*
1161
1099
1253
1478
513
450
*
524
402
*
461
24263
*
*
*
*
*
*
8684
*
*
*
*
*
*
326
*
*
*
*
*
*
638.4
*
*
*
*
*
*
1306
*
*
*
*
*
*
813
*
*
*
*
*
*
382
*
*
*
*
*
*
28988
*
*
*
*
*
*
12454
*
*
*
*
*
*
519.8
*
*
*
*
*
*
828.6
*
*
*
*
*
*
1692
*
*
*
*
*
*
1085
*
*
*
*
*
*
488
*
*
*
*
*
*
* = Not calculable, too few observations
                                                   A21

-------
Table A-10, Continued
Analyte
PCB 180






PCB 170






Day
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
4
2
0
1
2
2
2
4
2
0
1
2
2
2
Mean
(ng/g)
857
1094
*
1033
873
988
1258
544
679
*
683
488
492
771
Median
(ng/g)
816
1094
*
1033
873
988
1258
523
679
*
683
488
492
771
Standard
Deviation
140
193
*
*
121
184
640
83
137
*
*
41.1
109
195
Minimum
(ng/g)
742
957
*
1033
787
858
805
474
582
*
683
459
415
633
Maximum
(ng/g)
1053
1230
*
1033
958
1119
1710
658
776
*
683
518
569
909
First
Quartile
(ng/g)
750
*
*
*
*
*
*
478
*
*
*
*
*
*
Third
Quartile
(ng/g)
1004
*
*
*
*
*
*
632
*
*
*
*
*
*
                                          Tri-Cities, NY -20°C
Arochlor 1242






Arochlor 1260






PCB 8






PCB 52






PCB 153






0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
4
2
1
2
2
2
2
4
2
2
2
2
2
2
4
2
2
2
2
2
0
4
2
1
2
2
2
0
4
2
2
2
2
2
2
26239
23878
31722
29078
29366
31296
22570
10653
8976
12521
14145
14236
14984
11960
418
362
670
561
648
618
*
717
868
1013
1003
968
735
*
1463
1472
2055
2220
1816
1011
1112
25467
23878
31722
29078
29366
31296
22570
10820
8976
12521
14145
14236
14984
11960
407
362
670
561
648
618
*
684
868
1013
1003
968
735
*
1391
1472
2055
2220
1816
1011
1112
2598
4031
*
497
5015
1229
3594
1957
2775
1235
88
3058
317
1221
103
160
126
49
296
19
*
105
22.3
*
36.8
97.3
19.3
*
216
418
289
5.2
214
34.9
120
24178
21027
31722
28726
25820
30427
20029
8208
7014
11648
14082
12073
14760
11097
320
250
581
526
438
605
*
636
853
1013
977
899
722
*
1306
1176
1851
2216
1665
986
1027.5
29846
26728
31722
29429
32913
32165
25112
12763
10938
13394
14207
16398
15208
12823
536
475
759
595
857
631
*
864
884
1013
1029
1037
749
*
1765
1768
2260
2223.3
1967
1035.4
1197.1
24263
*
*
*
*
*
*
8684
*
*
*
*
*
*
326
*
*
*
*
*
*
638
*
*
*
*
*
*
1306
*
*
*
*
*
*
28988
*
*
*
*
*
*
12454
*
*
*
*
*
*
519.8
*
*
*
*
*
*
829
*
*
*
*
*
*
1692
*
*
*
*
*
*
* = Not calculable, too few observations
                                                A22

-------
Table A-10, Continued
Analyte
PCB 138






PCB 187






PCB 180






PCB 170






Day
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
4
2
2
2
2
2
2
4
2
2
0
2
0
1
4
2
2
2
2
2
2
4
2
2
2
2
2
1
Mean
(ng/g)
927
856
1215
1348
1219
1210
1228
425
388
534
*
482
*
586
857
854
1060
1292
1106
974
1038
544
518
708
824
623
490
750
Median
(ng/g)
884
856
1215
1348
1219
1210
1228
403
388
534
*
482
*
586
816
854
1060
1292
1106
974
1038
523
518
708
824
623
490
750
Standard
Deviation
150
320
164
4
301
43
127
60.6
141
73.5
*
18.2
*
*
140
277
129
24.7
124
57.4
153
83.1
156
77.6
28
52.2
31.8
*
Minimum
(ng/g)
810.5
630
1099
1345
1006
1180
1138
379
288
482
*
469
*
586
742
658
970
1275
1019
933
930
474
407
653
805
586
467
750
Maximum
(ng/g)
1130.7
1083
1330
1351
1432
1241
1318
513
487
586
*
495
*
586
1053
1050
1151
1310
1194
1014
1146
658
628
763
844
660
512
750
First
Quartile
(ng/g)
813
*
*
*
*
*
*
382
*
*
*
*
*
*
750
*
*
*
*
*
*
478
*
*
*
*
*
*
Third
Quartile
(ng/g)
1085
*
*
*
*
*
*
488
*
*
*
*
*
*
1004
*
*
*
*
*
*
632
*
*
*
*
*
*
* = Not calculable, too few observations
                                              A23

-------
Table A-ll. Pesticide descriptive statistics for Housatonic River sediment by day and
            holding condition.


Analyte


Day


N

Mean
(ng/g)

Median
(ng/g)

Standard
Deviation

Minimum
(ng/g)

Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
                                     Housatonic River 4°C
4,4-DDE






4,4-DDD






2,4-DDT






4,4-DDT






0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
0
7
14
28
42
84
168
4
2
2
2
2
2
0
4
2
2
2
2
2
2
4
2
2
2
2
2
1
4
2
2
2
2
2
2
139
147
121
131
132
113
*
36.4
20.0
18.4
21.0
21.5
31.8
26.6
197
211
169
180
184
155
220
1107
1213
990
1055
1069
840
1200
140
147
121
131
132
113
*
37.0
20.0
18.4
21.0
21.5
31.8
26.6
194
211
169
180
184
155
220
1101
1213
990
1055
1069
840
1200
3.51
1.44
3.27
7.57
25.2
1.86
*
13.0
1.63
0.163
1.11
5.58
0.622
3.99
9.43
0.78
0.38
8.26
43.9
5.25
*
46.7
16.4
53.9
33
225
1.25
65.2
134.47
146.23
119.16
125.98
113.8
111.72
*
23.18
18.83
18.3
20.21
17.52
31.34
23.79
188.75
210.81
169.19
174.65
153.3
151.04
220.21
1059.9
1201.6
951.9
1032
909
838.74
1154.3
142.03
148.27
123.78
136.68
149.5
114.35
*
48.29
21.13
18.53
21.777
25.41
32.22
29.43
209.8
211.92
169.73
186.33
215.4
158.46
220.21
1168
1224.8
1028.2
1078.7
1228
840.51
1246.4
135.57
*
*
*
*
*
*
24.2
*
*
*
*
*
*
189.33
*
*
*
*
*
*
1066.1
*
*
*
*
*
*
141.97
*
*
*
*
*
*
47.91
*
*
*
*
*
*
206.65
*
*
*
*
*
*
1155.2
*
*
*
*
*
*
                                    Housatonic River -20°C
4,4-DDE






4,4-DDD






0
7
14
28
42
84
168
0
7
14
28
42
84
168
4
2
0
2
1
2
0
4
2
0
2
1
2
2
139.29
146.68
*
126.99
118.59
123.59
*
36.38
35.8
*
18.865
18.21
35.715
26.34
140.33
146.68
*
126.99
118.59
123.59
*
37.03
35.8
*
18.865
18.21
35.715
26.34
3.51
1.15
*
0.3
*
1.85
*
13
22.1
*
0.021
*
0.488
0.424
134.47
145.86
*
126.78
118.59
122.28
*
23.18
20.1
*
18.85
18.21
35.37
26.04
142.03
147.49
*
127.2
118.59
124.89
*
48.29
51.4
*
18.88
18.21
36.06
26.64
135.57
*
*
*
*
*
*
24.2
*
*
*
*
*
*
141.97
*
*
*
*
*
*
47.91
*
*
*
*
*
*
 * = Not calculable, too few observations
                                           A24

-------
 Table A-ll, Continued
Analyte
2,4-DDT






4,4-DDT






Day
0
7
14
28
42
84
168
0
7
14
28
42
84
168
N
4
2
0
2
1
2
0
4
2
0
2
1
2
1
Mean
(ng/g)
196.7
200
*
177.78
162.06
165.87
*
1107.3
1113.2
*
1047.4
963.83
933.6
1250.3
Median
(ng/g)
194.12
200
*
177.78
162.06
165.87
*
1100.7
1113.2
*
1047.4
963.83
933.6
1250.3
Standard
Deviation
9.43
9.82
*
5.62
*
6.27
*
46.7
8.2
*
37.1
*
84.1
*
Minimum
(ng/g)
188.75
193.05
*
173.8
162.06
161.43
*
1059.9
1107.4
*
1021.2
963.83
874.2
1250.3
Maximum
(ng/g)
209.8
206.94
*
181.75
162.06
170.3
*
1168
1119
*
1073.6
963.83
993.1
1250.3
First
Quartile
(ng/g)
189.33
*
*
*
*
*
*
1066.1
*
*
*
*
*
*
Third
Quartile
(ng/g)
206.65
*
*
*
*
*
*
1155.2
*
*
*
*
*
*
* = Not calculable, too few observations
                                           A25

-------
Table A-12. Pesticide descriptive statistics for SQ-1 sediment by day and holding condition.


Analyte


Day


N

Mean
(ng/g)

Median
(ng/g)

Standard
Deviation

Minimum
(ng/g)

Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
                                 SQ-1 4°C (Surrogate Corrected)
a-BHC



y-BHC



2,4-DDE



a-Chlordane



Trans
Nonachlor


4,4-DDE



2,4-DDD



4,4-DDD




2,4-DDT




MIREX




0
28
70
154
0
28
70
154
0
28
70
154
0
28
70
154
0
28
70
154
0
28
70
154
0
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
1.37
1.08
1.31
1.55
1.34
1.11
1.02
1.81
3.98
3.50
4.37
7.65
10.4
7.91
10.1
15.2
2.30
1.70
2.08
2.14
3.04
2.37
3.00
4.33
0.735
2.04
2.39
3.31
2.85
2.52
1.60
3.19
2.76
0.915
0.985
0.745
1.15
1.24
2.02
1.88
1.34
1.80
2.15
1.37
1.08
1.31
1.55
1.34
1.11
1.02
1.81
3.98
3.50
4.37
7.65
10.4
7.91
10.1
15.2
2.30
1.70
2.08
2.14
3.04
2.37
3.00
4.33
0.735
2.04
2.39
3.31
2.85
2.52
1.60
3.19
2.76
0.915
0.985
0.745
1.15
1.24
2.02
1.88
1.34
1.80
2.15
0.092
0.219
0.035
0.078
0.106
0.141
0.035
0.184
0.078
0.092
1.09
0.516
0.679
1.80
1.04
0.742
0.099
0.339
0.247
0.141
0.191
0.495
0.431
0.304
0.021
0.417
0.283
0.325
0.141
0.156
0.184
0.297
0.071
0.148
0.219
0.233
0.205
0.099
0.014
0.021
0.354
0.318
0.085
1.30
0.920
1.28
1.49
1.26
1.01
0.990
1.68
3.92
3.43
3.60
7.28
9.89
6.64
9.32
14.7
2.23
1.46
1.90
2.04
2.90
2.02
2.69
4.11
0.720
1.74
2.19
3.08
2.75
2.41
1.47
2.98
2.71
0.810
0.830
0.580
1.00
1.17
2.01
1.86
1.09
1.57
2.09
1.43
1.23
1.33
1.60
1.41
1.21
1.04
1.94
4.03
3.56
5.14
8.01
10.9
9.19
10.8
15.7
2.37
1.94
2.25
2.24
3.17
2.72
3.3
4.54
0.750
2.33
2.59
3.54
2.95
2.63
1.73
3.40
2.81
1.02
1.14
0.910
1.29
1.31
2.03
1.89
1.59
2.02
2.21
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
 * = Not calculable, too few observations
                                           A26

-------
 Table A-12, Continued


Analyte


Day


N

Mean
(ng/g)

Median
(ng/g)

Standard
Deviation

Minimum
(ng/g)

Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
                                 SQ-1 -20°C (Surrogate Corrected)
a-BHC




y-BHC




2,4-DDE




a-Chlordane




Trans
Nonachlor



4,4-DDE




2,4-DDD




4,4-DDD




2,4-DDT




0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
0
14
28
70
154
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
1
2
2
2
2
1
2
2
2
1.37
1.15
1.26
1.36
1.52
1.34
1.11
1.26
0.940
1.68
3.98
5.35
3.89
3.37
6.73
10.4
10.1
8.80
9.86
13.8
2.30
2.22
1.96
2.01
2.09
3.04
2.76
2.58
2.83
3.94
0.735
0.605
2.39
2.38
3.17
2.85
2.69
2.09
2.90
2.55
0.915
1.00
0.795
0.815
0.920
1.37
1.15
1.26
1.36
1.52
1.34
1.11
1.26
0.940
1.68
3.98
5.35
3.89
3.37
6.73
10.4
10.1
8.80
9.86
13.8
2.30
2.22
1.96
2.01
2.09
3.04
2.76
2.58
2.83
3.94
0.735
0.605
2.39
2.38
3.17
2.85
2.69
2.09
2.90
2.55
0.915
1.00
0.795
0.815
0.920
0.092
0.106
0.035
0.156
0.092
0.106
0.163
0.050
0.255
0.134
0.078
1.63
0.481
0.064
1.308
0.679
0.304
0.028
0.078
2.73
0.099
0.099
0.014
0.050
0.382
0.191
0.035
0.028
0.191
0.834
0.021
0.106
0.064
0.050
0.658
0.141
*
0.099
0.304
0.396
0.148
*
0.021
0.050
0.071
1.30
1.07
1.23
1.25
1.45
1.26
0.990
1.22
0.760
1.58
3.92
4.19
3.55
3.32
5.80
9.89
9.86
8.78
9.80
11.9
2.23
2.15
1.95
1.97
1.82
2.90
2.73
2.56
2.69
3.35
0.720
0.530
2.34
2.34
2.70
2.75
2.69
2.02
2.68
2.27
0.810
1.00
0.780
0.780
0.870
1.43
1.22
1.28
1.47
1.58
1.41
1.22
1.29
1.12
1.77
4.03
6.50
4.23
3.41
7.65
10.9
10.3
8.82
9.91
15.7
2.37
2.29
1.97
2.04
2.36
3.17
2.78
2.60
2.96
4.53
0.750
0.680
2.43
2.41
3.63
2.95
2.69
2.16
3.11
2.83
1.02
1.00
0.810
0.850
0.970
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
* = Not calculable, too few observations
                                             A27

-------
 Table A-12, Continued


Analyte


Day


N

Mean
(ng/g)

Median
(ng/g)

Standard
Deviation

Minimum
(ng/g)

Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
                                 SQ-1 -20°C (Surrogate Corrected)
MIREX




0
14
28
70
154
2
1
2
2
2
2.02
2.04
1.63
1.78
2.03
2.02
2.04
1.63
1.78
2.03
0.014
*
0.085
0.057
0.247
2.01
2.04
1.57
1.74
1.85
2.03
2.04
1.69
1.82
2.20
*
*
*
*
*
*
*
*
*
*
* = Not calculable, too few observations
                                             A28

-------
Table A-13. Pesticide descriptive statistics for Tri-Cities NY sediment by day and
holding condition
Analyte

y-Chlordane






a-Chlordane




Trans
Nonachlor






y-Chlordane





a-Chlordane




Trans
Nonachlor






Day

0
7
14
28
42
84
168
0
7
14
28
42
84
0
7
14
28
42
84

0
7
14
28
42
84
0
7
14
28
42
84
0
7
14
28
42
84
0
N

4
2
1
1
2
2
2
4
2
1
1
2
2
4
2
1
1
2
2

4
2
2
2
2
2
4
2
2
2
2
2
4
2
2
2
2
2
4
Mean
(ng/g)

5326
5253
5375
4947
6432
7866
5682
5971
5869
6065
5556
6679
8227
3678
3669
3773
3475
4227
5387

5326
3784
6397
6595
6834
7762
5971
4333
7086
7309
7250
8117
3678
2670
4395
4611
4600
5279
5326
Median Standard Minimum
(ng/g) Deviation (ng/g)
Tri-Cities
5248
5253
5375
4947
6432
7866
5682
5853
5869
6065
5556
6679
8227
3571
3669
3773
3475
4227
5387
Tri-Cities,
5248
3784
6397
6595
6834
7762
5853
4333
7086
7309
7250
8117
3571
2670
4395
4611
4600
5279
5248
, NY4°C
1191
205
*
*
606
384
210
1304
217
*
*
551
377
867
141
*
*
367
191
NY -20°C
1191
2030
1221
1086
1149
47
1304
2137
1286
1107
915
92.4
867
1385
835
804
643
45.6
1191

4154
5108
5375
4947
6003
7594
5534
4685
5716
6065
5556
6290
7960
2865
3570
3773
3475
3968
5252

4154
2348
5534
5827
6021
7729
4685
2822
6176
6526
6603
8052
2865
1690
3805
4043
4146
5246
4154
Maximum
(ng/g)

6656
5398
5375
4947
6860
8137
5831
7493
6022
6065
5556
7069
8493
4706
3769
3773
3475
4486
5522

6656
5219
7260
7363
7646
7795
7493
5845
7995
8091
7897
8183
4706
3649
4985
5180
5054
5311
6656
First
Quartile
(ng/g)

4242
*
*
*
*
*
*
4792
*
*
*
*
2915
*
*
*
*
*

4242
*
*
*
*
*
4792
*
*
*
*
*
2915
*
*
*
*
*
4242
Third
Quartile
(ng/g)

6489
*
*
*
*
*
*
7269
*
*
*
*
4549
*
*
*
*
*

6489
*
*
*
*
*
7269
*
*
*
*
4549
*
*
*
*
*
6489
* = Not calculable, too few observations
                                           A29

-------
Table A-14. Pesticide descriptive statistics for Bedford-1 sediment by day and holding
condition
Analyte Day
N
Mean Median
(ng/g) (ng/g)
Standard
Deviation
Minimum
(ng/g)
Maximum
(ng/g)
First
Quartile
(ng/g)
Third
Quartile
(ng/g)
Bedford-1 4°C (Surrogate Corrected)
2,4-DDD 0
7
14
29
43
84
168
4,4-DDD 0
7
14
29
43
84
168
4,4-DDT 0
7
14
29
43
84
168

2,4-DDD 0
7
14
29
43
84
168
4,4-DDD 0
7
14
29
43
84
168
4,4-DDT 0
7
14
29
43
84
168
4
2
2
2
2
2
2
4
2
2
2
2
2
2
4
2
2
2
2
2
2

4
2
2
2
2
2
2
4
2
2
2
2
2
2
4
2
2
2
2
2
2
109
102
116
96.2
117
113
101
352
356
384
389
332
333
284
63.3
59.7
85.5
103
98.5
86.9
49.3
Bedford-1
109
111
111
94.0
120
107
111
352
387
379
375
346
308
320
63.3
63
68.1
101
85.8
80.4
71.4
112
102
116
96.2
117
113
101
359
356
384
389
332
333
284
63.1
59.7
85.5
103
98.5
86.9
49.3
-20°C
112
111
111
94.0
120
107
111
359
387
379
375
346
308
320
63.1
63
68.1
101
85.8
80.4
71.4
109
102
116
96.2
117
113
101
352
356
384
389
332
333
284
63.3
59.7
85.5
103
98.5
86.9
49.3
9.14
3.00
20.9
1.29
32.6
3.12
0.010
16.9
9.60
1.80
4.53
4.83
13.2
0.870
3.97
3.07
24.0
8.82
9.79
3.51
1.98
4.57
2.12
14.8
0.910
23.1
2.20
0.010
8.46
6.79
1.28
3.20
3.41
9.34
0.62
1.98
2.17
17.0
6.24
6.92
2.48
1.40
95.6
100
102
95.3
94.3
111
101
327
349
383
385
329
324
284
59.0
57.5
68.5
96.8
91.6
84.4
47.9
116
104
131
97.1
140
115
101
363
363
385
392
336
343
285
68.0
61.9
103
109
105
89.4
50.7
(Surrogate Corrected)
109
111
111
94.0
120
107
111
352
387
379
375
346
308
320
63.3
63
68.1
101
85.8
80.4
71.4
9.14
1.99
2.64
3.29
25.3
2.76
6.27
16.9
7.93
2.53
11.4
26.8
13.2
13.6
3.96
2.79
3.53
3.61
2.24
3.32
16.8
4.57
1.41
1.87
2.33
17.9
1.95
4.43
8.46
5.61
1.79
8.07
19.0
9.31
9.62
1.98
1.98
2.50
2.55
1.58
2.35
11.9
95.6
110
109
91.7
102
105
107
327
381
377
367
327
298
311
59.0
61.0
65.6
98.5
84.3
78.1
59.5
116
113
113
96.3
138
109
116
363
392
381
383
365
317
330
68.0
65.0
70.6
104
87.4
82.8
83.3
 ' = Not calculable, too few observations
                                           A30

-------
Table A-15. Heavy metal descriptive statistics for Sinclair sediment by day and holding
condition


Metal

As





Cu





Pb





Zn






Metal

As





Cu





Pb







Days

0
90
183
217
284
392
0
90
183
217
284
392
0
90
183
217
284
392
0
90
183
217
284
392

Days

0
90
183
217
284
392
0
90
183
217
284
392
0
90
183
217
284
392


N

5
2
1
1
2
2
5
2
1
1
2
2
4
2
1
1
2
2
5
2
1
1
2
2

N

5
2
1
1
2
2
5
2
1
1
2
2
4
2
1
1
2
2

Mean
(M.9/9)

22.5
21.7
23.6
17.9
25.3
22.1
504
548
574
538
491
461
164
155
179
156
191
149
470
465
512
456
481
442

Mean

22.5
20.1
19.3
16.2
22.1
18.6
504
489
508
511
472
434
164
159
151
134
254
196

Median
(M.9/9)

22.1
21.7
23.6
17.9
25.3
22.1
517
548
574
538
491
461
165
155
179
156
191
149
469
465
512
456
481
442

Median

22.1
20.1
19.3
16.2
22.1
18.6
517
489
508
511
472
434
165
159
151
134
254
196

Standard
Deviation
WET
1.44
0.85
*
*
1.06
2.74
52.1
133
*
*
62.2
1.90
26.1
17.7
*
*
52.3
2.83
28.8
27.6
*
*
6.36
18.6
Standard
Deviation
DRY
1.44
3.68
*
*
1.56
0.40
52.1
2.12
*
*
25.5
27.8
26.1
11.3
*
*
6.36
50.8

Minimum
(M.g/g)

20.8
21.1
23.6
17.9
24.5
20.2
419
454
574
538
447
460
135
142
179
156
154
147
437
445
512
456
476
429

Minimum

20.8
17.5
19.3
16.2
21.0
18.3
419
487
508
511
454
414
135
151
151
134
249
160

Maximum
(M.g/g)

24.4
22.3
23.6
17.9
26.0
24.0
548
642
574
538
535
462
191
167
179
156
228
151
515
484
512
456
485
455

Maximum

24.4
22.7
19.3
16.2
23.2
18.9
548
490
508
511
490
453
191
167
151
134
258
232
First
Quartile
(M.g/g)

21.2
*
*
*
*
*
458
*
*
*
*
*
139
*
*
*
*
*
447
*
*
*
*
*
First
Quartile

21.2
*
*
*
*
*
458
*
*
*
*
*
139
*
*
*
*
*
Third
Quartile
(ng/g)

23.9
*
*
*
*
*
545
*
*
*
*
*
188
*
*
*
*
*
494
*
*
*
*
*
Third
Quartile

23.9
*
*
*
*
*
545
*
*
*
*
*
188
*
*
*
*
*
                                        A31

-------
Metal
Zn





Days
0
90
183
217
284
392
N
5
2
1
1
2
2
Mean
(ng/g)
470
452
448
414
453
405
Median
(ng/g)
469
452
448
414
453
405
Standard
Deviation
28.8
41.7
*
*
17.7
2.80
Minimum
(ng/g)
437
422
448
414
440
403
Maximum
(ng/g)
515
481
448
414
465
407
First
Quartile
(ng/g)
447
*
*
*
*
*
Third
Quartile
(ng/g)
494
*
*
*
*
*
' = Not calculable
                                                 A32

-------
Table A-16. Heavy metal descriptive statistics for Wilmington sediment by day and
holding condition


Metal

As




Cu




Pb




Zn





Metal

As




Cu




Pb




Zn





Days

0
91
182
279
391
0
91
182
279
391
0
91
182
279
391
0
91
182
279
391

Days

0
91
182
279
391
0
91
182
279
391
0
91
182
279
391
0
91
182
279


N

5
2
2
2
2
5
2
2
2
2
5
2
2
2
2
4
2
2
2
2

N

5
2
2
2
2
5
2
2
2
2
5
2
2
2
2
4
2
2
2

Mean
(M.9/9)

63.4
66.6
62.7
60.6
64.3
122
131
124
136
117
5676
6595
5615
5775
4572
61.5
72.6
62.1
65.3
53.6

Mean

63.4
62.7
66.4
55.6
60.0
122
124
133
138
125
5676
6615
6160
5710
4839
61.5
56.4
66.5
68.2

Median
(M.9/9)

63.4
66.6
62.7
60.6
64.3
121
131
124
136
117
5700
6595
5615
5775
4572
61.3
72.6
62.1
65.3
53.6

Median

63.4
62.7
66.4
55.6
60.0
121
124
133
138
125
5700
6615
6160
5710
4839
61.3
56.4
66.5
68.2

Standard
Deviation
WET
3.05
7.35
0.508
2.33
6.29
7.26
14.1
0.980
3.54
6.32
471
1195
445
1124
124
4.82
6.58
1.32
13.2
3.83
Standard
Deviation
DRY
3.05
4.74
7.36
1.91
0.268
7.26
10.6
14.7
12.0
2.33
471
926
467
156
49.3
4.82
5.94
2.12
3.89

Minimum
(M.g/g)

60.5
61.4
62.3
58.9
59.9
111
121
123
133
113
5140
5750
5300
4980
4484
57.1
67.9
61.1
55.9
50.9

Minimum

60.5
59.3
61.2
54.2
59.9
111
116
123
129
124
5140
5960
5830
5600
4804
57.1
52.2
65.0
65.4

Maximum
(M.g/g)

67.7
71.8
63.0
62.2
68.8
129
141
125
138
122
6250
7440
5930
6570
4660
66.2
77.2
63.0
74.6
56.3

Maximum

67.7
66.0
71.6
56.9
60.2
129
131
144
146
127
6250
7270
6490
5820
4874
66.2
60.6
68.0
70.9
First
Quartile
(M.g/g)

60.6
*
*
*
*
116
*
*
*
*
5210
*
*
*
*
57.2
*
*
*
*
First
Quartile

60.6
*
*
*
*
116
*
*
*
*
5210
*
*
*
*
57.2
*
*
*
Third
Quartile
(ng/g)

66.4
*
*
*
*
129
*
*
*
*
6130
*
*
*
*
65.9
*
*
*
*
Third
Quartile

66.4
*
*
*
*
129
*
*
*
*
6130
*
*
*
*
65.9
*
*
*

-------
                                                                       First     Third
                    Mean  Median  Standard  Minimum  Maximum  Quartile   Quartile
 Metal   Days   N   (|ag/g)   (|ag/g)   Deviation    (|ag/g)      (|ag/g)     (|ag/g)     (|ag/g)
	391   2   68.0     68.0       2.04       66.6       69.4	*	*
= Not calculable, too few observations
                                          A34

-------
          Appendix B

Plots of Concentration vs. Time for
   All Sediment/Soil Extraction
      Holding Time Studies
                Bl

-------
PAHs
   B2

-------
Eagle Harbor:





1> 1000
c

g
° 400

200







1
c '
T 80 -
g
•£ 60-
c


20-

C



|400|
f 300

I 20°-
u
100-


c


a




• - -«- 	
*i " '
» »
• •
«

0 50 100 150 2
Days to Extraction



•

• *
*
*---•--; 	 r 	
*
* •
• •

*


50 100 150 2
Days to Extraction

•
••
•
• .
-* 	 •. 	
• .
•

* t

50 100 150 20
Days to Extraction





• naphthalene 4oC
• naphthalene -20oC
- - - - Lower Bound
a -20C Extreme Outliers




00






* Acenaphthalene 4oC
• Acenaphthalene -20oC
- - - - Upper Bound





)0



* dibenzothiophene 4oC
• dibenzothiophene -20oC
... -Upper Bound
... - Lower Bound




0

900


9i 70°
1 snn J
1 500
1 400

o 300
200





1400 -


-?
£, 100° ,
o '
1





C

6000
_ 5000
|
0
•£ 3000
c
0 2000





n





• •
• m
...*_, 	

*


50 100 150 200
Days to Extraction


•

_l
* • •


•
*


f

50 100 150 20
Days to Extraction

•
•
-f *
m * •
' 	 • 	 • 	
•• •


•

	 * 	

0 50 100 150
Daysto Extraction



• Imethyl naphthalene 4oC

• Imethyl naphthalene -
... Upper Bound


n -20C Extreme Outliers










• Acenaphthene 4oC
• Acenaphthene -20oC
- - - - Upper Bound





0



• phenanthrene 4oC
• phenanthrene -20oC
- - - - Upper Bound
- - - - Lower Bound




200




_
"5>
c '
0
" 1 '
g 100
c
u
50 -


0


1800-
1600-

n 1400 -
"5>
£ 1200-

1 800
° 600



200-


4500
4000
3 3500
D)
— 3000
c
= 2500
I
| 2000
O










ll . 1
•
• . 4. 	
» «
1 »


50 100 150 200
Daysto Extraction


•
•
• •
»
, * 1 " •

* • .




	 1-
) 50 100 150
Daysto Extraction

D




,1
t 1

»

0 50 100 150 20
Days to Extraction



* 2 methyl naphthalene 4oC

• 2 methyl naphthalene -
- - - - Upper Bound


n -20C Extreme Outliers










	 * Fluorene 4oC
• Fluorene -20oC
- - - - Upper Bound





200



• anthracene 4oC


a -20C Extreme Outliers




0
                                                              B3

-------


~ui |
_£_ 1
c
f 300-
O
O
100 -



•1
. .
• • .
. • »
$


0 50 100 150 200
Days to Extraction

* 1 Methyl phenanthrene
4oC
• 1 Methyl phenanthrene -
20oC
- - - - Upper Bound
- - - - Lower Bound


2000
1800
1600
n 1400
3)
— 1200
c
| 1000
1 800
o 600
o
400
200
0



•
•• • . • J
--••-.-- • • i • '
I








• benzo[a] anthracene
4oC
20oC
- - - - Upper Bound




D 50 100 150 200
Days to Extraction

Concentration (ng/g)
01 0 01 0 01 0 01
o o o o o o o
oooooooo




* . .
• i : '
•



* benzo [k] fluoranthene
4oC
• benzo [k] fluoranthene -
20oC
- - - - Upper Bound
- - - - Lower Bound

D 50 100 150 200
Days to Extraction
9000 -i



c '
= 5000 -
I 4000 -
|
o
o

1000-

. :
».. •
i * fluoranthene 4oC
- - - - Upper Round
- - - - Lower Bound
J


0 50 100 150 200
Days to Extraction


2500 -
_ '
|, 2000 !
c
o
"c
0>
o
o
500 -

•
*
-»*— i 	 | 	 1
" • • * * chrysene 4oC

* - - - - upper Bound
- - - - Lower Bound


0 50 100 150 200
Days to Extraction

6000 -
« 5000 i
O)
c
c 4000 -

c



. •
•• ! : . i
•




• pyrene4oC
- - - - Upper Bound
.... Lower Bound

0 50 100 150 200
Days to Extraction

3500 -i 	


n
c
0

-------


300
~UI
c
o
1
0>
c
50



•
• ' I
m *
•
*



• dibenzo [a,h] anthracene
4oC
• dibenzo [a,h] anthracene
-20oC
- - - - Upper Bound
• • • • Lower Bound

0 50 100 150 200
Days to Extraction

700
i
3
c 500
c
o
1
c
o
0 200



*
• .
; • »
• : :
•




» benzo[g,h,i] perylene
4oC
• benzo[g,h,i] perylene -
20oC
- - - - Upper Bound
- - - - Lower Bound

0 50 100 150 200
Days to Extraction
Sequim Bay:


100 -
"3
i> 80 -
c
S 60

1 4°-
3 20-



140 -



1 10°l
1 8°-
1 60-
I 40-
O




• *
• •
-r 	 y 	 : 	 • 	
» m *
• .
•


) 20 40 60 80 1
Days to Extraction




* u
~Ti '• •
i * 	 •- 	 ' 	
: •


) 20 40 60 80
Days to Extraction








0









1


















DO



» naphthalene 4C

--- Upper Bound









• Fluorene -20C
	 Upper Bound



16 -i
14 -
-3 12-
£ 10-
C I
S 8
1 6-
i 4
U







• — • R
0) D
"a
-£ 5
I4
o 2
u
1



•
-^ . I
1 •
•


20 40 60 80 1
Days to Extraction





•--;-; 	 	 	 * 	
f .


D 20 40 60 80 10
Days to Extraction








00









0



* Acenaphthalene 4C

	 Upper Bound









» dibenzothiophene 4C
• dibenzothiophene -20C
	 Upper Bound





120
? 100 -
_c_

1 60-
1 40
u

c


250


•a
01
I 15°
S
•E 100
" 50




• •
: • « • :
S *



20 40 60 80 10
Days to Extraction





•
"•n 	 	 	 •"" 	 ^r-
*


0 20 40 60 80 1
Days to Extraction



• Acenaphthene4C

	 Upper Bound


0






• phenanthrene 4C
• phenanthrene -20C
	 Upper Bound


00
                                                           B5

-------
  120 -

  100 ,
   40 -

   20 -
                            40         60
                          Days to Extraction
                                                                                               200
                                                                                            5
                                                                                            i1
                                                        40         60
                                                      Days to Extraction
                                                                                                                            160 ]
                                                                                                                         | 1«
                                                                                                                         -120
                                                                                                                         I 100
                                                                                                                                                                                              80
                                                                                                                                                                •   pyrene 4C
                                                                                                                                                                •   pyrene-20C
                                                                                                                                                               •	Upper Bound
                                                                                                                                                               	Lower Bound
                                                                                                                       40         60
                                                                                                                      Days to Extraction
  160 -
.  140 -
1  120'
  100 '
 benzo[a] anthracene 4C
 benzo[a] anthracene -20C
- Upper Bound
- Lower Bound
               20        40        60
                      Days to Extraction
                                                                                                200
                                                                                                180
120 ^
100
 80
                                                         40         60
                                                       Days to Extraction
                                                                                                                                                                                                .,..*..
                                                                                                                                                                                                 I  •
 »   benzo [b] fluoranthene 4C
 •   benzo [b] fluoranthene -20C
	Upper Bound
	Lower Bound
                                                                                                                                                                                                             Days to Extraction
  140 n

  120-

'  100-
  40-
  20-
               20        40         60        80
                       Days to Extraction
                                        20        40       60
                                                Days to Extraction
                                                                                                   20       40       60
                                                                                                          Days to Extraction
              20       40       60
                     Days to Extraction
                                                                                                                                    B6

-------
Bedford Harbor:
Concentration (ng/g)
0 § § § § I §

	 S

.
*
•







0 50 100 150 200
Days to Extraction

* naphthalene 4
- - - -Upper Bound
.... Lovver Bound
OC


140
120
1 60
ID
1 40
(J
20
0

•


• *
,*





* Fluorene 4C
• Fluorene -2
- . . -Lower Bou


D 50 100 150 200
Days to Extraction
OC
id
id


Concentration (ng/g)

• I

>.
_» •




* Acenaphthalene4C
• Acenaphthalene -20C
n -20C Ouliers
- - - -Upper Bound
- - - -Lower Bound

0 50 100 150 200
Days to Extraction

140 n


i 80i

c 40-
u


"
1* 1
•



0 50 100 150 200
Days to Extraction

Concentration (ng/gL)
ooooooooooo

n
*


-* 	

*


» dibenzothiophene 4C
a -20C Ouliers
- - - -Upper Bound


0 50 100 150 200
Days to Extraction
30
25
C I20
c
i 15
1 ..
5 5

* Acenaphthene 4C
• Acenaphthene -20C
o 4C Ouliers
n -20C Ouliers
... -Upper Bound
... -Lower Bound



00-
00 " *





• phenanthrene -20C
- - - -Upper Bound

0 50 100 150 200
Days to Extraction



1 500-

5 i
* 300 '
S '
(J


• t

"•
*





• anthracene -20C
a -20C Ouliers
- - -Upper Bound

0 50 100 150 200
Days to Extraction



1 0000 - -
3

| 6000 I -
o 4000 - -





i




• fluoranthene4C
• fluoranthene-20C
- - - -Upper Bound
... -Lower Bound


0 50 100 150 200
Days to Extraction
Concentration (ng/g)
o o o o o o o


.
» » pyrene 4C
* • pyrene -20C
! * - - - -Upper Bound
... -Lower Bound


0 50 100 150 200
Days to Extraction
                                                             B7

-------

7000 -
3 6000 -
— 5000 -
g '
^4000,
| 3000 -
o 2000 -
o

-* 	 • 	
I
m
•
^ 	










0 50 100 150 200
Days to Extraction
10000
9000
_ 8000
| 7000
•J 6000
| 5000
•£ 4000
c 3000
5 2000
1000
0

	 o 	




'••
:*




* benzo[a] anthracene 4C
• benzo[a] anthracene -20C
- - - -Upper Bound


» benzo [k] fluoranthene 4C
• benzo [k] fluoranthene -20C
o 4C Ouliers
n -20C Ouliers
- - - -Upper Bound
. - - -Lower Bound

0 50 100 150 200
Days to Extraction



U 1400
— 1200







9
•
•.
*






0 50 100 150 200
Days to Extraction
• dibenzo [a,h] anthracene -
20C
9 4C Ouliers
n -20C Ouliers
- - - -Upper Bound
- - - -Lower Bound


8000 -
— 7000 -
§ 5000 i


c
0


(
•






•





0 50 100 150
Days to Extraction
12000
10000
|> 8000
c
•| 6000
I 4000
c
U 2000
0

•





, •
•
, *


0 50 100 150
Days to Extraction



|> 6000 -
§ 5000 :
•a
2 3000 '
c


a
O

•
9




2

0


• chrysene -20C
- - - -UpperBound


» benzo [a] pyrene 4C
• benzo [a] pyrene -20C
o 4C Ouliers
n -20C Ouliers
- - - -Upper Bound
- - - -Lower Bound



200


• benzo[g,h,i] perylene 4C
• benzo[g,h,i] perylene -20C
0 4C Ouliers
a -20C Ouliers
- - - -Upper Bound
. - - -Lower Bound




0 50 100 150 200
Days to Extraction


B)
i i
1 600° \
c
o
° 2000 -



•
1



• benzo [b] fluoranthene 4C
- - - -Upper Bound

0 50 100 150 200
Days to Extraction
14000
12000
•fj 10000
c
= 8000
£ 6000
i
= 4000
2000
0

D
§


:•
• »

3 50 100 150 2
Days to Extraction

• indeno [1 ,2,3-c,d] pyrene -
20C
o 4C Ouliers
n -20C Ouliers
- - - -Upper Bound
... -Lower Bound
30


B8

-------
PCBs
   B9

-------
Housatonic
8000





a

g


c
o










!

^X^.^"- 	
• ""^^^^^
• ^""""•"•^^"'•'-x.,,^^
•^\^xx^^'<

^^

3 50 100 150 2
Days to Extraction















DO





• Arochlor1254-20C

	 Upper Bound

	 Lower Bound

	 Linear (Arochlor 1254 4C)

	 Linear (Arochlor 1254 -
20C)


















29000





u>

o


c

17000





-1 	 * 	
•

^^•»^
^^^5^

" ^^^^^^ ft





50 100 150 2
Days to Extraction















DO





• Arochlor 1260 -20C

	 Upper Bound

	 Lower Bound

	 Linear (Arochlor 1260 4C)

	 Linear (Arochlor 1260 -
20C)


Sequim Bay:



5 14° 1
i? 120 -

^ 80 -
c
K fin
o


e

'::i 	 i 	 •
*s :

•





• Arochlor 1254 4C
• Arochlor 1254 -20C
o 4C Extreme Outliers
a -20C Extreme
Outliers
	 Upper Bound
	 Lower Bound
0 50 100 150 200
Days to Extraction
                                                             BIO

-------
Tri-Cities, NY:







g
I

g








1
C 1
- 800
1 '
£ 600 '
0 400









o) 600 -
c


~ 400 |

0



0


o Q


---• 	 * 	


IB .


* :


0 50 100 150 200
Days to Extraction


o

i.'*
t





50 100 150
Days to Extraction


„

8

:* J


m
*



50 100 150 200
Days to Extraction







n 4C Outlier
o -20C Outlier
	 Upper Bound
	 Lower Bound








• PCB 52 4C
* PCB 52 -20C
- ... Upper Bound
.... Lower Bound



00





• PCB 187-20C
a 4C Outlier


- - - - Upper Bound
.... Lower Bound





















































o
I
r 10500

c

6500





2000-
3 '
c
o i
g 1000 -
c
o



0

1800 -,
1600


c
.2

c
c 600
0
400






ft
	 I 	 	
". * '

m *
*• *



*

0 50 100 150
Days to Extraction


,

t^i
^~"^~^~--^!~~~~^
• ^^"-^
.



50 100 150 2
Days to Extraction


"

. *
. t 	 .. 	 .«
• • • *
•• .
" m

*




50 100 150
Days to Extraction














2











DO






















* Arochlor 1260 -20C
... -Upper Bound
- ... Lower Bound




0




• PCB 1534C
--- -Upper Bound
.... Lower Bound
	 Linear (PCB 153 -20C)









• PCB 180 4C
* PCB 180-20C
n 4C Outlier


- - - - Lower Bound




200

















































g i
S i

Q 300 '


100




1200
-?
c 1000
c

c
o
0 400







"3 700
Ul
— 600
g
£


g 300






«

* • •
,


.


*


50 100 150
Days to Extraction


•
•-'-' 	 r 	 -*
* " *






) 50 100 150 2
Days to Extraction




•• *
* * •
• "
• •






50 100 150 2
Days to Extraction














2C











0














0







* PCB 8 -20C
- - - - Upper Bound
.... Lower Bound




0




• PCB1384C
* PCB138-20C
- - - - Upper Bound










* PCB170-20C
D 4C Outlier


- - - - Upper Bound
.... Lower Bound




                                                                     Bll

-------
Pesticides
     B12

-------
Housatonic:


a

C
O
O

0

ft
o


^"^^^«'
* *=5=::::::::^^
; ^^^^^^
20 40 60 80 100 120 140 160 1
Days to Extraction

* 4,4-DDE 4C
• 4,4-DDE -20C
o 4C Outlier
a -20C Outlier
	 Upper Bound
	 Lower Bound
	 Linear (4,4-DDE 4C)
	 Linear (4,4-DDE -20C)
30

Concentration (ng/g)
— i-KJCOJ^CriCD^ICaCO
OOOOOOOOOO




m
II

'' t * *
• ' «


* 4.4-DDD4C
• 4,4'-DDD-20C
	 Upper Bound
	 Lower Bound

0 50 100 150 200
Days to Extraction




c
1 1
o

0
1


i
^\^

• ^
:^"^\

• 2,4-DDT4C
• 2,4-DDT-20C
o 4C Outlier
D -20C Outlier
	 Lower Bound

20 40 60 80 100 120 140 160 180
Days to Extraction

140
130
I 120
I no
"c
o
|100
90
80


V
• *
..
o n|
* 1
o 	 i, 	
*
0 *


• 4,4'-DDT4C
• 4,4'-DDT-20C

	 Lower Bound

0 50 100 150 200
Days to Extraction
                                       B13

-------
Sequim Bay:

'


s L4"

o 1 0 -
« n°
- 0.8-

C
0 04 -

0.2






=,7.0-
0) en
S *n
1? in,

§ 20







2.5 -
_
•?
£ 2.0 -


•£
S 1.0-
c
o
0
0.5 -





3.5 -

= ,,
c 2.5-
o
•g 2.0 -
•H 1S

3 1-°;


c



1.2 -
? i n J
_c_
g 0.8 *
i

O






, • *
'.....» 	 1 	


•





D 50 100 150
Days to Extraction



a
0
D

..a.. a 	
• t



50 100 150
Days to Extraction




:.: 	 • 	 ;.
— * t







D 50 100 150 2
Days to Extraction




0 °
* 1
o




50 100 150
Days to Extraction


o o

*
•-*-• 	 • 	





D 50 100 150
Days to Extraction













2C












7














n












2












2













0












in




^



<


















in












DO


* a-BHC 4C




O 4C Extreme
Outliers

Outliers
	 Upper Bound






* 2,4-DDE4C
• 24-DDE-20C

o 4C Extreme

Outliers
	 Upper Bound






TRANS NONA 4C

200


Outliers
-200 Extreme
Outliers






* 2,4-DDD 40



Outliers
Q -200 Extreme
Outliers







• 2,4-DDT4C
• 2,4-DDT-20C
O 40 Extreme
Outliers
o -200 Extreme
Outliers
pper oun

	 Lower Bound






































































'


-?

g |

i
0)
i


C





o, 11."
c 120

? 80
S CO
1








— 4.0 -
0)
c 6^ .

~ 1C
r 9n -
i 2-°
c 1.5 -
o
0 1 0 -


c




B)
- 25-
c z'°
o
1 15-

o '•"


C




2.0 1
S1
i1
0
1

° 0 5 -


c





§

'.....1 	
. • i

•


50 100 150
Days to Extraction



9
O

;:i :
* t *
•



0 50 100 150 2C
Days to Extraction





	 » 	 ••

1 t «





50 100 150
Days to Extraction


o
	 J 	
.. *

* =
•




50 100 150
Days to Extraction


t>
*
.
• »

•




50 100 150
Days to Extraction













?












n














•>n












?n












2













10



























n












n












00


• g-BHC 4C




O 4C Extreme
Outliers
a 20C Extreme
Outliers
	 Upper Bound






» a-CHLORDANE
40
• a-CHLORDANE -
200
0 40 Extreme

Outliers
---- Upper Bound






* 4,4'-DDE4C




Outliers
n -200 Extreme
Outliers






* 4,4'-DDD4C


o 40 Extreme
Outliers
n -200 Extreme
Outliers







» MIREX4C
• MIREX-20C
O 4C Extrem e
Outliers
a -20C Extreme
Outliers
pper

	 Lower Bound

                                    B14

-------
Tri-Cities, NY:

9000















•&
2 5000

o










o


0



. . • •

•••' :


*

0 50 100 150 2C
Days to Extraction



•
• * ft

,• * :
• .


*

0 50 100 150 20
Days to Extraction





,•;'

*


50 100 150 1
Days to Extraction




• 9-CHLORDANE-20C
- - - - Upper Bound
.... Lower Bound



0





• a-CHLORDANE4C
... -Upper Bound
.... Lower Bound



0





• TRANS NONA 4C
• TRANS NONA -20C
- - - - Upper Bound
.... Lower Bound



00
                                          B15

-------
Bedford Harbor




0 130
=" 120

o 110
C 100
| 90

o






U)
Ul

c
o
S 60
2
| 40
c
o










?. • • '
r«



50 100 150 2
Days to Extraction


. So
1 I

I1



50 100 150 20
Days to Extraction













0










0





• 2,4-DDD4C


o 4C Outliers
	 Upper Bound
	 Lower Bound







* 4,4'-DDT 4C

	 Upper Bound
	 Lovver Bound
a -20C Outliers
































Ul
~" -^n '

1 ,nJ

C


C















•A 1
•t-* 	
l**"^"

*^*^=55Hk^

^%



50 100 150 2C
Days to Extraction























0














'

• 4,4-DDD-20C





	 Linear (4,4'-DDD

20C)











                                     B16

-------
                          Appendix C

               Chromate [Cr(VI)] Soil Extraction
Chromate [Cr(VI)] holding time extraction data for soils 123, 125A, 125B,
125C, 126D, and 138 (Bedford soil)

The laboratory control sample (LCS), soluble (K2Cr2O7) and insoluble
(PbCrO4) spikes, and the extract (K2Cr2O7) spike are listed in red for each
extraction along with the permissible QA/QC range.
                                ci

-------
C2

-------
Cr Soil Extraction
T=0 day
5/8/2003
12763-123
Stratford Con
Chrome VI dige:
Sample/STD
Blank
338
452
742
1300
1963
3311
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 thro
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
n.
ition assay
A540 ppb calc.
0.0007
0.2615
0.3530
0.5704
0.9834
1 .4575
2.3362
0.000699
0.049167
0.9989
0.6972
0.5503
0.7736
0.6980
0.7454
1 .0092
0.7451
0.4686
303.7
434.6
745.5
1336.2
2014.4
3271.2
ppb calc.
926.9
716.8
1036.2
928.0
995.8
1373.1
995.4
599.9
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
32
16
16
ppb in sol
7415.1
5734.2
8289.3
7424.3
7966.6
43940.6
15926.4
9598.7

S*
y = O.OOOJx + 0.0492 ^^^
R2 = 0.9989 ^^^


^
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
7365.9 985.12 2.5503 7.4151 333.3575 330.0 5.6
2.5069 5.7342 321.8176
2.5320 8.2893 327.2034
2.5453 7.4243 336.0315
2.5158 7.9666 331.7133
2.5875 43.9406 2561.7972
% recovery Range 2.5835 15.9264 923.9837
96.6 85-115% K2Cr2O7 Cr added
added (mg) |jg/g dry
5.0043 2159.345
ugh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9099
0.0055
Tare
1231
-62
Tin + Soil
0.9848 2.7566
0.9873 2.8639
0.9804 3.0794
105.0
wet
1.7718
1 .8766
2.0990
80-120%
Tin + Soil
2.5717
2.6655
2.8633
PbCrO4 Cr added
Added (mg) |jg/g dry
9.4 653.6
dry %moisture mean % Solid
1.5869 10.436
1.6782 10.572 10.434 89.566
1.8829 10.295
                                                                                                                                                Spike Recovery %
                                                                                                                                                Solution     Range
                                                                                                                                                  103     75-125%
                                                                                                                                                Spike Recovery %
                                                                                                                                                Solid        Range
                                                                                                                                                   91     75-125%
                                                                              C3

-------
Cr Soil Extraction
T=14day
12763-123
5/22/2003
Stratford Conn.
Chrome VI digestion assay

Sample/STD A540 ppb calc. Sample #

Blank
310
513
778
1159
2015
2991
0.0000
0.2469
0.3908
0.5660
0.8698
1 .5037
2.0974

296.0 9
501.5 10
751.8 11
1185.7 12
2091.2 13
2939.2 14

slope 0.0007
intercept 0.039695
RSQ 0.998055

Sample: ppb calc. dil. Factor ppb in sol
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20' C #6
-20° C #7 sol
-20° C #8 insol
Sample 2+spk
Sample 6+spk
0.6846
0.5640
0.7978
1 .0972
0.6128
0.5891
0.8265
0.8349
0.8657
0.8758
921.2
748.9
1082.9
1510.5
818.6
784.8
1123.9
1135.9
1179.8
1194.3
8.0
8.0
16.0
16.0
8.0
8.0
16.0
16.0
16.0
16.0
7369.4
5991.3
17325.8
24168.3
6548.9
6278.1
17981.7
18173.7
18877.6
19108.4















2 5

2 -

1.5-


1 -

0.5 -


Q



y = 0.0007X + 0.0397
R2 = 0.9981 S*





./
S
;r

-------
Cr Soil Extraction
|T=28day     \
 12763-123
 Stratford Conn.

