&EPA
United States
Environmental Protection
Agency
Office of Modeling. Monitoring
Systems, and Quality Assurance
Washington DC 20460
EPA/600/4-91/008
February 1991
Research and Development
Direct/Delayed
Response Project:
Soil Characterization
Comparison.
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DIRECT DELAYED RESPONSE PROJECT
SOIL CHARACTERIZATION COMPARISON
by
L. K. Fenstermaker, G. E. Byers", T. H. Starks, M. J. Miah",
C. J. Palmer, and K. D. Lauckner
Environmental Research Center
University of Nevada, Las Vegas
Cooperative Agreement No. CR814701-01
'Lockheed Engineering and Sciences Company
Las Vegas, Nevada
Contract No. 68-03-3249
Project Officers
L. J. Blume and D. T. Heggem
Exposure Assessment Research Division
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89193-3478
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89193-3478
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NOTICE
The information in this document has been funded wholly or in part by the United States
Environmental Protection Agency under cooperative agreement #CR814701-01 to the
Environmental Research Center, University of Nevada, Las Vegas and contract #68-03-3249 to
Lockheed Engineering and Sciences Company. It has been subjected to the Agency's peer and
administrative review, and it has been approved for publication as an EPA document. Mention of
trade names or commercial products does not constitute endorsement or recommendation for use.
11
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ABSTRACT
A large amount of soil characterization data has been collected as a component of the
Direct/Delayed Response Project (DDRP) in the acid rain Aquatic Effects Research Program. An
interlaboratory comparison study was undertaken to identify the comparability of this data to that
obtained from representative soil characterization laboratories. Participating laboratories were
selected at random from four regions of the U.S. and two regions of Canada. Two original DDRP
contract laboratories also participated. Duplicate samples of six soil audit materials and two liquid
soil extracts were sent to each of the laboratories in two separate batches. Laboratories used their
own protocols to perform the analyses requested except for the contract laboratories which followed
the DDRP protocol. Liquid audits were used in an effort to identify if interlaboratory differences
were due to extraction procedures or chemical measurements. A component of the variability in
the results was attributed to differences in the methods used such as soil/solution ratios, extractants
or extraction procedures. The largest number of different methods used was for the measurement
of cation exchange capacity. The results between the DDRP soil survey data and this study's results
were compared using Youden-pair plots. In addition, standard statistical tests were performed.
Overall, the DDRP data were comparable to the data from this study. However, out of the total
141 comparisons involving results from six or more laboratories, the results from the two contract
laboratories did not meet the comparison criteria in 19 cases. Since there was never a case in which
both contract laboratories failed, it would appear that the 19 cases which were not comparable were
due to random analytical errors, incorrectly reported results, or misapplication ofDDRP protocol
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CONTENTS
ABSTRACT iii
FIGURES vi
TABLES vi
ACKNOWLEDGEMENTS vii
1. INTRODUCTION 1
1.1 Background 1
1.2 Objective 2
2. PROCEDURE 3
2.1 Laboratory selection 3
2.2 Source of soil audit samples 5
2.3 Preparation of soil and aqueous audit samples 5
2.4 Distribution of audit samples 6
2.5 Laboratory protocols 6
2.6 Collection of data 8
2.7 Data verification 9
2.8 Workshop 9
2.9 Data analysis .10
2.91 Youden-pair plots 10
2.92 Box plots 11
2.93 Example of a Youden-pair plot 12
2.94 Supplemental statistical analyses 14
2.941 Time effect 14
2.942 Homogeneity of laboratory results 16
2.943 Pairwise comparisons 16
2.944 Group variability 17
2.945 Combined parameters 19
3. RESULTS 20
3.1 Natural and synthetic extracts 22
3.2 Supplemental statistical analyses 24
4. CONCLUSIONS 27
REFERENCES 28
APPENDDC A: Summary of NE and SBRP audit soil results A-l
APPENDIX B: Preparation of liquid audit samples B-l
APPENDDC C: Agenda for comparison workshop and list of workshop attendees .. C-l
APPENDDC D: Comparison study results D-l
Moisture (by wt %) D-3
Specific surface D-13
Total sand D-15
Very coarse sand D-23
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CONTENTS con't.