 Chrome VI digestion assay
Sample/STD    A540
                         6/6/2003
Blank
           306
           487
           734
          1330
          2056
          3150
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4" C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20'C #7 sol
-20°C #8 insol
Sample 2+spk
Sample 6+spk
                 0.0000
                 0.2436
                 0.3693
                 0.5485
                 0.7460
                 1.3193
                 2.1591
                 0.000659
                 0.011593
                 0.987509
                 0.7123
                 0.6151
                 0.8899
                 0.9129
                 0.6185
                 0.5488
                 0.7617
                 1.0616
                 0.8840
                 0.8499
                            ppb calc.   Sample #
   351.9
   542.6
   814.4
   1114.0
   1983.6
   3257.5
     9
    10
    11
    12
    13
    14
Samples # 1 through 8 had to
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
 ppb calc.
  1062.9
   915.4
  1332.3
  1367.2
   920.6
   814.9
  1137.8
  1592.7
  1323.3
  1271.6
be re-filtered

   1354
    -6
                                       dil. Factor
8.0
8.0
16.0
16.0
8.0
8.0
16.0
16.0
16.0
16.0
                                                            2.5
                                                             1.5 -
 0.5-
                                                                        y = 0.0007x + 0.0116
                                                                            R2 = 0.9875
                                                                     500    1000    1500    2000    2500
                                                                                                        3000
                                                                                                               3500
ave 1 &2
 7913.4
STD DEV
  834.05
                                                                                Sample Cone.
ave 5&6
 6941.9
STD DEV
  598.08
                                     after bringing
                                      % Recovery
                                         103.5
ppb in sol
 8503.1
 7323.6
 21316.6
 21874.8
 7364.9
 6519.0
 18205.2
 25483.8
 21173.4
 20345.8
 pH to the 7 range (because of precipitation).
 Range
80-120%
i Recovery
 104.9
 104.7
  Range
 85-115%
 85-115%
wet mass
 2.5952
 2.5160
 2.5481
 2.5790
 2.5844
 2.4949
 2.5042
 2.5161
 2.5160
 2.4949
ppm Calc.
 8.5031
 7.3236
 21.3166
 21.8748
 7.3649
 6.5190
 18.2052
 25.4838
 21.1734
 20.3458
     dry
386.4845
371.4873
1049.5987
1157.9653
372.5565
360.0934
1092.8049
1213.5254
765.9450
744.2267
                                                            0.9478
                                                            0.9058
                                                            0.9249
                               1.354
                              -0.006

                            %moisture
                              11.2131
                              9.5918
                              9.5983
                                                          dry
                                           %moisture
                                  0.9589     9.5548
                                  0.9478     10.2972
                                  0.9658     10.3915
                        mean

                       10.134


                        mean

                       10.081
                         % Solid

                         89.866


                         % Solid

                         89.919
ave 1 &2
 379.0
ave 5&6
 366.3
STD DEV
    10.6
STD DEV
    8.8
                                                         4°C
                                                        -20° C
                                                                                          4-C
                                                                                          -20-C
                                                      K2Cr2O7
                                                      added (mg)
                                                          1.5
                                                          1.5
                                                                             PbCrO4
                                                                           Added (mg)
                                                                               12.6
                                                                               12.1
                                                       Cr added  Spike Recovery %
                                                        |jg/g dry   Solution    Range
                                                          645        104    75-125%
                                                          657        111     75-125%
                                                       Cr added  Spike Recovery %
                                                        |jg/g dry   Solid       Range
                                                         874.7       89     75-125%
                                                         860.5       98     75-125%
                                                                                C5

-------
 Cr Soil Extraction
|T=55day  ~~|
 12763-123
 Stratford Conn.
         [7/2/2003     |
 Chrome VI digestion assay
 Sample/STD    A540
            ppb calc.   Sample #
 Blank
            231
            351
            836
            991
           1847
           2758
 0.0000
 0.1856
 0.2726
 0.3447
 0.7512
 1.3740
 1.9558
   303.3
   423.1
   522.5
   1082.5
   1940.4
   2741.9
 slope
 intercept
 RSQ

 Sample:
 4°C#1
 4"C#2
 4° C #3 sol
 4°C#4insol
 -20° C #5
 -20° C #6
 -20°C #7 sol
 -20'C #8 insol
 Sample 2+spk
 Sample 6+spk
 0.000726
-0.034547
  0.97371
 0.8435
 0.6739
 0.8176
 1.1164
 0.5952
 0.5454
 0.6976
 1.1677
 0.9285
  0.872
 Samples # 1 through 8 had to
 LCS#15
 Blank #16

 4oC
 Moisture A
 Moisture B
 Moisture C

 -20oC
 Moisture A
 Moisture B
 Moisture C
 ppb calc.
  1209.6
   976.0
  1173.9
  1585.6
   867.5
   798.9
  1008.6
  1656.2
  1326.7
  1248.9
be re-filtered

   1295
    55
                       dil. Factor
8.0
8.0
16.0
16.0
8.0
8.0
16.0
16.0
16.0
16.0
     9
    10
    11
    12
    13
    14
                                                             1.5-
   0.5 -
                                                                          y = 0.0007X - 0.0345
                                                                             R2 = 0.9737
                                                                       500      1000     1500
                                                                                               2000
                                                                                                       2500
                                                                                                               3000
                                                                Sample Cone.
  ave 1 &2
  8742.3
STD DEV
 1321.69
  ave 5&6
  6666.0
STD DEV
  388.09
                     after bringing
                      % Recover}
                         108.7
ppb in sol
 9676.9
 7807.7
 18782.9
 25369.0
 6940.4
 6391.6
 16137.9
 26499.8
 21227.4
 19982.0
 pH to the 7 range (because of precipitation).
 Range
80-120%
% Recovery
   101.7
   103.0
  Range
 85-115%
 85-115%
wet mass
 2.5530
 2.5039
 2.5140
 2.4947
 2.5083
 2.5059
 2.5190
 2.4971
 2.5039
 2.5059
                               1.295
                               0.055

                            %moisture
                              11.8710
                              12.0112
                              10.8513

                            %moisture
                              11.3553
                              11.2860
                              10.0381
                                                                   mean

                                                                   11.578


                                                                   mean

                                                                   10.893
ppm Calc.
 9.6769
 7.8077
 18.7829
 25.3690
 6.9404
 6.3916
 16.1379
 26.4998
 21.2274
 19.9820
                                                                    % Solid

                                                                    88.422


                                                                    % Solid

                                                                    89.107
 M9/9 dry
388.1729
346.7853
1014.1085
1331.4640
372.2948
376.8242
1083.2520
1646.9384
1035.7885
1019.7824
ave 1 &2
 367.5
ave 5&6
 374.6
STD DEV
    29.3
STD DEV
    3.2
                                                          4°C
                                                          -20-C
                                                          4'C
                                                          -20° C
                                                      K2Cr2O7
                                                      added (mg)
                                                          1.5
                                                          1.5
                                                        PbCrO4
                                                      Added (mg)
                                                          13.7
                                                          18.2
                                                       Cr added   Spike Recovery %
                                                       |jg/g dry   Solution   Range
                                                         670        97    75-125%
                                                         660        107   75-125%
                                                                                        Cr added   Spike Recovery %
                                                                                        |jg/g dry   Solid      Range
                                                                                         999.2       96    75-125%
                                                                                         1316.0       97    75-125%
                                                                                C6

-------
 Cr Soil Extraction
|T=112day~|
 12763-123
 Stratford Conn.
        [8/28/2003    |
 Chrome VI digestion assay
 Sample/STD    A540
           ppb calc.    Sample #
 Blank
            298
            369
            719
           1172
           1749
           2991
 0.0000
 0.2280
 0.2777
 0.5182
 0.8312
 1.2064
 1.9378
   266.8
   344.7
   722.1
   1213.1
   1801.8
   2949.3
 slope
 intercept
 RSQ

 Sample:
 4°C#1
 4"C#2
 4° C #3 sol
 4°C#4insol
 -20° C #5
 -20° C #6
 -20°C #7 sol
 -20'C #8 insol
 Sample 2+spk
 Sample 6+spk
0.000637
0.057967
0.998514
 0.4467
 0.5159
 1.0061
 0.4737
 0.6159
 0.5786
 0.6957
 0.4245
 0.7912
 0.8212
 Samples # 1 through 8 had to
 LCS#15
 Blank #16

 4oC
 Moisture A
 Moisture B
 Moisture C

 -20oC
 Moisture A
 Moisture B
 Moisture C
 ppb calc.
   609.9
   718.5
   1487.5
   652.2
   875.3
   816.8
   1000.5
   575.1
   1150.4
   1197.4
be re-filtered

   1156
    -81
                      dil. Factor
8.0
8.0
16.0
32.0
8.0
8.0
16.0
32.0
16.0
16.0
     9
    10
    11
    12
    13
    14
                                                             1.5-
   0.5 -
                                                                       y = 0.0006X + 0.058
                                                                           R2 = 0.9985
                                                                      500    1000   1500    2000    2500
                                                                                                        3000
                                                                                                               3500
                                                               Sample Cone.
  ave 1 &2
  5313.3
STD DEV
  614.15
  ave 5&6
  6768.6
STD DEV
  331.04
                     after bringing
                     % Recover}
                        103.1
ppb in sol
 4879.1
 5747.6
 23800.4
 20871.8
 7002.7
 6534.6
 16008.6
 18401.7
 18405.9
 19159.0
 pH to the 7 range (because of precipitation).
 Range
80-120%
% Recovery
   95.9
   95.6
  Range
 85-115%
 85-115%
wet mass
 2.4924
 2.5141
 2.5176
 2.5002
 2.5757
 2.5586
 2.5244
 2.4903
 2.5141
 2.5586
                               1.156
                              -0.081

                            %moisture
                              12.1316
                              13.4434
                              12.0853

                            %moisture
                              13.3231
                              12.8651
                              12.0395
                                                                   mean

                                                                  12.553


                                                                   mean

                                                                  12.743
ppm Calc.
 4.8791
 5.7476
 23.8004
 20.8718
 7.0027
 6.5346
 16.0086
 18.4017
 18.4059
 19.1590
                                                                    % Solid

                                                                    87.447


                                                                    % Solid

                                                                    87.257
 M9/9 dry
262.0265
283.7658
1023.0533
1486.8677
356.6772
347.3913
1049.8548
1232.7753
702.7883
930.5193
ave 1 &2
 272.9
ave 5&6
 352.0
STD DEV
    15.4
STD DEV
    6.6
                                                          4°C
                                                          -20°C
                                                          4'C
                                                          -20° C
                                                      K2Cr2O7
                                                      added (mg)
                                                          1.5
                                                          1.5
                                                        PbCrO4
                                                      Added (mg)
                                                          16.6
                                                          12.9
                                                       Cr added  Spike Recovery %
                                                       |jg/g dry   Solution   Range
                                                         675        111    75-125%
                                                         674        104   75-125%
                                                                                        Cr added   Spike Recovery %
                                                                                        |jg/g dry   Solid     Range
                                                                                         1221.6      99    75-125%
                                                                                         955.1       92    75-125%
                                                                                C7

-------
Cr Soil Extraction
|T=223 day
12763-123
Stratford Con
Chrome VI dige:
Sample/STD
Blank
305
558
952
1339
2502
3253
slope
intercept
RSQ
Sample:
4°C#1
4"C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20' C #8 insol
Sample 2+spk
Sample 6+spk
Samples # 1 thro
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
n.
ition assay
A540
0.0000
0.2288
0.4047
0.6557
0.9342
1 .6745
2.1619
0.000654
0.038555
0.999817

0.5944
0.4653
1.0151
0.7589
0.5363
0.6597
1.2319
0.6984
0.8258
0.9061
12/17/2003


ppb calc. Sample #
290.8 9
559.7 10
943.4 1 1
1369.1 12
2500.8 13
3245.8 14
ppb calc.
849.7
652.3
1492.8
1101.2
760.9
949.5
1824.2
1008.7
1203.4
1326.2
dil. Factor
8.0
8.0
16.0
32.0
8.0
8.0
16.0
32.0
16.0
16.0

2.5 -
2 -
1.5-
1 -

0.5 -
0 -
C



y = 0.0007X + 0.0386
R2 = 0.9998 ^S
S^
.s'
^r
j/^
*
) 500 1000 1500 2000 2500 3000 3500







Sample Cone.
ppb in sol ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
6797.5 6008.1 1116.37 2.5051 6.7975 297.9657 268.0 42.4
5218.7
23884.7
2.5176 5.2187 237.9736
2.5001 23.8847 1040.3410
35236.9 ave5&6 STD DEV 2.4992 35.2369 1603.7303 ave 5&6 STD DEV
6087.0 6841
7596.1
29187.2
.5 1067.08 2.4965 6.0870 358.5484 364.6 8.6
2.5389 7.5961 370.7039
2.5496 29.1872 1112.4293
32277.4 % Recovery Range 2.5025 32.2774 1772.2785
19254.7 106.3 85-115% 2.5176 19.2547 710.5829
21218.7 103.2 85-115% 2.5389 21.2187 663.6067
ugh 8 had to be re-filtered after bringing pH to the 7 range
% Recovery Range
0.8756
0.0063
Tare
1280
-49
Tin + Soil
0.9865 3.7284
0.9884 2.6400
0.9996 3.3259

Tare Tin + Soil
0.9978 3.1838
0.9941 3.2598
0.9807 3.1161
102.9
wet
2.7419
1.6516
2.3263
wet
2.1860
2.2657
2.1354
80-120%
Tin + Soil dry
3.4063
2.4479
3.0549

(because of precipitation). K2Cr2O7
added (mg)
1.280 4°C 1.5
-0.049 -20°C 1 .5
%moisture mean % Solid
2.4198 11.7473 PbCrO4
1.4595 11.6311 11.676 88.324 Added (mg)
2.0553 11.6494 4'C 17.1
-20° C 18.6
Tin + Soil dry
2.9732
%moisture mean % Solid
1 .9754 9.6340
3.0405 2.0464 9.6791 9.722 90.278
2.9057 1 .9250 9.8530
                                                                                                                                      Cr added  Spike Recovery %
                                                                                                                                       |jg/g dry  Solution  Range
                                                                                                                                         669       116   75-125%
                                                                                                                                         644       116   75-125%
                                                                                                                                      Cr added  Spike Recovery %
                                                                                                                                       |jg/g dry  Solid     Range
                                                                                                                                       1246.4      107   75-125%
                                                                                                                                       1324.6      106   75-125%
                                                                               C8

-------
Cr Soil Extraction
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI dige:
Sample/STD
Blank
112
302
543
793
1500
2316
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 thro
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
12/2/2002

ition assay
A540 ppb calc.
0.0000
0.2044
0.2488
0.3723
0.4467
0.6272
1 .3933
0.000508
0.077423
0.926539
0.4718
0.5896
0.6223
0.6018
0.5382
0.6504
0.7911
0.6479
249.8
337.2
580.2
726.6
1081.7
2589.0
ppb calc.
775.9
1007.7
1072.1
1031.7
906.6
1127.3
1404.2
1122.4
Sample #
9
10
11
12
13
14
dil. Factor
2
2
2
2
2
2
10
2
ppb in sol
1551.9
2015.4
2144.1
2063.4
1813.2
2254.7
14041.7
2244.8



1- _^
y = O.OOOSx + 0.0774 ^^^
1 R2 = 0.9265 ^^^^


^^"^
+^^^









0 500 1000 1500 2000 2500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1917.6 238.12 2.4804 1.5519 73.9567 91.6 11.7
2.4842 2.0154 95.6936
2.4878 2.1441 101.8125
2.4871 2.0634 100.6609
2.4927 1.8132 85.9600
2.4918 2.2547 110.7325 K2Cr2O7 Cr added Spike Recovery %
% recovery Range 2.4911 14.0417 665.9093 added (mg) |jg/g dry Solution Range
11.5 85-115% 0.5 23.724 81 75-125%
ugh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). PbCrO4 Cr added Spike Recovery %
% recovery Range Added (mg) |jg/g dry Solid Range
0.4992
0.0947
Tare
830
34
Tin + Soil
19.8396 21.3177
19.7107 21.2067
19.5329 20.6733
99.4
wet
1 .4781
1 .4960
1.1404
80-120%
Tin + Soil
21 .0882
20.9724
20.5014
19.8 1511.9 38 75-125%
dry %moisture mean % Solid \
1.2486 15.527
1.2617 15.662 15.421 84.579
0.9685 15.074
MOTE: There was a weighing error for the K2Cr2O7 addition 0.5 ml was
amended not .8422mL as stated.
A/hen 0.5 ml is calculated the recovery is:
K2Cr2O7 Cr added Spike Recovery %
added (mg) |jg/g dry Solution
0.05 23.724 82
C9

-------
Cr Soil Extraction
T=14day
12763-125A  |
Boom Snub 0.5'
                        [12/16/2002   |
Chrome VI digestion assay
Sample/STD    A540
Blank
           175
           321
           564
           892
          1463
          2396
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 5+spk
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
                0.0000
                0.2518
                0.3464
                0.5545
                0.8040
                0.9994
                1.3314
                0.000481
                0.248554
                 0.95965
                0.5454
                0.5600
                0.4118
                0.7300
                0.7708
                0.6324
                0.3631
                0.7220
                0.4258
                0.5362
                           ppb calc.    Sample #
  6.7
 203.3
 635.8
 1154.3
 1560.4
 2250.3
ppb calc.
 616.9
 647.2
 339.3
 1000.5
 1085.3
 797.7
 238.0
 983.9
 368.3
 597.8
        9
       10
       11
       12
       13
       14
                                      dil. Factor
   2.0
   2.0
   10.0
   20.0
   2.0
   2.0
   10.0
   20.0
   10.0
   10.0
ppb in sol
 1233.8
 1294.5
 3392.5
 20010.5
 2170.6
 1595.4
 2380.5
 19678.0
 3683.5
 5977.8
% Recover}  Range
   127.3    80-120%
            1.6-f

            1.4-

            1.2 -

              1 -

            0.8 -

            0.6 -

            0.4 -

            0.2 -
                                                             0
                                                                   y = O.OOOSx + 0.2486
                                                                       R2 = 0.9596
                                                               0
                                                                      500
                                                                              1000
                                                                                      1500
                                                                                              2000
                                                                                                      2500
                                                                                                              3000
ave1&2
 1264.1
ave5&6
 1883.0
           STD DEV
             42.91
           STD DEV
             406.75
% Recovery
   61.2
   95.2
                                                         dry
                                                            1.2179
                                                            1.1812
                                                            0.8242
                                                            1.8543
                                                            1.4593
                                                            1.1531
           Range
          85-115%
          85-115%
Sample Cone.
  wet mass
   2.4710
   2.4851
   2.4781
   2.4827
   2.4884
   2.4905
   2.4873
   2.4908
   2.4851
   2.4905
                       1.148
                       -0.272

                     %moisture
                      16.1341
                      16.3811
                      16.0863

                     %moisture
                      16.2201
                      15.9970
                      16.1016
                                             mean

                                             16.201


                                             mean

                                             16.106
ppm Calc.
 1.2338
 1 .2945
 3.3925
 20.0105
 2.1706
 1 .5954
 2.3805
 19.6780
 3.6835
 5.9778
                                  % Solid

                                  83.799


                                  % Solid

                                  83.894
 |jg/g dry
 59.5999
 63.3705
163.3472
961.6653
103.9638
 76.3421
118.6261
941.4566
176.8345
286.0593
ave1&2
  61.5
ave 5&6
  90.2
STD DEV
    2.7
STD DEV
    19.5
                                                                                                                          K2Cr2O7
                                                                                                                          added (mg)
                                                                                                                    4°C         0.5
                                                                                                                   -20' C       0.5
                                                                                                                    4'C
                                                                                                                   -20°C
                                                                   PbCrO4
                                                                 Added (mg)
                                                                     12.2
                                                                     11.4
                                                                                                            Cr added  Spike Recovery %
                                                                                                             |jg/g dry  Solution   Range
                                                                                                               222        46    75-125%
                                                                                                               222        13    75-125%
                                                                                                            Cr added  Spike Recovery %
                                                                                                             |jg/g dry  Solid      Range
                                                                                                              943.5       95    75-125%
                                                                                                              877.7       97    75-125%
                                                                               CIO

-------
Cr Soil Extraction
T=28 day
1 2763-1 25A
Boom Snub C
Chrome VI dige:
Sample/STD
Blank
254
402
617
988
1605
2472
slope
intercept
RSQ
Sample:
4°C#1
4"C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20' C #8 insol
Sample 2+spk
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
.5'
12/30/2002

ition assay
A540 ppb calc.
0.0001
0.2644
0.3081
0.5228
0.7825
1 .2240
1.7179
0.000673
0.091988
0.995075
0.5871
1 .0647
0.5624
0.6940
0.6656
0.9285
0.5091
0.6782
0.5415
0.5271

0.7592
0.0590
Tare
256.1
321.0
639.8
1025.5
1681.2
2414.7
ppb calc.
735.3
1444.6
698.6
894.1
851.9
1242.3
619.5
870.6
667.6
646.2
991
-49
Tin + Soil
19.3420 20.8832
19.6076 21.3381
19.7374 21.4651
Tare Tin + Soil
19.5603 21.4438
19.7100 21.8676
19.8187 21.4892
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
10.0
10.0
% Recover}
100.2
wet
1.5412
1 .7305
1 .7277
wet
1 .8835
2.1576
1 .6705
ppb in sol
1470.6
2889.2
6986.3
17881.5
1703.8
2484.7
6194.7
17412.2 c
6675.9
6462.0
Range
80-120%
Tin + Soil d
20.6488
21 .0736
21 .2052

2 	
1.8- y = 0.0007X + 0.092
1 6 R2 = 0.9951 ./*
0.6 - ^S^
0.2 - *^
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
2179.9 1003.11 2.5160 1.4706 68.0700 103.6 50.2
2.4887 2.8892 139.0523
2.4921 6.9863 337.2240
ave5&6 STD DEV 2.4888 17.8815 847.8067 ave 5&6 STD DEV
2094.2 552.17 2.4896 1.7038 89.4025 106.7 24.5
2.4999 2.4847 124.0120
2.4985 6.1947 301.2230
/o Recovery Range 2.4976 17.4122 878.8367
94.7 85-115% 2.4887 6.6759 317.4395
99.4 85-115% 2.4999 6.4620 307.1200
0.991 K2Cr2O7
-0.049 added (mg)
4°C 0.5
ry %moisture mean % Solid -20°C 0.5
1.3068 15.2089
1.4660 15.2846 15.179 84.821
1.4678 15.0431 PbCrO4
Added (mg)
Tin + Soil dry %moisture mean % Solid 4°C 1 1 .8
21.1454
21.5215
21 .2234
1.5851 15.8428 -20° C 11.5
1.8115 16.0410 15.932 84.068
1.4047 15.9114
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solution   Range
                                                           238        98    75-125%
                                                           239        81    75-125%
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solid     Range
                                                          899.3       83    75-125%
                                                          881.2       88    75-125%
Cll

-------
Cr Soil Extraction
T=56 day
1 2763-1 25A
Boom Snub C
Chrome VI dige:
Sample/STD
Blank
248
400
624
994
1621
2489
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 5+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
.5'
ition assay
A540
0.0000
0.2187
0.3005
0.4841
0.7665
1 .2376
1 .8300
0.000729
0.031248
0.99921 1
0.6732
0.6408
0.5183
0.6642
0.7184
0.7018
0.5153
0.7164
0.4352
0.4608

0.8308
0.0093
Tare
1/27/2003
ppb calc.
257.0
369.2
621.0
1008.2
1654.2
2466.5
ppb calc.
880.3
835.8
667.9
867.9
942.2
919.5
663.7
939.5
553.9
589.0
1096
-30
Tin + Soil
19.7954 21.9876
19.7345 21.9862
19.7810 21.6046
Tare Tin + Soil
19.8261 21.9127
19.7114 22.0397
19.6735 21.6767
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
10.0
10.0
% Recover}
109.9
wet
2.1922
2.2517
1 .8236
wet
2.0866
2.3283
2.0032
ppb in sol
1760.5
1671.7
6678.6
17358.4
1884.5
1839.0
6637.4
18789.9 c
5539.1
5890.1
Range
80-120%
Tin + Soil d
21.6310
21 .6280
21.3124

2 	
y = 0.0007x + 0.0312
18~ R2 = 0.9992 S*
0.8 - *S^
0.6- ^S
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
1716.1 62.83 2.4781 1.7605 84.6379 82.4 3.1
2.4841 1.6717 80.1995
2.5003 6.6786 318.1752
ave5&6 STD DEV 2.5076 17.3584 824.7940 ave 5&6 STD DEV
1861.7 32.19 2.4908 1.8845 96.3698 93.3 4.4
2.4894 1 .8390 90.2048
2.4899 6.6374 323.8396
/o Recovery Range 2.4943 18.7899 919.7484
94.5 85-115% 2.4841 5.5391 265.7255
100.1 85-115% 2.4894 5.8901 281.1931
K2Cr2O7
1.096 added (mg)
-0.030 4°C 0.5
-20' C 0.5
ry %moisture mean % Solid
1.8356 16.2668
1.8935 15.9080 16.066 83.934 PbCrO4
1.5314 16.0233 Added (mg)
4'C 10.7
Tin + Soil dry %moisture mean % Solid -20°C 11.1
21 .5824
21 .6740
21 .3572
1.7563 15.8296
1.9626 15.7067 15.829 84.171
1.6837 15.9495
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solution   Range
                                                           239        99    75-125%
                                                           238        97    75-125%
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solid     Range
                                                          817.9       91    75-125%
                                                          850.6       97    75-125%
C12

-------
Cr Soil Extraction
T=112day
1 2763-1 25A
Boom Snub C
Chrome VI dige:
Sample/STD
Blank
258
404
600
1029
1747
2481
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
.5'
ition assay
A540
0.0000
0.1924
0.3367
0.4852
0.8483
1.1287
1 .7739
0.000675
0.061295
0.985812
0.6675
0.5830
0.5409
0.6529
0.7956
1 .0480
0.5204
0.6521
0.4537
0.572

0.7964
0.0874
Tare
3/24/2003
ppb calc.
194.4
408.3
628.4
1166.7
1582.4
2538.9
ppb calc.
898.7
773.4
711.0
877.0
1088.6
1462.7
680.6
875.8
581.7
757.1
1090
39
Tin + Soil
19.3417 21.7911
19.6065 21.7224
19.7358 21.7559
Tare Tin + Soil
19.5585 22.0631
19.7090 21.5890
19.8173 23.2279
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
10.0
10.0
% Recover}
107.8
wet
2.4494
2.1159
2.0201
wet
2.5046
1 .8800
3.4106
ppb in sol
1797.3
1546.8
7109.9
17540.6
2177.2
2925.5
6806.0
17516.9 c
5817.2
7571.0
Range
80-120%
Tin + Soil d
21.4151
21 .4053
21 .4465

2 	
1.8- y = 0.0007x + 0.0613 *
16_ R2 = 0.9858 ^S
0.8 - ^S
0.6- s/^
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
1672.1 177.16 2.4926 1.7973 87.4911 80.4 10.1
2.4922 1.5468 73.2129
2.4925 7.1099 356.8683
ave5&6 STD DEV 2.4989 17.5406 889.8933 ave 5&6 STD DEV
2551.3 529.16 2.4965 2.1772 109.6109 123.8 20.0
2.5026 2.9255 137.8964
2.4998 6.8060 328.3862
/o Recovery Range 2.4964 17.5169 840.8832
100.5 85-115% 2.4922 5.8172 266.5535
116.1 85-115% 2.5026 7.5710 354.9008
1 .090 K2Cr2O7 Cr added Spike Recovery %
0.039 added (mg) |jg/g dry Solution Range
4°C 0.5 239 116 75-125%
ry %moisture mean % Solid -20° C 0.5 237 86 75-125%
2.0734 15.3507
1.7988 14.9865 15.218 84.782
1.7107 15.3161 PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid 4'C 10.4 789.8 103 75-125%
21 .6873
21.3019
22.7006
2.1288 15.0044 -20° C 9.9 752.8 95 75-125%
1.5929 15.2713 15.245 84.755
2.8833 15.4606
C12

-------
Cr Soil Extraction
T=224 day
1 2763-1 25A
Boom Snub C
Chrome VI dige:
Sample/STD
Blank
253
431
705
1225
1911
2878
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
.5'
ition assay
A540
0.0000
0.2111
0.3578
0.5767
0.9320
1 .4859
2.1372
0.000736
0.04272
0.999045
0.5361
1.1905
0.5714
0.6571
0.5340
0.4920
0.5544
0.6351
0.7079
0.7007

0.7412
0.0052
Tare
7/21/2003
ppb calc.
228.9
428.4
726.0
1209.0
1962.1
2847.6
ppb calc.
670.8
1560.5
718.8
835.3
667.9
610.8
695.7
805.4
904.4
894.6
950
-51
Tin + Soil
0.9951 2.0419
0.9902 2.0265
0.9890 2.0305
Tare Tin + Soil
0.9742 2.0594
0.9871 2.2308
0.9809 2.2078
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
16.0
16.0
2.0
2.0
16.0
16.0
16.0
16.0
% Recover}
103.1
wet
1 .0468
1 .0363
1.0415
wet
1 .0852
1 .2437
1 .2269
ppb in sol
1341.6
3121.0
11500.4
13364.6
1335.9
1221.6
11130.6
12886.1 c
14469.7
14313.1
Range
80-120%
Tin + Soil d
1 .8698
1 .8628
1 .8745


y = 0.0007X + 0.0427
2 - R2 = 0.999 ./*
0.5 - ^S^
0 500 1000 1500 2000 2500 3000 3500

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
2231.3 1258.22 2.5067 1.3416 96.8490 140.4 61.7
2.5124 3.1210 184.0433
2.5068 11.5004 712.2022
ave5&6 STD DEV 2.5159 13.3646 857.3423 ave 5&6 STD DEV
1278.8 80.75 2.5054 1.3359 83.3069 80.5 4.0
2.5629 1.2216 77.6785
2.5430 11.1306 719.4227
/o Recovery Range 2.5765 12.8861 781.6059
99.5 85-115% 2.5124 14.4697 670.6757
99.2 85-115% 2.5629 14.3131 601.5596
K2Cr2O7
0.950 added (mg)
-0.051 4°C 1.5
-20' C 1.5
ry %moisture mean % Solid
0.8747 16.4406
0.8726 15.7966 15.739 84.261 PbCrO4
0.8855 14.9784 Added (mg)
4'C 11.9
Tin + Soil dry %moisture mean % Solid -20°C 10.7
1 .8880
2.0394
2.0159
0.9138 15.7943
1.0523 15.3896 15.608 84.392
1.0350 15.6410
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solution   Range
                                                           704       81     75-125%
                                                           687       93     75-125%
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry  Solid      Range
                                                          903.1       79     75-125%
                                                          791.7       89     75-125%
C14

-------
Cr Soil Extraction
T=0 day
12763-125B
Boom Snub 3'
Chrome VI dige:
Sample/STD
Blank
141
289
510
885
1505
2283
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#3 + spike
Sol Spike 16
Insol Spike 17
Samples # 1 thro
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
12/5/2002

ition assay
A540 ppb calc.
0.0000
0.1391
0.2876
0.4551
0.7412
1.1482
1 .6280
0.000688
0.089921
0.996334
1.1091
1 .2784
1 .3386
1 .3371
0.9646
1 .9084
0.9768
0.9689
0.8928
1.2153
71.5
287.4
530.9
946.9
1538.6
2236.2
ppb calc.
1481.8
1727.9
1815.4
1813.2
1271.7
2643.8
1289.4
1277.9
1167.3
1636.2
Sample #
9
10
11
12
13
14
dil. Factor
4
4
4
4
4
4
10
8
4
10
ppb in sol
5927.0
6911.6
7261.7
7253.0
5086.7
10575.4
12894.1
10606.8
4669.1
16361.6


16 ^S+
y = O.OOOJx + 0.0899 ^^
1 1 R2 = 0.9963 4^^
^S^
>"


:; *<^
" ^
*
0 500 1000 1500 2000 2500


Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry
6488.0 954.14 2.4970 5.9270 302.6969
2.4877 6.9116 344.0335
2.4971 7.2617 360.2836
2.4854 7.2530 361.5936
2.5000 5.0867 272.0466
2.4920 10.5754 531.2729
% recovery Range 2.4953 12.8941 663.7368
83.6 85-115%
2.5050 4.6691 252.6520
2.4970 16.3616 811.7959
ugh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.6200
0.0770
Tare
771
-19
Tin + Soil
19.8674 20.9254
19.5268 20.9358
19.8872 21.7444
87.4
wet
1 .0580
1 .4090
1 .8572
80-120%
Tin + Soil dry %moisture mean % Solid
20.7227
20.6619
21 .3858
0.8553 19.159
1.1351 19.439 19.302 80.698
1.4986 19.309
                                  ave1-5  STD DEV
                                   328.1       39.4
                                 #6
                                 #16
                                 #7
                                 #17
K2Cr2O7
added (mg)
   0.421
   0.4291
  PbCrO4
 Added (mg)
    11.3
    11.2
Cr added   Spike Recovery %
|jg/g dry   Solution     Range
209.350      97     75-125%
212.270      -36     75-125%
Cr added   Spike Recovery %
|jg/g dry   Solid        Range
 902.9       37     75-125%
 894.3       54     75-125%
C15

-------
Cr Soil Extraction
T=14day
12763-125B
Boom Snub 2
Chrome VI dige:
Sample/STD
Blank
245
390
619
993
1602
2422
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 2+spk
Sample 5+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
ition assay
A540
0.0000
0.1874
0.3065
0.5360
0.7400
1 .2088
1.6125
0.000658
0.077547
0.989792
0.8461
1 .0647
0.8030
0.9230
1.0153
0.8904
0.8755
0.8495
0.8172
0.8153

0.7139
0.0291
Tare
12/19/2002
ppb calc.
167.0
348.0
696.9
1006.9
1719.5
2333.1
ppb calc.
1168.2
1500.5
1102.7
1285.1
1425.4
1235.5
1212.9
1173.4
1124.3
1121.4
967
-74
Tin + Soil
19.9482 21.8158
19.7961 21.2893
19.8302 21.1847
Tare Tin + Soil
19.7848 21.1949
19.8764 21.6101
19.8000 21.6226
Sample #
9
10
11
12
13
14
dil. Factor
5.0
5.0
10.0
20.0
5.0
5.0
10.0
20.0
10.0
10.0
% Recover}
99.6
wet
1 .8676
1 .4932
1 .3545
wet
1.4101
1 .7337
1 .8226
ppb in sol
5841.0
7502.4
11027.0
25701 .9
7127.0
6177.7
12129.0
23467.5 c
11242.8
11213.9
Range
80-120%
Tin + Soil d
21 .4670
21 .0096
20.9263

-i Q 	
y = 0.0007X + 0.0775
1.6- R2 = 0.9898 j/^
1.2 ^T
0.4- ^S
0.2- *
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
6671.7 1174.77 2.4885 5.8410 289.5714 330.8 58.3
2.4867 7.5024 372.0790
2.4809 11.0270 546.6162
ave5&6 STD DEV 2.4941 25.7019 1274.9069 ave 5&6 STD DEV
6652.3 671.22 2.4897 7.1270 361.3973 339.0 31.7
2.4898 6.1777 316.5294
2.4929 12.1290 601.6692
/o Recovery Range 2.4952 23.4675 1191.2400
93.5 85-115% 2.4867 11.2428 577.7701
102.2 85-115% 2.4898 11.2139 572.7093
K2Cr2O7
0.967 added (mg)
-0.074 4°C 0.5
-20' C 0.5
ry %moisture mean % Solid
1.5188 18.6764
1.2135 18.7316 18.828 81.172 PbCrO4
1.0961 19.0772 Added (mg)
4'C 11.7
Tin + Soil dry %moisture mean % Solid -20°C 10.8
20.9254
21 .2782
21 .2752
1.1406 19.1121
1.4018 19.1440 19.106 80.894
1.4752 19.0607
                                                        Cr added  Spike Recovery %
                                                        |jg/g dry  Solution   Range
                                                          249        87    75-125%
                                                          249       105    75-125%
                                                        Cr added  Spike Recovery %
                                                        |jg/g dry  Solid      Range
                                                         929.8      102    75-125%
                                                         860.8       99    75-125%
C16

-------
Cr Soil Extraction
T=28 day
12763-125B
Boom Snub 3'
1/2/2003 |




Chrome VI digestion assay

Sample/STD A540 ppb calc. Sample #
Blank
255
399
617
990
1616
2476
0.0000
0.2088
0.2915
0.4170
0.6798
1.1309
1 .6462
269.0 9
394.6 10
585.1 11
984.0 12
1668.7 13
2450.9 14

slope 0.000659
intercept 0.031 57

1 8 i

1.6 -
1.4 -
1.2 -
1 -
0.8 -

0.6-
0.4-

0.2 -
Q
y = 0.0007x + 0.0316
R2 = 0.9987 ./*
s/r
*S
.S
jf
jT
jf
*F
*












0 500 1000 1500 2000 2500 3000
















RSQ 0.998709
Sample Cone.
Sample: ppb calc. dil. Factor ppb in sol ave 4°C STD DEV wet mass ppm Calc. |jg/g dry ave 4°C STD DEV
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
4°C#17
4°C#18
4°C#19
Sample 1+spk
Sample 6+spk
0.9789
0.9847
0.7246
0.9075
1 .2002
0.8982
0.9215
0.8547
0.9743
0.9600
0.8921
0.7722
0.7112
1438.0
1446.8
1052.0
1329.6
1773.9
1315.5
1350.9
1249.5
1431.0
1409.3
1306.2
1124.2
1031.6
5.0
5.0
10.0
20.0
5.0
5.0
10.0
20.0
5.0
5.0
5.0
10.0
10.0
7189.9 7031.3 288.06 2.4946 7.1899 352.9911 348.2 12.8
7234.0 2.4841 7.2340 356.4302
10519.8 2.4863 10.5198 519.4723
26592.2 ave5&6 STD DEV 2.4839 26.5922 1314.3654 ave 5&6 STD DEV
8869.5 7723.5 1620.75 2.4950 8.8695 439.7822 383.4 79.8
6577.5 2.4895 6.5775 326.9493
13508.6 2.4957 13.5086 683.1715
24989.2 % Recovery Range 2.4931 24.9892 1256.8633
7155.0 2.4979 7.1550 355.2661
7046.5 2.4925 7.0465 350.6994
6531.2 2.4876 6.5312 325.7016
11242.3 101.3 85-115% 2.4841 11.2423 555.7706
10316.4 93.5 85-115% 2.4895 10.3164 514.0572
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
1081
 -60
% Recovery  Range
   109.2    80-120%
                               2.0480
                               1.5236
                               1.7815
                            dry
                               1.8545
                               2.1588
                               1.5825
  1.081
  -0.060

%moisture
 18.8107
 18.4281
 18.5004

%moisture
 18.7122
 19.1249
 20.3132
                             K2Cr2O7
                             added (mg)
                      4'C        0.5
                      -20-C      0.5
                     Cr added  Spike Recovery %
                     |jg/g dry  Solution   Range
                       248        69    75-125%
                       249       120    75-125%
                                              mean

                                             18.580


                                              mean

                                             19.383
% Solid

81.420


% Solid

80.617
 4°C
-20°C
  PbCrO4
Added (mg)
   11.8
    11
Cr added
M9/9 dry
  938.7
  880.6
Spike Recovery %
Solid      Range
   103    75-125%
   99     75-125%
                                                                               C17

-------
Cr Soil Extraction
T=56 day
12763-125B  |
Boom Snub 3'
         11/31/2003    |
          Color assay on 2/1703
Chrome VI digestion assay
Sample/STD    A540
Blank
           248
           400
           625
          1003
          1630
          2517
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20°C #7 sol
-20°C #8 insol
Sample 2+spk
Sample 6+spk
LCS#16
Blank #9

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
  0.0000
  0.2142
  0.3558
  0.5007
  0.7740
  1.2613
  1.8551
 0.000723
 0.052994
 0.999112
  1.0392
  1.0632
  1.2606
  1.2462
  1.2428
  0.9792
  0.9547
  1.0297
  0.8074
  0.7848
Tare
            ppb calc.    Sample #
    223.0
    418.9
    619.3
    997.3
   1671.4
   2492.8
  ppb calc.
   1364.2
   1397.4
   1670.4
   1650.5
   1645.8
   1281.2
   1247.3
   1351.0
   1043.5
   1012.3
              1005
              -46
Tin + Soil
    10
    11
    12
    13
    14
    15
                       dil. Factor
5.0
5.0
10.0
20.0
5.0
5.0
10.0
20.0
10.0
10.0
ppb in sol
 6820.9
 6986.9
 16704.4
 33010.5
 8229.1
 6406.0
 12473.0
 27020.9
 10435.5
 10122.8
            % Recover}  Range
                99.9    80-120%
                                                       y = 0.0007X + 0.053
                                                          R2 = 0.9991
                                                                      500
                                                                             1000
                                                                                     1500
                                                                                             2000
                                                                                                     2500
                                                                                                             3000
  ave 1 &2
  6903.9
  ave 5&6
  7317.5
STD DEV
  117.37
STD DEV
 1289.16
% Recovery
   86.2
   92.9
  Range
 85-115%
 85-115%
Sample Cone.
  wet mass
   2.4321
   2.5008
   2.4983
   2.5361
   2.5222
   2.5511
   2.5153
   2.5042
   2.5008
   2.5511
ppm Calc.
 6.8209
 6.9869
 16.7044
 33.0105
 8.2291
 6.4060
 12.4730
 27.0209
 10.4355
 10.1228


1
0.8684
0.8155
0.8232
i
0.8198
0.8164
0.8664
1.005
-0.046
%moisture mean
17.5544
18.0320 17.725
17.5893
%moisture mean
18.9681
18.9114 18.310
17.0512


% Solid

82.275

% Solid

81 .690

 M9/9 dry
388.1973
368.1854
864.1665
1665.0452
447.4099
333.5261
693.8972
1439.0825
506.5668
485.4914
ave 1 &2
 378.2
ave 5&6
 390.5
STD DEV
    14.2
STD DEV
    80.5
                                                                                  K2Cr2O7
                                                                                  added (mg)
                                                                           4°C       0.503
                                                                          -20'C      0.505
                                                                                                    4'C
                                                                                                   -20°C
                                                                                                   PbCrO4
                                                                                                  Added (mg)
                                                                                                     18.6
                                                                                                     14.3
                                                                                       Cr added  Spike Recovery %
                                                                                       |jg/g dry   Solution   Range
                                                                                         245        199   75-125%
                                                                                         246        124   75-125%
                                                                                               Cr added  Spike Recovery %
                                                                                               |jg/g dry  Solid      Range
                                                                                                1434.2       90     75-125%
                                                                                                1124.7       93     75-125%
                                                                               CIS

-------
Cr Soil Extraction
T=112day
12763-125B
Boom Snub 3'
Chrome VI dige:
Sample/STD
Blank
251
400
623
987
1623
2514
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 6+spk
3/27/2003

ition assay
A540 ppb calc.
0.0000
0.2136
0.3503
0.4829
0.8008
1 .2406
1 .8730
0.000731
0.047243
0.998983
1.1383
0.9950
0.9500
0.8886
1 .0832
0.9767
0.8504
0.8704
0.8621
0.7957
227.5
414.5
595.9
1030.7
1632.3
2497.3
ppb calc.
1492.4
1296.4
1234.8
1150.8
1417.0
1271.3
1098.6
1125.9
1114.6
1023.7
Sample #
9
10
11
12
13
14
dil. Factor
5.0
5.0
10.0
20.0
5.0
5.0
10.0
20.0
10.0
10.0
ppb in sol
7461.8
6481.8
12348.0
23016.3
7085.0
6356.6
10985.6
22518.4 c
11145.7
10237.5

2 	
1.8 -
1.6 -
1.4-
1.2 -
1 -
0.8 -
0.6-
0.4-
0.2 -
y = O.OOOTX + 0.0472
R2 = 0.999 S*

0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
6971.8 692.99 2.4963 7.4618 369.3629 343.6 36.5
2.4958 6.4818 317.7386
2.4964 12.3480 605.1111
ave5&6 STD DEV 2.5080 23.0163 1145.3535 ave 5&6 STD DEV
6720.8 515.03 2.4955 7.0850 350.7880 332.7 25.5
2.4960 6.3566 314.6842
2.4983 10.9856 538.5446
/o Recovery Range 2.4986 22.5184 1119.4296
92.1 85-115% 2.4958 11.1457 546.3363
97.0 85-115% 2.4960 10.2375 502.2555
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
% Recover}  Range
   99.2    80-120%
                       2.9220
                       2.5140
                       2.5892
                    dry
                       1.7939
                       1.9511
                       2.3396
  0.994
  -0.033

%moisture
 18.5210
 18.2891
 18.0192

%moisture
 18.2585
 18.4766
 18.3300
                                         K2Cr2O7
                                         added (mg)
                                  4°C        0.5
                                 -20'C       0.5
mean

18.276


mean

18.355
% Solid

81.724


% Solid

81.645
 4'C
-20°C
  PbCrO4
Added (mg)
   11.3
   10.5
                                           Cr added  Spike Recovery %
                                           |jg/g dry  Solution   Range
                                             247       106    75-125%
                                             247        83    75-125%
Cr added  Spike Recovery %
 |jg/g dry   Solid      Range
  887.0       90     75-125%
  828.1       95     75-125%
                                                                                C19

-------
Cr Soil Extraction
T=224 day
12763-125B
Boom Snub 2
Chrome VI dige:
Sample/STD
Blank
308
448
661
1251
2007
2961
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
ition assay
A540
0.0000
0.2182
0.3564
0.5249
0.8980
1 .5066
2.1520
0.000725
0.020661
0.998763
0.4724
0.4733
0.7348
0.8260
0.4369
0.4022
0.6573
0.8045
0.8125
0.7912

0.9504
0.0015
Tare
7/23/2003
ppb calc.
272.6
463.3
695.9
1210.7
2050.6
2941.3
ppb calc.
623.4
624.6
985.5
1111.4
574.4
526.5
878.6
1081.7
1092.7
1063.4
1283
-26
Tin + Soil
0.9918 2.1152
0.9960 2.1503
0.9916 2.1153
Tare Tin + Soil
0.9994 2.1569
0.9925 2.3563
1.0005 2.1066
Sample #
9
10
11
12
13
14
dil. Factor
8.0
8.0
16.0
16.0
8.0
8.0
16.0
16.0
16.0
16.0
% Recover}
103.6
wet
1.1234
1.1543
1.1237
wet
1.1575
1 .3638
1.1061
ppb in sol
4987.2
4997.2
15768.3
17782.0
4595.3
4212.2
14057.1
17307.3 c
17484.0
17013.6
Range
80-120%
Tin + Soil d
1.9114
1 .9441
1 .9093


y = 0.0007X + 0.0207
2 _ R2 = 0.9988 ;S
0 500 1000 1500 2000 2500 3000 3500

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
4992.2 7.03 2.5280 4.9872 309.7205 315.3 7.9
2.5700 4.9972 320.9336
2.5674 15.7683 997.6314
ave5&6 STD DEV 2.5315 17.7820 1275.8588 ave 5&6 STD DEV
4403.8 270.89 2.5383 4.5953 325.5971 309.5 22.8
2.5586 4.2122 293.4226
2.5090 14.0571 1061.3288
/o Recovery Range 2.5132 17.3073 1273.4296
94.7 85-115% 2.5700 17.4840 670.1402
97.0 85-115% 2.5586 17.0136 741.3416
K2Cr2O7
1.283 added (mg)
-0.026 4°C 1 .5
-20' C 1.5
ry %moisture mean % Solid
0.9196 18.1414
0.9481 17.8636 18.112 81.888 PbCrO4
0.9177 18.3323 Added (mg)
4'C 12.6
Tin + Soil dry %moisture mean % Solid -20°C 13.1
1 .9529
1 .9733
1.9141
0.9535 17.6242
0.9808 28.0833 21.037 78.963
0.9136 17.4035
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solution   Range
                                                          706        97    75-125%
                                                          744        101    75-125%
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solid     Range
                                                          977.9       98    75-125%
                                                         1062.1       91    75-125%
C20

-------
Cr Soil Extraction
T=0 day
12763-125C
Boom Snub 5.5'
Chrome VI dige:
Sample/STD
Blank
254
402
620
991
1612
3475
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Sample 5+spk
Samples # 1 thro
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
1/6/2003

ition assay
A540 ppb calc.
0.0000
0.2103
0.2671
0.4192
0.6681
1.1031
1 .6386
0.000452
0.163921
0.955981
0.4480
0.4361
0.4198
0.4152
0.4544
0.2355
0.6159
0.3420
0.3285
102.6
228.4
565.0
1115.9
2078.6
3263.8
ppb calc.
628.7
602.4
566.3
556.1
642.9
158.4
1000.3
394.1
364.3
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
10.0
ppb in sol
1257.5
1204.8
1132.6
1112.3
1285.8
792.1
20006.8
3941.3
3642.5




R2 = 0.956 ^^^^
_^S^
• .ff^


^^
o- *»

0 500 1000 1500 2000 2500 3000 3500 4000


Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry
1198.6 75.68 2.4837 1.2575 63.9753
2.4795 1 .2048 61 .3765
2.5041 1.1326 57.1793
2.5037 1.1123 56.1337
2.1961 1.2858 73.9816
2.4995 0.7921 40.0351
% recovery Range 2.4938 20.0068 1046.3221
70.7 85-115%
58.9 85-115%
ugh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.6707
-0.0470
Tare
1122
-467
Tin + Soil
19.8729 21.9668
19.6099 22.2456
19.8178 21.9820
113.3
wet
2.0939
2.6357
2.1642
80-120%
Tin + Soil
21 .5307
21 .6996
21 .5262
dry %moisture mean % Solid
1 .6578 20.827
2.0897 20.716 20.868 79.132
1 .7084 21 .061
                                  ave 1 -5
                                   62.5
STD DEV
    7.1
                                 #6
                                 #7
K2Cr2O7
added (mg)
   0.5013
  PbCrO4
 Added (mg)
     11
Cr added   Spike Recovery %
|jg/g dry   Solution     Range
253.450      -9     75-125%
Cr added   Spike Recovery %
|jg/g dry   Solid        Range
 896.8      110     75-125%
C21

-------
Cr Soil Extraction
T=14day
12763-125C
Boom Snub 5.5'
1/20/2003



Chrome VI digestion assay

Sample/STD A540 ppb calc.

Blank
254
408
617
993
1510
2476
0.0000
0.3684
0.4285
0.6209
0.8957
1 .2833
1 .8688

257.5
344.5
623.0
1020.8
1582.0
2429.6

slope 0.000691
intercept 0.190547
RSQ 0.99648

Sample: ppb calc.
4°C#1
4"C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20' C #8 insol
Sample 2+spk
Sample 6+spk
0.6008
0.6047
0.5221
0.6975
0.5889
0.5820
0.5457
0.7105
0.4621
0.4653
593.9
599.6
480.0
733.9
576.7
566.7
514.2
752.7
393.1
397.8






Sample #


9
10
11
12
13
14





dil. Factor
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
10.0
10.0




















1.8-
1.6 -
1.4 -
1.2 -
1 -

0.8 -
0.6 -
0.4 -

0.2 -
Q
R2 = 0.9965 ^X*
.S
.S
j^
yT
^S
.S
JT
*/+
*r














0 500 1000 1500 2000 2500 3000


















Sample Cone.
ppb in sol ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
1187.8 1193.5 7.98 2.4826 1.1878 59.9195 64.3 6.3
1199.1 2.1847 1.1991 68.7660
4799.9 2.4924 4.7999 244.5513
14678.2 ave5&6 STD DEV 2.4888 14.6782 738.7074 ave 5&6 STD DEV
1153.4 1143.4 14.13 2.4911 1.1534 58.7818 58.2 0.8
1133.4 2.4935 1.1334 57.7112
5141.5 2.4930 5.1415 261.7922
15054.6 % Recovery Range 2.4940 15.0546 782.4976
3931.3 68.3 85-115% 2.1847 3.9313 225.2913
3977.6 71.1 85-115% 2.4935 3.9776 200.4526
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
1024
-243
% Recover}  Range
   102.7    80-120%
                               2.2552
                               2.2717
                               1.6277
                             dry
                               3.7976
                               3.1990
                               3.1976
  1.024
  -0.243

%moisture
 20.3447
 20.1203
 20.0187

%moisture
 21.2116
 21.4391
 21.0722
       K2Cr2O7
       added (mg)
 4°C        0.5
-20° C       0.5
                                                      Cr added
                                                       |jg/g dry
                                                         251
                                                         254
                       Spike Recovery %
                       Solution   Range
                          72    75-125%
                          80    75-125%
 mean

20.161


 mean

21.241
                                                         % Solid

                                                         79.839


                                                         % Solid

                                                         78.759
 4°C
-20° C
  PbCrO4
Added (mg)
   10.4
   10.7
Cr added  Spike Recovery %
 |jg/g dry   Solid      Range
  842.1       80     75-125%
  876.4       83     75-125%
                                                                                C22

-------
Cr Soil Extraction
T=28 day
12763-125C
Boom Snub 5.5'
Chrome VI dige:
Sample/STD
Blank
253
407
628
999
1626
2493
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 5+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
2/3/2003

ition assay
A540 ppb calc.
0.0000
0.2557
0.3400
0.5464
0.7649
1 .2283
1 .6207
0.000624
0.126957
0.989632
0.5408
0.6172
0.4811
0.6904
0.5266
0.4989
0.4757
0.7384
0.4108
0.4028

0.7407
0.1762
Tare
206.5
341.7
672.7
1023.2
1766.4
2395.7
ppb calc.
663.7
786.3
568.0
903.7
641.0
596.5
559.3
980.7
455.2
442.4
984
79
Tin + Soil
19.8721 23.4469
19.6097 24.0281
18.7037 21.6442
Tare Tin + Soil
29.2382 35.0315
29.1906 34.4537
19.8555 23.2923
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
10.0
10.0
% Recover}
98.7
wet
3.5748
4.4184
2.9405
wet
5.7933
5.2631
3.4368
ppb in sol
1327.5
1572.5
5679.9
18073.4
1281.9
1193.1
5593.3
19613.1 c
4552.4
4424.1
Range
80-120%
Tin + Soil d
22.6928
23.0804
21 .0287

-1 Q _, 	 „
y = 0.0006x + 0.127
1.6- R2 = 0.9896 >^
1.2- +S
0.8 - ^S
0.2 -
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
1450.0 173.29 2.4921 1.3275 67.8305 76.6 12.4
2.4878 1.5725 85.3219
2.4926 5.6799 296.0176
ave5&6 STD DEV 2.4949 18.0734 950.5815 ave 5&6 STD DEV
1237.5 62.83 2.4805 1.2819 67.5748 65.5 2.9
2.4869 1.1931 63.4793
2.4908 5.5933 299.5098
/o Recovery Range 2.4945 19.6131 1001.6898
80.6 85-115% 2.4878 4.5524 232.0992
78.6 85-115% 2.4869 4.4241 226.5436
K2Cr2O7
0.984 added (mg)
0.079 4°C 0.5
-20' C 0.5
ry %moisture mean % Solid
2.8207 21 .0949
3.4707 21.4489 21.159 78.841 PbCrO4
2.3250 20.9318 Added (mg)
4'C 11.3
Tin + Soil dry %moisture mean % Solid -20°C 1 1
33.8136
33.3205
22.5425
4.5754 21 .0226
4.1299 21.5310 21.457 78.543
2.6870 21.8168
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solution   Range
                                                           256        86    75-125%
                                                           258        91    75-125%
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solid     Range
                                                          924.3       95    75-125%
                                                          903.3       104   75-125%
C23

-------
Cr Soil Extraction
T=56 day
12763-125C
Boom Snub 5.5'
3/3/2003 |



Chrome VI digestion assay

Sample/STD A540 ppb calc. Sample #

Blank
253
401
652
995
1645
2191
0.0000
0.1913
0.3564
0.5054
0.7378
1.2515
1 .7485

246.9 9
458.0 10
648.4 1 1
945.4 12
1602.0 13
2237.2 14

slope 0.000782
intercept -0.001904

2
1.8 -
1.6 -
1.4-
1.2 -
1 -

0.8 -
0.6-
0.4-

0.2 -
Q
y = 0.0008x-0.0019 j
R2 = 0.9966 ^S
S^
^^*
^r
^S^
^f
^^^
./^
}r
*













0 500 1000 1500 2000 2500

















RSQ 0.996615
Sample Cone.
Sample: ppb calc. dil. Factor ppb in sol ave 4°C STD DEV wet mass ppm Calc. |jg/g dry ave 4°C STD DEV
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
4°C#17
4°C#18
4°C#19
Sample 1+spk
Sample 6+spk
0.4847
0.4819
0.4810
0.6758
0.5385
0.5589
0.4999
0.6466
0.5543
0.4597
0.4249
0.3988
0.4151
621.9
618.4
617.2
866.2
690.7
716.8
641.4
828.9
710.9
590.0
545.5
512.1
533.0
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
2.0
2.0
2.0
10.0
10.0
1243.9 1234.7 121.17 2.4849 1.2439 62.7002 62.2 6.1
1236.7 2.4867 1.2367 62.3159
6172.0 2.4931 6.1720 310.2306
17323.6 ave5&6 STD DEV 2.4899 17.3236 871.6522 ave 5&6 STD DEV
1381.4 1407.5 36.87 2.4905 1.3814 69.6079 71.7 3.0
1433.5 2.4903 1.4335 73.8058
6413.6 2.4914 6.4136 323.0977
16577.2 % Recovery Range 2.4993 16.5772 832.4798
1421.8 2.4895 1.4218 71.7364
1180.0 2.4943 1.1800 59.3741
1091.0 2.4907 1.0910 55.0001
5121.4 96.9 85-115% 2.4867 5.1214 258.2886
5329.8 97.4 85-115% 2.4903 5.3298 268.6175
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
% Recovery  Range
   95.1    80-120%
                       2.6554
                       1.9295
                       1.8774
                    dry
                       2.8969
                       2.6941
                       3.2985
  0.947
  0.024

%moisture
 20.2031
 20.1035
 20.2227

%moisture
 20.8000
 20.4177
 19.6879
                                         K2Cr2O7
                                         added (mg)
                                  4'C        0.5
                                 -20-C       0.5
                                           Cr added   Spike Recovery %
                                           |jg/g dry   Solution   Range
                                             256        97    75-125%
                                             256        98    75-125%
 mean

20.176


 mean

20.302
% Solid

79.824


% Solid

79.698
 4°C
-20°C
  PbCrO4
Added (mg)
   10.8
   10.1
Cr added
 M9/9 dry
  874.3
  815.8
Spike Recovery %
Solid      Range
   93     75-125%
   93     75-125%
                                                                                C24

-------
Cr Soil Extraction
T=112day
12763-125C
Boom Snub 5.5'
Chrome VI dige:
Sample/STD
Blank
252
402
629
1004
1626
2503
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
4/28/2003

ition assay
A540 ppb calc.
0.0000
0.2314
0.4479
0.5374
0.8278
1 .2866
1 .8997
0.000724
0.098071
0.996731
0.5404
0.5314
0.4904
0.7320
0.5522
0.5616
0.4863
0.6261
0.4748
0.4823

0.7982
0.0525
Tare
184.3
483.4
607.1
1008.5
1642.5
2489.8
ppb calc.
611.3
598.8
542.2
876.1
627.6
640.6
536.5
729.7
520.6
531.0
968
-63
Tin + Soil
19.8724 23.9407
19.6100 23.4177
18.7034 21.6045
Tare Tin + Soil
29.2391 33.1208
29.1911 33.6385
19.8561 24.0327
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
10.0
20.0
2.0
2.0
10.0
20.0
10.0
10.0
% Recover}
94.3
wet
4.0683
3.8077
2.901 1
wet
3.8817
4.4474
4.1766
ppb in sol
1222.6
1197.7
5421.8
17521.3
1255.2
1281.2
5365.2
14594.3 c
5206.2
5309.9
Range
80-120%
Tin + Soil d
23.0941
22.6337
21.0186


2 - y = 0.0007X + 0.0981
R2 = 0.9967 .n/1*
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
1210.1 17.59 2.4856 1.2226 62.7878 62.1 1.0
2.4940 1.1977 61.3920
2.4944 5.4218 279.9077
ave5&6 STD DEV 2.4957 17.5213 896.3147 ave 5&6 STD DEV
1268.2 18.37 2.4859 1.2552 63.5286 65.1 2.2
2.4880 1.2812 66.5802
2.4835 5.3652 276.1352
/o Recovery Range 2.4905 14.5943 789.1480
99.6 85-115% 2.4940 5.2062 262.4960
100.7 85-115% 2.4880 5.3099 268.3889
K2Cr2O7
0.968 added (mg)
-0.063 4°C 0.6
-20' C 0.5
ry %moisture mean % Solid
3.2217 20.8097
3.0237 20.5899 20.532 79.468 PbCrO4
2.3152 20.1958 Added (mg)
4'C 11.1
Tin + Soil dry %moisture mean % Solid -20°C 10.2
32.3429
32.7119
23.1730
3.1038 20.0402
3.5208 20.8346 20.486 79.514
3.3169 20.5837
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solution   Range
                                                           278        78    75-125%
                                                           253        83    75-125%
                                                        Cr added  Spike Recovery %
                                                         |jg/g dry   Solid     Range
                                                          900.5       93    75-125%
                                                          828.7       87    75-125%
C25

-------
Cr Soil Extraction
T=224 day
12763-125C
Boom Snub 5.5'
Chrome VI dige:
Sample/STD
Blank
294
379
721
1213
1672
2818
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 2+spk
Sample 6+spk
8/26/2003

ition assay
A540 ppb calc.
0.0000
0.2379
0.3024
0.5668
0.9524
1 .2792
2.0259
0.000712
0.05145
0.997998
0.3216
0.3050
0.4746
0.3917
0.3571
0.3066
0.5407
0.5827
0.6723
0.6670
261.7
352.2
723.3
1264.6
1723.3
2771.3
ppb calc.
379.2
355.9
593.9
477.6
429.0
358.1
686.7
745.7
871.4
864.0
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
16.0
16.0
2.0
2.0
16.0
16.0
16.0
16.0
ppb in sol
758.4
711.8
9502.9
7641.2
858.0
716.3
10987.3
11930.6 c
13942.7
13823.7


2 -
1.5 -
1 -
0.5 -
y = 0.0007x + 0.0514
R2 = 0.998 .S*

0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
735.1 32.95 2.4666 0.7584 60.5766 60.4 0.2
2.5033 0.7118 60.2275
2.4960 9.5029 810.3800
ave5&6 STD DEV 2.5285 7.6412 654.3722 ave 5&6 STD DEV
787.1 100.24 2.4947 0.8580 61.5241 59.4 3.0
2.5349 0.7163 57.3336
2.4623 10.9873 814.0103
/o Recovery Range 2.5853 11.9306 926.7739
100.2 85-115% 2.5033 13.9427 601.7046
99.3 85-115% 2.5349 13.8237 700.6530
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
1162
 -65
% Recover}  Range
   102.5    80-120%
                               0.9765
                               0.9692
                               0.8935
                            dry
                               0.9330
                               0.9786
                               0.9211
  1.162
  -0.065

%moisture
 22.0546
 22.0838
 21.0410

%moisture
 20.8450
 18.9968
 16.5670
                             K2Cr2O7
                             added (mg)
                       4°C        1.5
                      -20'C       1.5
                                              mean

                                             21.726


                                              mean

                                             18.803
% Solid

78.274


% Solid

81.197
 4'C
-20°C
  PbCrO4
Added (mg)
   10.8
   11.5
                     Cr added   Spike Recovery %
                     |jg/g dry   Solution   Range
                       766        98    75-125%
                       747        101    75-125%
Cr added  Spike Recovery %
 |jg/g dry   Solid      Range
  878.0       68     75-125%
  881.4       98     75-125%
                                                                                C26

-------
Cr Soil Extraction
T=0 day
12763-126D
Frontier Hard Chrome,
Chrome VI dige:
Sample/STD
Blank
253
403
624
990
1616
2494
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 thro
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
1/9/2003
Sandy Soil
ition assay
A540 ppb calc.
0.0000
0.1825
0.2918
0.4279
0.7461
1 .2829
1 .7971
0.00074
0.000901
0.994374
1 .2325
1 .2686
1.1679
1 .2074
1 .2696
0.8889
0.6290
0.7278
245.4
393.1
577.0
1006.9
1732.2
2427.0
ppb calc.
1664.1
1712.9
1576.9
1630.2
1714.3
1199.9
848.7
982.2



Sample #
9
10
11
12
13
14
dil. Factor ppb in sol
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
16641.4
17129.2
15768.5
16302.3
17142.7
23997.3
33947.6
19643.8


1.8- 	 -^A 	
y = 0.0007x+ 0.0009 ^^








0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
16596.8 582.29 2.5137 16.6414 827.9809 815.3 30.6
2.5016 17.1292 840.0165
2.5146 15.7685 769.4911
2.5031 16.3023 799.0276
2.5034 17.1427 840.1259
2.5112 23.9973 1172.7190
% recovery Range 2.4527 33.9476 1697.3265
83.5 85-115% K2Cr2O7 Cr added
added (mg) |jg/g dry
ugh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). #6 0.5052 246.841
% recovery Range
0.8086
-0.0200
Tare
1091
-28
Tin + Soil
19.8132 22.8038
19.7520 23.0542
19.7401 22.9840
109.7
wet
2.9906
3.3022
3.2439
80-120% PbCrO4 Cr added
Added (mg) |jg/g dry
#7 10.9 877.3
Tin + Soil dry %moisture mean % Solid
22.2560
22.4510
22.3705
2.4428 18.317
2.6990 18.267 18.499 81.501
2.6304 18.912
                                                                 Spike Recovery %
                                                                 Solution    Range
                                                                    145    75-125%

                                                                 Spike Recovery %
                                                                 Solid       Range
                                                                    101     75-125%
C27

-------
Cr Soil Extraction
T=14day
12763-126D
Frontier Hard Chrome,
Chrome VI dige:
Sample/STD
Blank
254
407
623
995
1642
2487
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 5+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
-20oC
Moisture A
Moisture B
Moisture C
1/23/2003
Sandy Soil
ition assay
A540 ppb calc.
0.0000
0.2408
0.3927
0.5761
0.7775
1 .2693
1 .8534
0.00071
0.092824
0.998129
1.2149
1.1608
0.8472
0.6144
1.2611
1 .3042
0.8294
0.6100
0.7766
0.7726

0.7831
0.1247
Tare
208.3
422.1
680.3
963.7
1656.0
2478.2
ppb calc.
1579.4
1503.3
1061.8
734.2
1644.4
1705.1
1036.8
728.0
962.5
956.8
972
45
Tin + Soil
19.8140 23.0900
19.7528 22.2393
19.7412 23.8372
Tare Tin + Soil
18.6709 22.3224
18.5904 23.2159
18.3910 21.3296


Sample #
9
10
11
12
13
14
dil. Factor
10.0
10.0
20.0
40.0
10.0
10.0
20.0
40.0
20.0
20.0
% Recover}
97.7
wet
3.2760
2.4865
4.0960
wet
3.6515
4.6255
2.9386
ppb in sol
15794.2
15032.7
21237.0
29366.5
16444.5
17051.2
20735.9
29118.8 c
19249.5
19136.9
Range
80-120%
Tin + Soil d
22.5138
21.8014
23.0768

o _, 	 „
y = 0.0007X + 0.0928
18' R2 = 0.9981 ^S
0.8 - ^f
0.6- pS
0.4- tf
0.2 - *
0 500 1000 1500 2000 2500 3000

Sample Cone.
ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
15413.4 538.46 2.4981 15.7942 770.3265 770.6 0.4
2.5043 15.0327 770.9333
2.4990 21.2370 1046.1578
ave5&6 STD DEV 2.4857 29.3665 1439.0202 ave 5&6 STD DEV
16747.8 428.98 2.4976 16.4445 805.2203 819.7 20.5
2.4999 17.0512 834.1691
2.4959 20.7359 1015.9818
/o Recovery Range 2.4964 29.1188 1480.9667
86.4 85-115% 2.5043 19.2495 936.2300
67.3 85-115% 2.4999 19.1369 936.1486
K2Cr2O7
0.972 added (mg)
0.045 4°C 0.5
-20' C 0.5
ry %moisture mean % Solid
2.6998 17.5885
2.0486 17.6111 17.921 82.079 PbCrO4
3.3356 18.5645 Added (mg)
4'C 11.7
Tin + Soil dry %moisture mean % Solid -20°C 11.1
21 .6498
22.3889
20.7896
2.9789 18.4198
3.7985 17.8791 18.225 81.775
2.3986 18.3761
                                                        Cr added  Spike Recovery %
                                                        |jg/g dry   Solution   Range
                                                          228        121    75-125%
                                                          246        80    75-125%
                                                        Cr added   Spike Recovery %
                                                        |jg/g dry   Solid     Range
                                                          922.6       72    75-125%
                                                          874.8       76    75-125%
C28

-------
Cr Soil Extraction
T=28 day J2/6/2003
12763-126D
Frontier Hard Chrome, Sandy Soil

Chrome VI digestion assay

Sample/STD A540 ppb calc.
Blank
250
401
619
987
1614
2471
0.0000
0.1409
0.2392
0.5441
0.6960
1.1155
1 .6641
177.2
323.2
776.0
1001.6
1624.6
2439.3

slope 0.000673
intercept 0.021589
RSQ 0.98967

Sample: ppb calc.
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 2+spk
Sample 6+spk
1 .3283
1 .2370
0.8030
0.5449
1.2311
1.1374
0.7613
0.5448
0.7331
0.6846
1940.6
1805.0
1160.5
777.2
1796.2
1657.1
1098.5
777.0
1056.7
984.6









Sample #
9
10
11
12
13
14




1 8 i
1.6 -
1.4 -
1.2 -
1 -
0.8 -

0.6-
0.4-

0.2 -
Q
R2 = 0.9897 ./*
;T
./
.s
tf
+^r
^S
.g
•











0 500 1000 1500 2000 2500 3000
















Sample Cone.
dil. Factor ppb in sol ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
10.0
10.0
20.0
40.0
10.0
10.0
20.0
40.0
20.0
20.0
19405.8 18727.8 958.75 2.7612 19.4058 854.6062 867.6 18.3
18049.9 2.4927 18.0499 880.5297
23209.3 2.4964 23.2093 1130.5896
31086.5 ave5&6 STD DEV 2.4940 31.0865 1590.0454 ave 5&6 STD DEV
17962.3 17266.5 983.96 2.4945 17.9623 893.2512 874.2 27.0
16570.8 2.4945 16.5708 855.0766
21970.7 2.5001 21.9707 1143.1141
31080.5 % Recovery Range 2.4973 31.0805 1541.2779
21133.1 77.1 85-115% 2.4927 21.1331 1031.2855
19692.6 78.0 85-115% 2.4945 19.6926 973.1411
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
% Recover}  Range
   102.2    80-120%
   3.2216
   2.9445
   3.3058
dry
   4.9713
   4.5750
   6.2578
  1.024
  -0.003

%moisture
 17.6777
 17.9371
 17.6740

%moisture
 18.1099
 18.7129
 19.7028
                                                                  K2Cr2O7
                                                                  added (mg)
                                                           4°C        0.5
                                                          -20' C       0.5
mean

17.763


mean

18.842
% Solid

82.237


% Solid

81.158
 4'C
-20°C
  PbCrO4
Added (mg)
   11.6
   10.3
                     Cr added  Spike Recovery %
                     |jg/g dry  Solution   Range
                       245       107    75-125%
                       249       108    75-125%
                                                                                                   Cr added  Spike Recovery %
                                                                                                   |jg/g dry   Solid     Range
                                                                                                     910.0       79    75-125%
                                                                                                     817.6       82    75-125%
                                                                                C29

-------
Cr Soil Extraction
T=56 day J3/6/2003 |
12763-126D
Frontier Hard Chrome, Sandy Soil




Chrome VI digestion assay


Sample/STD A540 ppb calc. Sample #

Blank
253
401
621
989
1620
2476
0.0000
0.2021
0.3690
0.4857
0.8469
1.2156
1 .7892

184.6 9
421.9 10
587.7 1 1
1101.1 12
1625.2 13
2440.5 14

slope 0.000704
intercept 0.0722

2
1.8 -

1.6 -
1.4-
1.2 -
1 -

0.8 -
0.6-
0.4-

0.2 -
Q
y = 0.0007X + 0.0722
R2 = 0.9945 >^
^S
yS
*r
.S
^r
^^
^S
S*
J'
*














0 500 1000 1500 2000 2500 3000


















RSQ 0.994464
Sample Cone.
Sample: ppb calc. dil. Factor ppb in sol ave 4°C STD DEV wet mass ppm Calc. |jg/g dry ave 4°C STD DEV
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
4°C#17
4°C#18
4°C#19
Sample 1+spk
Sample 6+spk
1 .2409
1.2105
0.8514
0.6129
1 .2528
1 .2638
0.8705
0.6106
1 .2692
1 .2563
1.1188
0.7658
0.7915
1661.2
1618.0
1107.5
768.5
1678.1
1693.7
1134.7
765.3
1701.4
1683.1
1487.6
985.9
1022.4
10.0
10.0
20.0
40.0
10.0
10.0
20.0
40.0
10.0
10.0
10.0
20.0
20.0
16611.7 16302.4 855.88 2.4933 16.6117 811.5936 802.2 42.1
16179.6 2.4875 16.1796 792.5880
22150.8 2.4924 22.1508 1115.5730
30741.6 ave5&6 STD DEV 2.4889 30.7416 1505.0720 ave 5&6 STD DEV
16780.8 16859.0 110.56 2.4846 16.7808 848.8661 844.3 6.5
16937.2 2.4861 16.9372 839.6401
22693.8 2.4873 22.6938 1124.4287
30610.9 % Recovery Range 2.4925 30.6109 1529.9316
17013.9 2.4950 17.0139 840.1507
16830.6 2.4919 16.8306 832.1520
14876.2 2.4950 14.8762 734.6224
19717.4 77.6 85-115% 2.4875 19.7174 965.4305
20448.0 87.8 85-115% 2.4861 20.4480 1013.3662
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
Tare
              1125
               -51
Tin + Soil
            % Recovery   Range
               113.3   80-120%


1
3.7865
3.9428
3.9159
i
4.5854
1 .4971
3.3396
1.125
-0.051
%moisture mean
17.7617
18.0904 17.928
17.9315
%moisture mean
18.1778
18.8959 18.865
19.5219


% Solid

82.072

% Solid

81.135

       K2Cr2O7
       added (mg)
 4'C         0.5
-20-C       0.5
Cr added  Spike Recovery %
|jg/g dry   Solution   Range
  246        127   75-125%
  250        112   75-125%
                                                                                                     4°C
                                                                                                    -20°C
                                                                                                    PbCrO4
                                                                                                  Added (mg)
                                                                                                      10.4
                                                                                                      10
                     Cr added
                     M9/9 dry
                      819.1
                      795.6
          Spike Recovery %
          Solid     Range
             86    75-125%
             86    75-125%
                                                                               C30

-------
Cr Soil Extraction
T=112day |5/1/2003
12763-126D
Frontier Hard Chrome, Sandy Soil

Chrome VI digestion assay

Sample/STD A540 ppb calc.
Blank
145
296
520
898
1510
2399
0.0000
0.2077
0.3087
0.5501
0.8045
1.1673
1 .6300
55.9
216.2
599.5
1003.4
1579.4
2314.0

slope 0.00063
intercept 0.172512
RSQ 0.988215

Sample: ppb calc.
4'C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20° C #7 sol
-20° C #8 insol
Sample 1+spk
Sample 6+spk
1 .2450
1 .2387
0.7477
0.5816
1 .2354
1 .2227
0.8187
0.7906
0.7635
0.7283
1702.7
1692.7
913.2
649.5
1687.5
1667.3
1025.9
981.3
938.3
882.4









Sample #
9
10
11
12
13
14




1.8 -,
1.6 -
1.4 -
1.2 -
1 -
0.8 -

0.6-
0.4-

0.2 -
Q

y = 0.0006x + 0.1725
R2 = 0.9882 >"*
^T
»/
+S
-n/^
j/r
^S
^»
•












0 500 1000 1500 2000 2500 3000
















Sample Cone.
dil. Factor ppb in sol ave1&2 STD DEV wet mass ppm Calc. |jg/g dry ave1&2 STD DEV
10.0
10.0
20.0
40.0
10.0
10.0
20.0
40.0
20.0
20.0
17027.5 16977.5 70.73 2.5446 17.0275 826.7163 832.8 8.7
16927.5 2.4939 16.9275 838.9651
18264.1 2.4843 18.2641 1012.0140
25979.8 ave5&6 STD DEV 2.4838 25.9798 1500.7659 ave 5&6 STD DEV
16875.1 16774.3 142.58 2.5829 16.8751 792.0368 798.5 9.1
16673.5 2.5112 16.6735 804.9542
20518.6 2.5455 20.5186 977.1581
39252.6 % Recovery Range 2.5434 39.2526 1870.8486
18765.8 43.5 85-115% 2.4939 18.7658 929.9245
17648.1 24.4 85-115% 2.5112 17.6481 850.8789
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
% Recover}  Range
   104.5    80-120%
                       1.0406
                       1.3325
                       1.6228
                    dry
                      2.3279
                      1.2347
                      1.4411
  0.927
  -0.231

%moisture
 18.8932
 18.7995
 19.6952

%moisture
 16.0058
 18.2101
 18.4760
                                         K2Cr2O7
                                         added (mg)
                                  4'C        0.4
                                 -20'C       0.4
mean

19.129


mean

17.564
% Solid

80.871


% Solid

82.436
 4'C
-20'C
  PbCrO4
Added (mg)
   13.7
   16.6
                                           Cr added  Spike Recovery %
                                           |jg/g dry  Solution   Range
                                             192        93    75-125%
                                             191         94    75-125%
Cr added  Spike Recovery %
|jg/g dry   Solid      Range
 1097.3      61     75-125%
 1273.8      84     75-125%
                                                                                C31

-------
Cr Soil Extraction
T=224 day             [8/26/2003    \
12763-126D
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD    A540
Blank
           294
           379
           721
          1213
          1672
          2818
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4° C #3 sol
4°C#4insol
-20° C #5
-20° C #6
-20°C #7 sol
-20°C #8 insol
Sample 2+spk
Sample 5+spk
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C

-20oC
Moisture A
Moisture B
Moisture C
 0.0000
 0.2379
 0.3024
 0.5668
 0.9524
 1.2792
 2.0259
0.000712
 0.05145
0.997998
 0.6519
 0.7468
 0.7192
 0.7521
 0.7381
 0.7746
 0.6245
 0.7497
 0.6426
 0.6577
           ppb calc.   Sample #
 261.7
 352.2
 723.3
 1264.6
 1723.3
 2771.3
     9
    10
    11
    12
    13
    14
ppb calc.
 842.8
 976.0
 937.3
 983.4
 963.8
 1015.0
 804.3
 980.1
 829.7
 850.9
                      dil. Factor
16.0
16.0
32.0
32.0
16.0
16.0
32.0
32.0
32.0
32.0
ppb in sol
 13484.6
 15615.8
 29992.0
 31469.7
 15420.4
 16240.1
 25738.6
 31361.9
 26551.5
 27229.7
                                                             2 -
                                                            1.5 -
            0.5 -
                                                         y = 0.0007x + 0.0514
                                                             R2 = 0.998
                                                              0       500     1000     1500     2000
                                                                                                     2500
                                                                                                             3000
  ave 1 &2
  14550.2
  ave 5&6
  15830.3
STD DEV
 1507.00
STD DEV
  579.61
% Recovery
   82.8
   89.5
  Range
 85-115%
 85-115%
Sample Cone.
  wet mass
   2.4381
   2.5065
   2.4491
   2.5723
   2.4834
   2.4803
   2.4735
   2.5209
   2.5065
   2.4803
ppm Calc.
 13.4846
 15.6158
 29.9920
 31.4697
 15.4204
 16.2401
 25.7386
 31.3619
 26.5515
 27.2297
                     % Recover}  Range
                        102.5    80-120%
1.162
-0.065
%moisture
19.0261
18.1984
18.7909
%moisture
16.8091
16.5514


mean

18.672

mean

16.680


% Solid

81 .328

% Solid

83.320
 M9/9 dry
846.3754
943.4850
1607.5283
1605.9017
865.8760
825.3510
1545.7100
1697.3965
1101.3956
1374.5810
ave 1 &2
 894.9
ave 5&6
 845.6
STD DEV
    68.7
STD DEV
    28.7
                                                                                              K2Cr2O7
                                                                                              added (mg)
                                                                                        4°C        1.5
                                                                                       -20'C       1.5
                                                                                                   4'C
                                                                                                  -20°C
                                                                                                 PbCrO4
                                                                                               Added (mg)
                                                                                                  10.2
                                                                                                  11.5
                                                                                              Cr added  Spike Recovery %
                                                                                               |jg/g dry  Solution   Range
                                                                                                 749       95     75-125%
                                                                                                 726       96     75-125%
                                                                                              Cr added  Spike Recovery %
                                                                                               |jg/g dry  Solid      Range
                                                                                                784.4      91     75-125%
                                                                                                880.9      97     75-125%
                                                                              C32

-------
Cr Soil Extraction
T=0 day
Soil 138
Bradford Soil
Chrome VI digest
Sample/STD
Blank
150
400
625
1000
1625
2500
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike
Insol Spike
ion assay
A540
0.0000
0.1153
0.2974
0.4730
0.7693
1.1528
1 .7038
0.000675
0.043485
0.997348
0.3076
0.1903
0.2181
0.2054
0.2093
0.2343
0.2386

ppb calc.
-64.4
106.4
376.3
636.6
1075.7
1644.1
2460.8
ppb calc.
391.4
217.6
258.8
240.0
245.8
282.8
289.2








y = 0.0007X + 0.0224
R' = 0.9967 .^
/
S
/
/
'
0 200 400 600 800 1000 1200 1400 1600 18
00
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg/g dry
270.7 69.12 2.5134 0.3914 22.9857
2.5388 0.2176 12.6493
2.5033 0.2588 15.2579
2.5076 0.2400 14.1239
2.5286 0.2458 14.3440
2.5130 0.2828 16.6091
2.5251 0.2892 16.9020



TOC in sediment
16.24%
au DOC in five extracts (mg/L)
Sample 1 0.3076 419
Sample 2 0.1903 391
Samples 0.2181 372
Sample 4 0.2054 393
Sample 5 0.2093 390
Ave. 393
SD 16.8077363
ave 1-5 STD DEV
15.9 4.1
K2Cr2O7 Cr added Spike Recovery %
added (mg^ |jg/g dry Solution
0.1 58.729 1
LCS
Blank
Moisture A
Moisture B
Moisture C
0.8513
0.1069
1197
 94
Tare
19.8142
19.7399
19.5213
Tin + Soil
22.2120
22.1210
21.7092
wet
2.3978
2.381 1
2.1879
Tin + Soil
21 .4433
21 .3484
21 .0042


dry
1 .6291
1 .6085
1 .4829
1.197
0.094
%moisture mean
32.0586
32.4472 32.243
32.2227


% Solid

67.757

  PbCrO4   Cr added   Spike Recovery %
Added (nig)   |jg/g dry   Solid
I    20    I    18.8         5
                                                                                 C32

-------
Cr Soil Extraction
Re-extraction of soil 138 do to extremely
low soluble and insoluble spike recoveries

Bradford Soil

Chrome VI digestion assay
Sample/STD
Blank
250
400
625
1000
1625
2500
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike
Insol Spike
LCS
A540
0.0000
0.2603
0.3762
0.5207
0.7926
1 .2507
1.8154
0.000695
0.095052
0.999353

0.3635
0.2632
0.2945
0.2109
0.2520
0.1565
0.2325
0.8315
ppb calc.
-136.8
237.9
404.7
612.8
1004.2
1663.7
2476.7
ppb calc.
386.5
242.1
287.1
166.8
225.9
88.5
197.9
1060
Blank 0.0720 -33
Moisture A
Moisture B
Moisture C
Tare Tin + Soil
18.5202 19.5716
18.5027 19.6391
18.4899 19.7410
y = 0.0007X + 0.0803
    R2 = 0.9997
                                                                  z
                                                       0    200    400   600   800   1000   1200   1400   1600   1800
                                                                                 Sample Cone.
ave1-5 STDDEV
261.7 81.99






wet mass
2.5340
2.5749
2.5343
2.5283
2.5492
2.5719
2.5797
ppm Calc.
0.3865
0.2421
0.2871
0.1668
0.2259
0.0885
0.1979
M9/9 dry
22.0621
13.5995
16.3895
9.5423
12.8217
4.9756
1 1 .0959


dry
0.7250
0.7807
0.8724
1.060
-0.033
%moisture
31 .0443
31 .3006
30.2694


mean

30.871

                                                                                                ave 1-5
                                                                                                 14.9
                                    STD DEV
                                       4.7
                                                                                                                    K2Cr2O7    Cr added   Spike Recovery %
                                                                                                                    added (mg'   |jg/g dry   Solution
                                                                                                                   I    0.1    I    56.246       -18
                                                                                                                     PbCrO4    Cr added   Spike Recovery %
                                                                                                                   Added (mg)   |jg/g dry   Solid
                                                                                                                   I    11.6        10.5         -36
                                                                                                % Solid

                                                                                                69.129
                                                                                  C34

-------
                           Appendix D

          Chromate [Cr(VI)] Soil Extract Holding Time
Chromate [Cr(VI)] extract holding time data for soil extracts from 125A,
125B, 125C, and 126D

The laboratory control sample (LCS), soluble (K2Cr2O7) and insoluble
(PbCrO4) spikes, and the extract (K2Cr2O7) spike are listed in red for each
extraction along with the permissible QA/QC range. The soluble and
insoluble spike solutions were original to the initial extraction, but were
carried through the entire extract storage study as an additional check. The
solution spike and LCS were produced at each analysis point in this study.
                                 Dl

-------
D2

-------
i =u day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2358
0.3513
0.5624
0.8051
1 .2446
2.0481
0.000712
0.0354
0.999635
0.2286
0.2222
0.2785
0.4836
0.2475
0.5296
0.5345
0.3737
9/1 0/2003
storage = 4 C
ppb calc.
281.3
443.4
739.7
1080.3
1697.1
2824.9
ppb calc.
271.2
262.2
341.2
629.1
297.7
693.6
700.5
474.8
Day 1 Color
Sample #
9
10
11
12
13
14
dil. Factor
4
4
4
4
4
16
16
16
ppb in sol
1084.6
1048.7
1364.8
2516.2
1190.7
11097.9
11207.9
7596.9


>*
^^
R2 = 0 9996 ^^^^
^^
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg/g dry
1441.0 613.48 2.5422 1.0846 78.9476
2.5219 1.0487 74.8173
2.5169 1.3648 110.1043
2.5701 2.5162 184.4395
2.5415 1.1907 87.1019
2.5043 11.0979 773.9919
% recovery Range 2.4832 11.2079 1006.2799
96.3 85-115%
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9551
0.0058
Tare
1291
-42
Tin + Soil
0.9835 2.5068
0.9838 2.3479
0.9745 2.5483
101.8
wet
1 .5233
1 .3641
1 .5738
80-120%
Tin + Soil dry %moisture mean % Solid
2.2807
2.1500
2.3202
1.2972 14.843
1.1662 14.508 14.615 85.385
1.3457 14.494
                                   ave 1-5  STD DEV
                                   107.1
45.3
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   1.4893    696.487
        Spike Recovery %
        Solution      Range
            96     75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry  Solid        Range
                                    13.1       994.0        90     75-125%
D3

-------
T=0 day
12763-125A
Boom Snub 0.5'
         [9/12/2003     |Day3CoJor
          storage = 4 C
Chrome VI digestion assay
Sample/STD
A540
ppb calc.    Sample #
Blank
            297
            455
            730
           1072
           1669
           2843
slope
intercept
RSQ
0.0000
0.2254
0.3483
0.5482
0.8081
1 .2204
1 .9832

264.2
442.4
732.1
1108.9
1706.6
2812.4
0.00069
0.043155
0.998912
                                 9
                                10
                                11
                                12
                                13
                                14
                                                                               Sample Cone.
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                        "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1306
               -54
              103.0    80-120%
Tare
0.9835
0.9838
0.9745
Tin + Soil
2.5068
2.3479
2.5483
wet
1 .5233
1 .3641
1 .5738
Tin + Soil
2.2807
2.1500
2.3202
dry
1 .2972
1.1662
1 .3457
%moisture
14.843
14.508
14.494
                                                                                           % Solid
                                                                  14.615    85.385
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
0.4092
0.4117
0.5215
0.9009
0.4441
0.5268
0.5226
0.7162
530.6
534.3
693.4
1243.4
581.2
701.1
695.0
975.7
2
2
2
2
2
16
16
8
1061.3
1068.5
1386.9
2486.9
1162.5
11217.8
11120.4
7805.4
ave 1-5
1433.2





% recovery
99.1
STD DEV
603.52





Range
85-115%
wet mass
2.5422
2.5219
2.5169
2.5701
2.5415
2.5043
2.4832

ppm Calc.
1.0613
1 .0685
1 .3869
2.4869
1.1625
11.2178
11.1204

M9/9 dry
77.2469
76.2307
1 1 1 .8859
182.2870
85.0328
782.3584
998.4249

                                                                                                                ave 1 -5
                                                                                                                 106.5
                                                                                                         STD DEV
                                                                                                            44.7
                                                                                               K2Cr2O7    Cr added
                                                                                               added (mg)  |jg/g dry
                                                                                                 1.4893    696.487
                                                                                                PbCrO4
                                                                                              Added (mg)
                                                                                                  13.1
                                                                                              Cr added
                                                                                              M9/9 dry
                                                                                               994.0
                                                                                                       Spike Recovery %
                                                                                                       Solution     Range
                                                                                                           97     75-125%
Spike Recovery %
Solid        Range
    90     75-125%
                                                                              D4

-------
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
-0.0001
0.2190
0.3459
0.5480
0.7965
1 .2092
1.9816
0.00069
0.037455
0.999208
0.4371
0.4168
0.5240
0.8972
0.4633
0.5316
0.5391
0.7322
9/16/2003
Storage = 4 C
ppb calc.
263.1
447.1
740.0
1100.2
1698.3
2817.9
ppb calc.
579.2
549.8
705.2
1246.1
617.2
716.2
727.1
1007.0
Day 7 Color
Sample #
9
10
11
12
13
14
dil. Factor
2
2
2
2
2
16
16
8
ppb in sol
1158.5
1099.7
1410.4
2492.2
1234.4
11459.5
11633.4
8055.8



S^*
R2 = 0 9992 ^^^^
^^
X
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1479.0 578.32 2.5422 1.1585 84.3237 109.9 42.8
2.5219 1.0997 78.4518
2.5169 1.4104 113.7853
2.5701 2.4922 182.6821
2.5415 1.2344 90.2989
2.5043 11.4595 799.2125
% recovery Range 2.4832 11.6334 1044.4843
102.3 85-115%
K2Cr2O7 Cr added
added (mg) |jg/g dry
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). 1 .4893 696.487
% recovery Range
0.9267
0.0057
Tare
1289
-46
Tin + Soil
0.9835 2.5068
0.9838 2.3479
0.9745 2.5483
101.7
wet
1 .5233
1 .3641
1 .5738
80-120%
Tin + Soil
2.2807
2.1500
2.3202
PbCrO4 Cr added
dry %moisture mean % Solid Added (mg) |jg/g dry
1.2972 14.843 13.1 994.0
1.1662 14.508 14.615 85.385
1.3457 14.494
                                                      Spike Recovery %
                                                      Solution     Range
                                                          99     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          94     75-125%
D5

-------
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2397
0.3639
0.5714
0.8409
1 .2847
2.1014
0.000732
0.038247
0.999359
0.4548
0.4352
0.5370
0.9319
0.4737
0.5496
0.5483
0.7779
9/23/2003
Storage = 4 C
ppb calc.
275.2
444.9
728.4
1096.6
1702.9
2818.6
ppb calc.
569.1
542.3
681.4
1220.9
594.9
698.6
696.8
1010.5
Day 14 Colo
Sample #
9
10
11
12
13
14
dil. Factor
2
2
2
2
2
16
16
8
r
ppb in sol
1138.2
1084.6
1362.8
2441 .8
1189.8
11177.5
11149.1
8083.9


s+
l c y = 0 OOOTx + 0 0382 ^^^
R2 = 0 9994 ^^^
/
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1443.4 567.77 2.5422 1.1382 82.8438 107.2 42.0
2.5219 1.0846 77.3788
2.5169 1.3628 109.9418
2.5701 2.4418 178.9822
2.5415 1.1898 87.0335
2.5043 11.1775 779.5483
% recovery Range 2.4832 11.1491 1001.0024
102.9 85-115%
K2Cr2O7 Cr added
added (mg) |jg/g dry
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). 1 .4893 696.487
% recovery Range
0.9867
0.0046
Tare
1296
-46
Tin + Soil
0.9835 2.5068
0.9838 2.3479
0.9745 2.5483
102.2
wet
1 .5233
1 .3641
1 .5738
80-120%
Tin + Soil
2.2807
2.1500
2.3202
PbCrO4 Cr added
dry %moisture mean % Solid Added (mg) |jg/g dry
1.2972 14.843 13.1 994.0
1.1662 14.508 14.615 85.385
1.3457 14.494
                                                      Spike Recovery %
                                                      Solution     Range
                                                          97     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          90     75-125%
D6

-------
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2409
0.3640
0.5719
0.8369
1.2718
2.0641
0.000717
0.047574
0.999082
0.4469
0.4308
0.5380
0.9370
0.4821
0.5425
0.5450
0.7486
10/7/2003
Storage = 4 C
ppb calc.
269.8
441.5
731.6
1101.4
1708.3
2813.9
ppb calc.
557.2
534.8
684.3
1241.1
606.3
690.6
694.1
978.2
Day 28 Colo
Sample #
9
10
11
12
13
14
dil. Factor
2
2
2
2
2
16
16
8
r
ppb in sol
1114.4
1069.5
1368.7
2482.2
1212.7
11050.0
11105.8
7825.7


>»
! c V = 0 0007X + 0 0476 ^^^
R3 = 0 9991 ^^^^
j/r
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg/g dry
1449.5 588.60 2.5422 1.1144 81.1171
2.5219 1.0695 76.3015
2.5169 1.3687 110.4195
2.5701 2.4822 181.9473
2.5415 1.2127 88.7066
2.5043 1 1 .0500 770.6507
% recovery Range 2.4832 11.1058 997.1106
99.4 85-115%
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9801
0.0046
Tare
1301
-60
Tin + Soil
0.9835 2.5068
0.9838 2.3479
0.9745 2.5483
102.7
wet
1 .5233
1 .3641
1 .5738
80-120%
Tin + Soil dry %moisture mean % Solid
2.2807
2.1500
2.3202
1.2972 14.843
1.1662 14.508 14.615 85.385
1.3457 14.494
                                   ave 1 -5
                                   107.7
STD DEV
    43.5
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   1.4893    696.487
           Spike Recovery %
           Solution     Range
               95     75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry   Solid        Range
                                    13.1       994.0        89     75-125%
D7

-------
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
#2 + spike
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2429
0.3687
0.5690
0.8361
1 .2609
2.0970
0.000727
0.039858
0.999746
0.4512
0.4265
0.5425
0.9434
0.4842
0.5349
0.5325
0.7465
11/4/2003
storage = 4 C
ppb calc.
279.4
452.5
728.1
1095.7
1680.2
2830.7
ppb calc.
566.0
532.0
691.7
1243.3
611.4
681.2
677.9
972.4
Day 56 Colo
Sample #
9
10
11
12
13
14
dil. Factor
2
2
2
2
2
16
16
8
r
ppb in sol
1132.0
1064.1
1383.3
2486.6
1222.9
10899.1
10846.3
7778.9


>*
1 c y = 0 0007x + 0 0399 .^^
R2 = 0 9997 ^^^
/-
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg/g dry
1457.8 587.44 2.5422 1.1320 82.3979
2.5219 1.0641 75.9129
2.5169 1.3833 111.5988
2.5701 2.4866 182.2689
2.5415 1.2229 89.4512
2.5043 10.8991 760.1299
% recovery Range 2.4832 10.8463 973.8112
98.7 85-115%
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9744
0.0051
Tare
1286
-48
Tin + Soil
0.9835 2.5068
0.9838 2.3479
0.9745 2.5483
101.5
wet
1 .5233
1 .3641
1 .5738
80-120%
Tin + Soil dry %moisture mean % Solid
2.2807
2.1500
2.3202
1.2972 14.843
1.1662 14.508 14.615 85.385
1.3457 14.494
                                  ave 1 -5
                                   108.3
STD DEV
    43.5
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   1.4893    696.487
           Spike Recovery %
           Solution     Range
               94     75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry   Solid        Range
                                    13.1       994.0        87     75-125%
D8