APPENDIX D: Comparison study results continued
Coarse sand D-31
Medium sand D-39
Fine sand D-47
Very fine sand D-55
Total silt D-63
Coarse silt D-71
Clay D-73
pH in deionized water D-81
pH in 0.002M CaCl2 D-91
pH in 0.01M CaCl2 D-101
Calcium exchangeable in 1M NH4C1 D-lll
Magnesium exchangeable in 1M NH4C1 . / D-121
Potassium exchangeable in 1M NH4C1 D-123
Sodium exchangeable in 1M NH4C1 D-133
Calcium exchangeable in 1M NH4OAc D-135
Magnesium exchangeable in 1M NH4OAc D-147
Potassium exchangeable in 1M NH4OAc D-159
Sodium exchangeable in 1M NH4OAc D-171
Cation exchange capacity 1M NH4C1 D-183
Cation exchange capacity 1M NH4OAc D-193
Exchangeable acidity in 1M KC1 D-203
Exchangeable acidity in BaQ2 triethanolamine D-205
Calcium extractable in 0.002M CaCl2 D-207
Magnesium extractable in 0.002M CaCl2 D-207
Potassium extractable in 0.002M CaCl2 D-209
Sodium extractable in 0.002M CaCl2 D-209
Iron extractable in 0.002M CaCl2 D-211
Aluminum extractable in 0.002M CaCl2 D-211
Aluminum extractable in 1M KCl D-213
Iron extractable in sodium pyrophosphate D-223
Aluminum extractable in sodium pyrophosphate D-233
Iron extractable in citrate-dithionite D-243
Aluminum extractable in citrate-dithionite D-253
Sulfate extractable in deionized water D-263
Nitrate extractable in deionized water D-273
Sulfate adsorption 6-point isotherm D-275
Total carbon D-279
Total nitrogen D-289
Total sulfur D-299
Inorganic carbon • D-309
APPENDIX E: Audit sample standard deviations used to establish
the Youden-pair plot precision windows E-l
VI
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FIGURES
Number
1 Youden-pair plot of calcium extracted by 1M NH4OAc for audit sample Bs 13
TABLES
1 List of parameters analyzed for the DDRP surveys ; 4
2 Laboratories selected to participate for each region 4
3 Measurements of calcium extracted by 1M NH4OAc for audit sample Bs 12
4a Summary statistics for time effect for calcium extracted by 1M NH4OAc 15
4b Analysis of variance for time effect for calcium extracted by 1M NH4OAc 15
5 Analysis of variance for homogeneity of laboratory results for
calcium extracted by NH4OAc 16
6 Pairwise comparison for significant difference between DDRP and
non-contract laboratories for calcium extracted by 1M NH4OAc 17
7a DDRP and non-contract laboratory summary statistics for
calcium extracted by NH4OAc 18
7b Within-group and between-group variabilities for DDRP and
non-contract laboratories by audit sample for calcium extracted by NH4OAc 18
8 Variability between DDRP and non-contract laboratory results for
Ca, Mg, K, and Na in 1M NH4OAc by parameter 18
9 Critical probability and t-values for between-group statistical
analysis for DDRP vs. NC laboratory results for calcium in 1M NH4OAc
by audit, parameter, and parameter-group comparisons 19
10 Number of laboratories that reported measurements for each
parameter by audit sample 20
11 Parameter and audit samples for which the DDRP was not comparable
to other soil characterization laboratories 23
12 Critical probability and t-values for between-group statistical
analysis for DDRP vs. NC laboratories by audit, parameter, and
parameter-group comparisons 25
vu
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ACKNOWLEDGMENTS
The cooperation and assistance of each laboratory that participated in this study is greatly
appreciated. The laboratories voluntarily analyzed the study samples within a limited time frame.
Laboratory representatives also participated in a workshop to discuss results of the study which
were critical to the interpretation of the results and the conclusions drawn from them. Special
gratitude is extended to Dr. Chao-Lung Chen, Environmental Research Center, for his assistance
with the statistical computer programming; Amy Smiecinski and Marie Schnell,. Environmental
Research Center, for their technical assistance throughout the project; John Teberg and Aileen
Tansy, Lockheed Engineering & Sciences Company (LESC), for developing and producing the
Youden-pair plots; and Rob Tidwell, LESC, for preparing and packaging the samples. The
assistance of the U.S. Environmental Protection Agency personnel at both Las Vegas, Nevada, and
Corvallis, Oregon, is appreciated. A final word of appreciation is extended to the external peer
reviewers, Dr. J. Benton Jones of Benton Laboratories, Athens, GA, and Dr. Chang Wang of the
Land Resource Research Center, Central Experiment Farm, Ottawa, Ontario, Canada.