-------
Storage = Rm Temperature
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2334
0.3886
0.4305
0.9979
1 .3584
2.1543
0.000688
0.047839
0.986947
0.7529
0.9641
0.9507
0.8134
0.7279
0.8668
0.7475
5/12/2003

ppb calc.
269.7
495.3
556.2
1380.9
1904.9
3061.7
ppb calc.
1024.8
1331.8
1312.3
1112.7
988.4
1190.3
1016.9
Day 1 Color
Sample #
9
10
11
12
13
14
dil. Factor
1.0
1.0
1.0
4.0
1.0
4.0
16.0
ppb in sol
1024.8
1331.8
1312.3
4450.9
988.4
4761 .3
16271.0


J
y = 0 OOOTx + 0 0478 ^^
R2 = 0 9869 ^f^
./'
y
S
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1164.3 182.87 2.4933 1.0248 70.6682 82.6 11.9
2.4908 1.3318 98.9546
2.5072 1.3123 79.5580
2.5478 4.4509 323.3490 This samplewas not used due to varience
2.5003 0.9884 81.0965 from the other 4 samples
2.4942 4.7613 311.4414
2.5240 16.2710 1104.5402
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4974 234.271 98 75-125%
0.9130
0.0087
Tare
1257
-57
Tin + Soil
0.9651 2.1051
0.9643 2.1118
0.9605 2.0522
108.2
wet
1.1400
1.1475
1.0917
80-120%
Tin + Soil
1 .9346
1 .9370
1 .8946
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
dry %moisture mean % Solid #7 13.3 995.9 103 75-125%
0.9695 14.956
0.9727 15.233 14.875 85.125
0.9341 14.436
                         D9

-------
                                                   Storage = Rm Temperature
T=0 day
12763-125A
Boom Snub 0.5'
         [5/14/2003     [Day 2 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            286
            476
            557
           1273
           2128
           2949
  0.0000
  0.254
  0.3920
  0.4319
  1.0071
  1.3406
  2.1616
slope
intercept
RSQ
 0.000683
 0.057988
 0.983728
ppb calc.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
0.8010
0.9914
0.9636
0.7244
0.7508
0.8742
0.7046
0.2672
1087.5
1366.2
1325.5
975.4
1014.1
1194.7
946.4
306.2
ppb calc.    Sample #
 286.9              9
 488.9             10
 547.3             11
 1389.2             12
 1877.3             13
 3079.0             14
                                                                                Sample Cone.
                                         dil. Factor  ppb in sol    ave 1-5   STD DEV  wet mass  ppm Calc.
1.0
1.0
1.0
4.0
1.0
4.0
16.0
16.0
1087.5
1366.2
1325.5
3901 .6
1014.1
4778.7
15142.9
4899.5
                                                               1198.3
                                                          173.78
                                                               i recovery
                                                                88.3
                                                          Range
                                                         85-115%
                                                      2.4933
                                                      2.4908
                                                      2.5072
                                                      2.5478
                                                      2.5003
                                                      2.4942
                                                      2.5240
 1.0875
 1.3662
 1.3255
 3.9016
 1.0141
 4.7787
15.1429
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                        "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1269
               -76
              109.2     80-120%
Tare
0.9651
0.9643
0.9605
Tin + Soil
2.1051
2.1118
2.0522
wet
1.1400
1.1475
1.0917
Tin + Soil
1 .9346
1 .9370
1 .8946
dry
0.9695
0.9727
0.9341
%moisture
14.956
15.233
14.436
                                                                                             % Solid
                                                                   14.875    85.125
 M9/9 dry
 74.9950
 101.5148
 80.3608
 283.4482
 83.1972
 312.5758
1027.9615
ave 1 -5
 85.0
STD DEV
    11.5
                                                                                                                This samplewas not used due to varience
                                                                                                                from the other 4 samples
                    K2Cr2O7    Cr added  Spike Recovery %
                    added (mg)   |jg/g dry   Solution      Range
                 #6  0.4974     234.271       97     75-125%

                     PbCrO4   Cr added  Spike Recovery %
                    Added (mg)   |jg/g dry   Solid        Range
                 #7    13.3       995.9        95     75-125%
                                                                               DIG

-------
                                                   Storage = Rm Temperature
T=0 day
12763-125A
Boom Snub 0.5'
         [5/16/2003     [Day 4 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            286
            476
            557
           1273
           2128
           2949
  0.0000
  0.2355
  0.3829
  0.4289
  0.9815
  1.4647
  2.1787
slope
intercept
RSQ
 0.000712
 0.035579
 0.996189
ppb calc.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
0.8142
0.9924
0.9949
0.7244
0.7324
0.8664
0.7142
0.2713
1093.8
1344.2
1347.7
967.7
978.9
1167.2
953.3
331.1
ppb calc.    Sample #
 280.9              9
 487.9             10
 552.6             11
 1328.9             12
 2007.7             13
 3010.7             14
                                                                     z
                                                                                Sample Cone.
                                         dil. Factor  ppb in sol    ave 1-5   STD DEV  wet mass  ppm Calc.
1.0
1.0
1.0
4.0
1.0
4.0
16.0
16.0
1093.8
1344.2
1347.7
3870.7
978.9
4668.7
15253.6
5298.4
                                                               1191.2
                                                          184.78
                                                               i recovery
                                                                98.9
                                                          Range
                                                         85-115%
                                                      2.4933
                                                      2.4908
                                                      2.5072
                                                      2.5478
                                                      2.5003
                                                      2.4942
                                                      2.5240
                                         1.0938
                                         1.3442
                                         1.3477
                                         3.8707
                                         0.9789
                                         4.6687
                                         15.2536
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                         "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1246
               -42
              107.2
80-120%
Tare
0.9651
0.9643
0.9605
Tin + Soil
2.1051
2.1118
2.0522
wet
1.1400
1.1475
1.0917
Tin + Soil
1 .9346
1 .9370
1 .8946
dry
0.9695
0.9727
0.9341
%moisture
14.956
15.233
14.436
                                                                                             % Solid
                                                                   14.875    85.125
 M9/9 dry
 75.4297
 99.8772
 81.7044
281.2011
 80.3146
305.3792
1035.4762
ave 1 -5
 84.3
STD DEV
    10.7
                                                                                                                This samplewas not used due to varience
                                                                                                                from the other 4 samples
          K2Cr2O7    Cr added  Spike Recovery %
          added (mg)  |jg/g dry  Solution      Range
       #6   0.4974    234.271      94      75-125%

            PbCrO4    Cr added  Spike Recovery %
          Added (mg)  |jg/g dry  Solid         Range
       #7    13.3      995.9       96      75-125%
                                                                               Dll

-------
                                                   Storage = Rm Temperature
T=0 day
12763-125A
Boom Snub 0.5'
         [5/20/2003     [Day 8 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            286
            476
            557
           1273
           2128
           2949
  0.0000
  0.2394
  0.3781
  0.4245
  0.9314
  1.3877
  2.1176
slope
intercept
RSQ
 0.000683
  0.04038
 0.994006
ppb calc.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
0.8085
0.9789
0.9588
0.7064
0.7178
0.8406
0.6805
0.2637
1124.9
1374.4
1345.0
975.4
992.1
1171.9
937.4
327.0
ppb calc.    Sample #
 291.5              9
 494.6             10
 562.5             11
 1304.9             12
 1973.1             13
 3042.0             14
                                                                                Sample Cone.
                                         dil. Factor  ppb in sol    ave 1-5   STD DEV  wet mass  ppm Calc.
1.0
1.0
1.0
4.0
1.0
4.0
16.0
16.0
1124.9
1374.4
1345.0
3901 .5
992.1
4687.6
14999.0
5232.7
                                                               1209.1
                                                          182.58
                                                               i recovery    Range
                                                                96.5     85-115%
                                                      2.4933
                                                      2.4908
                                                      2.5072
                                                      2.5478
                                                      2.5003
                                                      2.4942
                                                      2.5240
                                         1.1249
                                         1.3744
                                         1.3450
                                         3.9015
                                         0.9921
                                         4.6876
                                         14.9990
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                         "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1239
               -45
              106.6
80-120%
Tare
0.9651
0.9643
0.9605
Tin + Soil
2.1051
2.1118
2.0522
wet
1.1400
1.1475
1.0917
Tin + Soil
1 .9346
1 .9370
1 .8946
dry
0.9695
0.9727
0.9341
%moisture
14.956
15.233
14.436
                                                                                             % Solid
                                                                   14.875    85.125
 M9/9 dry
 77.5715
 102.1259
 81.5417
 283.4358
 81.3932
 306.6184
1018.1951
ave 1 -5
 85.7
STD DEV
    11.1
                                                                                                                This samplewas not used due to varience
                                                                                                                from the other 4 samples
          K2Cr2O7    Cr added  Spike Recovery %
          added (mg)  |jg/g dry  Solution      Range
       #6   0.4974    234.271      94      75-125%

            PbCrO4    Cr added  Spike Recovery %
          Added (mg)  |jg/g dry  Solid         Range
       #7    13.3      995.9       94      75-125%
                                                                               D12

-------
Storage = Rm Temperature
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2599
0.3818
0.4260
0.9594
1 .5371
2.0623
0.000685
0.062744
0.99936
0.8307
1 .0035
0.9956
0.6979
0.7400
0.8356
0.7121
0.2664
5/27/2003

ppb calc.
288.0
466.0
530.6
1309.7
2153.6
2920.7
ppb calc.
1121.7
1374.1
1362.6
927.8
989.3
1128.9
948.5
297.5
Day 15 Colo
Sample #
9
10
11
12
13
14
dil. Factor
1.0
1.0
1.0
4.0
1.0
4.0
16.0
16.0
r
ppb in sol
1121.7
1374.1
1362.6
3711.0
989.3
4515.6
15176.0
4759.6


>»
y = 0 0007X + 0 0627 ^f"
R2 = 0 9994 ^^^
1- JT
/
/
S
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1211.9 188.62 2.4933 1.1217 77.3538 85.8 11.1
2.4908 1.3741 102.1038
2.5072 1 .3626 82.6086
2.5478 3.71 1 0 269.6000 This samplewas not used due to varience
2.5003 0.9893 81.1624 from the other 4 samples
2.4942 4.5156 295.3654
% recovery Range 2.5240 15.1760 1030.2072
84.6 85-115%
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4974 234.271 89 75-125%
0.8837
0.0062
Tare
1199
-83
Tin + Soil
0.9651 2.1051
0.9643 2.1118
0.9605 2.0522
103.2
wet
1.1400
1.1475
1.0917
80-120%
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid #7 13.3 995.9 95 75-125%
1 .9346
1 .9370
1 .8946
0.9695 14.956
0.9727 15.233 14.875 85.125
0.9341 14.436
                         D13

-------
Storage = Rm Temperature
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2332
0.3906
0.4296
0.9977
1.6102
2.1590
0.000727
0.040784
0.9991 1
0.8204
1.0017
0.9833
0.7158
0.7346
0.8626
0.6990
0.2714
6/10/2003

ppb calc.
264.6
481.1
534.8
1316.1
2158.6
2913.4
ppb calc.
1072.3
1321.6
1296.3
928.4
954.3
1130.3
905.3
317.2
Day 29 Colo
Sample #
9
10
11
12
13
14
dil. Factor
1.0
1.0
1.0
4.0
1.0
4.0
16.0
16.0
r
ppb in sol
1072.3
1321.6
1296.3
3713.6
954.3
4521 .3
14484.8
5075.0


X*
R3 = 0 9991 ^f
,r

/*
s
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1161.1 177.70 2.4933 1.0723 73.9430 82.3 10.8
2.4908 1.3216 98.2022
2.5072 1 .2963 78.5906
2.5478 3.7136 269.7892 This samplewas not used due to varience
2.5003 0.9543 78.2920 from the other 4 samples
2.4942 4.5213 295.7376
% recovery Range 2.5240 14.4848 983.2889
93.8 85-115%
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4974 234.271 91 75-125%
0.921 1
0.0047
Tare
1211
-50
Tin + Soil
0.9651 2.1051
0.9643 2.1118
0.9605 2.0522
104.2
wet
1.1400
1.1475
1.0917
80-120%
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid #7 13.3 995.9 90 75-125%
1 .9346
1 .9370
1 .8946
0.9695 14.956
0.9727 15.233 14.875 85.125
0.9341 14.436
                         D14

-------
Storage = Rm Temperature
T=0 day
1 2763-1 25A
Boom Snub 0.5'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2359
0.3891
0.4294
0.9280
1.2810
2.1416
0.000672
0.04152
0.979978
0.8309
0.9958
0.9775
0.7319
0.7467
0.8555
0.7273
0.2735
7/1/2003

ppb calc.
289.1
517.0
576.9
1318.5
1843.5
3123.6
ppb calc.
1174.1
1419.3
1392.1
1026.8
1048.8
1210.7
1020.0
345.0
Day 57 Colo
Sample #
9
10
11
12
13
14
dil. Factor
1.0
1.0
1.0
4.0
1.0
4.0
16.0
16.0
r
ppb in sol
1174.1
1419.3
1392.1
4107.3
1048.8
4842.7
16319.9
5520.6


•
y = 0 OOOTx + 0 0415 ^^^
R2 = 0 98 ^^^
^^ +
/
S
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
1258.6 177.77 2.4933 1.1741 80.9638 89.2 11.0
2.4908 1.4193 105.4630
2.5072 1 .3921 84.3989
2.5478 4.1073 298.3920 This samplewas not used due to varience
2.5003 1 .0488 86.0521 from the other 4 samples
2.4942 4.8427 316.7628
% recovery Range 2.5240 16.3199 1107.8630
102.5 85-115%
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4974 234.271 97 75-125%
0.9148
0.0089
Tare
1299
-49
Tin + Soil
0.9651 2.1051
0.9643 2.1118
0.9605 2.0522
111.8
wet
1.1400
1.1475
1.0917
80-120%
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid #7 13.3 995.9 102 75-125%
1 .9346
1 .9370
1 .8946
0.9695 14.956
0.9727 15.233 14.875 85.125
0.9341 14.436
                         D15

-------
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1 (#16)
Sample 2 (#17)
Sample 3 (#18)
Sample 4 (#19)
Sample 5 (#20)
Sol Spike 6 (#21)
Insol Spike 7 (#22)
#2 + spike (#17)
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2358
0.3513
0.5624
0.8051
1 .2446
2.0481
0.000712
0.0354
0.999635
0.4502
0.341 1
0.4688
0.4083
0.5025
0.7871
0.7771
0.4777
9/10/2003
Storage = 4 C
ppb calc.
281.3
443.4
739.7
1080.3
1697.1
2824.9
ppb calc.
582.2
429.1
608.3
523.4
655.6
1055.0
1041.0
620.8
Day 1 Color
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
16
16
16
ppb in sol
4657.4
3432.4
4866.3
4187.0
5244.7
16880.3
16655.8
9932.4


-A
.S'
R2 = 0 9996 ^^^
^T
X
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4477.5 697.96 2.5123 4.6574 310.5684 326.1 36.8
2.5458 3.4324 305.8664
2.5507 4.8663 346.5099
2.5737 4.1870 287.7671
2.5132 5.2447 379.8420
2.5359 16.8803 1146.7139
% recovery Range 2.5385 16.6558 1274.5568
95.6 85-115%
K2Cr2O7 Cr added
added (mg) |jg/g dry
1.4895 710.451
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9551
0.0058
Tare
1291
-42
Tin + Soil
0.9822 2.1423
0.9934 2.1163
0.9845 2.1086
101.8
wet
1.1601
1.1229
1.1241
80-120%
Tin + Soil
1 .9375
1 .9220
1.9173
PbCrO4 Cr added
Added (mg) |jg/g dry
dry %moisture mean % Solid 12.7 973.6
0.9553 17.654
0.9286 17.303 17.325 82.675
0.9328 17.018
                                                      Spike Recovery %
                                                      Solution      Range
                                                         116     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          97     75-125%
D16

-------
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1 (#16)
Sample 2 (#17)
Sample 3 (#18)
Sample 4 (#19)
Sample 5 (#20)
Sol Spike 6 (#21)
Insol Spike 7 (#22)
#2 + spike (#17)
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.232
0.3418
0.5484
0.7904
1.2178
2.0119
0.0007
0.032325
0.999716
0.4359
0.3389
0.4523
0.4002
0.4874
0.7729
0.7553
0.9163
9/12/2003
Storage = 4 C
ppb calc.
285.1
441.9
737.0
1082.6
1692.9
2827.0
ppb calc.
576.3
437.8
599.8
525.3
649.9
1057.6
1032.5
1262.4
Day 3 Color
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
16
16
8
ppb in sol
4610.6
3502.5
4798.0
4202.8
5199.0
16921.4
16519.2
10099.0


^^

R2 = 0 9997 ^^^^
S^
X
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4462.6 645.38 2.5123 4.6106 307.4491 325.3 34.3
2.5458 3.5025 312.1070
2.5507 4.7980 341 .6494
2.5737 4.2028 288.8547
2.5132 5.1990 376.5360
2.5359 16.9214 1149.5028
% recovery Range 2.5385 16.5192 1264.1093
97.0 85-115% K2Cr2O7 Cr added
added (mg) |jg/g dry
1.4895 710.451
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9487
0.0038
Tare
1309
-41
Tin + Soil
0.9822 2.1423
0.9934 2.1163
0.9845 2.1086
103.3
wet
1.1601
1.1229
1.1241
80-120%
Tin + Soil
1 .9375
1 .9220
1.9173
PbCrO4 Cr added
Added (mg) |jg/g dry
12.7 973.6
dry %moisture mean % Solid
0.9553 17.654
0.9286 17.303 17.325 82.675
0.9328 17.018
                                                       Spike Recovery %
                                                       Solution      Range
                                                          116     75-125%
                                                       Spike Recovery %
                                                       Solid        Range
                                                           96     75-125%
D17

-------
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1 (#16)
Sample 2 (#17)
Sample 3 (#18)
Sample 4 (#19)
Sample 5 (#20)
Sol Spike 6 (#21)
Insol Spike 7 (#22)
#2 + spike (#17)
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
-0.0001
0.2190
0.3459
0.5480
0.7965
1 .2092
1.9816
0.00069
0.037455
0.999208
0.4254
0.3437
0.4572
0.3993
0.4930
0.7877
0.7586
0.9341
9/16/2003
Storage = 4 C
ppb calc.
263.1
447.1
740.0
1100.2
1698.3
2817.9
ppb calc.
562.3
443.9
608.4
524.5
660.3
1087.4
1045.2
1299.6
Day 7 Color
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
16
16
8
ppb in sol
4498.3
3551 .0
4867.1
4195.7
5282.2
17398.6
16723.7
10396.8



S^*
R2 = 0 9992 ^^^^
^^
X
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4478.8 659.07 2.5123 4.4983 299.9597 326.8 38.1
2.5458 3.5510 316.4313
2.5507 4.8671 346.5664
2.5737 4.1957 288.3669
2.5132 5.2822 382.5591
2.5359 17.3986 1181.9197
% recovery Range 2.5385 16.7237 1279.7580
100.7 85-115% K2Cr2O7 Cr added
added (mg) |jg/g dry
1.4895 710.451
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9267
0.0057
Tare
1289
-46
Tin + Soil
0.9822 2.1423
0.9934 2.1163
0.9845 2.1086
101.7
wet
1.1601
1.1229
1.1241
80-120%
Tin + Soil
1 .9375
1 .9220
1.9173
PbCrO4 Cr added
Added (mg) |jg/g dry
12.7 973.6
dry %moisture mean % Solid
0.9553 17.654
0.9286 17.303 17.325 82.675
0.9328 17.018
                                                      Spike Recovery %
                                                      Solution      Range
                                                         120     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          98     75-125%
D18

-------
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1 (#16)
Sample 2 (#17)
Sample 3 (#18)
Sample 4 (#19)
Sample 5 (#20)
Sol Spike 6 (#21)
Insol Spike 7 (#22)
#2 + spike (#17)
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2397
0.3639
0.5714
0.8409
1 .2847
2.1014
0.000732
0.038247
0.999359
0.4597
0.3613
0.4816
0.4217
0.5161
0.8174
0.8064
0.9856
9/23/2003
Storage = 4 C
ppb calc.
275.2
444.9
728.4
1096.6
1702.9
2818.6
ppb calc.
575.8
441.3
605.7
523.9
652.8
1064.5
1049.4
1294.2
Day 14 Colo
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
16
16
8
r
ppb in sol
4606.2
3530.8
4845.6
4190.9
5222.6
17031.3
16790.9
10354.0


s+
l c y = 0 OOOTx + 0 0382 ^^^
R2 = 0 9994 ^^^
/
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4479.2 649.17 2.5123 4.6062 307.1540 326.6 35.4
2.5458 3.5308 314.6287
2.5507 4.8456 345.0364
2.5737 4.1909 288.0377
2.5132 5.2226 378.2474
2.5359 17.0313 1156.9700
% recovery Range 2.5385 16.7909 1284.8944
100.3 85-115% K2Cr2O7 Cr added
added (mg) |jg/g dry
1.4895 710.451
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9867
0.0046
Tare
1296
-46
Tin + Soil
0.9822 2.1423
0.9934 2.1163
0.9845 2.1086
102.2
wet
1.1601
1.1229
1.1241
80-120%
Tin + Soil
1 .9375
1 .9220
1.9173
PbCrO4 Cr added
Added (mg) |jg/g dry
12.7 973.6
dry %moisture mean % Solid
0.9553 17.654
0.9286 17.303 17.325 82.675
0.9328 17.018
                                                      Spike Recovery %
                                                      Solution      Range
                                                         117     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          98     75-125%
D19

-------
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1 (#16)
Sample 2 (#17)
Sample 3 (#18)
Sample 4 (#19)
Sample 5 (#20)
Sol Spike 6 (#21)
Insol Spike 7 (#22)
#2 + spike (#17)
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2409
0.3640
0.5719
0.8369
1.2718
2.0641
0.000717
0.047574
0.999082
0.4510
0.3481
0.4665
0.4085
0.5021
0.8098
0.7926
0.9571
10/7/2003
Storage = 4 C
ppb calc.
269.8
441.5
731.6
1101.4
1708.3
2813.9
ppb calc.
562.9
419.4
584.6
503.6
634.2
1063.6
1039.6
1269.2
Day 28 Colo
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
16
16
8
r
ppb in sol
4503.5
3354.8
4676.6
4029.1
5074.0
17017.8
16633.8
10153.3


>»
! c V = 0 0007X + 0 0476 ^^^
R3 = 0 9991 ^^^^
j/r
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4327.6 660.53 2.5123 4.5035 300.3074 315.3 35.4
2.5458 3.3548 298.9523
2.5507 4.6766 333.0026
2.5737 4.0291 276.9176
2.5132 5.0740 367.4815
2.5359 17.0178 1156.0538
% recovery Range 2.5385 16.6338 1272.8760
100.0 85-115%
K2Cr2O7 Cr added
added (mg) |jg/g dry
1.4895 710.451
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9801
0.0046
Tare
1301
-60
Tin + Soil
0.9822 2.1423
0.9934 2.1163
0.9845 2.1086
102.7
wet
1.1601
1.1229
1.1241
80-120%
PbCrO4 Cr added
Added (mg) |jg/g dry
Tin + Soil dry %moisture mean % Solid 12.7 973.6
1 .9375
1 .9220
1.9173
0.9553 17.654
0.9286 17.303 17.325 82.675
0.9328 17.018
                                                      Spike Recovery %
                                                      Solution      Range
                                                         118     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          98     75-125%
D20

-------
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
297
455
730
1072
1669
2843
slope
intercept
RSQ
Sample 1 (#16)
Sample 2 (#17)
Sample 3 (#18)
Sample 4 (#19)
Sample 5 (#20)
Sol Spike 6 (#21)
Insol Spike 7 (#22)
#2 + spike (#17)
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2429
0.3687
0.5690
0.8361
1 .2609
2.0970
0.000727
0.039858
0.999746
0.4525
0.351 1
0.4652
0.4088
0.5029
0.7955
0.7783
0.9576
11/4/2003
Storage = 4 C
ppb calc.
279.4
452.5
728.1
1095.7
1680.2
2830.7
ppb calc.
567.8
428.3
585.3
507.7
637.2
1039.8
1016.1
1262.8
Day 56 Colo
Sample #
9
10
11
12
13
14
dil. Factor
8
8
8
8
8
16
16
8
r
ppb in sol
4542.5
3426.2
4682.3
4061 .4
5097.3
16636.6
16257.9
10102.7


>*
1 c y = 0 0007x + 0 0399 .^^
R2 = 0 9997 ^^^
/-
S
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4361.9 640.66 2.5123 4.5425 302.9033 318.0 34.5
2.5458 3.4262 305.3139
2.5507 4.6823 333.4088
2.5737 4.0614 279.1380
2.5132 5.0973 369.1693
2.5359 16.6366 1130.1570
% recovery Range 2.5385 16.2579 1244.1120
98.2 85-115%
K2Cr2O7 Cr added
added (mg) |jg/g dry
1.4895 710.451
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.9744
0.0051
Tare
1286
-48
Tin + Soil
0.9822 2.1423
0.9934 2.1163
0.9845 2.1086
101.5
wet
1.1601
1.1229
1.1241
80-120%
PbCrO4 Cr added
Added (mg) |jg/g dry
Tin + Soil dry %moisture mean % Solid 12.7 973.6
1 .9375
1 .9220
1.9173
0.9553 17.654
0.9286 17.303 17.325 82.675
0.9328 17.018
                                                      Spike Recovery %
                                                      Solution      Range
                                                         114     75-125%
                                                      Spike Recovery %
                                                      Solid        Range
                                                          95     75-125%
D21

-------
Storage = Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2334
0.3886
0.4305
0.9979
1 .3584
2.1543
0.000688
0.047839
0.986947
0.9482
0.7528
0.8375
0.6906
0.8253
0.8507
0.5777
5/12/2003

ppb calc.
269.7
495.3
556.2
1380.9
1904.9
3061.7
ppb calc.
1308.6
1024.6
1147.7
934.2
1130.0
1166.9
770.1
Day 1 Color
Sample #
9
10
11
12
13
14
dil. Factor
4.0
4.0
4.0
8.0
4.0
8.0
16.0
ppb in sol
5234.6
4098.6
4591 .0
7473.9
4520.1
9335.5
12322.2


J
y = 0 OOOTx + 0 0478 ^^
R2 = 0 9869 ^f^
./'
y
S
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
5331.8 1503.08 2.5409 5.2346 382.5974 406.4 30.2
2.5396 4.0986 421 .2475
3.5382 4.591 0 222.3626 This sample was not used due to breakage of
2.5497 7.4739 441.8130 filter apparatus and loss of sample
2.5537 4.5201 379.9068
2.5431 9.3355 584.5286
2.5017 12.3222 1127.4072
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4947 237.167 75 75-125%
0.9130
0.0087
Tare
1257
-57
Tin + Soil
0.9598 2.0633
0.9582 2.3249
0.9641 2.2875
108.2
wet
1.1035
1 .3667
1 .3234
80-120%
Tin + Soil
1 .8669
2.0777
2.0486
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
dry %moisture mean % Solid #7 11.7 917.4 79 75-125%
0.9071 17.798
1.1195 18.087 17.979 82.021
1.0845 18.052
                         D22

-------
                                                   Storage = Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
         [5/14/2003     [Day 2 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            286
            476
            557
           1273
           2128
           2949
  0.0000
  0.254
  0.3920
  0.4319
  1.0071
  1.3406
  2.1616
slope
intercept
RSQ
 0.000683
 0.057988
 0.983728
ppb calc.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
0.8743
0.7431
0.8359
0.6907
0.8331
0.8449
0.5917
0.3891
1194.8
1002.8
1138.6
926.1
1134.5
1151.8
781.2
484.6
ppb calc.    Sample #
 286.9              9
 488.9             10
 547.3             11
 1389.2             12
 1877.3             13
 3079.0             14
                                                                                Sample Cone.
                                         dil. Factor  ppb in sol   ave 1-5   STD DEV  wet mass  ppm Calc.   |jg/g dry    ave1-5   STD DEV
4.0
4.0
4.0
8.0
4.0
8.0
16.0
16.0
4779.3
4011.1
4554.4
7408.7
4538.1
9214.3
12498.9
7754.3
                                                               5184.3
                                                         1517.22
                                                              i recovery
                                                                93.6
                                                         Range
                                                        85-115%
2.5409
2.5396
3.5382
2.5497
2.5537
2.5431
2.5017
4.7793
4.0111
4.5544
7.4087
4.5381
9.2143
12.4989
349.3178
412.2618
220.5925
437.9598
381.4188
576.9403
1143.5759
                                                                                     395.2
                                                                          38.4
                                                                                                                This sample was not used due to breakage of
                                                                                                                filter apparatus and loss of sample
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                        "') recovery  Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1269
               -76
              109.2
80-120%
Tare
0.9598
0.9582
0.9641
Tin + Soil
2.0633
2.3249
2.2875
wet
1.1035
1 .3667
1 .3234
Tin + Soil
1 .8669
2.0777
2.0486
dry
0.9071
1.1195
1 .0845
%moisture
17.798
18.087
18.052
                                                                                            % Solid
                                                                   17.979    82.021
   K2Cr2O7    Cr added  Spike Recovery %
   added (mg)   |jg/g dry   Solution      Range
#6   0.4947     237.167       77     75-125%

    PbCrO4   Cr added  Spike Recovery %
   Added (mg)   |jg/g dry   Solid        Range
#7    11.7       917.4        82     75-125%
                                                                              D23

-------
                                                   Storage = Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
         [5/16/2003     [Day 4 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            286
            476
            557
           1273
           2128
           2949
  0.0000
  0.2355
  0.3829
  0.4289
  0.9815
  1.4647
  2.1787
slope
intercept
RSQ
 0.000712
 0.035579
 0.996189
ppb calc.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
0.8656
0.7443
0.8270
0.6848
0.8269
0.8455
0.5813
0.3839
1166.0
995.6
1111.8
912.0
1111.7
1137.8
766.6
489.3
ppb calc.    Sample #
 280.9              9
 487.9             10
 552.6             11
 1328.9             12
 2007.7             13
 3010.7             14
                                                                     z
                                                                                Sample Cone.
                                         dil. Factor  ppb in sol    ave 1-5   STD DEV  wet mass  ppm Calc.
4.0
4.0
4.0
8.0
4.0
8.0
16.0
16.0
4664.2
3982.5
4447.3
7296.4
4446.7
9102.4
12266.4
7829.3
                                                               5097.4
                                                         1493.27
                                                               i recovery   Range
                                                                96.2     85-115%
                                                      2.5409
                                                      2.5396
                                                      3.5382
                                                      2.5497
                                                      2.5537
                                                      2.5431
                                                      2.5017
                                         4.6642
                                         3.9825
                                         4.4473
                                         7.2964
                                         4.4467
                                         9.1024
                                         12.2664
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                         "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1246
               -42
              107.2
80-120%
Tare
0.9598
0.9582
0.9641
Tin + Soil
2.0633
2.3249
2.2875
wet
1.1035
1 .3667
1 .3234
Tin + Soil
1 .8669
2.0777
2.0486
dry
0.9071
1.1195
1 .0845
%moisture
17.798
18.087
18.052
                                                                                             % Solid
                                                                   17.979    82.021
 M9/9 dry
340.9050
409.3234
215.4009
431.3209
373.7404
569.9372
1122.2988
ave 1 -5
 388.8
STD DEV
    39.8
                                                                                                                This sample was not used due to breakage of
                                                                                                                filter apparatus and loss of sample
          K2Cr2O7    Cr added  Spike Recovery %
          added (mg)  |jg/g dry  Solution      Range
       #6   0.4947    237.167      76      75-125%

            PbCrO4    Cr added  Spike Recovery %
          Added (mg)  |jg/g dry  Solid         Range
       #7    11.7      917.4       80      75-125%
                                                                               D24

-------
                                                   Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
         [5/20/2003     [Day 8 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            286
            476
            557
           1273
           2128
           2949
  0.0000
  0.2394
  0.3781
  0.4245
  0.9314
  1.3877
  2.1176
slope
intercept
RSQ
 0.000683
  0.04038
 0.994006
ppb calc.
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
0.8452
0.7271
0.8091
0.6644
0.7924
0.7992
0.5704
0.3733
1178.6
1005.7
1125.8
913.9
1101.3
1111.3
776.2
487.6
ppb calc.    Sample #
 291.5              9
 494.6             10
 562.5             11
 1304.9             12
 1973.1             13
 3042.0             14
                                                                                Sample Cone.
                                         dil. Factor  ppb in sol    ave 1-5   STD DEV  wet mass  ppm Calc.
4.0
4.0
4.0
8.0
4.0
8.0
16.0
16.0
4714.6
4022.7
4503.1
7310.9
4405.3
8890.2
12419.2
7800.8
                                                               5113.4
                                                         1492.10
                                                               i recovery   Range
                                                                94.5     85-115%
                                                       2.5409
                                                       2.5396
                                                       3.5382
                                                       2.5497
                                                       2.5537
                                                       2.5431
                                                       2.5017
                                         4.7146
                                         4.0227
                                         4.5031
                                         7.3109
                                         4.4053
                                         8.8902
                                         12.4192
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                         "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
              1239
               -45
              106.6
80-120%
Tare
0.9598
0.9582
0.9641
Tin + Soil
2.0633
2.3249
2.2875
wet
1.1035
1 .3667
1 .3234
Tin + Soil
1 .8669
2.0777
2.0486
dry
0.9071
1.1195
1 .0845
%moisture
17.798
18.087
18.052
                                                                                             % Solid
                                                                   17.979    82.021
 M9/9 dry
344.5877
413.4545
218.1047
432.1786
370.2572
556.6471
1136.2838
ave 1 -5
 390.1
STD DEV
    39.9
                                                                                                                This sample was not used due to breakage of
                                                                                                                filter apparatus and loss of sample
          K2Cr2O7    Cr added  Spike Recovery %
          added (mg)  |jg/g dry  Solution      Range
       #6   0.4947    237.167      70      75-125%

            PbCrO4    Cr added  Spike Recovery %
          Added (mg)  |jg/g dry  Solid         Range
       #7    11.7      917.4       81      75-125%
                                                                               D25

-------
Storage = Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2599
0.3818
0.4260
0.9594
1 .5371
2.0623
0.000685
0.062744
0.99936
0.8464
0.7201
0.8103
0.6843
0.7985
0.8220
0.5686
0.3769
5/27/2003

ppb calc.
288.0
466.0
530.6
1309.7
2153.6
2920.7
ppb calc.
1144.7
960.2
1091.9
907.9
1074.7
1109.0
738.9
458.9
Day 15 Colo
Sample #
9
10
11
12
13
14
dil. Factor
4.0
4.0
4.0
8.0
4.0
8.0
16.0
16.0
r
ppb in sol
4578.7
3840.7
4367.7
7263.1
4298.8
8872.2
11822.3
7342.1


>»
y = 0 0007X + 0 0627 ^f"
R2 = 0 9994 ^^^
1- JT
/
/
S
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4995.3 1542.16 2.5409 4.5787 334.6560 380.0 41.1
2.5396 3.8407 394.7488
3.5382 4.3677 21 1 .5498 This sample was not used due to breakage of
2.5497 7.2631 429.3556 filter apparatus and loss of sample
2.5537 4.2988 361.3101
2.5431 8.8722 555.5224
% recovery Range 2.5017 11.8223 1081.6669
87.5 85-115%
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4947 237.167 74 75-125%
0.8837
0.0062
Tare
1199
-83
Tin + Soil
0.9598 2.0633
0.9582 2.3249
0.9641 2.2875
103.2
wet
1.1035
1 .3667
1 .3234
80-120%
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid #7 11.7 917.4 76 75-125%
1 .8669
2.0777
2.0486
0.9071 17.798
1.1195 18.087 17.979 82.021
1.0845 18.052
                         D26

-------
Storage = Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2332
0.3906
0.4296
0.9977
1.6102
2.1590
0.000727
0.040784
0.9991 1
0.8564
0.7363
0.8207
0.6801
0.8112
0.8483
0.5704
0.3886
6/10/2003

ppb calc.
264.6
481.1
534.8
1316.1
2158.6
2913.4
ppb calc.
1121.8
956.6
1072.7
879.3
1059.6
1110.6
728.4
478.4
Day 29 Colo
Sample #
9
10
11
12
13
14
dil. Factor
4.0
4.0
4.0
8.0
4.0
8.0
16.0
16.0
r
ppb in sol
4487.2
3826.4
4290.7
7034.5
4238.5
8885.2
11654.8
7654.1


X*
R3 = 0 9991 ^f
,r

/*
s
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
4896.6 1451.03 2.5409 4.4872 327.9668 373.3 39.0
2.5396 3.8264 393.2767
3.5382 4.2907 207.8202 This sample was not used due to breakage of
2.5497 7.0345 415.8372 filter apparatus and loss of sample
2.5537 4.2385 356.2399
2.5431 8.8852 556.3338
% recovery Range 2.5017 11.6548 1066.3473
95.7 85-115%
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4947 237.167 77 75-125%
0.921 1
0.0047
Tare
1211
-50
Tin + Soil
0.9598 2.0633
0.9582 2.3249
0.9641 2.2875
104.2
wet
1.1035
1 .3667
1 .3234
80-120%
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid #7 11.7 917.4 76 75-125%
1 .8669
2.0777
2.0486
0.9071 17.798
1.1195 18.087 17.979 82.021
1.0845 18.052
                         D27

-------
Storage = Rm Temperature
T=0 day
12763-125B
Boom Snub 3'
Chrome VI digest
Sample/STD
Blank
286
476
557
1273
2128
2949
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 2+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2359
0.3891
0.4294
0.9280
1.2810
2.1416
0.000672
0.04152
0.979978
0.8644
0.7393
0.8268
0.6865
0.8173
0.8269
0.5897
0.3893
7/1/2003

ppb calc.
289.1
517.0
576.9
1318.5
1843.5
3123.6
ppb calc.
1223.9
1037.8
1168.0
959.3
1153.9
1168.1
815.3
517.3
Day 57 Colo
Sample #
9
10
11
12
13
14
dil. Factor
4.0
4.0
4.0
8.0
4.0
8.0
16.0
16.0
r
ppb in sol
4895.6
4151.4
4671 .9
7674.5
4615.4
9345.1
13045.4
8276.3


•
y = 0 OOOTx + 0 0415 ^^^
R2 = 0 98 ^^^
^^ +
/
S
0 500 1000 1500 2000 2500 3000 3500
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
5334.2 1590.07 2.5409 4.8956 357.8238 406.5 42.2
2.5396 4.1514 426.6759
3.5382 4.671 9 226.2836 This sample was not used due to breakage of
2.5497 7.6745 453.6726 filter apparatus and loss of sample
2.5537 4.6154 387.9220
2.5431 9.3451 585.1304
% recovery Range 2.5017 13.0454 1193.5740
103.1 85-115%
K2Cr2O7 Cr added Spike Recovery %
h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry Solution Range
% recovery Range #6 0.4947 237.167 75 75-125%
0.9148
0.0089
Tare
1299
-49
Tin + Soil
0.9598 2.0633
0.9582 2.3249
0.9641 2.2875
111.8
wet
1.1035
1 .3667
1 .3234
80-120%
PbCrO4 Cr added Spike Recovery %
Added (mg) |jg/g dry Solid Range
Tin + Soil dry %moisture mean % Solid #7 11.7 917.4 86 75-125%
1 .8669
2.0777
2.0486
0.9071 17.798
1.1195 18.087 17.979 82.021
1.0845 18.052
                         D28

-------
T=56 day
12763-125C
Boom Snub 5.5'
3/4/2003 |
Storage = 4 C
                                                   Day 1 color
Chrome VI digestion assay
Sample/STD
A540
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
   ppb calc.    Sample #
Blank
253
401
652
995
1645
2191
0.0000
0.1913
0.3564
0.5054
0.7378
1.2515
1 .7485

246.9
458.0
648.4
945.4
1602.0
2237.2
slope 0.000782
intercept -0.001904
RSQ 0.996615
Sample: ppb calc.
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 6+spk
0.4847
0.4819
0.5543
0.4597
0.4249
0.4810
0.6758
0.4151
621.9
618.4
710.9
590.0
545.5
617.2
866.2
532.9
Tare
     947
      24

Tin + Soil
                                                  9
                                                 10
                                                 11
                                                 12
                                                 13
                                                 14
1.4 -

1.2 -

 1 -

0.8 -

0.6

0.4 -

0.2 -

 0
                                                                          y = 0.0008x-0.0019
                                                                              R2 = 0.9966
                                                                                 Sample Cone.
                                         dil. Factor  ppb in sol   ave 4'C   STD DEV  wet mass  ppm Calc.
2.0
2.0
2.0
2.0
2.0
10.0
20.0
10.0
1243.9
1236.7
1421.8
1180.0
1091.0
6172.0
17323.6
5329.1
                                                                1234.7
                                                          121.17
                                                              % Recovery   Range
                                                          2.4849
                                                          2.4867
                                                          2.4895
                                                          2.4943
                                                          2.4907
                                                          2.4931
                                                          2.4899
                              1.2439
                              1.2367
                              1.4218
                              1.1800
                              1.0910
                              6.1720
                             17.3236
                                                                102.1
                                                         85-115%
19.8727
19.6098
18.7037
23.2004
22.0248
21.0570
% Recovery Range
95.1 80-120%

wet
3.3277
2.4150
2.3533
Tin + Soil
22.5281
21 .5393
20.581 1
dry
2.6554
1 .9295
1 .8774
0.947
0.024
%moisture
20.2031
20.1035
20.2227
                                                                    mean
                             % Solid
                                                                    20.176    79.824
     dry
62.7002
62.3159
71.7364
59.3741
55.0001
310.2306
871.6522
ave 4-C   STD DEV
 62.2        6.1
                                                                                                                 K2Cr2O7
                                                                                                                 added (mg)
                                                                                                                     0.5
                                                                                                             Cr added
                                                                                                             |jg/g dry
                                                                                                               256
                                                                                                             Spike Recovery %
                                                                                                             Solution    Range
                                                                                                                 97    75-125%
           PbCrO4    Cr added  Spike Recovery %
          Added (mg)   |jg/g dry  Solid       Range
             10.8       874.3       93     75-125%
                                                                                D29

-------
T=56 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
253
401
652
995
1645
2191
slope
intercept
RSQ
Sample:
4"C#1
4°C#2
4°C#17
4°C#18
4°C#19
4' C #3 sol
4°C#4insol
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.1908
0.3250
0.5052
0.8505
1 .2456
1 .8406
0.000824
-0.017153
0.992835
0.5020
0.4681
0.5642
0.4791
0.4399
0.4765
0.3241
0.4044

0.7657
0.0312
Tare
3/7/2003
Storage = 4 C
ppb calc.
252.2
415.0
633.5
1052.4
1531.6
2253.2
ppb calc.
629.7
588.6
705.1
601.9
554.3
598.7
413.9
517.9
950
59
Tin + Soil
19.8727 23.2004
19.6098 22.0248
18.7037 21.0570
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
10.0
40.0
10.0
% Recovery
95.4
wet
3.3277
2.4150
2.3533
Day 3 color
ppb in sol
1259.3
1177.1
1410.2
1203.8
1108.7
5987.4
16555.9
5179.0
Range
80-120%
Tin + Soil c
22.5281
21 .5393
20.581 1


18 y = 0.0008x-0.0172 *
R2 = 0.9928 ^S
S+
0.8 - }^
0.6 - ^T
0.4- ^^^
0.2 - 4f
0 500 1000 1500 2000 2500
Sample Cone.
ave 4'C STD DEV wet mass ppm Calc. |jg/g dry av
1231.8 113.49 2.4849 1.2593 63.4799 £
2.4867 1.1771 59.3124
2.4895 1.4102 71.1531
2.4943 1 .2038 60.5729
2.4907 1.1087 55.8920
2.4931 5.9874 300.9496
% Recovery Range 2.4899 16.5559 833.0242
98.0 85-115%
K2C
add
0.950 Pb
0.059 Add
1
ry %moisture mean % Solid
2.6554 20.2031
1.9295 20.1035 20.176 79.824
1 .8774 20.2227
                                   ave 4-C  STD DEV
                                     62.1        5.8
                                              Cr added   Spike Recovery %
                                          ig)  |jg/g dry   Solution     Range
                                     0.5        256         93     75-125%

                                          \    Cr added   Spike Recovery %
                                          ig)  |jg/g dry   Solid       Range
                                     10.8      874.3        88     75-125%
D30

-------
T=56 day
12763-125C
Boom Snub 5.5'
Chrome VI digestion assay
3/11/2003
Storage = 4 C
Sample/STD A540 ppb calc.
Blank
253
401
652
995
1645
2191
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 6+spk

0.0000
0.1727
0.2909
0.5071
0.7269
1.1923
1 .7921
0.000806
-0.044587
0.992067

0.4789
0.4560
0.5640
0.4688
0.4240
0.4713
0.6752
0.3964
269.5
416.0
684.1
956.7
1533.9
2277.7
ppb calc.
649.2
620.8
754.7
636.7
581.1
639.8
892.6
506.7

Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
10.0
20.0
10.0
Day 7 color





2
1.8
1.4
1.2
1
0.8
0.6
0.4
0.2
0
y = O.OOOSx - 0.0446 *
R2 = 0.9921 ^S
JT
>^»
^^^
/





500 1000 1500 2000 2500






Sample Cone.
ppb in sol ave 4'C STD DEV wet mass ppm Calc. |jg/g dry ave 4'C
1298.4 1297.0 129.36 2.4849 1.2984 65.4467 65.4
1241.6 2.4867 1.2416 62.5601
1509.4 2.4895 1.5094 76.1582
1273.3 2.4943 1.2733 64.0709
1162.2 2.4907 1.1622 58.5887
6397.5 2.4931 6.3975 321.5636
17852.2 % Recovery Range 2.4899 17.8522 898.2464
5066.7 94.2 85-115%
                                                                                                                           STD DEV
                                                                                                                               6.6
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
  0.7390
 -0.0150

Tare
     972
      37

Tin + Soil
19.8727
19.6098
18.7037
23.2004
22.0248
21.0570
% Recovery Range
97.7 80-120%

wet
3.3277
2.4150
2.3533
Tin + Soil
22.5281
21 .5393
20.581 1
dry
2.6554
1 .9295
1 .8774
0.972
0.037
%moisture
20.2031
20.1035
20.2227
                                                                    mean
% Solid
                                                                   20.176    79.824
K2Cr2O7    Cr added   Spike Recovery %
added (mg)  |jg/g dry   Solution    Range
    0.5        256        100    75-125%

  PbCrO4    Cr added   Spike Recovery %
Added (mg)  |jg/g dry   Solid       Range
   10.8      874.3       95     75-125%
                                                                               D31

-------
T=56 day
12763-125C
Boom Snub 5.5'
3/18/2003 |
Storage = 4 C
                                                   Day 14 color
Chrome VI digestion assay
Sample/STD
A540
Blank
253
401
652
995
1645
2191
0.0000
0.1741
0.3661
0.5545
0.7241
1.1747
1 .7496

214.6
466.4
713.4
935.9
1526.8
2280.8
slope 0.000762
intercept 0.010507
RSQ 0.987903
Sample: ppb calc.
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 6+spk
0.4784
0.4461
0.5704
0.4658
0.4314
0.4696
0.6766
0.4115
613.6
571.3
734.3
597.1
552.0
602.1
873.6
525.9
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
Tare
     942
     -28

Tin + Soil
   ppb calc.    Sample #
                                                 9
                                                10
                                                11
                                                12
                                                13
                                                14
1.4 -

1.2-
                                                                          y = 0.0008x + 0.0105
                                                                             R2 = 0.9879
                                                                                 Sample Cone.
                                         dil. Factor   ppb in sol   ave 4'C  STD DEV  wet mass ppm Calc.
2.0
2.0
2.0
2.0
2.0
10.0
20.0
10.0
1227.3
1142.6
1468.6
1194.2
1104.0
6021 .0
17471.6
5259.0
                                                                1227.3
                                                          142.92
                                                             % Recovery   Range
                                                          2.4849
                                                          2.4867
                                                          2.4895
                                                          2.4943
                                                          2.4907
                                                          2.4931
                                                          2.4899
                                                                95.8
                                                         85-115%
19.8727
19.6098
18.7037
23.2004
22.0248
21.0570
% Recovery Range
94.7 80-120%

wet Tin + Soil dry
3.3277
2.4150
2.3533
22.5281
21 .5393
20.581 1
2.6554
1 .9295
1 .8774

0.942
-0.028
%moisture
20.2031
20.1035
20.2227
                                                                    mean
                              1.2273
                              1.1426
                              1.4686
                              1.1942
                              1.1040
                              6.0210
                             17.4716
                             % Solid
                                                                    20.176    79.824
 M9/9 dry
 61.8643
 57.5719
 74.0988
 60.0923
 55.6554
302.6391
879.1002
ave 4-C   STD DEV
 61.9       7.2
                                                                                                 K2Cr2O7
                                                                                                 added (mg)
                                                                                                    0.5
                                                            Cr added
                                                             M9/9 dry
                                                               256
                               Spike Recovery %
                               Solution    Range
                                   94     75-125%
           PbCrO4   Cr added  Spike Recovery %
          Added (mg)   |jg/g dry  Solid       Range
             10.8       874.3       93     75-125%
                                                                               D32

-------
T=56 day
12763-125C
Boom Snub 5.5'
4/1/2003 |
Storage = 4 C
                                                    Day 28 color
Chrome VI digestion assay
Sample/STD
A540
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
   ppb calc.    Sample #
Blank
253
401
652
995
1645
2191
0.0000
0.1932
0.3295
0.5517
0.7903
1 .2051
1 .7887

240.1
413.2
695.3
998.3
1525.0
2266.1
slope 0.000788
intercept 0.004126
RSQ 0.99227
Sample: ppb calc.
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 6+spk
0.4985
0.4668
0.5504
0.4599
0.4283
0.4878
0.6847
0.4185
627.8
587.5
693.7
578.7
538.6
614.2
864.2
526.2
Tare
     928
      14

Tin + Soil
                                                  9
                                                 10
                                                 11
                                                 12
                                                 13
                                                 14
1.8

1.6-

1.4-

1.2 -

 1

0.8

0.6-

0.4 -

0.2 -

 0
                                                         y = O.OOOSx + 0.0041
                                                             R2 = 0.9923
                                                                                 Sample Cone.
                                         dil. Factor  ppb in sol   ave 4'C   STD DEV  wet mass  ppm Calc.
2.0
2.0
2.0
2.0
2.0
10.0
20.0
10.0
1255.5
1175.0
1387.3
1157.5
1077.2
6141.7
17283.9
5261 .7
                                                                1210.5
                                                          117.39
                                                              % Recovery   Range
                                                          2.4849
                                                          2.4867
                                                          2.4895
                                                          2.4943
                                                          2.4907
                                                          2.4931
                                                          2.4899
                              1.2555
                              1.1750
                              1.3873
                              1.1575
                              1.0772
                              6.1417
                              17.2839
                                                                 95.3
                                                         85-115%
19.8727
19.6098
18.7037
23.2004
22.0248
21.0570
% Recovery Range
93.3 80-120%

wet
3.3277
2.4150
2.3533
Tin + Soil
22.5281
21 .5393
20.581 1
dry
2.6554
1 .9295
1 .8774
0.928
0.014
%moisture
20.2031
20.1035
20.2227
                                                                     mean
                              % Solid
                                                                    20.176    79.824
 M9/9 dry
 63.2873
 59.2069
 69.9978
 58.2431
 54.3059
308.7057
869.6538
ave 4-C  STD DEV
 61.0        6.0
                                                                                                                  K2Cr2O7
                                                                                                                  added (mg)
                                                                                                                     0.5
                                                                                                             Cr added
                                                                                                             M9/9 dry
                                                                                                               256
                                                                                                             Spike Recovery %
                                                                                                             Solution    Range
                                                                                                                 97     75-125%
           PbCrO4    Cr added  Spike Recovery %
          Added (mg)  |jg/g dry  Solid       Range
             10.8       874.3       92     75-125%
                                                                                D33

-------
T=56 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
253
401
652
995
1645
2191
slope
intercept
RSQ
Sample:
4"C#1
4°C#2
4°C#17
4°C#18
4°C#19
4' C #3 sol
4°C#4insol
Sample 6+spk
LCS#15
Blank #16
4oC
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2420
0.3783
0.6467
0.8096
1 .2783
1 .8591
0.000796
0.054775
0.990201
0.5819
0.5459
0.6199
0.5246
0.5054
0.5382
0.7388
0.4697

0.8014
0.0552
Tare
4/29/2003
Storage = 4 C
ppb calc.
235.2
406.5
743.7
948.4
1537.2
2266.9
ppb calc.
662.3
617.0
710.0
590.3
566.2
607.4
859.4
521.3
938
1
Tin + Soil
19.8727 23.2004
19.6098 22.0248
18.7037 21.0570
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
10.0
20.0
10.0
% Recovery
94.3
wet
3.3277
2.4150
2.3533
Day 56 col
ppb in sol
1324.5
1234.1
1420.0
1180.6
1132.3
6073.7
17188.0
5213.1
Range
80-120%
Tin + Soil
22.5281
21 .5393
20.581 1
or

18 y = O.OOOSx + 0.0548 •
R2 = 0.9902 >/'
S^
0.8- ^^»
06 JS
0.4- j^^
0.2- *
0 500 1000 1500 2000 2500
Sample Cone.
ave 4'C STD DEV wet mass ppm Calc. |jg/g dry a
1258.3 115.16 2.4849 1.3245 66.7671
2.4867 1.2341 62.1838
2.4895 1 .4200 71 .6483
2.4943 1.1806 59.4045
2.4907 1.1323 57.0829
2.4931 6.0737 305.2873
% Recovery Range 2.4899 17.1880 864.8304
93.7 85-115%
K2
adc
0.938 P
0.001 Adc
dry %moisture mean % Solid
2.6554 20.2031
1.9295 20.1035 20.176 79.824
1 .8774 20.2227
                                  ave 4-C  STD DEV
                                    63.4        5.8
                                    >2O7   Cr added  Spike Recovery %
                                    ed (mg)   |jg/g dry  Solution    Range
                                    0.5        256        94     75-125%

                                  PbCrO4   Cr added  Spike Recovery %
                                    led (mg)   |jg/g dry  Solid       Range
                                    10.8       874.3        92     75-125%
D34

-------
Storage = Rm Temperature
T=0 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
254
402
620
991
1612
2475
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2103
0.2671
0.4192
0.6681
1.1031
1 .6386
0.000657
0.022154
0.999035
0.4480
0.4361
0.4198
0.4152
0.4544
0.2355
0.6159
0.3285
1/6/2003
ppb calc.
286.4
372.9
604.5
983.4
1645.7
2461.0
ppb calc.
648.3
630.2
605.4
598.4
658.1
324.8
904.0
466.4
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
Day 1 colo
ppb in sol
1296.7
1260.4
1210.8
1196.8
1316.2
1624.1
18079.3
4664.0
r

,6 >»
y = 0 0007X + 0 0222 ^T
i 1 R2 - n 993 ^T
/
/
/
S

-------
T=0 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
254
402
620
991
1612
2475
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2259
0.3422
0.5281
0.7670
1.1644
1 .7235
0.000667
0.085152
0.998487
0.5083
0.4889
0.4548
0.4670
0.5193
0.2823
0.6972
0.3809
1/10/2003
Day 3 color
Storage = Rm temperature
ppb calc.
210.9
385.2
663.8
1021.8
1617.3
2455.1
ppb calc.
634.1
605.0
553.9
572.2
650.6
295.4
917.2
443.2
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
ppb in sol
1268.2
1210.0
1107.9
1144.4
1301.2
1477.2
18343.3
4431 .8



,; .. .™...«, x*
R2 = 0 9985 ^^^
" X^
^
^
ST
X^
s

0 500 1000 1500 2000 2500 3000
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg
1206.3 81.19 2.4837 1.2682 64
2.4795 1.2100 61
2.5041 1.1079 55
2.5037 1.1444 57
2.1961 1.3012 74
2.4995 1 .4772 74
% recovery Range 2.4938 18.3433 95£
82.2 85-115%
|h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.7728
0.0201
Tare
1030
-97
Tin + Soil
19.8729 21.9668
19.6099 22.2456
19.8178 21.9820
104.1
wet
2.0939
2.6357
2.1642
80-120%
Tin + Soil dry %moisture
21 .5307
21 .6996
21 .5262
1.6578 20.827 mean % Solid
2.0897 20.716
1.7084 21.061 20.868 79.132
                                   ave 1-5
                                    62.9
STD DEV
    7.5
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   0.5013    253.450
           Spike Recovery %
           Solution     Range
               5      75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry   Solid        Range
                                     11        896.8        100     75-125%
D36

-------
T=0 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
254
402
620
991
1612
2475
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.1932
0.3968
0.5623
0.7463
1.1779
1 .6768
0.000645
0.109674
0.992218
0.4703
0.4527
0.4284
0.421 1
0.4820
0.6188
0.6572
0.3837
1/14/2003
Day 7 color
Storage = Rm Temperature
ppb calc.
129.6
445.5
702.3
987.8
1657.4
2431.5
ppb calc.
559.5
532.2
494.5
483.2
577.7
789.9
849.5
425.2
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
ppb in sol
1119.1
1064.4
989.0
966.4
1155.4
3949.7
16990.3
4251 .7


X»
1C (-99995..9I93, ^•
R2 = 9 9922 ^^^
" y
S
/
s
yr
s

0 509 1999 1599 2999 2599 3999
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg
1058.9 81.23 2.4837 1.1191 56
2.4795 1 .0644 54
2.5041 0.9890 49
2.5037 0.9664 48
2.1961 1.1554 66
2.4995 3.9497 19£
% recovery Range 2.4938 16.9903 888
82.1 85-115%
jh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.7414
0.0463
Tare
980
-98
Tin + Soil
19.8729 21.9668
19.6099 22.2456
19.8178 21.9820
99.0
wet
2.0939
2.6357
2.1642
80-120%
Tin + Soil
21 .5307
21 .6996
21 .5262
dry %moisture
1.6578 20.827 mean % Solid
2.0897 20.716
1.7084 21.061 20.868 79.132
                                   ave 1-5
                                    55.3
STD DEV
    7.1
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   0.5013    253.450
           Spike Recovery %
           Solution     Range
               57     75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry  Solid        Range
                                     11        896.8        93     75-125%
D37

-------
T=0 day
12763-125C
Boom Snub 5.5'
1/21/2003 |
Storage = Rm Temperature
                                                    Day 14 color
Chrome VI digestion assay
Sample/STD
A540
ppb calc.    Sample #
Blank
             254
             402
             620
             991
            1612
            2475
0.0000
0.2595
0.3690
0.5419
0.8250
1.1637
1.1471

220.9
384.2
641.9
1063.8
1568.7
1543.9
slope
intercept
RSQ
                                  9
                                 10
                                 11
                                 12
                                 13
                                 14
 0.000671
 0.111267 Linear regression without high standard
 0.992317
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
0.5219
0.4818
0.4416
0.4452
0.4845
0.6373
0.6675
0.3876
612.1
552.3
492.4
497.7
556.3
784.1
829.1
411.9
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
1224.1
1104.6
984.7
995.5
1112.6
3920.3
16581.4
4118.8
ave 1-5
1084.3





% recovery
78.1
STD DEV
98.19





Range
85-115%
                                                                                  Sample Cone.
                                                                                    wet mass ppm Calc.
                                                                                     2.4837
                                                                                     2.4795
                                                                                     2.5041
                                                                                     2.5037
                                                                                     2.1961
                                                                                     2.4995
                                                                                     2.4938
                                                                              1.2241
                                                                              1.1046
                                                                              0.9847
                                                                              0.9955
                                                                              1.1126
                                                                              3.9203
                                                                              16.5814
                                                                           M9/9 dry
                                                                           62.2780
                                                                           56.2706
                                                                           49.7122
                                                                           50.2382
                                                                           64.0171
                                                                           198.1407
                                                                           867.1839
                                                               ave 1-5
                                                                 56.5
STD DEV
    6.6
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                	               % recovery   Range
LCS#15
                                                                                                  K2Cr2O7    Cr added
                                                                                                  added (mg)   |jg/g dry
                                                                                                    0.5013    253.450
                                                                                                           Spike Recovery %
                                                                                                           Solution      Range
                                                                                                               56     75-125%
Blank #8
Moisture A
Moisture B
Moisture C
                Tare
               978
          Tin + Soil
               98.7
80-120%
19.8729
19.6099
19.8178
21.9668
22.2456
21.9820
wet Tin + Soil
2.0939
2.6357
2.1642
21 .5307
21 .6996
21 .5262
dry
1 .6578
2.0897
1 .7084
%moisture
20.827
20.716
21 .061
                                                                              % Solid
                                                                    20.868    79.132
                                                                                      PbCrO4    Cr added   Spike Recovery %
                                                                                     Added (mg)  |jg/g dry   Solid        Range
                                                                                         11        896.8        90     75-125%
                                                                                D38

-------
T=0 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
254
402
620
991
1612
2475
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2001
0.3552
0.6158
0.7290
1.2317
1.7173
0.000669
0.100071
0.987261
0.4885
0.471 1
0.4183
0.4833
0.4719
0.6293
0.6861
0.4067
2/3/2003
Day 28 color
Storage = Rm Temperature
ppb calc.
149.6
381.6
771.3
940.6
1692.4
2418.6
ppb calc.
580.9
554.9
475.9
573.1
556.1
791.5
876.4
458.6
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
ppb in sol
1161.8
1109.8
951.8
1146.3
1112.2
3957.4
17528.5
4585.7



1 E v - n nnn?y + n mm j^"*
R2 = 0 9873 ^^^
" */
^
/
+S*
^
f

0 500 1000 1500 2000 2500 3000
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg
1096.4 83.80 2.4837 1.1618 59
2.4795 1.1098 56
2.5041 0.9518 48
2.5037 1.1463 57
2.1961 1.1122 63
2.4995 3.9574 20C
% recovery Range 2.4938 17.5285 916
86.0 85-115%
jh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.6707
-0.0470
Tare
853
-220
Tin + Soil
19.8729 21.9668
19.6099 22.2456
19.8178 21.9820
86.2
wet
2.0939
2.6357
2.1642
80-120%
Tin + Soil
21 .5307
21 .6996
21 .5262
dry %moisture
1.6578 20.827 mean % Solid
2.0897 20.716
1.7084 21.061 20.868 79.132
                                   ave 1-5
                                    57.1
STD DEV
    5.8
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   0.5013    253.450
           Spike Recovery %
           Solution     Range
               56     75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry  Solid        Range
                                     11        896.8        96     75-125%
D39

-------
T=0 day
12763-125C
Boom Snub 5.5'
Chrome VI digest
Sample/STD
Blank
254
402
620
991
1612
2475
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.2008
0.3266
0.5143
0.7377
1.1766
1.6716
0.000659
0.0729
0.996398
0.4807
0.4828
0.4337
0.4280
0.4913
0.6359
0.6724
0.3822
3/4/2003
Day 56 color
Storage = Rm Temperature
ppb calc.
193.9
384.7
669.3
1008.1
1673.6
2424.3
ppb calc.
618.4
621.6
547.1
538.5
634.5
853.7
909.1
469.0
Sample #
9
10
11
12
13
14
dil. Factor
2.0
2.0
2.0
2.0
2.0
5.0
20.0
10.0
ppb in sol
1236.8
1243.1
1094.2
1076.9
1268.9
4268.7
18181.6
4690.2


	 X»
1C ,-0000,. .00,23 ^r
R2 = 0 9964 ^^^
" ./
s
/
s
S
s

0 500 1000 1500 2000 2500 3000
Sample Cone.
ave 1-5 STD DEV wet mass ppm Calc. |jg
1184.0 90.85 2.4837 1.2368 62
2.4795 1 .2431 63
2.5041 1 .0942 55
2.5037 1 .0769 54
2.1961 1.2689 73
2.4995 4.2687 21 £
% recovery Range 2.4938 18.1816 95C
90.3 85-115%
jh 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
% recovery Range
0.7061
0.0087
Tare
960
-97
Tin + Soil
19.8729 21.9668
19.6099 22.2456
19.8178 21.9820
97.0
wet
2.0939
2.6357
2.1642
80-120%
Tin + Soil
21 .5307
21 .6996
21 .5262
dry %moisture
1.6578 20.827 mean % Solid
2.0897 20.716
1.7084 21.061 20.868 79.132
                                   ave 1-5
                                    61.8
STD DEV
    7.5
                                 K2Cr2O7   Cr added
                                 added (mg)   |jg/g dry
                                   0.5013    253.450
           Spike Recovery %
           Solution     Range
               61      75-125%
                                  PbCrO4   Cr added  Spike Recovery %
                                 Added (mg)   |jg/g dry   Solid        Range
                                     11        896.8        99     75-125%
D40

-------
T=56 day
12763-126D
Frontier Hard Chrome, S
Chrome VI digest
Sample/STD
Blank
253
401
621
989
1620
2476
slope
intercept
RSQ
Sample:
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 1+spk
on assay
A540
0.0000
0.2021
0.3690
0.4857
0.8469
1.2156
1 .7892
0.000704
0.0722
0.994464
1 .2409
1.2105
1 .2692
1 .2563
1.1188
0.8514
0.6129
0.7658
3/6/2003
Storage = 4 C
Sandy Soil
ppb calc.
184.6
421.9
587.7
1101.1
1625.2
2440.5
ppb calc.
1661.2
1618.0
1701.4
1683.1
1487.6
1107.5
768.5
985.9

Sample #
9
10
11
12
13
14
dil. Factor
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
Day 1 colo
ppb in sol
16611.7
16179.6
17013.9
16830.6
14876.2
22150.8
30741 .6
19717.4
r

1.8 -
1.6-
1.4 -
1.2 -
1 -
0.8 -
0.6-
0.4-
0.2 -
o
y = 0.0007X + 0.0722
R2 = 0.9945 ^^
^^

0 500 1000 1500 2000 2500 3000

Sample Cone.
ave 4'C STD DEV wet mass ppm Calc. |jg/g dry ave 4'C
16302.4 855.88 2.4933 16.6117 811.5936 802.2
2.4875 16.1796 792.5880
2.4950 17.0139 840.1507
2.4919 16.8306 832.1520
2.4875 16.1796 792.5880
2.4950 14.8762 734.6224
% Recovery Range 2.4889 30.7416 1505.0720
77.6 85-115%
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
                                                                                                                           STD DEV
                                                                                                                               42.1
Tare
     1125
     -51

Tin + Soil
19.8159
19.7659
19.7540
24.4202
24.5795
24.5255
113.3 80-120%

wet Tin + Soil dry
4.6043
4.8136
4.7715
23.6024
23.7087
23.6699
3.7865
3.9428
3.9159
1.125
-0.051
%moisture
17.7617
18.0904
17.9315
                                                                             % Solid
                                                                    17.928    82.072
K2Cr2O7    Cr added   Spike Recovery %
added (mg)  |jg/g dry   Solution    Range
    0.5        246        127    75-125%

  PbCrO4    Cr added   Spike Recovery %
Added (mg)  |jg/g dry   Solid       Range
   10.4      819.1        86    75-125%
                                                                               D41

-------
T=56 day               [3/10/2003
12763-126D              Stroage = 4C
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
Blank
            253
            401
            621
            989
           1620
           2476
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 1+spk
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
  0.0000
  0.1998
  0.3006
  0.4751
  0.7456
  1.1934
  1.7390
 0.000697
 0.036977
 0.998788
  1.2519
  1.2104
  1.2491
  1.2341
  1.1220
  0.8254
  0.6661
  0.7699
Tare
   ppb calc.
    1743.9
    1684.3
    1739.9
    1718.3
    1557.4
    1131.7
    903.0
    1052.0
     1028
     -24

Tin + Soil
                                   Day 3 color
   ppb calc.    Sample #
    233.7              9
    378.4             10
    628.9             11
    1017.1             12
    1659.9             13
    2443.1             14
                       2 -

                      1.8-

                      1.6-

                      1.4-

                      1.2-

                       1 -

                      0.8-

                      0.6-

                      0.4-

                      0.2-

                       0-
                                                                      y = 0.0007X + 0.037
                                                                         R2 = 0.9988
                                       0
                                             500
                                                    1000
                                                            1500
                                                                   2000
                                                                           2500
                                                                                  3000
                                                                Sample Cone.
                         dil. Factor  ppb in sol    ave 4'C   STD DEV  wet mass  ppm Calc.
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
17438.8
16843.1
17398.6
17183.3
15574.3
22633.8
36121.4
21040.5
                       16887.6
  771.25
                     % Recovery   Range
2.4933
2.4875
2.4950
2.4919
2.4950
2.4924
2.4889
17.4388
16.8431
17.3986
17.1833
15.5743
22.6338
36.1214
                        90.0
19.8159
19.7659
19.7540
24.4202
24.5795
24.5255
                        % Recovery   Range
                           103.6     80-120%
wet        Tin + Soil  dry
   4.6043
   4.8136
   4.7715
                                               3.7865
                                               3.9428
                                               3.9159
 85-115%
  1.028
  -0.024

%moisture
 17.7617
 18.0904
 17.9315
                                                                   % Solid
                                                          17.928    82.072
 M9/9 dry
852.0053
825.0938
859.1474
849.5932
769.0957
1139.8986
1768.4560
ave 4-C   STD DEV
 831.0      36.9
                                                                                                                K2Cr2O7
                                                                                                                added (mg)
                                                                                                                    0.5
                                                                                                  Cr added
                                                                                                  M9/9 dry
                                                                                                    246
                                                                                              Spike Recovery %
                                                                                              Solution    Range
                                                                                                 126    75-125%
                              PbCrO4   Cr added  Spike Recovery %
                             Added (mg)   |jg/g dry  Solid       Range
                                10.4       819.1        114    75-125%
                                                                               D42

-------
T=56 day               [3/14/2003
12763-126D              Storage = 4C
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
Blank
            253
            401
            621
            989
           1620
           2476
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 1+spk
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
  0.0000
  0.1883
  0.2927
  0.4720
  0.7447
  1.2744
  1.7316
 0.000711
 0.030396
  0.99285
  1.2538
  1.2126
  1.2652
  1.2356
  1.1223
  0.8430
  0.6700
  0.783
Tare
   ppb calc.
    1721.2
    1663.3
    1737.3
    1695.6
    1536.2
    1143.3
    899.9
    1058.8
     1011
     -53

Tin + Soil
                                   Day 7 color
   ppb calc.    Sample #
    222.2              9
    369.0             10
    621.3             11
    1005.0             12
    1750.2             13
    2393.4             14
                         dil. Factor
    10.0
    10.0
    10.0
    10.0
    10.0
    20.0
    40.0
    20.0
                        % Recovery
                           101.8
ppb in sol
 17212.2
 16632.6
 17372.6
 16956.2
 15362.1
 22865.3
 35994.7
 21177.0
             Range
            80-120%
19.8159
19.7659
19.7540
24.4202
24.5795
24.5255
                        0.8

                        0.6-

                        0.4 -

                        0.2 -

                         0
                                                                       y = 0.0007X + 0.0304
                                                                          R2 = 0.9928
ave 4'C
16707.1
 99.1
        Sample Cone.
STD DEV  wet mass  ppm Calc.
  802.27    2.4933   17.2122
           2.4875   16.6326
           2.4950   17.3726
           2.4919   16.9562
           2.4950   15.3621
           2.4924   22.8653
           2.4889   35.9947
 85-115%
                       1.011
                      -0.053
 M9/9 dry
840.9342
814.7789
857.8624
838.3617
758.6203
1151.5546
1762.2541
ave 4-C   STD DEV
 822.1       38.7
                                                                                                                K2Cr2O7
                                                                                                                added (mg)
                                                                                                                    0.5
                                                                                                  Cr added
                                                                                                  M9/9 dry
                                                                                                    246
                                                                                  Spike Recovery %
                                                                                  Solution    Range
                                                                                      134    75-125%
wet        Tin + Soil  dry
   4.6043
   4.8136
   4.7715
                                               3.7865
                                               3.9428
                                               3.9159
                     %moisture
                      17.7617
                      18.0904
                      17.9315
                                                   PbCrO4   Cr added  Spike Recovery %
                                                 Added (mg)  |jg/g dry   Solid      Range
                                                     10.4       819.1       115    75-125%
                                                                   % Solid
                                                          17.928    82.072
                                                                               D43

-------
         [3/21/2003
T=56 day
12763-126D              Storage = 4C
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
Tare
     1085
     -59

Tin + Soil
   ppb calc.    Sample #
                         Day 14 color
Blank
253
401
621
989
1620
2476
0.0000
0.2171
0.3529
0.5160
0.8313
1.1996
1 .7753

195.4 9
391.7 10
627.4 1 1
1083.2 12
1615.6 13
2447.8 14
slope 0.000692
intercept 0.081 936
RSQ 0.996383
Sample: ppb calc. dil. Factor
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 1+spk
1 .2572
1 .2308
1 .3086
1 .2585
1.1436
0.8515
0.6741
0.7696
1698.9
1660.7
1773.2
1700.7
1534.7
1112.4
856.0
994.0
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
 2

1.8-

1.6 -

1.4 -

1.2 -

 1 -

0.8-

0.6 -

0.4 -

0.2 -
                                                                0
                                                                      y = 0.0007x + 0.0819
                                                                         R2 = 0.9964
                                                                        500
                                                                               1000
                                                                                      1500
                                                                                              2000
                                                                                                     2500
                                                                                                            3000
                                                                                Sample Cone.
                                                   ppb in sol   ave 4'C  STD DEV  wet mass  ppm Calc.
                                                    16988.6    16736.2    876.93
                                                    16607.0
                                                    17731.6
                                                    17007.4
                                                    15346.5
                                                    22248.3
                                                    34239.3   % Recovery   Range
                                                                   2.4933
                                                                   2.4875
                                                                   2.4950
                                                                   2.4919
                                                                   2.4950
                                                                   2.4924
                                                                   2.4889
                                                                  16.9886
                                                                  16.6070
                                                                  17.7316
                                                                  17.0074
                                                                  15.3465
                                                                  22.2483
                                                                  34.2393
                                                    19880.6
                                        % Recovery  Range
                                                72.3
                                               85-115%
19.8159
19.7659
19.7540
24.4202
24.5795
24.5255
109.3 80-120%

wet Tin + Soil dry
4.6043
4.8136
4.7715
23.6024
23.7087
23.6699
3.7865
3.9428
3.9159
1.085
-0.059
%moisture
17.7617
18.0904
17.9315
                                                                            % Solid
                                                                   17.928    82.072
                                            dry
                                       830.0092
                                       813.5258
                                       875.5896
                                       840.8950
                                       757.8486
                                       1120.4840
                                       1676.3112
ave 4-C   STD DEV
 823.6       43.2
                                                                                                K2Cr2O7
                                                                                                added (mg)
                                                                                                   0.5
                                                                                                 Cr added
                                                                                                  |jg/g dry
                                                                                                    246
                                                                      Spike Recovery %
                                                                      Solution     Range
                                                                         121     75-125%
                                                  PbCrO4   Cr added  Spike Recovery %
                                                 Added (mg)   |jg/g dry   Solid       Range
                                                    10.4       819.1        104     75-125%
                                                                              D44

-------
         [4/4/2003
T=56 day
12763-126D              Storage = 4C
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
Blank
            253
            401
            621
            989
           1620
           2476
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 1+spk
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
  0.0000
  0.2041
  0.3150
  0.4944
  0.8031
  1.2868
  1.7776
 0.000719
 0.050924
 0.994134
  1.2537
  1.2230
  1.2889
  1.2686
  1.1434
  0.8429
  0.6744
  0.7768
Tare
   ppb calc.
    1672.2
    1629.5
    1721.1
    1692.9
    1518.8
    1101.1
    866.8
    1009.2
     1104
      42

Tin + Soil
                         Day 28 color
   ppb calc.    Sample #
    213.0              9
    367.1             10
    616.6             11
    1045.7             12
    1718.2             13
    2400.5             14
                                                       y = 0.0007X + 0.0509
                                                          R2 = 0.9941
                                                                Sample Cone.
                         dil. Factor  ppb in sol   ave 4'C  STD DEV wet mass  ppm Calc.
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
16721.8
16295.0
17211.2
16929.0
15188.3
22021 .2
34671 .9
20183.2
16469.1





% Recovery
86.5
790.04





Range
85-115%
2.4933
2.4875
2.4950
2.4919
2.4950
2.4924
2.4889
16.7218
16.2950
17.2112
16.9290
15.1883
22.0212
34.6719
                                                               M9/9 dry
                                                              816.9737
                                                              798.2415
                                                              849.8906
                                                              837.0160
                                                              750.0377
                                                              1109.0442
                                                              1697.4946
                                         ave 4-C  STD DEV
                                          810.4      39.1
19.8159
19.7659
19.7540
24.4202
24.5795
24.5255
                        % Recovery  Range
                          111.1    80-120%
wet        Tin + Soil  dry
   4.6043
   4.8136
   4.7715
                                                                                                               K2Cr2O7
                                                                                                               added (mg)
                                                                                                                   0.5
                                                                                                 Cr added
                                                                                                 M9/9 dry
                                                                                                   246
                                                                                             Spike Recovery %
                                                                                             Solution     Range
                                                                                                121     75-125%
                                               3.7865
                                               3.9428
                                               3.9159
  1.104
  0.042

%moisture
 17.7617
 18.0904
 17.9315
  PbCrO4    Cr added  Spike Recovery %
Added (mg)  |jg/g dry  Solid       Range
   10.4      819.1        108    75-125%
                                                                  % Solid
                                                         17.928    82.072
                                                                              D45

-------
         |5/2/2003
T=56 day
12763-126D              Storage = 4C
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
Blank
            253
            401
            621
            989
           1620
           2476
slope
intercept
RSQ

Sample:
4°C#1
4°C#2
4°C#17
4°C#18
4°C#19
4° C #3 sol
4°C#4insol
Sample 1+spk
LCS#15
Blank #16

4oC
Moisture A
Moisture B
Moisture C
  0.0000
  0.1912
  0.3403
  0.4656
  0.7573
  1.2548
  1.7549
 0.000708
 0.043346
 0.995853
  1.2469
  1.2195
  1.2412
  1.2385
  1.1208
  0.8134
  0.6502
  0.7572
Tare
   ppb calc.
    1699.8
    1661.1
    1691.7
    1687.9
    1521.7
    1087.6
    857.1
    1008.2
Tin + Soil
                         Day 56 color
   ppb calc.    Sample #
    208.8              9
    419.4             10
    596.4             11
    1008.3             12
    1711.0             13
    2417.3             14
                         dil. Factor
    10.0
    10.0
    10.0
    10.0
    10.0
    20.0
    40.0
    20.0
ppb in sol
 16998.0
 16611.0
 16917.5
 16879.4
 15217.1
 21751.2
 34282.8
 20163.8
                        % Recovery   Range
              1015         102.2     80-120%
               -61
19.8159
19.7659
19.7540
24.4202
24.5795
24.5255
                         1.4 -

                         1.2-

                          1 -

                         0.8 -

                         0.6-

                         0.4-

                         0.2 -
                                                                        y = 0.0007X + 0.0433
                                                                           R2 = 0.9959
ave 4'C
16524.6
 79.1
wet        Tin + Soil  dry
   4.6043
   4.8136
   4.7715
                                               3.7865
                                               3.9428
                                               3.9159
STD DEV
  745.23
                                         Sample Cone.
                                          wet mass  ppm Calc.
2.4933
2.4875
2.4950
2.4919
2.4950
2.4924
2.4889
16.9980
16.6110
16.9175
16.8794
15.2171
21.7512
34.2828
 M9/9 dry
830.4675
813.7227
835.3883
834.5639
751.4562
1095.4478
1678.4427
ave 4-C   STD DEV
 813.1       35.6
 85-115%
                       1.015
                      -0.061

                     %moisture
                      17.7617
                      18.0904
                      17.9315
                                                                                                                K2Cr2O7
                                                                                                                added (mg)
                                                                                                                    0.5
                                                                                                  Cr added
                                                                                                  M9/9 dry
                                                                                                    246
                                                                                              Spike Recovery %
                                                                                              Solution     Range
                                                                                                 115     75-125%
                                                   PbCrO4   Cr added  Spike Recovery %
                                                 Added (mg)   |jg/g dry   Solid       Range
                                                     10.4       819.1        106     75-125%
                                                                   % Solid
                                                          17.928    82.072
                                                                               D46

-------
                                       Storage =  Rm Temperature
T=0 day
12763-126D
Frontier Hard Chrome, Sandy Soil
         11/10/2003     | Day 1 Color
Chrome VI digestion assay
Sample/STD

Blank
A540
            253
            403
            624
            990
           1616
           2494
  0.0000
  0.1825
  0.2918
  0.4279
  0.7461
  1.2829
  1.7971
ppb calc.    Sample #
 245.4              9
 393.1             10
 577.0             11
 1006.9             12
 1732.2             13
 2427.0             14
slope
intercept
RSQ
  0.00074
 0.000901
 0.994374
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
1 .2325
1 .2686
1.1679
1 .2074
1 .2696
0.8889
0.6290
0.7278
1664.1
1712.9
1576.9
1630.2
1714.3
1199.9
848.7
982.2
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
16641.4
17129.2
15768.5
16302.3
17142.7
23997.3
33947.6
19643.8
                                                                               Sample Cone.
ave 1-5
16596.8





b recovery
83.5
STD DEV
582.29





Range
85-115%
wet mass
2.5137
2.5016
2.5146
2.5031
2.5034
2.5112
2.4527

ppm Calc.
16.6414
17.1292
15.7685
16.3023
17.1427
23.9973
33.9476

M9/9 dry
827.9809
840.0165
769.491 1
799.0276
840.1259
1172.7190
1697.3265

ave 1-5 STD DEV
815.3 30.6







Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
               	               % recovery   Range
LCS#15
                                                                                               K2Cr2O7    Cr added
                                                                                               added (mg)   |jg/g dry
                                                                                                 0.5052     246.841
                                                                                                       Spike Recovery %
                                                                                                       Solution      Range
                                                                                                           145     75-125%
Blank #8
Moisture A
Moisture B
Moisture C
                Tare
              1091
               -28
          Tin + Soil
              109.7
80-120%
19.8132
19.7520
19.7401
22.8038
23.0542
22.9840
wet Tin + Soil
2.9906
3.3022
3.2439
22.2560
22.4510
22.3705
dry
2.4428
2.6990
2.6304
%moisture
18.317
18.267
18.912
                                                                                    PbCrO4    Cr added  Spike Recovery %
                                                                                  Added (mg)  |jg/g dry  Solid         Range
                                                                                     10.9      877.3       101      75-125%
                                                                            % Solid
                                                                  18.499    81.501
                                                                              D47

-------
T=0 day
12763-126D
Frontier Hard
1 1/1 3/2003 JDaySColor
Storage = Rm Temperature
Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
     A540
ppb calc.    Sample #
Blank
 253
 403
 624
 990
1616
2494
slope
intercept
RSQ
0.0000
0.2115
0.3399
0.4487
0.8195
1 .2876
1 .7884

222.0
400.8
552.3
1068.6
1720.3
2417.6
0.000718
0.052028
0.992114
                                                  9
                                                 10
                                                 11
                                                 12
                                                 13
                                                 14
                                                                                 Sample Cone.
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
1 .2436
1 .3047
1 .2470
1 .2488
1 .2858
0.8675
0.5640
0.7985
1659.0
1744.1
1663.8
1666.3
1717.8
1135.4
712.8
1039.3
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
16590.5
17441.2
16637.8
16662.9
17178.0
22707.9
28513.1
20786.5
ave 1-5
16902.1





% recovery
103.1
STD DEV
384.36





Range
85-115%
wet mass
2.5137
2.5016
2.5146
2.5031
2.5034
2.5112
2.4527

ppm Calc.
16.5905
17.4412
16.6378
16.6629
17.1780
22.7079
28.5131

[ig/g dry
825.4460
855.3157
811.9107
816.7020
841 .8566
1109.7060
1425.6103

ave 1-5 STD DEV
830.2 18.1







Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                         "') recovery   Range
LCS#15
                                                                                                      K2Cr2O7    Cr added
                                                                                                      added (mg)  |jg/g dry
                                                                                                        0.5052    246.841
Blank #8
Moisture A
Moisture B
Moisture C
                Tare
                    971
                    -16
               Tin + Soil
               97.6
80-120%
19.8132
19.7520
19.7401
22.8038
23.0542
22.9840
wet Tin + Soil
2.9906
3.3022
3.2439
22.2560
22.4510
22.3705
dry
2.4428
2.6990
2.6304
%moisture
18.317
18.267
18.912
                                                                                      PbCrO4
                                                                                    Added (mg)
                                                                                       10.9
                                                                         Cr added
                                                                         M9/9 dry
                                                                          877.3
Spike Recovery %
Solution      Range
    113    75-125%

Spike Recovery %
Solid         Range
    68     75-125%
                                                                         mean
                                                                                  % Solid
                                                                         18.499    81.501
                                                                                D48

-------
T=0 day
12763-126D
Frontier Hard
|1/17/2003 |Day7Color
Storage = Rm Temperature
Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
ppb calc.    Sample #
Blank
            253
            403
            624
            990
           1616
           2494
slope
intercept
RSQ
0.0000
0.2379
0.4498
0.5067
0.7939
1 .2838
1.7018

156.2
481.5
568.8
1009.7
1761.8
2403.5
0.000651
0.136174
0.986886
                                 9
                                10
                                11
                                12
                                13
                                14
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
1.2610
1 .2971
1.2716
1 .2463
1 .3305
0.8578
0.6657
0.7677
1726.8
1782.2
1743.1
1704.3
1833.5
1107.8
812.9
969.5
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
17268.3
17822.5
17431.0
17042.6
18335.3
22156.8
32517.1
19390.3
                                                                                 Sample Cone.
ave 1-5
17579.9





b recovery
STD DEV
509.25





Range
wet mass
2.5137
2.5016
2.5146
2.5031
2.5034
2.5112
2.4527
ppm Calc.
17.2683
17.8225
17.4310
17.0426
18.3353
22.1568
32.5171
M9/9 dry
859.1709
874.0161
850.6192
835.3150
898.5700
1082.7717
1625.8025
ave 1-5 STD DEV
863.5 24.1






                                                                 58.7
                                                         85-115%
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                         "') recovery   Range
LCS#15
                                                                                                 K2Cr2O7    Cr added
                                                                                                 added (mg)   |jg/g dry
                                                                                                   0.5052    246.841
Blank #8
Moisture A
Moisture B
Moisture C
                Tare
               1038
               51
          Tin + Soil
              104.3
80-120%
19.8132
19.7520
19.7401
22.8038
23.0542
22.9840
wet Tin + Soil
2.9906
3.3022
3.2439
22.2560
22.4510
22.3705
dry
2.4428
2.6990
2.6304
%moisture
18.317
18.267
18.912
                                                                                      PbCrO4
                                                                                    Added (mg)
                                                                                       10.9
                                                                         Cr added
                                                                         M9/9 dry
                                                                          877.3
Spike Recovery %
Solution      Range
    89     75-125%

Spike Recovery %
Solid         Range
    87     75-125%
                                                                    mean
                                                                             % Solid
                                                                    18.499    81.501
                                                                                D49

-------
T=0 day                 11/24/2003     |Day 14 Color
12763-126D             Storage = Rm Temperature I
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
ppb calc.    Sample #
Blank
            253
            403
            624
            990
           1616
           2494
slope
intercept
RSQ
0.0000
0.2066
0.4450
0.4796
0.8827
1.3196
1 .8281

150.3
483.4
531.7
1094.9
1705.4
2415.9
0.000716
0.099039
0.986293
                                 9
                                10
                                11
                                12
                                13
                                14
                                         500     1000    1500    2000    2500    3000
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
1 .2485
1 .3063
1 .2697
1.2415
1 .2972
0.8737
0.5736
0.7674
1606.0
1686.8
1635.7
1596.3
1674.1
1082.4
663.1
933.8
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
16060.4
16868.0
16356.6
15962.6
16740.9
21647.4
26522.5
18676.9
ave 1-5
16397.7





% recovery
67.9
STD DEV
401.15





Range
85-115%
                                                                                Sample Cone.
                                                                                  wet mass
                                                                                   2.5137
                                                                                   2.5016
                                                                                   2.5146
                                                                                   2.5031
                                                                                   2.5034
                                                                                   2.5112
                                                                                   2.4527
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                        "') recovery   Range
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
                Tare
               970
               -131
          Tin + Soil
              97.4
80-120%
19.8132
19.7520
19.7401
22.8038
23.0542
22.9840
wet Tin + Soil
2.9906
3.3022
3.2439
22.2560
22.4510
22.3705
dry
2.4428
2.6990
2.6304
%moisture
18.317
18.267
18.912
>pm Calc.
16.0604
16.8680
16.3566
15.9626
16.7409
21 .6474
26.5225






M9/9 dry
799.0751
827.2089
798.1907
782.3815
820.4334
1057.8779
1326.0859






ave 1-5 STD DEV
805.5






K2Cr2O7
added (mg)
0.5052
PbCrO4
Added (mg)
10.9
18.2






Cr added
M9/9 dry
246.841
Cr added
M9/9 dry
877.3
Spike Recovery %
Solution     Range
    102    75-125%

Spike Recovery %
Solid        Range
    59     75-125%
                                                                   mean
                                                                            % Solid
                                                                   18.499    81.501
                                                                              D50

-------
T=0 day
12763-126D
Frontier Hard Chrome, £
Chrome VI digest
Sample/STD
Blank
253
403
624
990
1616
2494
slope
intercept
RSQ
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
Samples # 1 throuc
LCS#15
Blank #8
Moisture A
Moisture B
Moisture C
on assay
A540
0.0000
0.1692
0.3289
0.5039
0.8023
1 .2768
1 .7670
0.000713
0.049379
0.991781
1.2121
1 .2542
1 .2072
1.1842
1 .2463
0.8137
0.5154
0.7055
2/7/2003
Storage = Rm T
Sandy Soil
ppb calc.
168.0
391.9
637.2
1055.6
1720.8
2408.1
ppb calc.
1630.1
1689.1
1623.2
1591.0
1678.1
1071.6
653.4
919.9
Day 28 Colo
emperature
Sample #
9
10
11
12
13
14
dil. Factor
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
r
ppb in sol
16301.2
16891.4
16232.5
15910.0
16780.6
21431.3
26134.2
18397.4



y = 0 OOOTx + 0 0494 _^^

yS
S
>S
,S
/
s
+
0 500 1000 1500 2000 2500 3000
Sample Cone.
ave1-5 STD DEV wet mass ppm Calc. |jg/g dry ave1-5 STD DEV
16423.1 406.70 2.5137 16.3012 811.0525 806.7 20.4
2.5016 16.8914 828.3553
2.5146 16.2325 792.1310
2.5031 15.9100 779.8025
2.5034 16.7806 822.3823
2.5112 21.4313 1047.3210
% recovery Range 2.4527 26.1342 1306.6684
62.2 85-115%
K2Cr2O7 Cr added
|h 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation). added (mg) |jg/g dry
% recovery Range 0.5052 246.841
0.7514
-0.0240
Tare
984
-103
Tin + Soil
19.8132 22.8038
19.7520 23.0542
19.7401 22.9840
98.9
wet
2.9906
3.3022
3.2439
80-120%
Tin + Soil
22.2560
22.4510
22.3705
PbCrO4 Cr added
Added (mg) |jg/g dry
dry %moisture 10.9 877.3
2.4428 18.317 mean % Solid
2.6990 18.267
2.6304 18.912 18.499 81.501
                                                      Spike Recovery %
                                                      Solution     Range
                                                          97     75-125%

                                                      Spike Recovery %
                                                      Solid        Range
                                                          57     75-125%
D51

-------
T=0 day                 [3/7/2003      [Day 56 Color
12763-126D              Storage = Rm Temperature I
Frontier Hard Chrome, Sandy Soil
Chrome VI digestion assay
Sample/STD
A540
ppb calc.    Sample #
Blank
            253
            403
            624
            990
           1616
           2494
slope
intercept
RSQ
0.0000
0.2266
0.3766
0.5545
0.8758
1.3130
1 .8437

176.8
385.1
632.2
1078.6
1685.9
2423.1
0.00072
0.099359
0.993468
                                 9
                                10
                                11
                                12
                                13
                                14
ppb calc. dil. Factor ppb in sol
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sol Spike 6
Insol Spike 7
Sample 4+spk
1 .2322
1 .271 1
1.2610
1.2512
1 .2842
0.8637
0.5893
0.7671
1573.6
1627.7
1613.6
1600.0
1645.9
1061.7
680.6
927.6
10.0
10.0
10.0
10.0
10.0
20.0
40.0
20.0
15736.3
16276.7
16136.4
16000.2
16458.6
21234.9
27223.1
18551.2
                                         500     1000     1500    2000    2500    3000
                                                                               Sample Cone.
ave 1-5
16121.6





b recovery
STD DEV
274.34





Range
wet mass
2.5137
2.5016
2.5146
2.5031
2.5034
2.5112
2.4527
ppm Calc.
15.7363
16.2767
16.1364
16.0002
16.4586
21 .2349
27.2231
M9/9 dry
782.9477
798.2081
787.4407
784.2240
806.6009
1037.7231
1361.1122
ave 1-5 STD DEV
791.9 10.2






                                                               63.8
                                                        85-115%
Samples # 1 through 7 had to be re-filtered after bringing pH to the 7 range (because of precipitation).
                                        "') recovery   Range
LCS#15
                                                                                               K2Cr2O7    Cr added
                                                                                               added (mg)   |jg/g dry
                                                                                                 0.5052    246.841
Blank #8
Moisture A
Moisture B
Moisture C
                Tare
              1067
              -126
          Tin + Soil
              107.2
80-120%
19.8132
19.7520
19.7401
22.8038
23.0542
22.9840
wet Tin + Soil
2.9906
3.3022
3.2439
22.2560
22.4510
22.3705
dry
2.4428
2.6990
2.6304
%moisture
18.317
18.267
18.912
                                                                                    PbCrO4
                                                                                  Added (mg)
                                                                                      10.9
                                                                       Cr added
                                                                        M9/9 dry
                                                                         877.3
Spike Recovery %
Solution     Range
    100    75-125%

Spike Recovery %
Solid        Range
    65     75-125%
                                                                   mean
                                                                            % Solid
                                                                   18.499    81.501
                                                                              D52

-------
                Appendix E



Semi-Volatile Organic Compound Extraction Data
                     El

-------
E2

-------
                                                                                     Bedford, Plot 1  PAH Data
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
MSL Sample ID
1790-9abBlkA
1790-9ab Blk Spk A
1790-9aBlkB
1790-9a Blk Spk B
1790-9a-BlkSpkC
1790-9ab-7 MS
1790-9a-12 MS
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9a-10
1790-9a-11
1790-9a-24
1790-9a-25
1790-9a-26
1790-9a-13
1790-9a-14
1790-9a-27
1790-9a-15
1790-9a-16
1790-9a-28
1790-9a-29
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
Extraction Date
12/30/2003
1/6/2004
1/27/2004
3/23/2004
6/15/2004
1/13/2004
2/11/2004
12/30/2003
12/30/2003
12/30/2003
12/30/2003
1/6/2004
1/6/2004
1/6/2004
1/6/2004
1/13/2004
1/13/2004
1/13/2004
1/13/2004
1/28/2004
1/28/2004
1/28/2004
1/28/2004
2/11/2004
2/11/2004
2/11/2004
2/11/2004
3/23/2004
3/23/2004
3/23/2004
3/23/2004
6/15/2004
6/15/2004
6/15/2004
6/15/2004
Analysis Date
1/24/2004
1/24/2004
4/16/2004
4/17/2004
6/18/2004
1/24/2004
4/16/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
4/16/2004
4/16/2004
4/16/2004
4/16/2004
4/17/2004
4/16/2004
4/16/2004
4/17/2004
4/17/2004
4/17/2004
4/17/2004
4/17/2004
6/18/2004
6/18/2004
6/18/2004
6/18/2004
Days held from
Extraction to Analysis
25
18
80
25
3
11
65
25
25
25
25
18
18
18
18
11
11
11
11
79
79
79
79
66
65
65
66
25
25
25
25
3
3
3
3
Storage Temperature
NA
NA
NA
NA
NA
-20C
-20C
-20C
-20C
-20C
-20C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
4C
-20C
-20C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
PAH'S
naphthalene
61.87 U
2019.08
68.76 U
3795.58
3831.39
3097.71
2910.75
356.71
233.04
210.06
331.22
348.04
326.39
156.75
285.33
470.99
364.52
319.9
427.45
453.71
541.59
579.88
547.39
464.54
511.04
458.96
547.97
511.11
557.24
592.68
639.6
509.04
542.46
520.49
485.9



r



r






E





r
r
r
r
r
r
r
r
r
r
r
r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
units are ng/g
                                                                                           E3

-------
BATTELLE MARINE SCIENCES LAi
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                Bedford, Plot 1 PAH Data
       MSL Sample ID
Acenaphthalene
Acenaphthene
                                                                                    Fluorene
dibenzothiophene
phenanthrene
                                                                                                                                                                 anthracene
1790-9abBlkA
1790-9ab BlkSpk A
1790-9aBlkB
1790-9a BlkSpk B
1790-9a-BlkSpkC
1790-9ab-7 MS
1790-9a-12 MS
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9a-10
1790-9a-11
1790-9a-24
1790-9a-25
1790-9a-26
1790-9a-13
1790-9a-14
1790-9a-27
1790-9a-15
1790-9a-16
1790-9a-28
1790-9a-29
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
69.41 U
1877.54
77.13 U r
3610.45 r
3699.63
3131.56
2625.71 r
411.49
352.89
318.61
301.97
403.31
350.42
308.37 E
309.23
531.97
367.33
322.72
516.72
228.88 r
156.33 r
273.18 r
317.02 r
344.12 r
391.55 r
354.09 r
411.37 r
420.37 r
411.83 r
428.63 r
539.83 r
522.37
489.63
450.11
502.42
77.28
2065.63
85.89
4001 .59
3754.82
2730.23
2522.14
82.44
69.73
71.24
74.89
88.39
81.42
72.05
73.46
114.91
78.22
82.63
93.76
74.24
111.07
165.16
184.24
141.91
153.66
133.34
177.51
74.88
75.33
99.08
79.51
90.28
94.48
96.84
92.28
U