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1. INTRODUCTION
1.1 BACKGROUND
This study was designed and implemented to answer questions regarding data comparability
and accuracy related to the Direct Delayed Response Project (DDRP) soil surveys.(U) The DDRP
is an integral part of the Aquatic Effects Research Program (AERP), a U.S. Environmental
Protection Agency (EPA) program. The AERP is a component of the federally mandated National
Acid Precipitation Assessment Program (NAPAP) which addresses the concern of potential
acidification of surface waters by atmospheric deposition. The purpose of the DDRP was to
characterize and predict the long-term response of watersheds and surface waters to acidic
deposition for several geographic regions of the United States. The projected responses of
watershed systems typical of the regional population can then be extrapolated to a larger regional
or national scale.
Specific goals of the DDRP are to: 1) define physical, chemical, and mineralogical
characteristics of the soils and define other watershed properties within the regions of interest; 2)
assess the variability of these characteristics; 3) determine which of these characteristics are most
strongly related to surface water chemistry; 4) estimate the relative importance of key watershed
processes in controlling surface water chemistry across regions of special interest; and 5) classify
the survey watersheds with regard to their response to sulfur deposition and extrapolate the results
from the survey watersheds to the regions of concern. A variety of data sources and methods of
analysis are being used to address these goals.
The DDRP surveys entailed the collection of soil samples from the Northeastern region, the
Southern Blue Ridge Province, and the Mid-Appalachian region, and characterization of these
samples for a number of soil chemical and physical properties. Four contract laboratories analyzed
these soil samples according to strict quality assurance and quality control guidelines that included
specific analytical protocols, laboratory training, audits, and data verification/3'4* Quality assurance
assessments were made using analytical results from blind and non-blind samples that were included
with the routine samples.
An important component of the quality assurance program within the DDRP is the
assessment of the data quality. One of the attributes of data quality is comparability.
Comparability is of particular importance for two reasons. First, it was recognized that it would be
necessary to develop a standardized analytical methods manual for the DDRP soil survey analyses.
Although many excellent methods manuals were available from soil characterization laboratories,
these manuals often differed in the choice of methods, in the details of procedures for any given
method, and in the nature of quality control procedures associated with these methods. Information
was compiled from many of these manuals in the development of the DDRP methods manual.
Although this manualw was subjected to extensive peer review, the question still remains as to the
comparability of data resulting from these methods to those obtained by the methods presently in
use by soil characterization laboratories in the U.S. and Canada. It is possible that the DDRP
protocols provide results that are not comparable to results from other protocols.
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Second, although the DDRP soil surveys do cover broad land areas of particular interest to
the issue of acid depositions effects, there are other regions in the U.S. and Canada of similar
importance. To make predictions for these regions, it would be necessary to rely on existing soil
characterization information. Are these data comparable to the DDRP data, or will there need to
be adjustments in the data or in the DDRP models to account for existing differences? If the data
from this study are comparable, then it is possible that the various soil characterization data bases
in existence elsewhere may be comparable to the DDRP data bases.
12 OBJECTIVE
The objective of this study was to investigate whether the analytical data obtained by
laboratories using DDRP soil analysis protocols are comparable to data for the same audit materials
analyzed by other soil characterization laboratories in Canada and the U.S. not using DDRP
protocols.
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2. PROCEDURE
2.1 LABORATORY SELECTION
The first step in the selection of laboratories for this study was which type of laboratory to
include. It was decided to limit participation to university laboratories since university laboratories
perform the bulk of the soil analyses for the U.S. Soil Conservation Service, and therefore, use of
these laboratories would provide a comparison between the DDRP data bases and the SCS data
bases for future potential modeling. Also university laboratories typically explore new
methodologies and improvements of old methods and would provide an assessment of current
methods for comparison with the DDRP methods. It was also decided to include laboratories from
Canada due to that nation's strong acid deposition assessment programs, and to assess the
comparability of U.S. and Canadian laboratory data. Comparable data will enable trend analyses
to be performed along the U.S./Canadian border.
A list of 50 U.S. university laboratories was obtained from the "Survey of State Soil Testing
Laboratories in the United States" prepared by the Soil Testing and Plant Analysis Committee -
S877 of the Soil Science Society of America.(S) A list of 29 Canadian laboratories was acquired from
the Canadian Forestry Service, the Land Resources Research Institute of Agriculture Canada, and
from a soil testing manual by McKeague.(6) The laboratories from both lists were grouped into six
regions, four for the U.S. and two for Canada. The separation into regions provided a mechanism
for examining variation between regions. Previous surveys have shown that soils vary from region
to region and that soil analytical methods vary according to the soil properties within a region.