U r
r


r

U
U
U

U
U E
U

U
U

U r
r
r
r
r
r
r
r
r
U r
r
U r




50.43 U
1703.59
56.04 U r
3901 .81 r
3618.13
2587.22
2448.42 r
96.77
59.93
46.48 U
79.19
78.98
78.49
47.01 U E
67.94
129.41
51.03 U
53.91 U
76.48
63.03 r
84.66 r
104.72 r
108.02 r
85.04 r
126.65 r
90.43 r
136.52 r
97.34 r
99.5 r
121.14 r
118.3 r
113.47
99.21
90.05
100.57
15.00 U
15.00 U
16.67 U r
98.81 r
33.94
187.89
217.12 r
126.44
102.82
86.46
115.70
120.24
93.68
13.98 U
81.36
183.49
136.57
128.36
172.09
101.08 r
81.42 r
162.34 r
183.19 r
139.84 r
157.68 r
144.74 r
146.00 r
166.26 r
162.85 r
199.88 r
196.16 r
180.26
138.97
160.86
148.68
301.85 U
1997.00
335.46 U r
3976.05 r
3722.66
4747.06
4168.28 r
1724.22
1307.04
1005.31
1705.25
1772.08
1327.29
1159.04
1278.40
2276.67
1548.46
1575.01
2145.24
1769.27 r
2094.31 r
2417.99 r
2326.09 r
1617.68 r
1875.07 r
1669.99 r
1692.81 r
1917.54 r
1834.43 r
2258.36 r
2194.89 r
2351 .42
2196.08
2214.53
2319.56
74.76 U
1755.91
98.96
3957.20
3665.44
3233.47
2828.20
417.40
321.60
270.26
361.10
376.30
308.53
264.45
284.38
523.49
342.12
352.91
466.69
312.3
294.54
434.74
500.22
381.44
453.11
393.5
460.31
471.05
478.29
571.68
560.27
598.39
524.37
492.68
543.22
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
units are ng/g
                                                                                      E4

-------
BATTELLE MARINE SCIENCES LAi
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                  Bedford, Plot 1 PAH Data
       MSL Sample ID
                                   fluoranthene
                                                          pyrene
benzo[a] anthracene
chrysene
benzo [b] fluoranthene
1790-9abBlkA
1790-9ab BlkSpk A
1790-9aBlkB r
1790-9a BlkSpk B r
1790-9a-BlkSpkC
1790-9ab-7 MS
1790-9a-12 MS r
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9a-10 r
1790-9a-11 r
1790-9a-24 r
1790-9a-25 r
1790-9a-26 r
1790-9a-13 r
1790-9a-14 r
1790-9a-27 r
1790-9a-15 r
1790-9a-16 r
1790-9a-28 r
1790-9a-29 r
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
621 .85 U
2120.15
691 .08 U
5073.10
3508.86
12307.40
11210.46
7686.81
6005.38
5000.55
7862.68
7746.39
5564.92
5323.41
6038.10
9622.91
7074.77
7111.59
9547.98
7574.75
8308.18
10528.31
9903.44
6904.57
8109.25
7433.89
7615.36
8729.33
8631 .98
9319.07
9966.47
8468.45
8148.56
8114.49
8089.78
r 300.02 U r
2480.94
r 333.42 U r
r 4437.86 r
3566.22
12483.48
r 10266.99 r
7805.67
r 6195.85 r
r 5260.90 r
r 8143.23 r
r 8292.86 r
5948.03
5669.79
6473.97
10026.36
7608.21
7574.17
10044.03
r 7582.4 r
r 8399.1 r
r 10057 r
r 9326.91 r
r 6387.68 r
r 7481 .37 r
r 6858.53 r
r 7079.51 r
r 8172.63 r
r 7977.11 r
r 8614.85 r
r 9193.17 r
8795.07
8491 .29
8365.28
8264.93
113.02 U
1730.21
125.60 U
5700.57
3387.77
9640.52
10897.84
5471.76
4540.26
3849.66
5487.89
5813.48
4115.97
3908.43
4677.71
7091.81
5339.21
5359.7
6911.24
5755.59
5177.65
8524.09
8589.05
5893.57
6946.89
6649.17
6788.77
7812.02
7929.62
8338.62
8764.77
7091.42
6557.53
6371.32
6387.88
r 108.81 U r
2065.82
r 120.92 U r
r 4658.01 r
3440.73
10245.19
r 9189.71 r
5900.89
r 4973.34 r
r 4190.35 r
r 6046.56 r
r 6298.97 r
4478.80
4288.50
5171.30
7626.49
5749.16
5787.72
7533.94
r 5244.74 r
r 5264.72 r
r 7816.97 r
r 7494.29 r
r 5101.89 r
r 6037.52 r
r 5712.87 r
r 5821 .2 r
r 6742.49 r
r 6653.69 r
r 7105.63 r
r 7577.42 r
7674.34
7262.26
7076.98
7180.47
104.60 U
1712.54
116.25 U
4698.79
2938.85
11126.34
10316.46
7500.36
6478.63
5509.08
8124.27
7973.28
5789.67
5463.25
6752.95
9583.58
7246.62
7421 .37
9620.56
5008.71
6635.7
8132.03
8222.01
5821.14
7059.88
14381.88
6914.14
7246.9
7849.52
18159.77
19400.7
7837.37
7305.1
7058.63
7096.91
r
r
r
r


r

r
r
r
r
r

r




r
r
r
r
r
r
r
r
r
r
r
r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
units are ng/g
                                                                                       E5

-------
BATTELLE MARINE SCIENCES LAi
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                  Bedford, Plot 1 PAH Data
       MSL Sample ID
benzo [k] fluoranthene
benzo [a] pyrene
indeno [1,2,3-c,d] pyrene
di benzo [a,h] anthracene
1790-9abBlkA
1790-9ab BlkSpk A
1790-9aBlkB
1790-9a BlkSpk B
1790-9a-BlkSpkC
1790-9ab-7 MS
1790-9a-12 MS
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9a-10
1790-9a-11
1790-9a-24
1790-9a-25
1790-9a-26
1790-9a-13
1790-9a-14
1790-9a-27
1790-9a-15
1790-9a-16
1790-9a-28
1790-9a-29
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
108.72 U r
1839.42 r
120.82 U r
3689.19 r
3034.41
6379.44
7393.42 r
3052.81
2584.58 r
2198.53 r
3211.47 r
3229.73 r
2356.97 r
2277.27
2724.74 r
3908.2
2870.17
3043.93
3828.22
5164.13 r
6452.6 r
7559.04 r
7021 .7 r
4663.85 r
5500.44 r
5131.01 r
5308.7 r
6418.09 r
6171.74 r
6503.53 r
6950.65 r
9128.14
8292.84
8154.28
8366.57
112.84 U r
1755.44 r
125.40 U r
4043.96 r
3217.64
9995.82
10661.06 r
6347.75
5446.99
4643.88
6732.79
6816.61
4857.24
4618.76
5694.93
8100.9
6139.64
6350.35
8213.51
6768.34 r
7916.9 r
10131.73 r
9857.93 r
6526.98 r
7727.15 r
7142.18 r
7517.12 r
8554.36 r
8618.45 r
9123.51 r
9779.33 r
11082.57
10175.2
10054.83
9936.05
137.85 U r
1458.95 r
153.20 U r
4259.32 r
2616.74
7478.81
13883.72 r
4855.15
4225.68
3598.97
5137.14
5163.73
3766.98
3566.08
4339.55
6147.07
4661.41
4808.89
6317.43
7072.32 r
8150.99 r
11082.41 r
11397.56 r
8052.33 r
9553.32 r
8871.31 r
9493.65 r
10254.97 r
10967.84 r
11490.11 r
12275.79 r
12300.57
11136.57
10615.47
10925.72
116.74 U
1313.65
129.73 U
4067.17
2781.19
3591.30
4786.74
1018.65
919.76
780.57
1077.08
1090.74
796.74
748.58
904.40
1354.67
1000.13
1018.33
1349.62
616.13
357.67
1080.17
1271.46
1727.75
499.31
1996.6
1317.39
1179.01
1461.56
1575.29
670.58
1801.84
1595.37
1443.81
1494.43
r
r
r
r


r












r
r
r
r
r
r
r
r
r
r
r
r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
units are ng/g
                                                                                        E6

-------
                                                                                Bedford, Plot 1 PAH Data
BATTELLE MARINE SCIENCES LAi
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
       MSL Sample ID
benzo[g,h,i] perylene
Surrogate Recovery
  d8 naphthalene
d10 Acenaphthene
d10 phenanthrene
d12 chrysene
1790-9abBlkA
1790-9ab BlkSpk A
1790-9aBlkB
1790-9a BlkSpk B
1790-9a-BlkSpkC
1790-9ab-7 MS
1790-9a-12 MS
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9a-10
1790-9a-11
1790-9a-24
1790-9a-25
1790-9a-26
1790-9a-13
1790-9a-14
1790-9a-27
1790-9a-15
1790-9a-16
1790-9a-28
1790-9a-29
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
127.43 U r
1602.09 r
141.61 U r
3762.39 r
3161.24
7593.96
7993.97 r
4449.29
3857.71
3304.13
4738.92
4791.46
3474.15
3301.79
4018.31
5638.97
4317.52
4435.1
5785.88
4420.88 r
5534.88 r
7062.56 r
6646.32 r
4647.28 r
5608.1 r
5134.06 r
5526.72 r
6058.37 r
6319.68 r
6500.29 r
7159.8 r
8369.36
7774.11
7711.21
7746.62
81.60%
65.50%
102.90% r
95.30% r
102.80%
83.20%
160.60% # r
65.60%
55.40%
58.80%
84.70%
69.40%
65.10%
39.10% #
63.40%
89.40%
72.60%
74.30%
80.40%
88.50% r
103.40% r
108.50% r
101.90% r
149.20% r
173.90% # r
157.40% # r
162.30% # r
85.70% r
84.70% r
85.80% r
91.40% r
93.60%
103.30%
107.90%
104.40%
80.40%
64.40%
100.50% r
99.90% r
102.20%
84.20%
167.10% # r
64.90%
56.20%
54.00%
82.30%
71.10%
64.20%
46.20% #
63.50%
92.20%
74.50%
74.30%
81.90%
88.10% r
98.70% r
112.30% r
101.90% r
154.30% # r
178.70% # r
164.20% # r
170.90% # r
89.70% r
89.90% r
90.10% r
96.60% r
98.40%
107.90%
112.00%
108.20%
80.80%
63.50%
106.60% r
110.50% r
100.40%
89.60%
179.70% # r
68.80%
59.90%
51 .60%
85.20%
76.30%
59.50%
54.20%
61 .00%
98.50%
74.10%
74.40%
87.00%
90.30% r
99.40% r
120.20% r
108.70% r
162.20% # r
187.10% # r
176.50% # r
179.00% # r
100.50% r
96.20% r
97.10% r
104.30% r
106.70%
116.40%
117.80%
115.40%
39.10%
51.80%
217.70%
147.90%
93.00%
97.70%
191.20%
85.80%
35.10%
32.00%
38.60%
290.10%
60.60%
102.10%
50.30%
133.90%
93.60%
92.00%
104.50%
155.30%
138.70%
138.80%
270.80%
158.90%
193.10%
171.30%
184.60%
117.60%
106.20%
108.00%
117.20%
137.20%
281.50%
132.20%
144.40%
#

#



#

#
#
#
#







#


#
#
#
#
#





#




r
r


r












r
r
r
r
r
r
r
r
r
r
r
r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
units are ng/g
                                                                                      E7

-------
                                                                                 Bedford, Plot 1  PAH Data
BATTELLE MARINE SCIENCES LAi
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
       MSL Sample ID
d12 perylene
Internal Std. Recovery
 d8 acenaphthylene
d10 pyrene
d12 benzo [a] pyrene
1790-9abBlkA
1790-9ab BlkSpk A
1790-9aBlkB
1790-9a BlkSpk B
1790-9a-BlkSpkC
1790-9ab-7 MS
1790-9a-12 MS
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9a-10
1790-9a-11
1790-9a-24
1790-9a-25
1790-9a-26
1790-9a-13
1790-9a-14
1790-9a-27
1790-9a-15
1790-9a-16
1790-9a-28
1790-9a-29
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
46.80% #
37.70% #
141.40% r
89.60% r
76.00%
58.70%
149.00% r
85.70%
39.60%
35.10% #
45.00% #
151.60% #
40.80% #
75.80%
40.30% #
121.30%
71 .50%
70.00%
92.50%
78.50% r
60.40% r
82.80% r
113.40% r
107.70% r
147.10% r
122.20% r
132.70% r
80.10% r
60.30% r
62.60% r
67.80% r
111.60%
127.00%
118.80%
102.70%
151.50%
146.40%
100.00%
97.40%
83.70%
139.00%
123.70%
172.40%
189.50%
180.30%
140.00%
169.40%
158.90%
148.90%
179.90%
125.20%
146.90%
144.80%
161.80%
120.50%
87.80%
96.10%
105.00%
132.70%
115.80%
125.70%
139.10%
111.30%
191.90%
106.90%
103.40%
87.00%
79.50%
80.90%
81.70%
123.10%
121.10%
r 80.30% r
r 75.90% r
58.80%
121.90%
r 95.10% r
144.10%
157.40%
151.80%
117.30%
142.30%
134.10%
123.10%
147.40%
108.10%
123.90%
121.80%
136.20%
r 94.70% r
r 70.10% r
r 75.50% r
r 82.70% r
r 100.80% r
r 88.60% r
r 96.80% r
r 103.40% r
r 86.60% r
r 141.50% r
r 81 .00% r
r 78.70% r
64.20%
58.60%
60.50%
60.30%
137.30%
103.30%
90.30%
121.40%
72.40%
143.10%
177.80%
168.00%
185.20%
178.30%
130.90%
166.90%
156.50%
144.50%
172.70%
129.20%
149.20%
142.40%
159.80%
150.30%
77.20%
123.50%
143.20%
178.10%
156.40%
173.10%
189.00%
152.00%
267.30% #
146.10%
142.70%
94.50%
85.00%
86.90%
86.80%


r
r


r












r
r
r
r
r
r
r
r
r
r
r
r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
units are ng/g
                                                                                       E8

-------
                                                                                         QC
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
MSL Sample ID Extraction Date
BLANKS
1790-9ab Blk A 12/30/2003
1790-9a Blk B 1/27/2004
BLANK SPIKES
1790-9ab Blk Spk A 1/6/2004
1790-9a Blk Spk B 3/23/2004
1790-9a-Blk Spk C 6/15/2004
Spike concentration A
Spike concentration B
Spike concentration C
percent recovery A
percent recovery B
percent recovery C
MATRIX SPIKES
1790-9 Average NA
1790-9ab-7 MS 1/13/2004
1790-9a-12 MS 2/11/2004
Spike concentration 7
Spike concentration 1 2
percent recovery 7
percent recovery 1 2
Days held from
Analysis Date Extraction to Analysis

1/24/2004 25
4/16/2004 80

1/24/2004 18
4/17/2004 25
6/18/2004 3







NA NA
1/24/2004 11
4/16/2004 65




PAH'S
Storage Temperature naphthalene

NA 61.87 U
NA 68.76 U

NA 2019.08
NA 3795.58
NA 3831 .39
3000.00
3333.40
3333.40
67.30%
113.87%
114.94%

NA 439.07
-20C 3097.71
-20C 2910.75
3080.60
3184.80
86.30%
77.61%
Acenaphthalene

69.41 U
r 77.13 U

1877.54
r 3610.45
3699.63
3000.00
3333.40
3333.40
62.58%
108.31%
110.99%

383.46
3131.56
r 2625.71
3080.60
3184.80
89.21%
70.40%
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
R=data is rejected
r=data is an estimate
                                                                                    E9

-------
                                                                                   QC
BA TTELLE MARINE SCIENCES LA
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
       MSL Sample ID
Acenaphthene
                         Fluorene
dibenzothiophene
phenanthrene
                                                                                               anthracene
                                                                                                                    fluoranthene
BLANKS
1790-9ab Blk A
1790-9a Blk B r

77.28
85.89

U
U r

50.43
56.04

U
U r

15.00
16.67

U
U r

301.85
335.46

U
U r

74.76 U
98.96 r

621 .85
691 .08

U
U
BLANK SPIKES
          1790-9ab Blk Spk A
           1790-9a Blk Spk B
           1790-9a-Blk Spk C
         Spike concentration A
         Spike concentration B
         Spike concentration C
            percent recovery A
            percent recovery B
            percent recovery C
2065.63
4001 .59 r
3754.82
3000.00
3333.40
3333.40
68.85%
120.05% #
112.64%
1703.59
3901 .81
3618.13
3000.00
3333.40
3333.40
56.79%
117.05%
108.54%
15.00 U
98.81 r
33.94
NA
NA
NA
NA
NA
NA
1997.00
3976.05
3722.66
3000.00
3333.40
3333.40
66.57%
119.28%
111.68%
1755.91
3957.20 r
3665.44
3000.00
3333.40
3333.40
58.53%
118.71%
109.96%
2120.15
5073.10
3508.86
3000.00
3333.40
3333.40
70.67%
152.19%
105.26%
MATRIX SPIKES
              1790-9 Average
               1790-9ab-7 MS
               1790-9a-12 MS
         Spike concentration 7
        Spike concentration 12
            percent recovery 7
           percent recovery 12
80.42
2730.23
2522.14
3080.60
3184.80
86.02%
76.67%
82.35
2587.22
r 2448.42
3080.60
3184.80
81.31%
74.29%
136.34
187.89
217.12 r
NA
NA
NA
NA
1841.93
4747.06
4168.28
3080.60
3184.80
94.30%
73.05%
419.98
3233.47
2828.20 r
3080.60
3184.80
91 .33%
75.62%
7872.55
12307.40
11210.46
3080.60
3184.80
143.96%
104.81%
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
R=data is rejected
r=data is an estimate
                                                                               E10

-------
BA TTELLE MARINE SCIENCES LA
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
                                                                                     QC
       MSL Sample ID
                                   pyrene
benzo[a] anthracene
chrysene
benzo [b] fluoranthene
benzo [k] fluoranthene
BLANKS
1790-9ab Blk A
1790-9a Blk B
BLANK SPIKES
1790-9ab Blk Spk A
1790-9a Blk Spk B
1790-9a-Blk Spk C
Spike concentration A
Spike concentration B
Spike concentration C
percent recovery A
percent recovery B
percent recovery C
MATRIX SPIKES
1790-9 Average
1790-9ab-7 MS
1790-9a-12 MS
Spike concentration 7
Spike concentration 1 2
percent recovery 7
percent recovery 1 2

r 300.02 U r
r 333.42 U r

2480.94
r 4437.86 r
3566.22
3000.00
3333.40
3333.40
82.70%
133.13% #
106.98%

7860.35
12483.48
r 10266.99 r
3080.60
3184.80
150.07% #
75.57%

113.02 U
125.60 U

1730.21
5700.57
3387.77
3000.00
3333.40
3333.40
57.67%
171.01% #
101.63%

6290.90
9640.52
10897.84
3080.60
3184.80
108.73%
144.65% #

r 108.81 U r
r 120.92 U r

2065.82
r 4658.01 r
3440.73
3000.00
3333.40
3333.40
68.86%
139.74% #
103.22%

6207.63
10245.19
r 9189.71 r
3080.60
3184.80
131.06% #
93.63%

104.60 U r
116.25 U r

1712.54 r
4698.79 r
2938.85
3000.00
3333.40
3333.40
57.08%
140.96% #
88.16%

8271 .21
11126.34
10316.46 r
3080.60
3184.80
92.68%
64.22%

108.72 U
120.82 U

1839.42
3689.19
3034.41
3000.00
3333.40
3333.40
61.31%
110.67%
91 .03%

5074.07
6379.44
7393.42
3080.60
3184.80
42.37% #
72.83%

r
r

r
r










r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
R=data is rejected
r=data is an estimate
                                                                                Ell

-------
BA TTELLE MARINE SCIENCES LA
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
                                                                                      QC
       MSL Sample ID
benzo [a] pyrene
indeno [1,2,3-c,d] pyrene
dibenzo [a,h] anthracene
benzo[g,h,i] perylene
BLANKS
1790-9ab Blk A
1790-9a Blk B
BLANK SPIKES
1790-9ab Blk Spk A
1790-9a Blk Spk B
1790-9a-Blk Spk C
Spike concentration A
Spike concentration B
Spike concentration C
percent recovery A
percent recovery B
percent recovery C
MATRIX SPIKES
1790-9 Average
1790-9ab-7 MS
1790-9a-12 MS
Spike concentration 7
Spike concentration 1 2
percent recovery 7
percent recovery 1 2

112.84 U r
125.40 U r

1755.44 r
4043.96 r
3217.64
3000.00
3333.40
3333.40
58.51%
121.32% #
96.53%

7674.14
9995.82
10661.06 r
3080.60
3184.80
75.36%
93.79%

137.85 U r
153.20 U r

1458.95 r
4259.32 r
2616.74
3000.00
3333.40
3333.40
48.63%
127.78% #
78.50%

7865.32
7478.81
13883.72 r
3080.60
3184.80
-12.55% #
188.97% #

116.74 U r
129.73 U r

1313.65 r
4067.17 r
2781.19
3000.00
3333.40
3333.40
43.79%
122.01% #
83.43%

1148.13
3591.30
4786.74 r
3080.60
3184.80
79.31%
114.25%

127.43 U
141.61 U

1602.09
3762.39
3161.24
3000.00
3333.4
3333.4
53.40%
112.87%
94.84%

5511.91
7593.96
7993.97
3080.60
3184.80
67.59%
77.93%

r
r

r
r










r




#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
R=data is rejected
r=data is an estimate
                                                                                 E12

-------
                                                                                 QC
BA TTELLE MARINE SCIENCES LA
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
       MSL Sample ID
Surrogate Recovery
  d8 naphthalene
d10 Acenaphthene
d10 phenanthrene
d12 chrysene
d12 perylene
BLANKS
1790-9ab Blk A
1790-9a Blk B

81 .60%
102.90% r

80.40%
100.50% r

80.80%
106.60% r

39.10%
217.70%

#
# r

46.80% #
141.40%


r
BLANK SPIKES
          1790-9ab Blk Spk A
           1790-9a Blk Spk B
           1790-9a-Blk Spk C
         Spike concentration A
         Spike concentration B
         Spike concentration C
           percent recovery A
           percent recovery B
           percent recovery C
MATRIX SPIKES
             65.50%
             95.30%
            102.80%
             64.40%
             99.90%
            102.20%
           63.50%
          110.50%      r
          100.40%
        51.80%
       147.90%       r
        93.00%
      37.70%
      89.60%
      76.00%
              1790-9 Average
              1790-9ab-7 MS
              1790-9a-12 MS
         Spike concentration 7
        Spike concentration 12
            percent recovery 7
           percent recovery 12
             83.20%
            160.60%
             84.20%
            167.10%   #   r
           89.60%
          179.70%  #   r
        97.70%
       191.20%   #   r
      58.70%
     149.00%       r
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
R=data is rejected
r=data is an estimate
                                                                            E13

-------
                                                                                 QC
BA TTELLE MARINE SCIENCES LA
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
       MSL Sample ID
Internal Std. Recovery
 d8 acenaphthylene
d10 pyrene
d12 benzo [a] pyrene
BLANKS
              1790-9ab Blk A
               1790-9a Blk B
BLANK SPIKES
          1790-9ab Blk Spk A
           1790-9a Blk Spk B
           1790-9a-Blk Spk C
         Spike concentration A
         Spike concentration B
         Spike concentration C
           percent recovery A
           percent recovery B
           percent recovery C
               151.50%
               100.00%
               146.40%
                97.40%
                83.70%
     123.10%
      80.30%
     121.10%
      75.90%
      58.80%
              137.30%
               90.30%
              103.30%
              121.40%
               72.40%
MATRIX SPIKES
              1790-9 Average
              1790-9ab-7 MS
              1790-9a-12 MS
         Spike concentration 7
        Spike concentration 12
            percent recovery 7
           percent recovery 12
               139.00%
               123.70%
     121.90%
      95.10%
              143.10%
              177.80%
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
R=data is rejected
r=data is an estimate
                                                                            E14

-------
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564

Units are ng/g
                                                                                         Eagle Harbor
PAH Results
Storage
MSL Sample ID Extraction Date Days held to extraction Analysis Date Temperature
1790-7 Blankl
1790-7 Blank 2
1790-7-7 MS
1790-7 -12 MS
1790 Spike Blank B
1790-7 Spike Blank C
1790-7-1
1790-7-2
1790-7-3
1790-7-4
1790-7-6
1790-7-21
1790-7-22
1790-7-8
1790-7-9
1790-7-23
1790-7-10
1790-7-11
1790-7-25
1790-7-26
1790-7-13
1790-7-14
1790-7-27
1790-7-28
1790-15
1790-16
1790-29
1790-30
1790-7-17
1790-7-18
1790-7-31
1790-7-32
r=data points rejected
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
11/25/2002
12/2/2002
12/9/2002
1/6/2003
2/17/2003
5/12/2003
11/25/2002
11/25/2002
11/25/2002
11/25/2002
12/2/2002
12/2/2002
12/2/2002
12/9/2002
12/9/2002
12/9/2002
12/23/2002
12/23/2002
12/23/2002
12/23/2002
1/6/2003
1/6/2003
1/6/2003
1/6/2003
2/17/2003
2/17/2003
2/17/2003
2/17/2003
5/12/2003
5/12/2003
5/12/2003
5/12/2003




0
7
14
42
84
168
0
0
0
0
7
7
7
14
14
14
28
28
28
28
42
42
42
42
84
84
84
84
168
168
168
168




1/17/2003
1/18/2003
1/18/2003
2/5/2003
3/21/2003
5/20/2003
1/17/2003
1/17/2003
1/17/2003
1/18/2003
1/18/2003
1/18/2003
1/18/2003
1/18/2003
1/18/2003
1/18/2003
2/5/2003
2/5/2003
2/5/2003
2/5/2003
2/6/2003
2/6/2003
2/6/2003
2/6/2003
3/21/2003
3/21/2003
3/21/2003
3/21/2003
5/20/2003
5/20/2003
5/21/2003
5/21/2003




NA
NA
-20C
-20C
NA
NA
-20C
-20C
-20C
-20C
-20C
4C
4C
-20C
-20C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C




1 methyl 2 methyl
naphthalene napthalene naphthalene Acenaphthalene Acenaphthene
30.08 U
26.77 U
1011.31
756.00
358.12
220.93
414.60
540.55
600.79
400.87
548.30
568.24
365.11
472.49
476.59
507.28
1344.00
595.06
504.54
744.01
465.53
544.55
441.98
866.39
251.84 E
255.26 E
241.9
169.48 E
561.87
479.5
461.31
340.76




72.44
46.75
465.73
516.97
27.47 U
55.12
393.68
503.18
573.80
356.90 B
469.83 B
457.21 B
319.23 B
424.58 B
462.47 B
407.35 B
947.59
413.74
368.32
349.17
399.02
466.12
319.11
260.15
194 E
206.11 E
175.7
128.31 E
470.4
417.86
300.94
237.74




30.08 U
26.77 U
135.22
143.02
27.47 U
26.94 U
109.56
142.71
218.59
105.84
129.73
122.94
86.74
129.44
136.00
99.13
224.22
122.58
84.34
79.28
109.03
129.48
69.96
58.48
60.83 E
64.68 E
46.28
32.17 E
133.24
129.75
71.34
56.04




30.08 U
26.77 U
632.34
66.38
407.05
173.12
96.25
108.30
239.58
87.48
91.81
59.38
72.78
119.12
108.16
92.13
73.08
52.89
53.76
62.99
47.14
56.8
70.02
475.89
68.36
74.83
87.78
76.45
44.49
46.07
46.36
33.33




30.08 U
26.77 U
1759.96
1121.60
425.33
217.42
885.19
1233.00
2941.64
943.63
1127.31
1038.78
786.28
1152.16
1191.81
977.36
1459.65
1031.89
1108.38
911.03
868.1
1029.91
866.38
801.03
583.81
694.23
772.48
525.26
1112.3
1118.02
232.99
206.43




B=blank Contamination
E=Estimate
units are ng/g
        Eagle Harbor
                                                                                             E15

-------
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564

Units are ng/g
                                                                                         Eagle Harbor
MSL Sample ID Extraction Date Days held to extraction Fluorene dibenzothiophene phenanthrene anthracene 1 methyl phenanthrene fluoranthene
1790-7 Blankl
1790-7 Blank 2
1790-7 -7 MS
1790-7 -12 MS
1790 Spike Blank B
1790-7 Spike Blank C
1790-7-1
1790-7-2
1790-7-3
1790-7-4
1790-7-6
1790-7-21
1790-7-22
1790-7-8
1790-7-9
1790-7-23
1790-7-10
1790-7-11
1790-7-25
1790-7-26
1790-7-13
1790-7-14
1790-7-27
1790-7-28
1790-15
1790-16
1790-29
1790-30
1790-7-17
1790-7-18
1790-7-31
1790-7-32
r=data points rejected
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
11/25/2002
12/2/2002
12/9/2002
1/6/2003
2/17/2003
5/12/2003
11/25/2002
11/25/2002
11/25/2002
11/25/2002
12/2/2002
12/2/2002
12/2/2002
12/9/2002
12/9/2002
12/9/2002
12/23/2002
12/23/2002
12/23/2002
12/23/2002
1/6/2003
1/6/2003
1/6/2003
1/6/2003
2/17/2003
2/17/2003
2/17/2003
2/17/2003
5/12/2003
5/12/2003
5/12/2003
5/12/2003




0
7
14
42
84
168
0
0
0
0
7
7
7
14
14
14
28
28
28
28
42
42
42
42
84
84
84
84
168
168
168
168




30.08 U
26.77 U
2134.82
1301.68
497.85
208.63
1121.86
1554.81
3576.40
1132.80
1420.91
1338.98
985.71
1440.18
1455.52
1184.71
1865.24
1190.06
1156.54
952.09
1088.4
1202.57
797.04
890.06
924.98
1121.3
772.99
569.63
1359.36
1256.76
245.9
202.52




30.08 U
26.77 U
505.49
435.50
27.47
26.94
367.67
488.07
1684.57
373.65
445.94
437.27
323.55
454.67
446.17
274.33
567.36
385.39
292.87
220.85
347.81
349.56
210.22
135.49
263.77
312.21
139.69
84.46
400.07
378.64
84.93
70.61




30.08 U
26.77 U
6171.75
4635.26
500.45
232.66
4190.02
5412.64
19204.57
3988.23
4961.24
4893.29
3540.91
5169.25
4992.05
3413.68
6448.62
4270.59
3462.42
2222.76
3923.44
4396.62
2193.86
1750.91
3286.88
3994.97
1760.66
1099.66
5029.06
4385.68
1006.12
815.84




30.08 U
26.77 U
3008.51
1593.60
476.33
184.66
1686.64
1756.17
3170.17
1234.44
1594.90
1533.30
1516.32
1709.13
1731.91
1629.72
4607.50
1243.26
1305.88
1361.93
1185.15
1251.94
1253.47
1335.66
1042.89
1191.33
1210.83
1829.3
1946.81
1281.15
492.24
530.64




30.08 U
26.77 U
549.64
389.70
27.47
26.94
411.60
477.63
1321.12
370.78
422.19
474.32
377.41
464.60
457.19
471.99
498.64
333.59
417.64
376.04
347.05
372.09
374.45
310.85
304.41
347.38
435.59
344.3
454.15
389.35
297.76
286.39




30.08 U
26.77 U
8044.54
6695.10
559.97
218.95
6462.21
7317.84
17596.65
5733.24
6334.23
7188.55
6133.64
6824.85
6367.32
6925.52
7489.70
6113.67
7279.30
6209.34
5376.97
6460.04
6443.24
6065.62
5039.82
5684.69
6563.86
5635.82
6700.98
5889.1
2858.61
2656.96




B=blank Contamination
E=Estimate
units are ng/g
        Eagle Harbor
                                                                                             E16

-------
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564

Units are ng/g
                                                                                         Eagle Harbor
benzo[a] benzo [b] benzo [k] benzo [a] indeno [1,2,3-
MSL Sample ID Extraction Date Days held to extraction pyrene anthracene chrysene fluoranthene fluoranthene pyrene c,d] pyrene
1790-7 Blankl
1790-7 Blank 2
1790-7 -7 MS
1790-7 -12 MS
1790 Spike Blank B
1790-7 Spike Blank C
1790-7-1
1790-7-2
1790-7-3
1790-7-4
1790-7-6
1790-7-21
1790-7-22
1790-7-8
1790-7-9
1790-7-23
1790-7-10
1790-7-11
1790-7-25
1790-7-26
1790-7-13
1790-7-14
1790-7-27
1790-7-28
1790-15
1790-16
1790-29
1790-30
1790-7-17
1790-7-18
1790-7-31
1790-7-32
r=data points rejected
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
11/25/2002
12/2/2002
12/9/2002
1/6/2003
2/17/2003
5/12/2003
11/25/2002
11/25/2002
11/25/2002
11/25/2002
12/2/2002
12/2/2002
12/2/2002
12/9/2002
12/9/2002
12/9/2002
12/23/2002
12/23/2002
12/23/2002
12/23/2002
1/6/2003
1/6/2003
1/6/2003
1/6/2003
2/17/2003
2/17/2003
2/17/2003
2/17/2003
5/12/2003
5/12/2003
5/12/2003
5/12/2003




0
7
14
42
84
168
0
0
0
0
7
7
7
14
14
14
28
28
28
28
42
42
42
42
84
84
84
84
168
168
168
168




30.08 U
26.77 U
5950.21
4752.94
527.97
228.92
4886.71
5304.42
12472.52
4229.30
4592.64
5180.74
4503.45
4967.59
4631.72
5018.87
5315.51
4309.58
5264.50
4545.92
3870.80
4685.71
4601.16
4854.68
3500.82
3969.53
4855.97
4138.68
4856.32
4330.06
4525.13
4160.66




30.08
26.77
2296.21
1411.66
497.14
190.47
1714.13
1626.99
2790.85
1473.37
1356.69
1551.61
1426.87
1612.01
1461.18
1616.48
1465.52
1343.52
1627.69
1363.11
1148.56
1405.7
1346.67
1906.24
1185.63
1312.3
1302.99
1431.05
1412.87
1184.24
1386.34
1097.79




30.08 U
26.77 U
2606.94
1766.36
600.11
207.06
2210.96
2040.51
3323.71
1825.36
1735.59
2181.18
1933.55
1992.81
1821.34
1918.12
1917.08
1773.36
1944.41
1684.47
1432.65
1757.31
1703.81
2208.55
1544.43
1657.89
1844.96
2091.06
1800.09
1776.22
1856.34
1389.18




30.08 U
26.77 U
3110.67 r
2014.07
581.36
189.13
2537.48
2225.11
2933.74
2179.77
1776.00
2144.13
1902.71
1901.67 r
1758.53 r
1948.57 r
2024.18
1913.26
2299.81
1960.96
1645.53
2129.9
1928.87
2925.32
1889.19
1854.64
1972.67
2024.1
1483.94
1316.61
1539.25
1179.54




30.08 U
26.77 U
3063.93 r
1716.88
579.20
197.04
2501.76
2192.41
2889.37
2148.40
1750.55
2113.28
1877.41
1873.12 r
1734.44 r
1921.20 r
1727.24
1629.18
1962.53
1670.07
1399.59
1815.66
1640.08
2506.68
1883.85
1846.73
1960.13
2019.26
492.82
438.63
517.94
393.84




30.08 U
26.77 U
1361.45 r
713.42
512.73
163.41
942.67
879.51
1177.05
862.20
719.68
849.18
771.37
768.59 r
706.70 r
793.53 r
706.98
671.90
797.85
684.82
591.47
717.66
666.7
1113.2
648.89
774.79
792.27
806.31
744
749.38
760.98
612.39




30.08
26.77
1423.83
404.42
475.26
132.50
671.87
649.27
848.43
689.24
546.91
683.92
643.69
646.88
580.14
671.71
356.75
378.89
440.86
393.14
326.04
418.05
368.15
886.57
493.35
388.66
398.6
417.31
464.73
656.52
530.57
377.86




U
U
r


E

r
r
r
r

r
r
r
r




















B=blank Contamination
E=Estimate
units are ng/g
        Eagle Harbor
                                                                                             E17

-------
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564

Units are ng/g
                                                                                         Eagle Harbor
dibenzo
[a,h] benzo [g,h,i]
MSL Sample ID Extraction Date Days held to extraction anthracene perylene
1790-7 Blankl
1790-7 Blank 2
1790-7 -7 MS
1790-7 -12 MS
1790 Spike Blank B
1790-7 Spike Blank C
1790-7-1
1790-7-2
1790-7-3
1790-7-4
1790-7-6
1790-7-21
1790-7-22
1790-7-8
1790-7-9
1790-7-23
1790-7-10
1790-7-11
1790-7-25
1790-7-26
1790-7-13
1790-7-14
1790-7-27
1790-7-28
1790-15
1790-16
1790-29
1790-30
1790-7-17
1790-7-18
1790-7-31
1790-7-32
r=data points rejected
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
11/25/2002
12/2/2002
12/9/2002
1/6/2003
2/17/2003
5/12/2003
11/25/2002
11/25/2002
11/25/2002
11/25/2002
12/2/2002
12/2/2002
12/2/2002
12/9/2002
12/9/2002
12/9/2002
12/23/2002
12/23/2002
12/23/2002
12/23/2002
1/6/2003
1/6/2003
1/6/2003
1/6/2003
2/17/2003
2/17/2003
2/17/2003
2/17/2003
5/12/2003
5/12/2003
5/12/2003
5/12/2003




0
7
14
42
84
168
0
0
0
0
7
7
7
14
14
14
28
28
28
28
42
42
42
42
84
84
84
84
168
168
168
168




30.08 U
26.77 U
1124.54 r
161.52
412.66
110.56 E
330.48
323.50 r
85.84 r
86.61 r
271.76 r
309.10
309.48 r
324.75 r
287.99 r
328.92 r
136.90
146.66
171.41
154.12
120.36
161.25
147.77
640.21
143.83
126.4
134.31
142.76
103.7
133.15
121.29
81.78




30.08 U
26.77 U
1 372.52 r
427.05
372.22
95.89 E
650.95
600.97 r
784.55 r
661.70 r
515.55 r
674.31
605.58 r
610.77 r
543.59 r
617.80 r
366.24
400.85
461.66
416.72
347.92
448.72
391.87
932.72
574.36
403.84
437.68
450.97
357.1
557.14
388.35
273.17




B=blank Contamination
E=Estimate
units are ng/g
        Eagle Harbor
                                                                                             E18

-------
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564

Units are ng/g
                                                                                         Eagle Harbor
Surrogate PR
dill
MSL Sample ID Extraction Date Days held to extraction (IS naphthalene Acenaphthene
1790-7 Blankl
1790-7 Blank 2
1790-7 -7 MS
1790-7 -12 MS
1790 Spike Blank B
1790-7 Spike Blank C
1790-7-1
1790-7-2
1790-7-3
1790-7-4
1790-7-6
1790-7-21
1790-7-22
1790-7-8
1790-7-9
1790-7-23
1790-7-10
1790-7-11
1790-7-25
1790-7-26
1790-7-13
1790-7-14
1790-7-27
1790-7-28
1790-15
1790-16
1790-29
1790-30
1790-7-17
1790-7-18
1790-7-31
1790-7-32
r=data points rejected
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
11/25/2002
12/2/2002
12/9/2002
1/6/2003
2/17/2003
5/12/2003
11/25/2002
11/25/2002
11/25/2002
11/25/2002
12/2/2002
12/2/2002
12/2/2002
12/9/2002
12/9/2002
12/9/2002
12/23/2002
12/23/2002
12/23/2002
12/23/2002
1/6/2003
1/6/2003
1/6/2003
1/6/2003
2/17/2003
2/17/2003
2/17/2003
2/17/2003
5/12/2003
5/12/2003
5/12/2003
5/12/2003




0
7
14
42
84
168
0
0
0
0
7
7
7
14
14
14
28
28
28
28
42
42
42
42
84
84
84
84
168
168
168
168




97.13%
67.13%
91 .00%
88.25%
63.38%
73.38%
58.38%
91 .00%
90.75%
64.88%
82.13%
83.25%
68.38%
86.63%
88.50%
81.13%
99.13%
86.75%
94.00%
87.50%
72.50%
94.25%
84.13%
82.00%
40.00% #
43.75% #
54.75%
41.50% #
83.88%
77.38%
84.25%
73.25%




95.75%
67.75%
96.75%
85.63%
74.50%
77.25%
59.63%
94.75%
91.13%
65.75%
86.00%
85.00%
73.13%
91.88%
93.50%
86.50%
95.63%
84.00%
91.88%
84.50%
70.63%
90.13%
84.13%
80.50%
51.00%
57.38%
72.13%
54.25%
81.88%
76.25%
84.00%
74.00%




dill
phenanthrene
108.25%
72.00%
1 1 1 .63%
92.50%
95.13%
87.63%
79.25%
110.50%
109.00%
77.00%
102.88%
98.75%
89.38%
109.50%
108.38%
100.38%
100.63%
90.63%
100.25%
92.13%
75.38%
96.13%
90.88%
90.75%
68.13%
81.50%
99.13%
78.38%
92.50%
85.13%
93.25%
82.88%




d!2 chrysene
87.38%
70.88%
117.63%
100.75%
96.00%
79.00%
106.88%
111.50%
118.63%
99.13%
99.88%
104.25%
106.25%
116.88%
112.13%
106.50%
96.00%
98.13%
104.75%
98.88%
77.38%
102.00%
97.13%
101.25%
73.38%
85.63%
91.88%
84.25%
93.13%
85.13%
98.38%
81.63%




d!2
perylene
58.50%
42.25% #
60.38%
71.13%
101.25%
57.88%
58.38%
60.75%
61.75%
55.13%
53.00%
54.63%
58.25%
58.50%
55.50%
54.88%
64.50%
70.00%
74.13%
70.50%
53.38%
71.50%
68.00%
71.88%
90.88%
96.25%
98.88%
96.88%
64.38%
59.88%
68.75%
55.25%




d!4 dibenzo (a,h,)
anthracene
74.75%
74.13%
1 95.25% #
112.38%
76.63%
46.50% #
144.88%
1 59.88% #
177.88%#
1 52.75% #
144.88%
144.25%
167.50%#
190.00%#
1 76.38% #
1 79.50% #
90.00%
108.25%
113.13%
109.00%
79.13%
1 1 1 .25%
101.38%
116.50%
85.00%
95.13%
101.13%
96.75%
92.63%
87.50%
1 1 1 .00%
77.63%




B=blank Contamination
E=Estimate
units are ng/g
        Eagle Harbor
                                                                                             E19

-------
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564

Units are ng/g
                                                                                         Eagle Harbor
Internal Standard PR
MSL Sample ID Extraction Date Days held to extraction
1790-7 Blankl
1790-7 Blank 2
1790-7 -7 MS
1790-7 -12 MS
1790 Spike Blank B
1790-7 Spike Blank C
1790-7-1
1790-7-2
1790-7-3
1790-7-4
1790-7-6
1790-7-21
1790-7-22
1790-7-8
1790-7-9
1790-7-23
1790-7-10
1790-7-11
1790-7-25
1790-7-26
1790-7-13
1790-7-14
1790-7-27
1790-7-28
1790-15
1790-16
1790-29
1790-30
1790-7-17
1790-7-18
1790-7-31
1790-7-32
r=data points rejected
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
11/25/2002
12/2/2002
12/9/2002
1/6/2003
2/17/2003
5/12/2003
11/25/2002
11/25/2002
11/25/2002
11/25/2002
12/2/2002
12/2/2002
12/2/2002
12/9/2002
12/9/2002
12/9/2002
12/23/2002
12/23/2002
12/23/2002
12/23/2002
1/6/2003
1/6/2003
1/6/2003
1/6/2003
2/17/2003
2/17/2003
2/17/2003
2/17/2003
5/12/2003
5/12/2003
5/12/2003
5/12/2003




0
7
14
42
84
168
0
0
0
0
7
7
7
14
14
14
28
28
28
28
42
42
42
42
84
84
84
84
168
168
168
168




dS acenaphthylene
95.40%
106.00%
1 1 1 .20%
126.20%
93.00%
102.40%
97.30%
105.30%
101.20%
104.40%
102.60%
102.80%
108.20%
101.30%
110.40%
115.40%
110.00%
120.40%
116.50%
121.70%
119.50%
119.90%
120.20%
128.40%
98.00%
94.60%
86.50%
95.00%
105.90%
113.30%
112.20%
108.60%




dlO pyrene d!2 benzo [a] pyrene
110.70%
117.80%
128.80%
128.10%
100.10%
110.10%
115.80%
121.30%
115.40%
122.50%
119.10%
118.90%
121.70%
122.20%
131.30%
137.20%
115.80%
123.10%
119.60%
123.60%
121.20%
119.80%
119.10%
125.80%
107.30%
104.90%
101.60%
107.60%
113.70%
119.20%
119.30%
116.00%




88.10%
134.50%
215.50%
148.20%
92.70%
101.70%
160.00%
178.40%
181.40%
181.80%
178.10%
183.90%
189.20%
212.20%
227.00%
234.10%
129.10%
140.60%
136.50%
139.90%
139.40%
135.40%
136.50%
147.90%
99.40%
98.00%
92.30%
98.10%
113.70%
122.40%
125.60%
116.40%






#










#
#
#




















B=blank Contamination
E=Estimate
units are ng/g
        Eagle Harbor
                                                                                             E20

-------
                                                                               QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4583
                                                                                                  PAH Results
Storage
MSL Sample ID Extraction Date Days held to extraction Analysis Date Temperature
BLANKS
1790-7 Blank! 11/25/2002 0 1/17/2003 NA
1790-7 Blank 2 12/2/2002 7 1/18/2003 NA
BLANK SPIKES
1790 Spike Blank B 2/17/2003 84 3/21/2003 NA
1790-7 Spike Blank C 5/12/2003 168 5/20/2003 NA
BS B concentration
BS C concentration
PRBSB
PRBSC
MATRIX SPIKES
1790-7-7 MS 12/9/2002 14 1/18/2003 -20C
1790-7-12 MS 1/6/2003 42 2/5/2003 -20C
1790-7 (ave)
1790-7-7MS concentration
1 790-7-1 2MS concentration
PR 7-MS
PR 12-MS
1 methyl 2 methyl
naphthalene napthalene naphthalene
30.08 U 72.44 30.08 U
26.77 U 46.75 26.77 U
358.12 27.47 U 27.47 U
220.93 55.12 26.94 U
576.70 NA NA
538.80 NA NA
62.10% NA NA
41.00% NA NA
1011.31 465.73 B 135.22
756.00 516.97 143.02
506.26 385.48 105.86
495.00 NA NA
469.50 NA NA
102.02% NA NA
53.19% NA NA
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
r=data points rejected
B=blank Contamination
E=Estimate
                                                                           E21

-------
                                                                               QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4583
MSL Sample ID Extraction Date Days held to extraction Acenaphthalene Acenaphthene Fluorene dibenzothiophene
BLANKS
1790-7 Blank! 11/25/2002 0
1790-7 Blank 2 12/2/2002 7
BLANK SPIKES
1790 Spike Blank B 2/17/2003 84
1790-7 Spike Blank C 5/12/2003 168
BS B concentration
BS C concentration
PRBSB
PRBSC
MATRIX SPIKES
1790-7-7 MS 12/9/2002 14
1790-7-12 MS 1/6/2003 42
1790-7 (ave)
1790-7-7MS concentration
1 790-7-1 2MS concentration
PR 7-MS
PR 12-MS

30.08 U
26.77 U

407.05
173.12
576.70
538.80
70.58%
32.13% #

632.34
66.38
94.05
495.00
469.50
108.74%
-5.89% #

30.08 U
26.77 U

425.33
217.42
576.70
538.80
73.75%
40.35%

1759.96
1121.60
984.58
495.00
469.50
156.63% #
29.19% #

30.08 U
26.77 U

497.85
208.63
576.70
538.80
86.33%
38.72% #

2134.82
1301.68
1184.90
495.00
469.50
191.88% #
24.87% #

30.08
26.77

27.47
26.94
NA
NA
NA
NA

505.49
435.50
366.92
NA
NA
NA
NA

U
U

U
U












U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
r=data points rejected
B=blank Contamination
E=Estimate
                                                                           E22

-------
                                                                               QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4583
MSL Sample ID Extraction Date Days held to extraction
BLANKS
1790-7 Blank! 11/25/2002 0
1790-7 Blank 2 12/2/2002 7
BLANK SPIKES
1790 Spike Blank B 2/17/2003 84
1790-7 Spike Blank C 5/12/2003 168
BS B concentration
BS C concentration
PRBSB
PRBSC
MATRIX SPIKES
1790-7-7 MS 12/9/2002 14
1790-7-12 MS 1/6/2003 42
1790-7 (ave)
1790-7-7MS concentration
1 790-7-1 2MS concentration
PR 7-MS
PR 12-MS
phenanthrene anthracene 1 methyl phenanthrene fluoranthene

30.08 U
26.77 U

500.45
232.66
576.70
538.80
86.78%
43.18%

6171.75
4635.26
4223.61
495.00
469.50
393.52% #
87.68%

30.08 U
26.77 U

476.33
184.66
576.70
538.80
82.60%
34.27% #

3008.51
1593.60
1562.80
495.00
469.50
292.03% #
6.56% #

30.08 U
26.77 U

27.47 U
26.94 U
NA
NA
NA
NA

549.64
389.70
428.40
NA
NA
NA
NA

30.08 U
26.77 U

559.97
218.95
576.70
538.80
97.10%
40.64%

8044.54
6695.10
6513.53
495.00
469.50
309.26% #
38.67% #
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
r=data points rejected
B=blank Contamination
E=Estimate
                                                                           E23

-------
                                                                               QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4583
MSL Sample ID Extraction Date Days held to extraction
BLANKS
1790-7 Blank! 11/25/2002 0
1790-7 Blank 2 12/2/2002 7
BLANK SPIKES
1790 Spike Blank B 2/17/2003 84
1790-7 Spike Blank C 5/12/2003 168
BS B concentration
BS C concentration
PRBSB
PRBSC
MATRIX SPIKES
1790-7-7 MS 12/9/2002 14
1790-7-12 MS 1/6/2003 42
1790-7 (ave)
1790-7-7MS concentration
1 790-7-1 2MS concentration
PR 7-MS
PR 12-MS
benzo[a] benzo [b] benzo [k]
pyrene anthracene chrysene fluoranthene fluoranthene
30.08 U
26.77 U
527.97
228.92
576.70
538.80
91.55%
42.49%
5950.21
4752.94
4906.65
495.00
469.50
210.80% #
-32.74% #
30.08 U
26.77 U
497.14
190.47
576.70
538.80
86.20%
35.35% #
2296.21
1411.66
1482.71
495.00
469.50
164.33% #
-15.13% #
30.08 U
26.77 U
600.11
207.06
576.70
538.80
104.06%
38.43% #
2606.94
1766.36
1898.65
495.00
469.50
143.07% #
-28.18% #
30.08 U
26.77 U
581.36
189.13
576.70
538.80
100.81%
35.10% #
3110.67 r
2014.07
1976.75
495.00
469.50
229.05% #
7.95% #
30.08 U
26.77 U
579.20
197.04
576.70
538.80
100.43%
36.57% #
3063.93 r
1716.88
1727.16
495.00
469.50
270.03% #
-2.19% #
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
r=data points rejected
B=blank Contamination
E=Estimate
                                                                          E24

-------
                                                                               QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4583
                                                                                                                                     Surrogate PR
dibenzo
benzo [a] indeno [1,2,3- [a,h] benzo [g,h,i]
MSL Sample ID Extraction Date Days held to extraction pyrene c,d] pyrene anthracene perylene d8 naphthalene
BLANKS
1790-7 Blank! 11/25/2002 0
1790-7 Blank 2 12/2/2002 7
BLANK SPIKES
1790 Spike Blank B 2/17/2003 84
1790-7 Spike Blank C 5/12/2003 168
BS B concentration
BS C concentration
PRBSB
PRBSC
MATRIX SPIKES
1790-7-7 MS 12/9/2002 14
1790-7-12 MS 1/6/2003 42
1790-7 (ave)
1790-7-7MS concentration
1 790-7-1 2MS concentration
PR 7-MS
PR 12-MS

30.08 U
26.77 U

512.73
163.41
576.70
538.80
88.91%
30.33% #

1361.45 r
713.42
781.16
495.00
469.50
117.22%
-14.430/0 #

30.08 U
26.77 U

475.26
132.50 E
576.70
538.80
82.41%
24.59% #

1423.83 r
404.42
535.70
495.00
469.50
179.40% #
-27.96% #

30.08 U
26.77 U

412.66
110.56 E
576.70
538.80
71.56%
20.52% #

1124.54 r
161.52
204.78
495.00
469.50
185.79% #
-9.21% #

30.08 U
26.77 U

372.22
95.89 E
576.70
538.80
64.54%
17.80% #

1372.52 r
427.05
518.27
495.00
469.50
172.56% #
-19.43% #

97.13%
67.13%

63.38%
73.38%





91.00%
88.25%





U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
r=data points rejected
B=blank Contamination
E=Estimate
                                                                          E25

-------
                                                                         QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4583
MSL Sample ID
                        Extraction Date
           Days held to extraction
                      dlO
              Acenaphthene
                    dlO
            phenanthrene
           d!2 chrysene
                 d!2
             perylene
                                                                                                                                d!4 dibenzo (a,h,)
                                                                                                                                     anthracene
BLANKS
          1790-7 Blank!
          1790-7 Blank 2
11/25/2002
 12/2/2002
                  95.75%
                  67.75%
               108.25%
                72.00%
              87.38%
              70.88%
             58.50%
             42.25% #
                          74.75%
                          74.13%
BLANK SPIKES
      1790 Spike Blank B
    1790-7 Spike Blank C

BS B concentration
BS C concentration
PRBSB
PRBSC
 2/17/2003
 5/12/2003
84
168
74.50%
77.25%
95.13%
87.63%
96.00%
79.00%
101.25%
 57.88%
76.63%
46.50% #
MATRIX SPIKES
            1790-7-7 MS        12/9/2002
           1790-7-12 MS         1/6/2003
                   14
                   42
                  96.75%
                  85.63%
               111.63%
                92.50%
             117.63%
             100.75%
             60.38%
             71.13%
                         195.25% #
                         112.38%
1790-7 (ave)
1790-7-7MS concentration
1790-7-12MS concentration
PR 7-MS
PR 12-MS
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
r=data points rejected
B=blank Contamination
E=Estimate
                                                                    E26

-------
                                                                                      Sequim-1 PAH Data
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
MSL Sample ID
1790-8b-Blk Spk A
1790-8bBlkA
1790-8bBlkB
1790-8abBlkSpkB
1790-8bBlkSpkC
1790-8b-7 Spk
1790-8b-12spk
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4 (20)
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8ab-15
1790-8ab-16
1790-8ab-29
1790-8ab-30
1790-8b-17
1790-8b-18
1790-8b-31
1790-8b-32
Extraction Date
12/8/2003
12/15/2003
1/5/2004
3/1/2004
5/24/2004
12/22/2003
1/19/2004
12/8/2003
12/8/2003
12/8/2003
12/8/2003
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/22/2003
12/22/2003
12/22/2003
12/22/2003
1/5/2004
1/5/2004
1/5/2004
1/5/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
Days held from
Analysis Date Extraction to Analysis
1/22/2004
1/23/2004
1/23/2004
4/17/2004
6/17/2004
1/23/2004
1/23/2004
1/22/2004
1/22/2004
1/22/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
1/23/2004
4/17/2004
4/17/2004
4/17/2004
4/17/2004
6/18/2004
6/18/2004
6/18/2004
6/18/2004
45
39
18
47
24
32
4
45
45
45
46
39
39
39
39
32
32
32
32
18
18
18
18
4
4
4
4
47
47
47
47
25
25
25
25
Storage
Temperature
NA
NA
NA
NA
NA
-20C
-20C
-20C
-20C
-20C
-20C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
-20C
-20C
4C
4C
PAH Results
naphthalene Acenaphthylene Acenaphthene
70.53
0.52
0.46 U
45.18
71.81
130.94
151.97
42.52
87.81
91.32
103.22
71.01
64.03 r
65.27
67.70
94.83
86.59
56.73
78.27
62.91
53.78
85.01
74.05
80.38
78.83
95.09
66.3
83.41
46.77
61.86
69.46
142.49 r
133.53 r
83.43 r
72.27 r
61.48
0.51 U
0.51 U
49.09
65.91
96.10
68.51
4.28
9.20
10.75
8.34
10.20
9.92
8.92
9.74
13.04
14.08
9.03
10.39
7.98
9.8
7.54
8.47
8.82
10.69
9.72
6.55
10.77
8.56
8.41
8.82
14.78 r
13.73 r
11.88 r
10.02 r
68.13
0.57 U
0.57 U
52.07
71.34
179.21
166.57
45.87
108.70
119.29
113.94
96.18
87.52
86.58
93.60
99.33
107.12
90.57
100.89
71.84
77.89
88.65
91.23
92.54
95.32
110.05
75.19
104.28
83.71
94.48
93.94
145.28
122.72
119.39
97.77
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
E=data is an estimate
r=data is rejected
                                                                                         E27

-------
BATTELLE MARINE SCIENC
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                     Sequim-1 PAH Data
MSL Sample ID
                               Fluorene
dibenzothiophene
phenanthrene
                                                                                                       anthracene
                                                                                                                                fluoranthene
                                                                                                                                                       pyrene
benzo[a] anthracene
1790-8b-BlkSpkA
1790-8bBlkA
1790-8bBlkB
1790-8abBlkSpkB
1790-8bBlkSpkC
1790-8b-7 Spk
1790-8b-12spk
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4(20)
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8ab-15
1790-8ab-16
1790-8ab-29
1790-8ab-30
1790-8b-17 r
1790-8b-18 r
1790-8b-31 r
1790-8b-32 r
55.40
0.66
0.37 U
54.75
75.41
178.61
161.43
44.17
99.15
116.11
100.68
96.49
88.39
85.14
93.24
91.59
106.89
90.55
94.16
71.1
79.09
78.57
89.28
91.05
97.39
112.64
74.5
107.84
96.46
101.53
100.38
143.27 r
121.07 r
126.61 r
107.66 r
9.26
2.71
2.22 U
51.73
70.86
65.60
70.95
3.58
6.20
7.08
6.81
6.26
5.42
5.54
5.53
6.11
6.35
5.29
5.52
4.31
4.76
5
5.19
5.68
5.56
7.08
4.56
6.29
6.39
6.18
6.07
6.98 r
7.01 r
7.49 r
6.49 r
63.73
16.29
2.24 U
52.01
79.70
226.43
238.02
79.02
175.56
200.30
191.49
169.96
147.35
143.66
150.63
161.94
164.9
149.42
154.82
119.27
128.67
140.81
143.71
151.82
150.62
183.15
121.46
154.54
140.67
145.22
142.11
229.2 r
230.51 r
198.19 r
186.5 r
54.29
1.52
0.55 U
51.52
82.31
195.46
157.21
40.03
79.18
97.22
69.96
104.03
89.88
88.99
95.48
104.1
112.08
88.08
94.12
72.57
79.59
82.23
85.23
87.32
96.09
108.69
69.61
81.4
83.91
80.69
79.43
118.95 r
123.79 r
120.92 r
108.22 r
69.56
29.73
4.61 U
80.41
87.07
280.54
293.86
103.91
171.33
185.16
164.29
188.89
171.29
187.45
179.49
202.7
210
192.27
191.02
154.41
165.54
172.87
184.24
179.79
175.25
216.52
142.59
215.76
190.5
196.88
204.85
228.93 r
259.9 r
221.98 r
218.61 r
78.23
12.00
2.22 U
70.33
80.13
254.81
264.44
83.93
156.29
161.45
152.99
164.45
147.09
161.98
154.13
176.34
183.83
168.56
167.88
132.82
143.09
151.96
156.48
154.98
151.95
187.65
123.03
169.9
150.79
156.57
163.26
185.25 r
207.07 r
187.67 r
182.27 r
51.61
0.87
0.84
89.07
86.11
217.18
228.89
59.83
102.27
120.27
93.38
143.43
129.64
148.56
133.61
152.98
162.63
149.33
130.98
105.22
122.38
117.8
123.98
128.02
126.94
150.72
93.75
159.54
152.96
149.28
156.67
88.86
107
169.48
162.43
#=outside project DQO's
U=not detected at or above IV
NA = not applicable
E=data is an estimate
r=data is rejected
                                                                                        E28

-------
BATTELLE MARINE SCIENC
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                     Sequim-1 PAH Data
MSL Sample ID
chrysene
benzo [b] fluoranthene
benzo [a] pyrene
indeno [1,2,3-c,d] pyrene
dibenzo [a,h] anthracene
1790-8b-BlkSpkA
1790-8bBlkA
1790-8bBlkB U
1790-8abBlkSpkB
1790-8bBlkSpkC
1790-8b-7 Spk
1790-8b-12spk
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4(20)
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8ab-15
1790-8ab-16
1790-8ab-29
1790-8ab-30
1790-8b-17 r
1790-8b-18 r
1790-8b-31 r
1790-8b-32 r
55.91
1.54
0.81 U
66.64
83.24
232.65
232.99
66.71
119.05
141.14
116.67
153.03
138.15
157.29
140.85
169
177.53
159.73
142.86
111.22
130.29
127.78
135.26
137.2
133.56
162.92
102.34
136.97
130.35
128.79
132.85
105.09 r
122.62 r
172.93 r
164.39 r
56.39 r
0.77 U r
0.77 U
66.17
71.87
169.44 E
166.99
39.99
99.47
108.52
116.91
111.74 E
108.33 E
124.31 E
114.71 E
138.55 E
137.88 E
134.4 E
113.35 E
90.43
106.58
98.86
105.24
99.4
98.06
124.92
79.27
185.14
148.4
162.17
195.98
99.48 r
115.8 r
198.45 r
196.12 r
57.76 r
0.84 U r
0.84 U
52.87
73.26
175.18 E
147.66
35.82
80.00
84.04
81.96
98.83 E
90.82 E
104.28 E
98.26 E
122.89 E
124.65 E
112.11 E
89.51 E
75.51
91.61
82.97
84.78
88.35
91
107.9
62.64
118
100.96
108.92
128.03
58.99 r
68.8 r
145.78 r
131.43 r
50.34 r
1.02 U r
1.02 U
74.00
64.40
58.75 E
57.28
2.10
4.04
4.99
4.33
4.31 E
4.06 E
4.69 E
4.16 E
5.17 E
5.11 E
5.04 E
4.18 E
3
4.12
3.33
3.93
4.51
4.3
5.66
2.79
7.68
6.85
7.75
9.07
1.08 r
1.32 r
4.63 r
4.24 r
38.95
0.86
0.86
59.43
69.45
168.52
136.11
34.40
65.08
86.64
70.86
90.89
86.90
99.12
98.56
110.2
124.1
98.16
71.63
54.57
71.94
62.87
66.81
85.98
89.34
98.05
52.68
94.98
82.32
93.85
106.84
16.13
20.78
78.65
72.68
r
U r
U


E





E
E
E
E
E
E
E
E












r
r
r
r
#=outside project DQO's
U=not detected at or above IV
NA = not applicable
E=data is an estimate
r=data is rejected
                                                                                         E29

-------
BATTELLE MARINE SCIENC
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                   Sequim-1 PAH Data
MSL Sample  ID
benzo[g,h,i] perylene
Surrogate Recovery
   d8 naphthalene
d10 Acenaphthene
d10 phenanthrene
d12 chrysene
d12 perylene
1790-8b-BlkSpkA
1790-8bBlkA
1790-8bBlkB
1790-8abBlkSpkB
1790-8bBlkSpkC
1790-8b-7 Spk
1790-8b-12spk
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4(20)
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8ab-15
1790-8ab-16
1790-8ab-29
1790-8ab-30
1790-8b-17
1790-8b-18
1790-8b-31
1790-8b-32
55.78 r
0.94 U r
0.94 U
49.49
70.58
157.03 E
135.07
34.46
82.08
95.43
95.38
88.93 E
83.97 E
95.06 E
95.44 E
91.53 E
102.82 E
77.54 E
54.94 E
47.56
65.52
52.64
61.85
84.12
86.36
98.35
52.55
86.96
76.01
89.21
96.6
11.54 r
14.31 r
62.99 r
51.39 r
104.00%
62.00%
66.70%
76.30%
98.80%
68.60%
86.70%
64.30%
87.00%
99.20%
93.80%
65.50%
60.70%
60.90%
70.20%
74.20%
73.60%
62.20%
80.30%
51 .90%
57.50%
67.80%
67.50%
70.90%
73.70%
86.70%
83.20%
81 .80%
60.10%
75.50%
71.20%
116.20% r
100.70% r
100.70% r
61.10% r
94.30%
66.50%
69.70%
83.80%
100.20%
74.90%
90.50%
65.50%
86.30%
100.00%
92.40%
68.40%
66.30%
64.40%
73.80%
79.20%
78.60%
76.70%
82.20%
54.60%
61 .90%
68.90%
71 .20%
76.00%
78.10%
90.30%
84.70%
87.60%
72.10%
85.00%
79.80%
120.50% r
107.20% r
106.60% r
80.70% r
93.70%
83.70%
78.70%
92.00%
115.30%
90.20%
103.70%
75.50%
95.70%
123.50%
108.90%
94.20%
85.80%
81 .80%
89.50%
95.00%
93.80%
90.10%
92.80%
66.80%
75.30%
77.60%
82.60%
93.90%
91 .50%
107.80%
95.40%
93.90%
86.10%
94.70%
86.10%
131.00% r
121.40% r
114.30% r
100.30% r
81 .60%
112.50%
92.50%
128.00%
128.70%
110.90%
122.90%
96.60%
86.40%
125.50%
87.40%
106.30%
95.60%
105.80%
103.90%
111.30%
116.30%
113.20%
103.10%
74.60%
89.80%
84.20%
93.50%
111.80%
106.90%
122.90%
106.10%
109.70%
112.20%
114.40%
105.90%
75.50% r
71 .30% r
112.90% r
106.00% r
65.80%
79.70%
73.50%
77.10%
120.40%
91 .50%
88.90%
67.30%
59.90%
83.50%
60.70%
80.60%
73.10%
82.20%
82.60%
92.80%
91.70%
89.60%
77.40%
59.60%
71 .60%
65.10%
72.90%
85.70%
82.30%
95.60%
81.10%
83.00%
77.30%
82.00%
83.90%
43.40%
40.00%
93.10%
82.60%
#=outside project DQO's
U=not detected at or above IV
NA = not applicable
E=data is an estimate
r=data is rejected
                                                                                       E30

-------
BATTELLE MARINE SCIENC
1529 West Sequim Bay Road
Sequim, Washington 98382
(360) 681-4564
                                                                                    Sequim-1 PAH Data
MSL Sample  ID
Internal Std. Recovery
  d8 acenaphthylene
d10 pyrene
d12 benzo [a] pyrene
1790-8b-BlkSpkA
1790-8bBlkA
1790-8bBlkB
1790-8abBlkSpkB
1790-8bBlkSpkC
1790-8b-7 Spk
1790-8b-12spk
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4(20)
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8ab-15
1790-8ab-16
1790-8ab-29
1790-8ab-30
1790-8b-17 r
1790-8b-18 r
1790-8b-31 r
1790-8b-32 r
81.30%
174.40%
171.60%
106.70%
85.90%
187.10%
133.10%
168.10%
109.50%
118.80%
118.10%
182.60%
208.20% #
165.90%
148.20%
139.40%
146.10%
199.60%
144.90%
165.60%
174.60%
166.70%
166.70%
152.60%
183.50%
152.00%
144.30%
140.00%
118.90%
158.00%
123.80%
78.30% r
73.30% r
88.60% r
89.00% r
64.80%
144.60%
139.90%
92.30%
76.20%
149.70%
115.40%
135.80%
120.50%
135.90%
132.40%
178.60%
189.00%
142.40%
123.10%
113.50%
118.70%
163.90%
119.50%
135.40%
143.30%
135.40%
133.80%
128.50%
152.70%
120.40%
116.40%
107.80%
95.70%
128.20%
95.30%
81 .20% r
70.50% r
82.00% r
86.00% r
47.40% #
219.70% #
168.40%
142.70%
73.30%
176.70%
149.00%
191.50%
118.20%
156.90%
108.20%
233.30% #
240.00% #
179.70%
149.80%
131.40%
144.10%
194.30%
144.50%
157.20%
171.00%
157.70%
157.30%
166.00%
194.20%
143.20%
137.10%
131.20%
132.90%
166.00%
113.50%
26.70% # r
24.10% # r
67.00% r
64.00% r
#=outside project DQO's
U=not detected at or above IV
NA = not applicable
E=data is an estimate
r=data is rejected
                                                                                       E31

-------
                                                                                       QC
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
MSL Sample ID Extraction Date
BLANKS
1790-8bBlkA 12/15/2003
1790-8bBlkB 1/5/2004
BLANK SPIKES
1790-8b-BlkSpkA 12/8/2003
1 790-8ab Bl k Spk B 3/1 /2004
1790-8b Blk Spk C 5/24/2004
spk concentration A
spk concentration B
spk concentration C
percent recovery A
percent recovery B
percent recovery C
MATRIX SPIKES
1790-8b-7Spk 12/22/2003
1790-8b-12Spk 1/19/2004
1790-8b-Ave NA
spk concentration 7
spk concentration 1 2
percent recovery 7 Spk
percent recovery 1 2 Spk
Days held from
Analysis Date Extraction to Analysis

1/23/2004 39
1/23/2004 18

1/22/2004 45
4/17/2004 47
6/17/2004 24







1/23/2004 32
1/23/2004 4
NA NA




Storage
Temperature

NA
NA

NA
NA
NA







-20C
-20C
NA




PAH Results
naphthalene

0.52
0.46 U

70.53
45.18
71.81
66.90
62.50
69.40
105.4%
72.3%
103.5%

130.94
151.97
73.04
69.00
68.00
83.9%
116.1%
Acenaphthylene

0.51 U
0.51 U

61.48
49.09
65.91
NA
NA
NA
NA
NA
NA

96.10
68.51
9.37
NA
NA
NA
NA
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
                                                                                  E32

-------
                                                                                QC
BA TTELLE MARINE SCIENCES I
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
MSL Sample ID Acenaphthene Fluorene dibenzothiophene phenanthrene anthracene fluoranthene pyrene
BLANKS
1790-8bBlkA 0.57 U 0.66
1790-8bBlkB 0.57 U 0.37 U

2.71 16.29 1.52 29.73 12.00
2.22 U 2.24 U 0.55 U 4.61 U 2.22 U
BLANK SPIKES
         1790-8b-BlkSpkA
        1790-8abBlkSpkB
         1790-8bBlkSpkC

         spk concentration A
         spk concentration B
         spk concentration C
         percent recovery A
         percent recovery B
         percent recovery C

MATRIX SPIKES

            1790-8b-7Spk
           1790-8b-12Spk

              1790-8b-Ave
         spk concentration 7
        spk concentration 12
      percent recovery 7 Spk
     percent recovery 12 Spk
68.13
52.07
71.34
66.90
62.50
69.40
101.8%
83.3%
102.8%
55.40
54.75
75.41
66.90
62.50
69.40
82.8%
87.6%
108.7%
 179.21
 166.57

  92.78
  69.00
  68.00
125.3%  #
108.5%
 178.61
 161.43

  92.75
  69.00
  68.00
124.4%  #
101.0%
                                           9.26
                                          51.73
                                          70.86

                                            NA
                                            NA
                                            NA
                                            NA
                                            NA
                                            NA
65.60
70.95

 5.72
  NA
  NA
  NA
  NA
                                           63.73
                                           52.01
                                           79.70

                                           66.90
                                           62.50
                                           69.40
                                          95.3%
                                          83.2%
                                          114.8%
 226.43
 238.02

 149.65
  69.00
  68.00
111.3%
130.0%#
                                      54.29
                                      51.52
                                      82.31

                                      66.90
                                      62.50
                                      69.40
                                     81.2%
                                     82.4%
                                    118.6%
 195.46
 157.21

  86.75
  69.00
  68.00
157.6%   #
103.6%
69.56
80.41
87.07
66.90
62.50
69.40
104.0%
128.7% #
125.5% #
280.54
293.86
178.92
69.00
68.00
147.3% #
169.0% #
78.23
70.33
80.13
66.90
62.50
69.40
116.9%
112.5%
115.5%
254.81
264.44
154.50
69.00
68.00
145.4% #
161.7% #
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
                                                                            E33

-------
                                                                                 QC
BA TTELLE MARINE SCIENCES I
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
MSL Sample ID benzo[a] anthracene chrysene benzo [b] fluoranthene benzo [a] pyrene indeno [1 ,2,3-c,d] pyrene
BLANKS
1790-8bBlkA 0.87 1.54 0.77 U r 0.84 U r
1790-8bBlkB 0.84 U 0.81 U 0.77 U 0.84 U

1.02 U r
1.02 U
BLANK SPIKES
         1790-8b-BlkSpkA
        1790-8abBlkSpkB
         1790-8bBlkSpkC

         spk concentration A
         spk concentration B
         spk concentration C
         percent recovery A
         percent recovery B
         percent recovery C

MATRIX SPIKES

             1790-8b-7Spk
           1790-8b-12Spk

              1790-8b-Ave
         spk concentration 7
        spk concentration 12
      percent recovery 7 Spk
     percent recovery 12 Spk
51.61
89.07
86.11
66.90
62.50
69.40
77.1%
142.5% #
124.1% #
217.18
228.89
132.27
69.00
68.00
123.1% #
142.1%#
55.91
66.64
83.24
66.90
62.50
69.40
83.6%
106.6%
119.9%
232.65
232.99
135.89
69.00
68.00
140.2% #
142.8% #
  56.39
  66.17
  71.87

  66.90
  62.50
  69.40
 84.3%
105.9%
103.6%
 169.44
 166.99

 118.33
  69.00
  68.00
 74.1%
 71.6%
  57.76
  52.87
  73.26

  66.90
  62.50
  69.40
 86.3%
 84.6%
105.6%
 175.18
 147.66

  93.68
  69.00
  68.00
118.1%
 79.4%
  50.34
  74.00
  64.40

  66.90
  62.50
  69.40
 75.2%
118.4%
 92.8%
  58.75    E
  57.28

   4.83
  69.00
  68.00
 78.1%
 77.1%
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
                                                                             E34

-------
                                                                                QC
BA TTELLE MARINE SCIENCES I
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
                                                                                    Surrogate Recovery
MSL Sample ID dibenzo [a,h] anthracene benzo[g,h,i] perylene d8
BLANKS
1790-8bBlkA
1790-8bBlkB
0.86 U r
0.86 U
0.94 U r
0.94 U
naphthalene d10 Acenaphthene d10 phenanthrene
62.00%
66.70%
66.50%
69.70%
83.70%
78.70%
BLANK SPIKES
         1790-8b-BlkSpkA
        1790-8abBlkSpkB
         1790-8bBlkSpkC

         spk concentration A
         spk concentration B
         spk concentration C
         percent recovery A
         percent recovery B
         percent recovery C

MATRIX SPIKES

            1790-8b-7Spk
           1790-8b-12Spk

              1790-8b-Ave
         spk concentration 7
        spk concentration 12
      percent recovery 7 Spk
     percent recovery 12 Spk
  38.95
  59.43
  69.45

  66.90
  62.50
  69.40
 58.2%
 95.1%
100.1%
 168.52
 136.11

  83.23
  69.00
  68.00
123.6%  #
 77.8%
  55.78
  49.49
  70.58

  66.90
  62.50
  69.40
 83.4%
 79.2%
101.7%
 157.03
 135.07

  78.47
  69.00
  68.00
113.9%
 83.2%
104.00%
 76.30%
 98.80%
 94.30%
 83.80%
100.20%
 93.70%
 92.00%
115.30%
 68.60%
 86.70%
 74.90%
 90.50%
 90.20%
103.70%
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
                                                                           E35

-------
                                                                              QC
BA TTELLE MARINE SCIENCES I
1529 West Sequim Bay Road
Sequim, Washington 98382
(360)681-4564
MSL Sample ID
d12 chrysene
d12 perylene
Internal Std. Recovery
  d8 acenaphthylene
d10 pyrene
d12 benzo [a] pyrene
BLANKS
             1790-8bBlkA
             1790-8bBlkB
     112.50%
      92.50%
       79.70%
       73.50%
              174.40%
              171.60%
      144.60%
      139.90%
            219.70% #
            168.40%
BLANK SPIKES
         1790-8b-BlkSpkA
        1790-8abBlkSpkB
         1790-8bBlkSpkC

        spk concentration A
        spk concentration B
        spk concentration C
         percent recovery A
         percent recovery B
         percent recovery C

MATRIX SPIKES

            1790-8b-7Spk
           1790-8b-12Spk

              1790-8b-Ave
         spk concentration 7
        spk concentration 12
     percent recovery 7 Spk
    percent recovery 12 Spk
      81.60%
     128.00%
     128.70%
       65.80%
       77.10%
      120.40%
               81.30%
              106.70%
               85.90%
       64.80%
       92.30%
       76.20%
             47.40% #
            142.70%
             73.30%
     110.90%
     122.90%
       91.50%
       88.90%
              187.10%
              133.10%
      149.70%
      115.40%
            176.70%
            149.00%
#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
                                                                          E36

-------
                                                                               Bedford, Plot 1 Pesticide Data
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
1790-9ab blkA
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9abspkblkA
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-7 MS
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9abblkB
1790-9ab-10
1790-9ab-11
1790-9ab-24
1790-9ab-25
1790-9ab-26
1790-9ab-13
1790-9ab-14
1790-9ab-12 MS
1790-9ab-27
1790-9 Spk Blank B
1790-9-15
1790-9-16
1790-9-28
1790-9-29
1790-9a-BlkSpkC
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
Average
Extraction Date
12/30/2003
12/30/2003
12/30/2003
12/30/2003
12/30/2003
1/6/2004
1/6/2004
1/6/2004
1/6/2004
1/6/2004
1/13/2004
1/13/2004
1/13/2004
1/13/2004
1/13/2004
1/27/2004
1/28/2004
1/28/2004
1/28/2004
1/28/2004
2/11/2004
2/11/2004
2/11/2004
2/11/2004
2/11/2004
3/23/2004
3/23/2004
3/23/2004
3/23/2004
3/23/2004
6/15/2004
6/15/2004
6/15/2004
6/15/2004
6/15/2004

Storage
Temperature
NA
-20C
-20C
-20C
-20C
NA
-20C
-20C
4C
4C
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
4C
-20C
-20C
-20C
4C
NA
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C

Days held from
Analysis Date Extraction to Analysis a-BHC
1/18/2004
1/18/2004
1/18/2004
1/18/2004
1/18/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
3/4/2004
3/5/2004
3/5/2004
3/5/2004
3/5/2004
3/5/2004
3/5/2004
3/5/2004
3/5/2004
3/5/2004
4/16/2004
4/17/2004
4/17/2004
4/17/2004
4/17/2004
6/18/2004
6/18/2004
6/18/2004
6/18/2004
6/18/2004

19
19
19
19
19
13
13
13
13
13
6
6
6
6
6
37
37
37
37
37
23
23
23
23
23
24
25
25
25
25
3
3
3
3
3

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

d-BHC
16.67
14.84
19.16
20.62
14.53
16.67
21.76
15.82
13.97
14.25
29.83
24.85
15.20
24.11
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
18.78
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
16.10
HEPTACLOR
U
U


U
U

U
U
U


U

U
U
U
U
U
U
U
U
U
U

U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
13.81
14.53
163.62
14.97
15.82
13.97
14.25
311.46
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
277.16
14.58
132.35
13.97
14.62
15.63
15.43
301 .52
13.77
14.53
13.30
13.48
23.92
U
U
U
U
U

U
U
U
U

U
U
U
U
U
U
U
U
U
U
U
U

U

U
U
U
U

U
U
U
U

ALDRIN
16.67
14.84
13.55
13.81
14.53
320.43
14.97
15.82
13.97
14.62
337.65
14.16
16.77
16.03
19.25
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
294.98
14.58
293.66
13.97
14.62
15.63
15.43
299.67
13.77
14.53
13.30
13.48
24.76

U
U
U
U
U

U
U
U


U

U

U
U
U
U
U
U
U
U

U

U
U
U
U

U
U
U
U

#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
                                                                                       E37

-------
                                                                           Bedford, Plot 1 Pesticide Data
BATTELLE MARINE SCIEN
1529 West Sequim Bay Roai
Sequim, Washington 98382
360-681-4583
        MSL Sample ID
                           HEPT EPOXIDE
                                                 a-CHLORDANE
                                                                        TRANS NONA
                                                                                           DIELDRIN
4,4'-DDE
2,4-DDD
                                                                                                                                        ENDRIN
                                                                                                                                                      ENDO II
#=outside project DQO's
U=not detected at or above t
NA = not applicable
r=data is rejected
E=data is an estimate
4,4'-ODD
1790-9ab blkA
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9abspkblkA
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-7 MS
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9abblkB
1790-9ab-10
1790-9ab-11
1790-9ab-24
1790-9ab-25
1790-9ab-26
1790-9ab-13
1790-9ab-14
1790-9ab-12 MS
1790-9ab-27
1790-9 Spk Blank B
1790-9-15
1790-9-16
1790-9-28
1790-9-29
1790-9a-BlkSpkC
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
Average
16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
16.49
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.69
U
U
U

U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
13.81
14.53
588.89
14.97
15.82
13.97
14.25
610.92
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
609.59
14.58
746.85
38.44
36.60
15.63
39.99
811.32
41.32
35.13
33.96
33.14
41.49
U
U
U
U
U

U
U
U
U

U
U
U
U
U
U
U
U
U
U
U
U

U



U







16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
43.16
14.16
15.20
16.03
15.38
36.93
44.43
40.13
38.84
43.83
42.96
13.55
35.86
25.61
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
19.57
U
U
U
U
U
U
U
U
U
U

U
U
U
U




U

U


U
U
U
U
U
U
U
U
U
U
U

16.67 U
102.94
95.05
86.06
87.89
16.67 U
99.61
103.58
88.72
98.46
116.82
110.77
116.56
129.47
118.65
16.67 U
70.04
67.03
66.19
67.99
61.62
65.56
64.54
66.99
77.39
14.29 U
117.61
113.32
114.42
122.52
16.67 U
123.55
104.01
105.68
100.96
95.91
16.67
14.84
13.55
13.81
14.53
683.66
14.97
15.82
13.97
14.25
716.50
14.16
15.20
16.03
17.13
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
646.96
14.58
766.45
13.97
15.84
16.46
15.43
844.29
17.92
14.53
13.30
13.48
37.41
U
U
U
U
U

U
U
U
U

U
U
U

U
U
U
U
U
U
U
U

U

U


U


U
U
U

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
15.06
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.64
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
357.40
344.98
363.96
353.79
16.67
392.42
377.25
341.74
353.07
461.76
427.51
429.04
414.33
444.23
16.67
452.00
465.74
470.02
459.90
425.31
380.39
424.02
445.22
428.25
14.29
394.12
382.67
387.89
418.93
70.24
445.76
370.30
398.56
364.45
403.14
                                                                                  E38

-------
                                                                           Bedford, Plot 1 Pesticide Data
BATTELLE MARINE SCIEN
1529 West Sequim Bay Roai
Sequim, Washington 98382
360-681-4583
        MSL Sample ID
2,4-DDT
                                           ENDRIN ALDY.
                                                                  ENDO SULFATE
4,4'-DDT
                                                                                                      ENDRIN KET.
                                                                                                                           METHOXYCLOR
                                                                                                                                                  MIREX
                                                                                                                                                            PCB-103Surr
1790-9abblkA U
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9abspkblkA U
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-7 MS
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9abblkB U
1790-9ab-10
1790-9ab-11
1790-9ab-24
1790-9ab-25
1790-9ab-26
1790-9ab-13
1790-9ab-14
1790-9ab-12 MS
1790-9ab-27
1790-9 Spk Blank B U
1790-9-15
1790-9-16
1790-9-28
1790-9-29
1790-9a-BlkSpkC
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
Average
16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67 U
60.41
57.21
72.13
66.18
677.25
65.02
60.43
56.24
60.16
837.29
79.19
74.55
74.14
118.10
16.67 U
121.40
126.02
131.03
115.46
133.51
87.87
113.44
704.31
119.21
751 .26
103.11
99.90
101.05
109.26
667.53
80.40
99.32
71.24
61.28
110.29
16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
20.96
16.67
14.41
14.33
15.48
25.81
27.72
13.55
25.36
15.92
14.58
14.29
41.51
14.62
32.89
40.63
54.52
65.74
54.49
61.11
13.48
23.07
U
U
U
U
U
U
U
U
U
U
U
U
U
U

U
U
U
U


U

U
U
U

U






U

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
126.00
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

16.67
14.84
13.55
13.81
14.53
16.67
14.97
15.82
13.97
14.25
15.38
14.16
15.20
16.03
15.38
16.67
14.41
14.33
15.48
14.84
14.97
13.55
14.16
15.92
14.58
14.29
13.97
14.62
15.63
15.43
16.67
13.77
14.53
13.30
13.48
14.59
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U

83.98%
88.47%
84.11%
90.03%
79.90%
97.46%
90.64%
91.91%
88.61%
94.34%
108.79%
101.43%
103.20%
98.86%
116.95%
68.53%
72.72%
73.13%
68.17%
71.36%
65.37%
47.60%
63.33%
49.06%
55.13%
98.70%
112.38%
104.38%
103.05%
106.13%
96.82%
106.86%
97.43%
104.75%
100.06%

#=outside project DQO's
U=not detected at or above t
NA = not applicable
r=data is rejected
E=data is an estimate
                                                                                  E39

-------
                                                                              Bedford, Plot 1 Pesticide Data
BATTELLE MARINE SCIEN
1529 West Sequim Bay Roai
Sequim, Washington 98382
360-681-4583
        MSL Sample ID PCB-198 Surr     TCMX ris
                                                        HBBris
#=outside project DQO's
U=not detected at or above t
NA = not applicable
r=data is rejected
E=data is an estimate
                                                                     OCN ris
1790-9ab blkA
1790-9ab-1
1790-9ab-2
1790-9ab-3
1790-9ab-4
1790-9abspkblkA
1790-9ab-5
1790-9ab-6
1790-9ab-20
1790-9ab-21
1790-9ab-7 MS
1790-9ab-8
1790-9ab-9
1790-9ab-22
1790-9ab-23
1790-9abblkB
1790-9ab-10
1790-9ab-11
1790-9ab-24
1790-9ab-25
1790-9ab-26
1790-9ab-13
1790-9ab-14
1790-9ab-12 MS
1790-9ab-27
1790-9 Spk Blank B
1790-9-15
1790-9-16
1790-9-28
1790-9-29
1790-9a-BlkSpkC
1790-9a-17
1790-9a-18
1790-9a-30
1790-9a-31
Average
99.33%
98.56%
96.98%
111.14%
97.34%
102.13%
100.06%
99.02%
97.79%
97.25%
116.95%
112.22%
113.69%
108.22%
115.26%
122.72%
123.30%
121.69%
119.96%
119.33%
126.62%
104.30%
129.76%
116.15%
130.15%
111.06%
132.05%
120.69%
119.72%
122.25%
114.96%
135.12%
119.20%
140.58%
128.00%

125.44%
125.80%
127.45%
119.80%
120.53%
105.36%
1 1 1 .24%
109.12%
114.94%
108.29%
89.63%
86.41%
90.86%
90.68%
78.96%
109.41%
110.74%
108.44%
124.09%
116.13%
113.76%
160.52%
133.85%
161.34%
149.57%
97.66%
90.62%
97.94%
101.56%
99.38%
92.12%
84.54%
93.23%
87.73%
95.97%

113.92%
116.25%
113.49%
105.81%
107.12%
103.62%
105.65%
108.50%
110.95%
110.46%
85.39%
81.14%
89.34%
87.76%
86.04%
63.51%
65.01%
63.39%
72.20%
69.15%
67.59%
86.14%
80.92%
83.75%
80.27%
99.03%
80.43%
88.69%
91 .87%
88.49%
94.90%
76.64%
86.49%
78.13%
89.97%

120.56%
97.72%
101.69%
95.05%
98.13%
120.46%
96.69%
102.18%
103.79%
103.51%
82.45%
80.72%
87.12%
86.59%
83.06%
63.75%
62.92%
58.61%
69.29%
67.40%
60.50%
71 .38%
72.50%
76.20%
72.31%
98.58%
78.74%
84.96%
87.48%
84.77%
95.44%
84.19%
96.37%
86.73%
102.02%

                                                                                      E40

-------
                                                                                QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
BLANKS
1790-9abblkA
1790-9abblkB
BLANK SPIKES
1790-9abBlkSpkA
1790-9 BlkSpkB
1790-9a-BlkSpkC
Spike concentration A
Spike concentration B
Spike concentration C
percent recovery A
percent recovery B
percent recovery C
MATRIX SPIKES
1790-9ab Average
1790-9ab-7 MS
1790-9ab-12 MS
Spike concentration 7
Spike concentration 12
percent recovery 7
percent recovery 1 2
Storage
Extraction Date Temperature

12/30/2003 NA
1/27/2004 NA

1/6/2004 NA
3/23/2004 NA
6/15/2004 NA








1/13/2004 -20C
2/11/2004 -20C




Days held from
Analysis Date Extraction to Analysis

1/18/2004 19
3/4/2004 37

1/19/2004 13
4/16/2004 24
6/18/2004 3








1/19/2004 6
3/5/2004 23




a-BHC d-BHC HEPTACLOR

16.67 U 16.67 U 16.67
16.67 U 16.67 U 16.67

16.67 U 16.67 U 163.62
14.29 U 14.29 U 132.35
16.67 U 16.67 U 301.52
333.33
285.71
333.33
49.09%
46.32%
90.46%

0.00
15.38 U 29.83 311.46
15.92 U 15.92 U 277.16
307.69
299.40
101.23%
92.57%


U
U







#
#









#=outside project DQO's
U=not detected at or above MDL
NA = not applicable
r=data is rejected
E=data is an estimate
                                                                            E41

-------
BATTELLE MARINE SCIEI
1529 West Sequim Bay ROJ
Sequim, Washington 98382
360-681-4583
                                                                            QC
        MSL Sample ID   ALDRIN
HEPT EPOXIDE
a-CHLORDANE
TRANS NONA
DIELDRIN
4,4'-DDE
2,4-DDD
ENDRIN
BLANKS
1790-9abblkA
1790-9abblkB
BLANK SPIKES
1790-9abBlkSpkA
1790-9 BlkSpkB
1790-9a-BlkSpkC
Spike concentration A
Spike concentration B
Spike concentration C
percent recovery A
percent recovery B
percent recovery C
MATRIX SPIKES
1790-9ab Average
1790-9ab-7 MS
1790-9ab-12 MS
Spike concentration 7
Spike concentration 12
percent recovery 7
percent recovery 1 2

16.67 U
16.67 U

320.43
293.66
299.67
333.33
285.71
333.33
96.13%
102.78%
89.90%

0.00
337.65
294.98
307.69
299.40
109.74%
98.52%

16.67 U 16.67 U 16.67 U
16.67 U 16.67 U 16.67 U

16.67 U 16.67 U 16.67 U
14.29 U 14.29 U 14.29 U
16.67 U 16.67 U 16.67 U








15.38 U 15.38 U 15.38 U
15.92 U 15.92 U 15.92 U





16.67 U
16.67 U

588.89
746.85
811.32
666.66
571.42
666.66
88.33%
130.70%
121.70% #

21.11
610.92
609.59
615.38
598.80
95.84%
98.28%

16.67 U 16.67 U 16.67
36.93 16.67 U 16.67

16.67 U 16.67 U 683.66
14.29 U 14.29 U 766.45
16.67 U 16.67 U 844.29
666.66
571.42
666.66
102.55%
134.13%
126.65%

0.00
43.16 116.82 716.50
25.61 66.99 646.96
615.38
598.80
116.43%
108.04%
#=outside project DQO's
U=not detected at or above
NA = not applicable
r=data is rejected
E=data is an estimate
                                                                       E42

-------
                                                                            QC
BATTELLE MARINE SCIEI
1529 West Sequim Bay ROJ
Sequim, Washington 98382
360-681-4583
        MSL Sample ID
ENDOI
4,4'-DDD
2,4-DDT
ENDRIN ALDY.
ENDO SULFATE
4,4'-DDT
#=outside project DQO's
U=not detected at or above
NA = not applicable
r=data is rejected
E=data is an estimate
ENDRIN KET.
BLANKS
1790-9abblkA U 16.67 U 16.67 U 16.67 U 16.67 U
1790-9abblkB U 16.67 U 16.67 U 16.67 U 16.67 U
BLANK SPIKES
1790-9abBlkSpkA 16.67 U 16.67 U 16.67 U 16.67 U
1790-9 BlkSpkB 14.29 U 14.29 U 14.29 U 14.29 U
1790-9a-BlkSpkC 16.67 U 70.24 16.67 U 16.67 U
Spike concentration A
Spike concentration B
Spike concentration C
percent recovery A
percent recovery B #
percent recovery C #
MATRIX SPIKES
1790-9ab Average
1790-9ab-7 MS 15.38 U 461.76 15.38 U 15.38 U
1790-9ab-12 MS 15.92 U 445.22 15.92 U 15.92 U
Spike concentration 7
Spike concentration 12
percent recovery 7
percent recovery 1 2

16.67 U 16.67 U
16.67 U 16.67 U

16.67 U 677.25
14.29 U 751.26
16.67 U 667.53
666.66
571.42
666.66
101.59%
131.47%
100.13%

110.29
15.38 U 837.29
15.92 U 704.31
615.38
598.80
118.14%
99.20%

16.67 U
16.67 U

16.67 U
14.29 U
54.52








15.38 U
15.92 U




                                                                        E43

-------
                                                                           QC


BATTELLE MARINE SCIEI
1529 West Sequim Bay ROJ
Sequim, Washington 98382
360-681-4583


	MSL Sample ID     METHOXYCLOR	MIREX    PCB-103Surr    PCB-198Surr     TCMX ris       HBB ris      OCN ris
BLANKS
        1790-9abblkA               16.67  U      16.67 U       83.98%          99.33%     125.44%       113.92%      120.56%
        1790-9abblkB              126.00         16.67 U       68.53%         122.72%     109.41%        63.51%      63.75%

 BLANK SPIKES	
    1790-9abBlkSpkA               16.67  U      16.67 U       97.46%         102.13%     105.36%       103.62%      120.46%
      1790-9 BlkSpkB               14.29  U      14.29 U       98.70%         111.06%      97.66%        99.03%      98.58%
     1790-9a-BlkSpkC               16.67  U      16.67 U       96.82%         114.96%      92.12%        94.90%      95.44%

   Spike concentration A
   Spike concentration B
   Spike concentration C
      percent recovery A
      percent recovery B
      percent recovery C

 MATRIX SPIKES
     1790-9ab Average
        1790-9ab-7 MS               15.38  U      15.38 U      108.79%         116.95%      89.63%        85.39%       82.45%
       1790-9ab-12 MS               15.92  U      15.92 U       49.06%         116.15%     161.34%        83.75%       76.20%

   Spike concentration 7
  Spike concentration 12
      percent recovery 7
     percent recovery 12

#=outside project DQO's
U=not detected at or above
NA = not applicable
r=data is rejected
E=data is an estimate
                                                                      E44

-------
                                                                                                       Housatonic River
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
Days held
to
MSL Sample ID Extraction date extraction
17901 Blank
1790-2-1
1790-2-2
1790-2-3
1790-2-4
17902 Blank
1790-2-21
1790-2-22
1790-2-5
1790-2-6
1790-2-23
1790-2-24
1790-2-7 MS
1790-2-8
1790-2-9
1790-2-10
1790-2-11
1790-2-25
1790-2-26
1790-2-Blank Spike
1790-2-1 2 MS
1790-2-13
1790-2-27
1790-2-28
1790SpkBlkB
1790-2-15
1790-2-16
1790-2-29
1790-2-30
1790SpkBlkC
1790-2-17
1790-2-18
1790-2-31
1790-2-32
10/30/2002
10/30/2002
10/30/2002
10/30/2002
10/30/2002
11/6/2002
11/6/2002
11/6/2002
11/6/2002
11/6/2002
11/13/2002
11/13/2002
11/13/2002
11/13/2002
11/13/2002
11/27/2002
11/27/2002
11/27/2002
11/27/2002
11/27/2002
12/11/2002
12/11/2002
12/11/2002
12/11/2002
1/22/2003
1/22/2003
1/22/2003
1/22/2003
1/22/2003
4/16/2003
4/16/2003
4/16/2003
4/16/2003
4/16/2003
0
0
0
0
0
7
7
7
7
7
14
14
14
14
14
28
28
28
28
28
42
42
42
42
84
84
84
84
84
168
168
168
168
168
Aroc lor 1254
Aroclor Days held from
analysis extraction to
date analysis
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
03/14/03
03/14/03
03/14/03
03/14/03
03/14/03
04/09/04
04/09/04
04/09/04
04/09/04
04/09/04
47
47
47
47
47
40
40
40
40
40
33
33
33
33
33
19
19
19
19
19
5
5
5
5
51
51
51
51
51
359
359
359
359
359
Aroc lor 1260
Days held from
Aroclor 1260 extraction to
analysis date analysis
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
03/14/03
03/14/03
03/14/03
03/14/03
03/14/03
04/09/04
04/09/04
04/09/04
04/09/04
04/09/04
47
47
47
47
47
40
40
40
40
40
33
33
33
33
33
19
19
19
19
19
5
5
5
5
51
51
51
51
51
359
359
359
359
359
Pesticides
Days held from
Pesticide extraction to Storage
analysis date analysis Temp
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
12/16/02
03/14/03
03/14/03
03/14/03
03/14/03
03/14/03
04/09/04
04/09/04
04/09/04
04/09/04
04/09/04
47
47
47
47
47
40
40
40
40
40
33
33
33
33
33
19
19
19
19
19
5
5
5
5
51
51
51
51
51
359
359
359
359
359
NA
-20C
-20C
-20C
-20C
NA
4C
4C
-20C
-20C
4C
4C
-20C
-20C
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
Arochlor
4,4'-DDE 4,4'-DDD 2,4-DDT 4,4'-DDT 1254
15.63 U
141.77
138.89
142.03
134.47
15.63 U r
148.27
146.23
147.49
145.86
123.78
119.16
138.31 r
141.26 r
131.52 r
126.78
127.20
125.98
136.68
15.63 U
119.78
118.59
149.51
113.82
15.63 U
122.28
124.89
111.72
114.35
15.63 U
152.90
149.31
144.33
149.17
15.63 U
48.29
27.27
23.18
46.78
15.63 U r
21.13
18.83
51.42
20.13
18.53
18.30
16.90 r
17.55 r
16.82 r
18.85
18.88
21.78 U
20.21
15.63 U
16.98
18.21
25.41
17.52
15.63 U
35.37
36.06
32.22
31.34
15.63 U
53.32
50.31
50.25
52.82
15.63 U
209.80
191.05
197.18
188.75
15.63 U r
211.92
210.81
206.94
193.05
169.73
169.19
198.38 r
213.93 r
187.39 r
173.80
181.75
174.65
186.33
15.63 U
163.57
162.06
215.38
153.26
15.63 U
161.43
170.30
151.04
158.46
15.63 U
211.46
219.02
203.67
199.47
15.63 U
1116.78
1084.52
1168.03
1059.90
15.63 U r
1224.81
1201.60
1107.43
1118.97
1028.16
951.87
1051.99 r
1008.30 r
990.56 r
1021.18
1073.64
1031.98
1078.65
15.63 U
941.60
963.83
1228.06
909.31
15.63 U
874.17
993.10
838.74
840.51
15.63 U
1194.21
1135.42
1109.43
1097.43
312.5 U
7150.9
6509.9
6877.5
7282.6
312.5 U E
6586.7
6757.7
7738.4
6696.3
5029.9
5470.9
11556.2 E
5725.5 E
5843.1 E
5572.4
5754.5
5820.2
5908.6
6524.4
10170.0
4882.4
6162.9
5069.0
6173.1
5332.0
5224.3
4917.3
5063.0
4840.6
4726.0
4668.4
4566.7
4814.4
Arochlor
1260
312.5
25304.4
25532.1
25257.6
23427.9
312.5
26637.2
26835.7
26521.5
25270.3
22670.5
22384.9
26645.6
24050.2
24279.8
22775.2
25859.6
22657.6
23641.3
312.5
20816.3
21563.5
26962.7
20355.4
312.5
19066.0
20390.8
18607.5
18245.1
328.6
24026.3
22600.1
23418.8
24137.7
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
all units are ng/g
E=values are estimated
r=data is rejected
                                                                                                         E45