Four regions defined by the Soil Science Society of America were used for the separation of
laboratories in the U.S. These regions were the North Central, Northeast, West, and South. The
Canadian laboratories were separated into Eastern and Western regions. Eleven to thkteen
laboratories were in each of four regions within the U.S. and the Western region in Canada. The
Eastern region of Canada had 18 laboratories.
The process used for laboratory selection was initiated by a pre-selection survey in which
laboratories within each region were randomly numbered. Those numbered 1 to 4 were mailed
letters explaining the objectives of the study, asking a series of questions to assist in final participant
selection, and containing a list of the analyses required by the DDRP survey (Table 1). These
laboratories were then contacted by telephone to ascertain the number of analyses they routinely
performed common to the DDRP survey analyses. If the laboratories performed at least 50 percent
of the analyses and agreed to participate in the study, they met the criteria for participant selection.
However, if fewer than two of the first four laboratories met the criterion, then the next two
sequentially numbered laboratories were contacted. Two U.S. regions, West and North Central,
required additional contact to identify laboratories for participation. The selection process resulted
in two laboratories randomly selected for participation in the study from each of the six regions.
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Table 1. List of Parameters Analyzed for the DDRP Surveys
Moisture (by wt%)
Specific surface
Total Sand (2.0-0.05)
Very Coarse Sand (2.0-1.0)
Coarse Sand (1.0-0.5)
Medium Sand (05-0.25)
Fine Sand (0.25-0.1)
Very Fine Sand (0.1-0.05)
Total Silt (0.05-0.002)
Coarse Silt (0.05-0.02)
Fine Silt (0.02-0.002)
Clay (<.002)
pH in deionized water
pH in 0.002 M CaClj pH in 0.01 M CaClj
Ca, Mg, K, Na Exchangeable in 1M NH4C1
Ca, Mg, K, Na Exchangeable in 1M NH4OAc
CECinlM1NH4Cl
CEC in 1M NH«OAc
Exchangeable acidity in 1M KC1
Exchangeable acidity in BaCl2 Triethanolamine
Al Extractable b 1 M KC1
Ca, Mg, K, Na Exchangeable in 0.002M CaCl2
Fe, Al Exchangeable in CaClj
Fe, Al Extractable in pyrophosphate
Fe, Al Extractable in acid oxalate
Fe, Al Extractable b dtrate-dithionite
Sulfate, Nitrate extractable b deionized H2O
Sulfate extractable b 0.016M sodium phosphate
Sulfate adsorption 6-pobt isotherm
Total Carbon
Total Nitrogen
Total Sulfur
Table 2. Laboratories Selected to Participate for Each Region.
U.S. Laboratories
Canadian Laboratories
North Central
Northeast
West
South
West
East
Iowa State University, IA
Purdue University, IN
Pennsylvania State University, PA
Rutgers State University, NJ
New Mexico State University, NM
Utah State University, UT
University of Florida, FL
Texas A&M University, TX
Northern Forestry Centre, AL
Alberta Environment, AL
Ontario Agricultural College, ON
Newfoundland Forestry Centre, NF
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Two DDRP contract laboratories were included in this study to address two issues related
to data comparability. The first issue addressed was the assessment of whether the DDRP audit
samples used in the study had changed over time. These audit samples had been used in 1985 and
1986 for the Northeastern and Southern Blue Ridge Province surveys, respectively. It is possible
that changes could have occurred in the samples due to soil degradation and contamination during
storage or transit. Also, analytical results may differ due to changes in the DDRP laboratory
operating procedures (i.e.^ instrumentation, personnel, reagents, etc.). The second issue concerned
the introduction of new audit materials (B and O soil horizons) for the final DDRP Mid-
Appalachian survey. By including the contract laboratories in the study, a basis for comparability
was established between the first two surveys and the final survey which used the new audit samples.
This study also provided an opportunity to build acceptability windows for the new audit materials.
Seven special interest laboratories were also invited to participate. These laboratories
included: the U.S. National Soil Survey Laboratory in Lincoln, Nebraska; the Canadian Land
Resources Research Institute in Ottawa, Ontario; the Alberta Research Council Laboratory in
Edmonton, Alberta; and four laboratories conducting specific soil analyses for the NAPAP
Watershed Manipulation Project.
22 SOURCE OF SOIL AUDIT SAMPLES
The six different soil audit samples used in the study were chosen from, bulk soil samples
which had been previously prepared for use in the Northeastern and Southern Blue Ridge Province
DDRP soil surveys (A, Bs, Bw, and C horizons), and the Mid-Appalachian DDRP soil survey (O,
A, Bw, and B). The bulk soil samples originated in the northeastern United States and represented
the major soils of the region. The audit samples included five mineral soils and one organic soil.