-------
                                                                                                       Housatonic River
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
Days held
to PCB-103
MSL Sample ID Extraction date extraction Surr
17901 Blank
1790-2-1
1790-2-2
1790-2-3
1790-2-4
17902 Blank
1790-2-21
1790-2-22
1790-2-5
1790-2-6
1790-2-23
1790-2-24
1790-2-7 MS
1790-2-8
1790-2-9
1790-2-10
1790-2-11
1790-2-25
1790-2-26
1790-2-Blank Spike
1790-2-1 2 MS
1790-2-13
1790-2-27
1790-2-28
1790SpkBlkB
1790-2-15
1790-2-16
1790-2-29
1790-2-30
1790SpkBlkC
1790-2-17
1790-2-18
1790-2-31
1790-2-32
10/30/2002
10/30/2002
10/30/2002
10/30/2002
10/30/2002
11/6/2002
11/6/2002
11/6/2002
11/6/2002
11/6/2002
11/13/2002
11/13/2002
11/13/2002
11/13/2002
11/13/2002
11/27/2002
11/27/2002
11/27/2002
11/27/2002
11/27/2002
12/11/2002
12/11/2002
12/11/2002
12/11/2002
1/22/2003
1/22/2003
1/22/2003
1/22/2003
1/22/2003
4/16/2003
4/16/2003
4/16/2003
4/16/2003
4/16/2003
0
0
0
0
0
7
7
7
7
7
14
14
14
14
14
28
28
28
28
28
42
42
42
42
84
84
84
84
84
168
168
168
168
168
U 72.74%
73.11%
77.47%
76.28%
70.72%
U E 76.65%
74.80%
83.10%
80.23%
76.40%
67.12%
69.64%
E 71.81%
E 78.28%
E 72.24%
79.57%
73.01%
69.12%
71.90%
U 66.45%
68.87%
71.70%
60.70%
71.80%
U 68.40%
70.00%
65.88%
62.63%
65.75%
U 113.28%
105.58%
101.50%
100.24%
108.32%
PCB-198
Surr
68.41%
70.60%
76.59%
73.22%
72.46%
70.37%
76.62%
79.59%
77.59%
64.27%
71.84%
72.02%
76.61%
73.22%
67.90%
78.36%
74.40%
69.81%
73.41%
71.06%
75.79%
72.58%
70.08%
66.88%
58.13%
61.97%
59.18%
57.52%
57.74%
116.56%
114.64%
111.39%
107.70%
113.37%
TCMX ris
76.41%
79.47%
69.62%
76.72%
74.52%
60.72%
74.43%
70.66%
68.13%
70.79%
90.18%
78.64%
53.45%
59.79%
58.44%
71.73%
88.17%
93.00%
86.75%
88.34%
90.20%
88.27%
72.13%
93.56%
104.42%
97.48%
104.84%
107.48%
106.44%
111.20%
116.08%
117.94%
120.46%
99.24%
HBB ris
58.13%
59.38%
54.51%
57.80%
57.56%
46.97% #
54.78%
55.94%
51.65%
52.47%
71.57%
63.13%
40.61% ##
47.17% #
43.16% #
62.48%
69.91%
71.72%
69.21%
67.85%
73.33%
70.13%
50.24%
74.82%
82.79%
77.34%
78.25%
84.03%
86.62%
1 04.24%
104.80%
110.91%
109.66%
94.18%
OCN ris
85.43%
89.74%
77.62%
86.42%
87.82%
66.19%
86.45%
85.84%
78.97%
81.41%
107.74%
92.10%
66.65%
70.39%
65.11%
93.19%
113.19%
111.35%
105.66%
103.73%
107.38%
105.34%
80.27%
116.04%
116.95%
116.48%
125.51%
125.68%
135.63%
104.70%
137.22%
142.54%
140.25%
119.75%
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
all units are ng/g
E=values are estimated
r=data is rejected
                                                                                                         E46

-------
                                                                                      QC
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
Days held
to
Extraction date extraction
Aroclor
analysis
date
Aroclor 1254
Days held from
extraction to
analysis
Aroclor 1260
analysis date
Aroclor 1260
Days held from
extraction to
analysis
Pesticide
analysis date
Pesticides
Days held from
extraction to
analysis
Storage
Temp
4,4'-DDE
BLANKS
                       17901 Blank
                       17902 Blank
10/30/2002      0
 11/6/2002      7
         12/16/02
         12/16/02
              47
              40
               12/16/02
               12/16/02
              47
              40
               12/16/02
               12/16/02
              47
              40
             NA
             NA
            15.63 U
            15.63 U r
BLANK SPIKES (Aroclor 1254)
                1790-2-Blank Spike
                    1790 Spk Blk B
                    1790SpkBlkC

Spike concentration BS
Spike concentration BS B
Spike concentration BS C
Percent Recovery BS
Percent Recovery BS B
Percent Recovery BS C

MATRIX SPIKES (Aroclor 1254)
                      1790-2-7 MS
                      1790-2-12 MS
11/27/2002      28
 1/22/2003      84
 4/16/2003     168
         12/16/02
         03/14/03
         04/09/04
              19
              51
              359
               12/16/02
               03/14/03
               04/09/04
               19
               51
              359
               12/16/02
               03/14/03
               04/09/04
               19
               51
              359
             NA
             NA
             NA
            15.63 U
            15.63 U
            15.63 U
11/13/2002
12/11/2002
14
42
12/16/02
12/16/02
33
5
12/16/02
12/16/02
33
5
12/16/02
12/16/02
33
5
-20C
-20C
138.31    r
119.78
1790-2 (ave)
Spike concentration 7-MS
Spike concentration 12-MS
Percent Recovery 7-MS
Percent Recovery 12-MS
U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
all units are ng/g
E=values are estimated
r=data is rejected
                                                                                  E47

-------
                                                                                    QC
BA TTELLE MARINE SCIENCES LABORA TORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
BLANKS
17901 Blank
17902 Blank
BLANK SPIKES (Aroclor 1254)
1790-2 -Blank Spike
1790 Spk Blk B
1790SpkBlkC
Spike concentration BS
Spike concentration BS B
Spike concentration BS C
Percent Recovery BS
Percent Recovery BS B
Percent Recovery BS C
MATRIX SPIKES (Aroclor 1254)
1790-2-7 MS
1790-2-12 MS
1790-2 (ave)
Spike concentration 7-MS
Spike concentration 12-MS
Percent Recovery 7-MS
Percent Recovery 12-MS
Days held
to
Extraction date extraction 4,4'-DDD 2,4-DDT

10/30/2002 0 15.63 U 15.63 U
11/6/2002 7 15.63 U r 15.63 U r

11/27/2002 28 16.18 15.63 U
1/22/2003 84 15.63 U 15.63 U
4/16/2003 168 15.63 U 15.63 U







11/13/2002 14 16.90 r 198.38 r
12/11/2002 42 16.98 163.57





Arochlor Arochlor PCB-103
4,4'-DDT 1254 1260 Surr

15.63 U 312.5 U 312.5 U 72.74%
15.63 U r 312.5 U E 312.5 U E 76.65%

15.63 U 6524.4 312.5 U 66.45%
15.63 U 6173.1 312.5 U 68.40%
15.63 U 4840.6 328.6 U 113.28%
6250.0
6250.0
6250.0
104.4
98.8
77.5

1051.99 r 11556.2 E 26645.6 E 71.81%
941.60 10170.0 20816.3 68.87%
6433.3
6068.0
5800.0
84.4
64.4
PCB-198
Surr

68.41%
70.37%

71.06%
58.13%
116.56%







76.61%
75.79%





U=not detected at or above MDL
NA = not applicable
#=outside project DQO's
all units are ng/g
E=values are estimated
r=data is rejected
                                                                                E48

-------
                                                                               Sequim-1 Pesticide Data
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
1790-8bblkspkA
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4 (20)
1790-8b blk
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-7Spk
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8bblk2
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-12Spk
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8b blk Spk B
1790-8b-15
1790-8b-16
1790-8b-29
1790-8b-30
1790-8b-BlkSpkC
1790-8b-17
1790-8b-18
1790-8b-31
1790-8b-32
Extraction Date
12/8/2003
12/8/2003
12/8/2003
12/8/2003
12/8/2003
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/22/2003
12/22/2003
12/22/2003
12/22/2003
12/22/2003
1/5/2004
1/5/2004
1/5/2004
1/5/2004
1/5/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
Storage Temp
NA
-20C
-20C
-20C
-20C
NA
-20C
-20C
4C
4C
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
Pesticides: Arolchlor 1254:
Pesticides Days held from Arolchlor 1254 Days held from
Analysis Date Extraction to Analysis Analysis Date Extraction to Analysis a-BHC
1/16/2004
1/16/2004
1/16/2004
1/16/2004
1/17/2004
1/17/2004
1/17/2004
1/17/2004
1/17/2004
1/17/2004
1/21/2004
1/21/2004
1/21/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/28/2004
1/28/2004
1/28/2004
1/29/2004
1/29/2004
3/5/2004
3/5/2004
3/5/2004
3/6/2004
3/6/2004
6/3/2004
6/4/2004
6/4/2004
6/4/2004
6/4/2004
39
39
39
39
40
33
33
33
33
33
30
30
30
31
31
17
17
17
17
17
9
9
9
10
10
4
4
4
5
5
10
11
11
11
11
1/16/2004
1/16/2004
1/16/2004
1/16/2004
1/17/2004
1/17/2004
1/17/2004
1/17/2004
1/17/2004
1/17/2004
1/21/2004
1/21/2004
1/21/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/22/2004
1/28/2004
1/28/2004
1/28/2004
1/29/2004
1/29/2004
3/5/2004
3/5/2004
3/5/2004
3/6/2004
3/6/2004
6/3/2004
6/4/2004
6/4/2004
6/4/2004
6/4/2004
39
39
39
39
40
33
33
33
33
33
30
30
30
31
31
17
17
17
17
17
9
9
9
10
10
4
4
4
5
5
10
11
11
11
11
0.11 U r
0.64 E
0.65 E
0.69 E
0.33 r
0.11 U
0.78
0.75
0.54
0.66
6.55
1.12
1.29
1.15 r
1.06
0.11 U r
0.73
1.07
1.14 r
1.03 r
8.20
1.31
1.31
1.57
0.88
3.71
1.42
1.29
1.35
1.36
5.16
1.44
1.44
1.59
1.35
g-BHC
0.50
0.69
0.55
0.68
0.22
0.11 U
0.63
0.68
0.57
0.74
5.59
1.11
1.25
1.15
1.17
0.11 U
0.67
1.07
1.85
1.14
8.13
1.37
1.26
1.55
0.97
3.64
0.87
0.98
1.05
1.06
5.67
1.57
1.61
1.67
1.77
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
units are ng/g
                                                                                     E49

-------
                                                                           Sequim-1 Pesticide Data
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
                         Extraction Date
2,4-DDE
                                                                 a-CHLORDANE
                                                                                       TRANS NONA
4,4'-DDE
2,4-DDD
4,4'-DDD
2,4-DDT
1790-8bblkspkA
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4(20)
1790-8b blk
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-7 Spk
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8bblk2
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-12Spk
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8b blk Spk B
1790-8b-15
1790-8b-16
1790-8b-29
1790-8b-30
1790-8b-BlkSpkC
1790-8b-17
1790-8b-18
1790-8b-31
1790-8b-32
12/8/2003 r
12/8/2003 E
12/8/2003 E
12/8/2003 E
12/8/2003 r
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/22/2003
12/22/2003
12/22/2003
12/22/2003 r
12/22/2003
1/5/2004 r
1/5/2004
1/5/2004
1/5/2004 r
1/5/2004 r
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
0.11 U r
0.88 E
1.35 E
1.51 E
0.32 r
0.11 U
1.63
1.66
1.51
2.12
7.81
3.15
3.89
3.27 r
3.28
0.11 U r
2.84
5.69
2.56 r
4.45 r
7.00
3.76
4.35
4.55
3.29
3.39
3.78
2.99
3.82
5.25
6.49
5.75
6.98
7.23
7.30
0.20 r
2.99 E
4.99 E
5.31 E
1.23 r
0.22
5.60
4.47
3.17
4.28
14.93
8.49
9.81
8.81 r
8.62
0.13 r
6.98
8.64
7.05 r
8.29 r
18.14
9.30
9.06
11.75
6.37
5.05
11.29
8.58
9.89
11.03
6.47
11.76
14.34
14.55
14.30
0.15 r
0.67 E
1.27 E
1.20 E
0.43 r
0.17
1.18
0.96
0.79
0.94
7.45
1.86
2.21
1.94 r
1.91
0.11 U r
1.55
1.89
1.56 r
1.72 r
8.90
2.08
2.00
2.48
1.40
4.93
2.33
1.73
2.01
2.30
6.46
1.81
2.15
2.02
2.04
0.21 r
0.88 E
1.64 E
1.57 E
0.45 r
0.17
1.35
1.04
0.74
1.01
9.72
2.48
2.87
2.74 r
2.46
0.13 r
1.85
2.44
1.92 r
2.21 r
9.33
2.75
2.63
3.47
1.94
5.31
3.37
2.35
2.85
3.38
6.77
3.32
4.13
4.09
4.14
0.88 r
0.40 E
0.60 E
0.46 E
0.29 r
0.11 U
0.56
0.35
0.27
0.29
5.96
0.59
0.72
0.61 r
0.48
0.11 U r
0.36
0.59
0.33 r
1.02 r
10.91
2.48
2.49
2.97
1.67
4.73
2.75
2.05
2.33
2.64
6.84
2.67
3.31
3.06
3.22
0.11 r
0.70 E
1.12 E
1.31 E
0.32 r
0.11 U
1.12 r
0.87 r
0.64
0.83 r
8.99
2.62
2.65
2.42 r
2.16
0.11
1.65
1.77 r
1.82
1.99
13.75
1.90
1.74
1.84
1.52
5.08
3.27
2.37
3.14
3.24
6.06
2.48
3.25
3.07
3.16
0.11 U
0.25
0.53
0.44
0.24
0.11 U
0.39
0.32
0.22
0.30
6.23
0.77
0.92
0.90
0.92
0.11 U
0.61
0.69
0.63
0.86
7.83
0.74
0.65
0.96
0.61
5.15
0.89
0.69
1.05
1.23
6.24
0.95
1.12
1.48
1.31
r
E
E
E
r

r
r

r



r



r

















U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
units are ng/g
                                                                                 E50

-------
                                                                            Sequim-1 Pesticide Data
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
                         Extraction Date
                                              MIREX
                                                             Arochlor 1254
                                                                                 PCB-103Surr
                                                                                                    PCB-198Surr
                                                                                                                        TCMX ris
                                                                                                                                       HBB ris
                                                                                                                                                            OCN ris
1790-8bblkspkA
1790-8b-1
1790-8b-2
1790-8b-3
1790-8b-4(20)
1790-8b blk
1790-8b-5
1790-8b-6
1790-8b-21
1790-8b-22
1790-8b-7 Spk
1790-8b-8
1790-8b-9
1790-8b-23
1790-8b-24
1790-8bblk2
1790-8b-10
1790-8b-11
1790-8b-25
1790-8b-26
1790-8b-12Spk
1790-8b-13
1790-8b-14
1790-8b-27
1790-8b-28
1790-8b blk Spk B
1790-8b-15
1790-8b-16
1790-8b-29
1790-8b-30
1790-8b-BlkSpkC
1790-8b-17
1790-8b-18
1790-8b-31
1790-8b-32
12/8/2003
12/8/2003
12/8/2003
12/8/2003
12/8/2003
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/15/2003
12/22/2003
12/22/2003
12/22/2003
12/22/2003
12/22/2003
1/5/2004
1/5/2004
1/5/2004
1/5/2004
1/5/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
1/19/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
3/1/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
5/24/2004
0.11 U r
0.47 E
0.93 E
0.99 E
0.28 r
0.11 U
0.78 r
0.63 r
0.48
0.63 r
7.13
1.94
1.81
1.64 r
1.67
0.11 U
1.25
1.28 r
1.43
1.41
8.09
1.47
1.36
1.69
1.13
6.22
1.91
1.54
1.66
1.93
6.62
2.03
2.53
2.36
2.48
16.4 r
28.7 E
54.4 E
57.4 E
14.2 r
4.2
47.44 E
35.29 E
29.75
34.75 E
92.25
128.15
121.9
112.11 r
115.87
2.22 E
78.66 E
84.9 E
86.44 E
91.15 E
152.93
94.67
88.19
115.16
73.5
9.6
133.1
100.0
109.7
125.6
25.4
144.8
192.4
168.8
192.1
63.37%
70.58%
74.45%
63.32%
56.24%
79.00%
91 .29%
85.88%
81.61%
98.12%
100.98%
78.24%
99.15%
96.07%
102.59%
73.90%
67.76%
87.61%
58.84%
75.87%
116.63%
105.87%
102.76%
127.79%
95.94%
97.29%
113.89%
87.54%
106.16%
102.21%
106.81%
99.14%
91.19%
99.30%
91 .07%
66.31%
66.73%
71.61%
61.05%
63.83%
96.45%
79.94%
71.38%
60.66%
82.35%
85.97%
95.25%
89.84%
90.67%
94.09%
91.85%
61.43%
65.55%
75.56%
75.92%
131.88%
94.08%
80.42%
106.15%
103.89%
133.23%
104.98%
88.24%
105.29%
95.50%
122.68%
109.34%
115.15%
113.26%
112.28%
168.22% #
149.38%
140.54%
134.20%
162.63% #
131.23%
140.73%
136.43%
130.39%
136.61%
126.83%
138.01%
121.89%
162.71% #
136.34%
156.91% #
142.75%
129.22%
171.81% #
152.48% #
84.06%
98.85%
105.73%
85.50%
110.99%
86.91%
83.40%
88.05%
86.78%
80.16%
79.01%
84.76%
76.70%
84.60%
76.69%
174.34% #
168.28% #
153.13% #
145.27%
165.07% #
126.71%
159.47% #
153.12% #
146.27%
151.97% #
137.58%
109.67%
120.53%
158.79% #
124.55%
147.82%
141.34%
153.28% #
144.95%
141.82%
70.16%
109.02%
122.09%
97.95%
104.88%
76.70%
81 .07%
83.34%
82.28%
78.71%
88.13%
91.31%
78.14%
91.31%
85.41%
189.38% #
187.58% #
170.25% #
161.00% #
181.93% #
140.22%
181.57% #
171.04% #
164.37% #
168.53% #
157.15% #
114.42%
141.34%
191.08% #
147.36%
170.18% #
158.49% #
175.24% #
58.61%
160.22% #
79.08%
122.42%
138.05%
110.97%
120.65%
83.39%
90.43%
94.40%
91.10%
75.59%
93.11%
95.56%
82.12%
97.81%
90.73%
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
units are ng/g
                                                                                 E51

-------
                                                                                 QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
                          Extraction Date
                  Storage Temp
               Pesticides
              Analysis Date
                    Pesticides:
                  Days held from
               Extraction to Analysis
               Arolchlor 1254
               Analysis Date
                 Arolchlor 1254:
                 Days held from
               Extraction to Analysis
                                                                                                                                                       a-BHC
BLANKS
           1790-8b blk
          1790-8bblk2
12/15/2003
 1/5/2004
NA
NA
1/17/2004
1/22/2004
33
17
1/17/2004
1/22/2004
33
17
0.11  U
0.11  U
BLANK SPIKES
      1790-8b blk spk A       12/8/2003
      1790-8b blk Spk B       3/1/2004
     1790-8b- Blk Spk C       5/24/2004

Spike Concentration A
Spike Concentration B
Spike Concentration C
Percent Recovery A
Percent Recovery B
Percent Recovery C

MATRIX SPIKES
            1780-8 Ave
         1790-8b-7Spk      12/22/2003
        1790-8b-12Spk       1/19/2004

Spike Concentration 7
Spike Concentration 12
Percent Recovery 7
Percent Recovery 12
                        NA
                        NA
                        NA
                1/16/2004

                6/3/2004
                        39

                        10
                  1/16/2004

                  6/3/2004
                       39

                       10
                       -20C
                       -20C
                1/21/2004
                1/28/2004
                        30
                         9
                  1/21/2004
                  1/28/2004
                       30
                        9
                      0.11  U
                      3.71
                      5.16

                      5.55
                      5.55
                      5.55
                    0.00%  #
                   64.78%
                   92.95%
                      1.21
                      6.55
                      8.20

                      5.52
                      5.44
                   96.66%
                  128.42% #
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
                                                                             E52

-------
                                                                                QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
                          Extraction Date
                  g-BHC
                2,4-DDE
                                                                              a-CHLORDANE
                                            TRANS NONA
                                         4,4'-DDE
                                 2,4-DDD
BLANKS
           1790-8b blk
          1790-8bblk2
BLANK SPIKES
      1790-8b blk spk A
      1790-8b blk Spk B
     1790-8b-BlkSpkC

Spike Concentration A
Spike Concentration B
Spike Concentration C
Percent Recovery A
Percent Recovery B
Percent Recovery C

MATRIX SPIKES
            1780-8 Ave
         1790-8b-7Spk
        1790-8b-12Spk

Spike Concentration 7
Spike Concentration 12
Percent Recovery 7
Percent Recovery 12
12/15/2003
 1/5/2004
 12/8/2003
 3/1/2004
 5/24/2004
12/22/2003
 1/19/2004
    0.11 U
    0.11 U
    0.50
    3.64
    5.67

    5.55
    5.55
    5.55
  8.95%  #
 65.57%
102.10%
    1.23
    5.59
    8.13

    5.52
    5.44
 79.05%
126.81% #
    0.11 U
    0.11 U
    0.11  U
    3.39
    6.49

    5.55
    5.55
    5.55
  0.00%  #
 61.05%
116.94%
    3.69
    7.81
    7.00

    5.52
    5.44
 74.72%
 60.92%
    0.22
    0.13
    0.20
    5.05
    6.47

    5.55
    5.55
    5.55
  1.19%  #
 88.69%
116.59%
    9.03
   14.93
   18.14

    5.52
    5.44
106.90%
167.52% #
    0.17
    0.11 U
    0.15
    4.93
    6.46

    5.55
    5.55
    5.55
  2.72%  #
 88.77%
116.36%
    1.99
    7.45
    8.90

    5.52
    5.44
 98.98%
127.11% #
    0.17
    0.13
    0.21
    5.31
    6.77

    5.55
    5.55
    5.55
  1.49%  #
 93.29%
121.94%#
    2.67
    9.72
    9.27

    5.52
    5.44
127.77%#
121.32%#
    0.11
    0.11
    0.88
    4.73
    6.84

    5.55
    5.55
    5.55
 15.92%  #
 85.31%
123.20% #
    1.26
    5.96
    7.17

    5.52
    5.44
 85.08%
108.64%
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
                                                                            E53

-------
                                                                                QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
                          Extraction Date
                  4,4'-DDD
             2,4-DDT
                                                                                MIREX
                              Arochlor1254
                                  PC B-103 Sim-
                              PC B-198 Surr
BLANKS
           1790-8b blk
          1790-8bblk2
12/15/2003
 1/5/2004
0.11  U
0.11  U
0.11  U
0.11  U
0.11
0.11
 4.2
2.22
79.00%
73.90%
96.45%
91.85%
BLANK SPIKES
      1790-8b blk spk A      12/8/2003              0.11    r        0.11  U  r      0.11   U
      1790-8b blk Spk B       3/1/2004              5.08             5.15           6.22
     1790-8b-BlkSpkC      5/24/2004              6.06             6.24           6.62

Spike Concentration A                               5.55             5.55           5.55
Spike Concentration B                               5.55             5.55           5.55
Spike Concentration C                               5.55             5.55           5.55
Percent Recovery A                                0.00% #         0.00% #       0.00%   #
Percent Recovery B                              91.57%          92.80%       112.03%
Percent Recovery C                             109.13%         112.39%       119.25%

MATRIX SPIKES
            1780-8 Ave                            2.11             0.81            1.59
         1790-8b-7Spk      12/22/2003             8.99             6.23           7.13
        1790-8b-12Spk      1/19/2004             13.75             7.83           8.09

Spike Concentration 7                               5.52             5.52           5.52
Spike Concentration 12                              5.44             5.44           5.44
Percent Recovery 7                             124.57% #         98.16%       100.44%
Percent Recovery 12                             213.94% #        129.01 % #      119.48%
                                                                              16.4
                                                                               9.6
                                                                              25.4
                                                                         63.37%
                                                                         97.29%
                                                                        106.81%
                                                                           66.31%
                                                                          133.23%
                                                                          122.68%
                                                                             92.25
                                                                            152.93
                                                                        100.98%
                                                                        116.63%
                                                                           85.97%
                                                                          131.88%
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
                                                                            E54

-------
                                                                               QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
MSL Sample ID
                         Extraction Date    TCMX ris
                              HBB ris
                                OCN ris
BLANKS
           1790-8b blk
         1790-8bblk2
12/15/2003
 1/5/2004
131.23%
156.91%#
126.71%
147.82%
140.22%
170.18%#
BLANK SPIKES
      1790-8b blk spk A       12/8/2003        168.22% #        174.34% #       189.38%  #
      1790-8b blk Spk B       3/1/2004          86.91%           76.70%          83.39%
     1790-8b-BlkSpkC       5/24/2004         79.01%           88.13%          93.11%

Spike Concentration A
Spike Concentration B
Spike Concentration C
Percent Recovery A
Percent Recovery B
Percent Recovery C

MATRIX SPIKES
            1780-8 Ave
         1790-8b-7Spk      12/22/2003        126.83%          137.58%         157.15% #
       1790-8b-12Spk       1/19/2004         84.06%           70.16%          79.08%

Spike Concentration 7
Spike Concentration 12
Percent Recovery 7
Percent Recovery 12
U=not detected at or above MDL
NA = not applicable
#=outside Project DQO's
r=values are rejected
E=values are estimated
                                                                           E55

-------
                                                                                                   Tri-Cities
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583




































MSLSamplelD
2056Blank1
2056-1-1
2056-1-2
2056-1-3
2056-1-4
2056-1-5
2056-1-6
2056-1-21
2056-1-22
2056-1 SpkBlkA
2056-1-7 MS
2056-1-8
2056-1-9
2056-1-23
2056-1-24
2056-1 Blank 2
2056-1-10
2056-1-11
2056-1-25
2056-1-26
2056-1 Spk Blk B
2056-1-15
2056-1-16
2056-1-29
2056-1-30
2056-1 -12 MS
2056-1-13
2056-1-14
2056-1-27
2056-1-28
2056-1 Spk Blk C
2056-1-17
2056-1-18
2056-1-31
2056-1-32
Storage Aroc lor 1260 Aroclor1242 Pesticide
Extraction Date Temperature Analysis Date Analysis Date Analysis Date g-CHLORDANE a-CHLORDANE TRANS NONA
9/25/2003
9/25/2003
9/25/2003
9/25/2003
9/25/2003
10/02/03
10/02/03
10/02/03
10/02/03
10/02/03
10/9/2003
10/9/2003
10/9/2003
10/9/2003
10/9/2003
10/23/2003
10/23/2003
10/23/2003
10/23/2003
10/23/2003
12/18/2003
12/18/2003
12/18/2003
12/18/2003
12/18/2003
11/6/2003
11/6/2003
11/6/2003
11/6/2003
11/6/2003
3/11/2004
3/11/2004
3/11/2004
3/11/2004
3/11/2004
-20C
-20C
-20C
-20C
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
-20C
-20C
-20C
4C
4C
NA
-20C
-20C
4C
4C
10/2/2003
10/2/2003
10/2/2003
10/2/2003
10/2/2003
10/31/2003
10/31/2003
10/31/2003
10/31/03
10/31/03
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
11/19/2003
11/19/2003
11/19/2003
11/19/2003
11/19/2003
3/16/2004
3/16/2004
3/16/2004
3/17/2004
3/17/2004
10/2/2003
10/2/2003
10/2/2003
10/2/2003
10/2/2003
10/31/2003
10/31/2003
10/31/2003
10/31/2003
10/31/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
11/19/2003
11/19/2003
11/19/2003
11/19/2003
11/19/2003
3/16/2004
3/16/2004
3/16/2004
3/17/2004
3/17/2004
10/2/2003
10/2/2003
10/2/2003
10/2/2003
10/2/2003
10/31/2003
10/31/2003
10/31/2003
10/31/2003
10/31/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
11/1/2003
1/24/2004
1/24/2004
1/24/2004
1/24/2004
1/24/2004
11/19/2003
11/19/2003
11/19/2003
11/19/2003
11/19/2003
3/16/2004
3/16/2004
3/16/2004
3/17/2004
3/17/2004
62.50 U
4506.70
4153.74
5988.78
6656.28
5219.43
2348.28 E
5397.90
5107.54
1964.27
9684.58
5533.67
7260.37
5374.99
3574.41 r
62.50 U
5827.50
7363.31
4947.25
3779.94 r
2605.84
7795.42
7729.30
8137.04
7594.36
9066.92
6020.98
7646.19
6859.77
6003.33
2456.92 r
6383.76 r
5882.05 r
5830.76 r
5533.64 r
62.50 U
5111.45
4685.38
6595.08
7493.35
5844.65
2821.81 E
6021.90
5715.59
2706.45
10758.57
6176.27
7995.00
6065.01
4088.98 r
62.50 U
6526.00
8091.35
5555.65
4308.55 r
3223.06
8182.71
8052.02
8493.33
7959.89
10168.05
6602.86
7896.78
7068.64
6289.87
3204.48 r
7513.58 r
6143.78 r
6162.69 r
5840.46 r
62.50 U
3063.27
2865.40
4079.23
4705.70
3648.83
1690.18
3768.89
3569.86
62.50 U
4824.32
3804.62
4985.15
3773.27
2534.55
62.50 U
4042.63
5180.12
3475.13
2694.14
55.56 U
5310.80
5246.33
5521.57
5252.04
4118.55
4145.63
5054.39
4486.34
3967.55
62.50 U
4609.32
4181.56
4144.59
3978.01
# outside Project DQO
U=undetected
r=rejected


















E=estimated value
units are ng/g









                                                                                                  E56

-------
BATTELLE MARINE SCIENCES LAI
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
                                                                                               Tri-Cities
              MSLSamplelD
                                   Arochlor1242
                                                            Arochlor1260
                                                                              PCB-103 Surr
                                                                                                     PCB-198 Surr
                                                                                                                             TCMX ris
                                                                                                                                               HBB ris
                                                                                                                                                              OCN ris
                                                                                                                                                                                PCB8
                                                                                                                                                                                              PCB52



































2056Blank1
2056-1-1
2056-1-2
2056-1-3
2056-1-4
2056-1-5
2056-1-6 E
2056-1-21
2056-1-22
2056-1 Spk Blk A
2056-1-7 MS
2056-1-8
2056-1-9
2056-1-23
2056-1-24 r
2056-1 Blank 2
2056-1-10
2056-1-11
2056-1-25
2056-1-26 r
2056-1 Spk Blk B
2056-1-15
2056-1-16
2056-1-29
2056-1-30
2056-1 -12 MS
2056-1-13
2056-1-14
2056-1-27
2056-1-28
2056-1 Spk Blk C r
2056-1-17 r
2056-1-18 r
2056-1-31 r
2056-1-32 r
1250.0 U
24177.9
24518.1
29845.8
26415.3
26728.2
21027.2 E
26392.6
26845.4
1250.0 U
27922.98
31721.71
36796.08
25479.28 E
23057.99 r
1250.00
28725.92
29429.26
29211.35
21316.36 r
1111.11 E
30426.96
32165.07
35173.17
29957.54
22741.5
25819.9
32912.7
36196.0
28566.1
1250.0 E
25112.0 E
20028.8 E
21524.7 E
20921.4 E
1250.0 U
8207.6
10114.8
12763.2
11526.1
10937.8
7013.5 E
13975.1
10450.0
12033.6
24759.00
11647.60
13394.13
10838.90
7494.27 r
1250.00
14207.29
14082.39
11774.98
8312.50 r
11226.50
14759.55
15208.49
14953.08
15394.04
24370.9
12073.4
16397.6
16126.0
13855.8
11965.1 E
12822.9 E
11096.7 E
14464.8 E
8733.6 E
87.30%
84.80%
78.71%
105.32%
88.63%
89.86%
46.61% n
98.76%
93.23%
95.04%
122.14%
109.03%
134.26%
96.41%
63.54% n
102.97%
106.18%
111.80%
87.11%
70.77% #
103.01%
116.99%
107.08%
108.40%
105.12%
126.93%
102.96%
131.60%
118.94%
101.66%
56.32%
103.63%
97.43%
100.43%
97.37%
88.85%
76.16%
73.51%
103.34%
86.82%
91 .24%
45.08% n
92.23%
85.62%
94.68%
123.63%
99.39%
121.68%
82.60%
61 .68%
97.50%
108.44%
105.21%
90.59%
62.70%
89.10%
105.66%
103.20%
100.49%
98.28%
118.39%
97.44%
112.63%
107.43%
82.27%
85.49%
98.78%
95.85%
97.00%
96.37%
118.79%
125.21%
115.35%
107.52%
116.41%
121.84%
138.29%
114.61%
124.67%
128.73%
99.99%
84.77%
92.76%
143.23%
204.55% n
120.04%
113.91%
112.59%
147.49%
175.51% #
135.16%
119.99%
141.59%
126.59%
128.70%
96.46%
107.95%
95.64%
99.33%
123.25%
161.52% n
167.88% #
168.68% n
174.43% n
176.45% n
120.73%
134.51%
121.71%
1 1 1 .49%
126.58%
119.66%
131.71%
122.09%
132.86%
115.87%
97.39%
90.28%
102.21%
159.72% n
206.48% n
121.08%
110.55%
118.00%
136.58%
191.71% #
162.36% n
127.19%
149.52%
133.07%
138.11%
94.45%
102.97%
92.32%
98.18%
126.45%
80.38%
86.21%
86.01%
88.33%
93.73%
144.73%
163.35% #
145.01%
134.99%
152.67% #
143.13%
153.58% #
144.38%
158.74% #
136.68%
121.73%
107.14%
124.21%
188.46% #
244.82% #
138.29%
134.35%
144.16%
167.49% #
225.87% #
165.37% #
148.90%
175.79% #
152.28% #
166.70% #
120.91%
130.39%
117.31%
124.12%
156.55% #
74.73%
91.02%
90.46%
93.42%
96.16%
62.50 U
344.05
319.97
536.22
470.63
475.15
249.54 E
506.50
488.05
62.50 U
58.48 U
580.47
758.80
565.98
438.13 r
62.50 U
525.77
595.27
519.05
356.97 r
55.56 U
604.52
630.89
759.89
638.27
60.02 U
438.10
857.29
924.87
749.01
62.50 U r
806.97 r
741.23 r
653.58 r
682.93 r
125.65
645.93
635.95
864.27
721.73
884.05
852.48
929.65
874.47
62.50
1124.50
1012.57
1287.46
860.36
580.22
62.50
977.03
1029.13
786.35
617.37
55.56
748.84
721.57
789.99
731.26
1077.81
899.05
1036.66
959.20
805.84
62.50
769.05
769.63
750.94
737.07
# outside Project DQO
U=undetected
r=rejected




















E=estimated value
units are ng/g










                                                                                              E57

-------
BATTELLE MARINE SCIENCES LAI
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
                                                                                                Tri-Cities
               MSLSamplelD
                                   PCB 153
                                                 PCB 138
                                                                 PCB 187
                                                                               PCB 180
                                                                                             PCB 170



































2056Blank1
2056-1-1
2056-1-2
2056-1-3
2056-1-4
2056-1-5
2056-1-6 E
2056-1-21
2056-1-22
2056-1 SpkBlkA U
2056-1-7 MS
2056-1-8
2056-1-9
2056-1-23
2056-1-24 r
2056-1 Blank 2 U
2056-1-10
2056-1-11
2056-1-25
2056-1-26 r
2056-1 Spk Blk B U
2056-1-15
2056-1-16
2056-1-29
2056-1-30
2056-1 -12 MS
2056-1-13
2056-1-14
2056-1-27
2056-1-28
2056-1 Spk Blk C U r
2056-1-17 r
2056-1-18 r
2056-1-31 r
2056-1-32 r
62.50 U
1305.78
1308.52
1764.89
1474.30
1767.88
1176.45 E
2139.99
1659.67
62.50 U
4622.27
1850.59
2259.72
1732.18 r
1222.95 r
62.50 U
2223.33
2216.04
1923.18
1352.42 r
55.56 U r
986.03
1035.37
842.04
994.05
3831.40
1665.03
1967.13
1349.31
1496.73
62.50 U
1197.08
1027.55
1372.50
789.75
62.50 U
810.53
819.01
1130.71
948.19
1082.88
630.07 E
1286.96
1004.16
62.50 U
58.48 U
1098.73
1330.44
975.87 r
700.26 r
62.50 U
1345.07
1350.79
1160.59
789.80 r
55.56 U r
1179.78
1240.57
1058.50
1252.81
60.02 U
1006.33
1432.37
1062.19
1098.84
62.50 U
1317.54
1138.21
1477.99
934.10
62.50 U
391.43
379.16
512.68
415.17
487.15
287.94 E
611.01
450.22
704.60
1389.57
481.89
585.80
429.11 r
329.72 r
62.50 U
648.13
633.97
524.35
374.59 r
638.98 r
662.25
706.91
618.32
735.05
1288.26
468.88
494.68
309.23
402.35
778.33
685.32
586.23
842.96
460.69
0.00 U
773.24
741.56
1052.74
858.46
1049.53
657.63 E
1230.17
957.10
1400.50
2896.37
969.55
1151.24
921.43 r
675.06 r
62.50 U
1274.69
1309.61
1032.52
731.30 r
874.60 r
933.21
1014.39
857.80
1118.62
2324.86
1018.82
1193.48
787.20
957.85
1070.41
1146.17
929.75
1710.43
805.26
62.50 U
473.89
491.66
657.81
553.53
627.82
407.40 E
776.04
581.95
62.50
58.48 U
653.04
762.82
564.38 r
424.49 r
62.50 U
844.06
804.48
682.92
492.40 r
55.56 U r
466.95
511.99
414.84
568.83
60.02 U
586.30
660.19
459.36
517.46
62.50 U
916.88
750.49
908.81
633.30
# outside Project DQO
U=undetected
r=rejected












E=estimated value
units are ng/g






                                                                                               E58

-------
                                                                 QC
BATTELLE MARINE SCIENCES LABORATORIES
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583

BLANKS
MSL Sample ID
2056 Blank 1
2056-1 Blank 2
Extraction Date
9/25/2003
10/23/2003
Storage
Temperature
-20C
NA
Aroclor 1260
Analysis Date
10/2/2003
11/1/2003
Aroclor 1242
Analysis Date
10/2/2003
11/1/2003
BLANK SPIKES
                 2056-1 Spk Blk A
                 2056-1 Spk Blk B
                 2056-1 Spk Blk C
  10/02/03
12/18/2003
 3/11/2004
Spike Concentration BSA
Spike Concentration BSB
Spike concentration BSC
Perceny Recovery BSA
Perceny Recovery BSB
Perceny Recovery BSC

MATRIX SPIKES
                     2056-1-7 MS
                    2056-1-12 MS
 10/9/2003
 11/6/2003
 NA
 NA
 NA
-20C
-20C
  10/31/03
 1/24/2004
 3/16/2004
 11/1/2003
11/19/2003
10/31/2003
 1/24/2004
 3/16/2004
 11/1/2003
11/19/2003
2056-1 (ave)
Spike Concentration 7-MS
Spike Concentration 12-MS
Percent Recovery 7-MS
Percent Recovery 12-MS

# outside Project DQO
U=undetected
r=rejected
E=estimated value
                                                             E59

-------
                                                               QC
BATTELLE MARINE SCIENCES LABOR
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
Pesticide
MSL Sample ID Analysis Date g-CHLORDANE a-CHLORDANE TRANS NONA
BLANKS
2056 Blank 1
2056-1 Blank 2
BLANK SPIKES
2056-1 Spk Blk A
2056-1 Spk Blk B
2056-1 Spk Blk C
Spike Concentration BSA
Spike Concentration BSB
Spike concentration BSC
Perceny Recovery BSA
Perceny Recovery BSB
Perceny Recovery BSC
MATRIX SPIKES
2056-1 -7 MS
2056-1 -12 MS
2056-1 (ave)
Spike Concentration 7-MS
Spike Concentration 12-MS
Percent Recovery 7-MS
Percent Recovery 12-MS

10/2/2003 62.50 U
11/1/2003 62.50 U

10/31/2003 1964.27
1/24/2004 2605.84
3/16/2004 2456.92 r
3125.00
2777.78
3125.00
62.86
93.81
78.62

11/1/2003 9684.58
11/19/2003 9066.92
5873.45
2923.98
3001.20
130.34 #
106.41

62.50 U
62.50 U

2706.45
3223.06
3204.48 r
3125.00
2777.78
3125.00
86.61
116.03
102.54

10758.57
10168.05
6403.67
2923.98
3001.20
148.94 #
125.43 #

62.50 U
62.50 U

62.50 U
55.56 U
62.50 U r
NS
NS
NS




4824.32
4118.55
4063.54
NS
NS


# outside Project DQO
U=undetected
r=rejected
E=estimated value
                                                            E60

-------
BATTELLE MARINE SCIENCES LABOR
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
                                                               QC
                  MSL Sample ID     Arochlor 1242
                     Arochlor1260    PCB-103Surr
                                               PCB-198Surr
BLANKS
                    2056 Blank 1
                 2056-1  Blank 2
  1250.0  U
 1250.00
                  1250.0
                 1250.00
          U
 87.30%
102.97%
88.85%
97.50%
BLANK SPIKES
                2056-1 Spk Blk A
                2056-1 Spk Blk B
                2056-1 Spk Blk C
Spike Concentration BSA
Spike Concentration BSB
Spike concentration BSC
Perceny Recovery BSA
Perceny Recovery BSB
Perceny Recovery BSC

MATRIX SPIKES
  1250.0
 1111.11
  1250.0
U
    E
    E
 12033.6
11226.50
 11965.1   E
 95.04%
103.01%
 56.32%
94.68%
89.10%
85.49%
                    2056-1-7 MS
                   2056-1-12 MS
27922.98
 22741.5
               24759.00
                24370.9
                    122.14%
                    126.93%
                       123.63%
                       118.39%
2056-1  (ave)
Spike Concentration 7-MS
Spike Concentration 12-MS
Percent Recovery 7-MS
Percent Recovery 12-MS

# outside Project DQO
U=undetected
r=rejected
E=estimated value
                                                           E61

-------
                                                            QC
BATTELLE MARINE SCIENCES LABOR
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
                 MSL Sample ID TCMX ris	HBB ris      OCN ris	PCB 8	PCB 52	PCB 153     PCB138
BLANKS
2056 Blank 1 118.79% 120.73% 144.73%
2056-1 Blank 2 120.04% 121.08% 138.29%
BLANK SPIKES
2056-1 Spk Blk A 128.73% 115.87% 136.68%
2056-1 Spk Blk B 135.16% 162.36% # 165.37% #
2056-1 Spk Blk C 161. 52% # 80.38% 74.73%
Spike Concentration BSA
Spike Concentration BSB
Spike concentration BSC
Perceny Recovery BSA
Perceny Recovery BSB
Perceny Recovery BSC
MATRIX SPIKES
2056-1-7 MS 99.99% 97.39% 121.73%
2056-1-12 MS 96.46% 94.45% 120.91%
2056-1 (ave)
Spike Concentration 7-MS
Spike Concentration 12-MS

62.50 U
62.50 U

62.50 U
55.56 U
62.50 U r
NA
NA
NA




58.48 U
60.02 U

NA
NA

125.65
62.50 U

62.50 U
55.56 U
62.50 U r
NA
NA
NA




1124.50
1077.81

NA
NA

62.50 U
62.50 U

62.50 U
55.56 U
62.50 U
NA
NA
NA




4622.27
3831.40

NA
NA

62.50
62.50

62.50
55.56
62.50
NA
NA
NA




58.48
60.02

NA
NA

U
U

U
U
U







U
U



Percent Recovery 7-MS
Percent Recovery 12-MS

# outside Project DQO
U=undetected
r=rejected
E=estimated value
                                                         E62

-------
                                                              QC
BATTELLE MARINE SCIENCES LABOR
1529 West Sequim Bay Road
Sequim, Washington 98382
360-681-4583
                  MSL Sample ID  PCB 187     PCB180     PCB170
BLANKS


BLANK SPIKES



Spike Concentration
Spike Concentration
Spike concentration

2056 Blank 1
2056-1 Blank 2

2056-1 Spk Blk A
2056-1 Spk Blk B
2056-1 Spk Blk C
BSA
BSB
BSC

62.50 U
62.50 U

704.60
638.98
778.33
NA
NA
NA

0.00 U
62.50 U

1400.50
874.60
1070.41
NA
NA
NA

62.50 U
62.50 U

62.50
55.56 U
62.50 U
NA
NA
NA
Perceny Recovery BSA
Perceny Recovery BSB
Perceny Recovery BSC

MATRIX SPIKES
                    2056-1-7 MS   1389.57      2896.37        58.48 U
                   2056-1-12 MS   1288.26      2324.86        60.02 U

2056-1  (ave)
Spike Concentration 7-MS                 NA          NA          NA
Spike Concentration 12-MS                NA          NA          NA
Percent Recovery 7-MS
Percent Recovery 12-MS

# outside Project DQO
U=undetected
r=rejected
E=estimated value
                                                           E63

-------
E64

-------
                     Appendix F



Metals Data for the Sinclair Sediment and Wilmington Soil
                          Fl

-------
F2

-------
                                               Sinclair Sediment
Dry
Age of Sediment
days
0
0
0
0
0
92
92
182
216
283
283
391
391
mean
STD
CV
As
Cu
Pb
Zn
As
ng/g
23.4
24.4
22.1
21.6
20.8
22.7
17.5
19.3
16.2
23.2
21.0
18.3
18.9
20.7
2.51
12.09
548
542
517
496
419
490
487
508
511
490
454
414
453
486.9
41.77
8.58
DR1
149
191
180
135
151
167
151
134
258
249
232
160
179.7
43.70
24.32
456
515
437
473
469
481
422
448
414
465
440
403
407
448.4
32.61
7.27
23.4
24.4
22.1
21.6
20.8
22.3
21.1
23.6
17.9
24.5
26.0
20.2
24.0
22.5
2.18
9.69
Wet
Cu
Pb
Zn
ng/g
548
542
517
496
419
642
454
574
538
447
535
462
460
510.4
61.80
12.11
DR1
149
191
180
135
167
142
179
156
154
228
147
151
164.9
26.08
15.82
456
515
437
473
469
484
445
512
456
476
485
429
455
468.6
26.12
5.57
1
 DR = Data removed because of possible contamination
                                                   F3

-------
                                                Wilmington Soil
Dry
Age of Sediment
days
0
0
0
0
0
90
90
183
183
280
280
392
392
mean
STD
CV
As

60.6
63.4
65.0
60.5
67.7
66.0
59.3
71.6
61.2
56.9
54.2
60.2
59.9
62.0
4.64
7.48
Cu
«
128
129
111
121
120
131
116
144
123
146
129
127
124
126.8
9.84
7.76
Pb
j/g
5140
5700
5280
6010
6250
7270
5960
8139
6883
5820
5600
4874
4804
5979.2
968.90
16.20
Zn

DR1
57.1
66.2
65.0
57.5
60.6
52.2
65.0
68.0
70.9
65.4
69.4
66.6
63.7
5.62
8.83
As

60.6
63.4
65.0
60.5
67.7
71.8
61.4
62.3
63.0
62.2
58.9
59.9
68.8
63.5
3.83
6.03
Wet
Cu
«
128
129
111
121
120
141
121
125
123
133
138
122
113
125.0
8.77
7.02
Pb
3/g
5140
5700
5280
6010
6250
7440
5750
7020
6160
4980
6570
4484
4660
5803.4
893.00
15.39
Zn

DR1
57.1
66.2
65.0
57.5
77.2
67.9
63.0
61.1
55.9
74.6
56.3
50.9
62.7
7.89
12.57
1
 DR = Data removed because of possible contamination
                                                   F4

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