The analytical results from the Northeastern and Southern Blue Ridge Province surveys are
summarized in Appendix A.
2 J PREPARATION OF SOIL AND AQUEOUS AUDIT SAMPLES
The soil audit samples each consisted initially of approximately 500 kilograms of soil Each
bulk sample was air-dried, coned and quartered, tested for homogeneity, bottled into smaller sample
volumes of approximately one kilogram, and retained in cold storage at four degrees centigrade.
Subsamples of the audits were used as the six soils for this study. The selected 1 kg soil
samples were retrieved from cold storage, brought to room temperature, riffle-split into two 500 g
samples to conserve the number of audit samples, and placed in 500 mL amber plastic bottles for
shipment to the laboratories.
In addition to the soil audit samples, two aqueous audit samples were submitted in each of
the two batches to the laboratories. One of the aqueous samples was an extraction of the Bs audit
soil using 1M NtLpAc. An audit soil sample was used for extraction purposes to provide the
laboratories with an extract which contained elemental concentrations approximating one of the
audit samples. The other liquid extract was a synthetic sample of 1M NH4OAc. This sample
contained a predetermined concentration of Ca, Mg, K, and Na which approximated the mid-range
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concentration using the DDRP soil-to-solution ratio for an initial readout. See Appendix B. The
aqueous audit samples were included to distinguish between error due to soil extraction techniques
and instrumental analysis. For example, if the laboratory data agreed for the analyses of the
aqueous audit samples, then any differences in the laboratory data for the soil audit samples would
indicate a difference in extraction protocol or an extraction error. If the laboratory data on the
analyses of the aqueous audit samples did not agree, then differences in the data for the soil audit
samples would indicate both extraction and instrumental error. The synthetic sample was used to
provide a sample of known concentrations to assess accuracy and precision. The aqueous audit
samples were prepared in bulk and retained in cold storage at four degrees centigrade. Prior to
distribution, subsamples were placed in 125 mL amber bottles for inclusion with the soil samples
in the two batches which were shipped to the laboratories.
2.4 DISTRIBUTION OF AUDIT SAMPLES
Labels were affixed to the bottles containing the soil and aqueous samples to ensure that
the samples were properly identified yet remained blind to the analytical laboratories. Each
laboratory received six soil samples and two liquid samples per batch. Two batches of eight samples
were sent to each laboratory six weeks apart. Samples were shipped for next-day receipt by the
laboratories to minimize exposure to heat and other possible contamination in transit. The
laboratories were instructed to store the samples at four degrees centigrade immediately upon
receipt. Each participating laboratory analyzed the six soil samples for at least 26 parameters and
the two liquid extracts for four parameters. All noncontract laboratories were instructed to analyze
the samples according to methods currently in use in their laboratory for any given soil parameter.
A copy of the methods used by each noncontract laboratory was requested to assist in the
interpretation of analytical results.
2.5 LABORATORY PROTOCOLS
Throughout this report laboratories and data are grouped into three categories. The first
category is the audit data and laboratories from the Northeast and Southern Blue Ridge Province
DDRP soil surveys which are referred to as the DDRP data and DDRP laboratories. Second are
two laboratories which had been contracted for the DDRP soil surveys and also participated in this
study. These two laboratories are called the contract (C) laboratories or data in this report. The
third category, which consists of all other laboratories participating in this study, are referred to as
the noncontract (NC) laboratories or data.
Detailed procedures for the soil analytical protocols to be used by the NC laboratories were
not specified for this study. Only the general method was specified for each group of parameters,
e.g., calcium exchangeable in ammonium acetate. The purpose of this study was to compare the
analytical results from different laboratories, not to compare their protocols. Therefore, this section
does not discuss laboratory procedural differences in detail, but provides only general information
about protocols which may have led to different analytical results. The NC laboratories referenced
various publications as sources of their procedures for the specified parameters.(<>7A9) In addition,
many of the NC laboratories submitted protocols that were modifications of standard methods
tailored to accommodate their own specific laboratory facilities and equipment. However, most NC
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laboratories had protocols that did not deviate markedly from the relatively few universally accepted
protocols. None of the NC laboratories used the exact protocol specified in DDRP. The C
laboratories used the DDRP protocols as specified (4).
Of the 22 laboratories initially included in the study, 17 submitted data. Five of the original
laboratories had internal problems which caused incomplete and/or late data submissions. Included
in the final data set were the two C laboratories, 10 regional laboratories, three Water Manipulation
Project laboratories, one special interest laboratory, and one national laboratory (Canada). Of the
53 parameters analyzed, there were 30 parameters for which data from six or more laboratories
were reported. Only data from a minimum of six laboratories were chosen to be plotted and
discussed in this report. Two of the six laboratories are the G laboratories, leaving a minimum of
four NC laboratories for which there were data for comparison to the DDRP data.
The following paragraphs discuss some of the differences noted among laboratory protocols.
These are not detailed discussions, as it is not the purpose of this report to compare methodologies.
One interesting note is that one of the NC laboratories used calibrated scoops to measure aliquots
rather than gravimetric means.
MOISTURE Mineral soils were dried at 105° C and organic soils at 60° C by the DDRP and C
laboratories. The NC laboratories had varied drying temperatures, such as 60 to 70° C for organic
soils, and varied drying times.
PARTICLE SIZE (sand, silt, and clay) Various modifications of the pipet method were used by
the NC laboratories, e.g., some laboratories substituted the pipet/centrifuge washing system with
the pipet/filter candle system to reduce the various washing procedures required in the former
method. Both hydrogen peroxide and calcium hypochlorite were used for dissolution of organic
matter. One laboratory used the hydrometer method for the particle size determinations.
pH pH was determined in three different extracts by the DDRP and C laboratories: deionized
water, 0.002M CaCl2, and 0.01M CaCl2. Methods used by the C laboratories for water and 0.01M
CaClj used 1:1 mineral soil-to-solution ratio and 1:5 organic soil-to-solution ratio. The 0.002M
CaQ2 method used 1:1 mineral soil-to-solution ratio and 1:10 organic soil-to-solution ratio. The pH
was measured with a pH meter and combination electrode. The NC laboratories used various soil
to solution ratios including 1:1, 1:2, 1:5, and saturated paste, which generally gives pH of 0.2 units
below the 1:1 water extract pH. The NC laboratories also differed in stirring times and had
equilibration times ranging from 15 minutes to four hours.
EXCHANGEABLE CATIONS Exchangeable cations were determined with an unbuffered 1M
ammonium chloride solution and buffered 1M ammonium acetate at pH 7.0 by the DDRP and C
laboratories. A 1:26 mineral soil-to-solution ratio and 1:52 organic soil-to-solution ratio were used
for the DDRP methods, which also specified the use of a mechanical extractor for the exchange
reaction. The NC laboratories used various ratios, shaking times, and equipment. Atomic
absorption spectrometry or inductively coupled plasma-atomic emission spectrometry was specified
for measurement readings by all laboratories.
CATION EXCHANGE CAPACITY Cation exchange capacity (CEC) was determined using two
methods by the DDRP and C laboratories. CEC determined in an unbuffered 1M ammonium
chloride solution is the effective CEC which occurs at approximately the field pH when combined
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with the total acidity component. CEC determined with 1M ammonium acetate solution buffered
at pH 7.0 is the theoretical estimate of the maximum potential CEC for a specific soil when
combined with the acidity component. A 1:26 mineral soil-to-solution ratio and 1:52 organic soil
to solution ratio were used with a soil weight of 2.5 grams. Samples were analyzed for ammonium
content by one of three methods: automated distillation/titration; manual distillation/automated
titration; or ammonium displacement/flow injection analysis. The CEC methods used by the NC
laboratories varied widely, including summation of cations plus acidity. Various extracting solutions
were used, for example, the standard barium chloride to strontium chloride, sodium acetate, and
ammonium acetate. The weight of soil used ranged from 2.5 to 10 g, with the extract volume
ranging from 25 to 400 mL. Both ethanol and propanol were used as wash solutions. Extractors
and oscillating equipment were used for agitation. Several different replacement solutions were
used, and some were reversed, e.g., ammonium acetate was used as the saturating ion replaced by
sodium by most of the laboratories, and sodium was used as the saturating ion replaced by
ammonium by one of the NC laboratories. Some laboratories used Buchner funnels and vacuum
for extraction. Equilibrium times varied from several hours to overnight. Various measurement
equipment was also used, e.g., distillation, flame photometry.
TOTAL CARBON Total carbon was determined by the DDRP and C laboratories using rapid
oxidation followed by thermal conductivity detection with an automated C, H, N- analyzer. The NC
laboratories used a Leco-600 furnace, Walkley-Black wet combustion method, and one lab used a
Carlo Erba auto-analyzer. Some laboratories ground the dry samples to 60 mesh and dried the
samples at 60° C.
TOTAL NITROGEN Total nitrogen was determined by the DDRP and C laboratories using
rapid oxidation followed by thermal conductivity detection using an automated C, H, N- analyzer.
Half of the NC laboratories used the Kjeldahl method, some laboratories used a Leco-600 furnace,
and one used a Carlo Erba auto-analyzer. Differences were also noted in digestion times which
ranged from one hour to three hours.
TOTAL SULFUR The DDRP and C laboratories performed a total sulfur determination by
automated sample combustion followed by infrared detection or titration of evolved sulfur dioxide.
The NC laboratories used Leco furnaces, Fisher sulfur analyzers, and wet digestion.
2.6 COLLECTION OF DATA
This study required the management, manipulation, and assessment of data from 21
laboratories. To ease the task of managing these data, a DBASEHI program was designed and
developed to allow each laboratory to enter its final data using formatted input screens. Each entry
screen contained records with fixed decimal point lengths and reporting units for each parameter
analyzed. Upon completion of the analyses for the two batches of samples, each laboratory
submitted a floppy diskette containing its results. The data received from each laboratory were
identified by a laboratory code and compiled into one database by parameter. Statistical analyses
were performed with the use of SAS PC* and mainframe software.
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2.7 DATA VERIFICATION
The results generated by the laboratories were thoroughly reviewed for transcription and
data entry errors, as well as correct units. Each laboratory was given the opportunity to review its
own data on hardcopy and return the corrected data points for entry into the compiled database.
The corrected data were further verified by review of all data points, statistical manipulations, and
graphical displays for the results of each parameter generated for this report.
2.8 WORKSHOP
A workshop was held on April 19,1988, in Las Vegas, Nevada, to discuss the preliminary
results from this study. The agenda for the workshop is in Appendix C. Representatives from
twelve of the laboratories attended, as well as EPA representatives and contractors from Las Vegas,
NV, and Corvallis, OR. (See Appendix C.) The purpose of the workshop was to provide a forum
for the discussion and verification of results and differences in methods. Each participant was
provided with a summary of the data prior to the workshop to allow them to compare their results
with those from all other laboratories in advance.
Several errors in the original data set were identified at the workshop. A common error was
that of reporting units. Although the reporting units had been included on the data entry screens,
the results were often given in the units customarily reported by the laboratory. An adjustment for
this factor greatly reduced many of the initial differences identified among the laboratories. Other
errors included incorrect decimal places and transposed numbers.
The results were discussed on a parameter-by-parameter basis. As the results were
presented, each laboratory was given an opportunity to discuss the methods which it used. It was
recognized that the differences in results could be due to differences in methods and procedures,
laboratory performance of any given method, and/or variability in the audit material. Due to
concerns regarding the possibility of error resulting from laboratory performance in addition to
methodology, no attempt was made to compare analytical results according to each laboratory's
methods. A general conclusion of the group, however, was that the range in results was very narrow
considering the wide variety of methods used and the number of participating laboratories. Some
attendees expressed the opinion that the data quality objectives (DQOs) required for the DDRP
soil survey were too stringent, especially when compared to the relative lack of homogeneity found
in soil samples and the natural variability of soil units in the field. It was explained to the group
that the DQOs were set for the surveys so that measurement error would be small relative to
natural variability. During the course of the workshop, the participants expressed their opinions
of the study. Almost all the participants stated that this study and comparability studies in general
provide valuable information for their laboratories. It gives them an opportunity to assess how their
laboratory compares with other laboratories across the country, and to discuss new methods,
equipment, and related issues. All the laboratories expressed an interest in the continuation of
nationwide comparison studies.
-------
2.9 DATA ANALYSIS
The purpose of this study was to determine whether data obtained by using the DDRP
protocol to measure soil parameters are comparable with data obtained from other soil
characterization laboratories that use their own individual protocols. It was anticipated that, for any
particular soil audit material, the expected measurements of a soil parameter obtained from
laboratories outside the DDRP program would differ from one another and from those of the
DDRP laboratories owing to differences in methodology, equipment, and personnel. It was decided
that the principal interest of this comparability study was whether the expected measurements
obtained by use of the DDRP protocol would lie near the center of the distribution of expected
measurements from soil laboratories outside DDRP, or whether the DDRP protocol produced
expected results considerably larger or considerably smaller than the expected results obtained from
most soil characterization laboratories outside DDRP. Therefore, in this study, if the results from
the C laboratories that used the DDRP protocol are near the center of the distribution of the
results from the NC laboratories, then the DDRP protocol are considered to produce results that
are "comparable" to results being obtained by soil laboratories outside the DDRP program. The
quantification of what is meant by "near the center of the distribution" will be explained in terms
of Youden-pair plots(10) and box plots.(ai2)
2.91 Youden-pair Plots
In a Youden-pair plot a point (xlt x2) is plotted on a graph where Xi and x2 represent batch
1 and batch 2 measurements of a soil parameter. A Youden-pair plot will contain such points for
all the laboratories participating in the comparison study. The perpendicular distance of a point
from the diagonal line, Xt = Xv is the usual sample standard deviation (s) of the two measurements
xt and x2. The perpendicular projection of the point (xt, x2) onto the diagonal line is the point (x~,
x), where x" is the sample mean of the two measurements. A Youden-pair plot was prepared for
each combination of measured soil parameter and type of soil audit material if six or more
laboratories reported these measurements.
Four DDRP laboratories analyzed some of the soil audit materials used in this comparability
study during the DDRP Northeastern and Southern Blue Ridge Province soil surveys. From these
analyses, an estimate s_ of the standard deviation of the analytical error was obtained for each
combination of soil audit material and soil parameter measured. In each case, this estimate, sp, was
calculated by taking the square root of the pooled (over the four laboratories) estimate of the
analytical error variance. A point representing the results for each of the four laboratories was
plotted on the Youden-pair plot by starting at the mean point (x, 7) for each laboratory on the
diagonal line and moving perpendicular to the line a distance sp. Since these points must be placed
above or below the diagonal line, an arbitrary decision was made to place them all above the line.
These points representing the earlier results of the four DDRP laboratories are labeled 1,2,3, and
4 on the Youden-pair plots.
The points labeled a and b on the Youden-pair plots correspond to results obtained in this
study by the two C laboratories. (In printing the Youden-pair plots in Appendix D, it was found
that the a and b designations of the results from two laboratories were often hard to find on the
plots because of overstrikes of labels for other laboratories that had similar results. For this reason,
a decision was made to replace the symbols a and b with a triangle (A) and a square (D),
10
-------
respectively, which are more easily distinguished from the letter designations of the other
laboratories. Nevertheless, in the text, these two laboratories will continue to be designated by a
and 6.) If no changes in the soil audit materials or in the interpretation of the DDRP protocol has
occurred between the DDRP surveys and this study, one would expect the perpendicular projections
of the points a and b to lie near those of points 1, 2, 3, and 4.
As a visual means for comparing the precision of the laboratories in the study and of the
DDRP laboratories in the previous soil surveys, lines are drawn parallel to and at a distance of 2s
(in a perpendicular direction) on either side of the diagonal line. The area between these two outer
lines will be referred to as the "precision window." If the analytical error in the measurement of
a soil parameter were normally distributed with mean 0 and standard deviation sp, then the
probability that a point representing two repeat measurements (xlf x2) will fall between these two
outer lines is approximately 95 percent. Note that the points 1, 2, 3, and 4, representing the results
from the DDRP soil survey, will always k'e half way between the diagonal line and the upper
precision window boundary.
2.92 Box Plots
The box plot is a widely used procedure for looking at the distribution of data and
identifying extreme (outlying) observations. This procedure identifies observations that lie more
than 1.5 interquartile ranges from the median of the data as extreme or outlying observations. (To
define the median and quartiles, the default definition for the pth percentile given in the PC SAS
computer software package program PROC UNIVARIATE is employed. The first quartile
corresponds to a p = 25, the median to p = 50, and the third quartile to p = 75. If the n
observations are ordered from smallest to largest, then for
np/lOQ *j + g
where/ is the greatest integer less than or equal np/100 andg is a nonnegative number less than
one, then the pth percentile of the data set is defined to be the value in position (/ + 1) if g > 0;
while, if g - 0, the pth percentile is defined to be the arithmetic average of the values in positions
; and (/+ !)• An interquartile range is the difference between the third and first quartiles.)
For this study, the quantitative criterion used to determine -whether the DDRP protocol gives
results comparable to those obtained by other soil characterization laboratories is that if the sample
means from the C laboratories are not extremes in a box plot of the sample means of att participating
laboratories mat measured a parameter of 'a soB audit material, then the results an comparable for that
parameter and soil audit material combination. The actual box plots are not presented in this report.
Instead, the comparability or lack of comparability of the DDRP protocol results according to the
box-plot criterion are illustrated in the Youden-pair plots. The median M and the interquartile
range R of the sample means of the C and NC laboratory results for each soil parameter in each
soil audit material were calculated. In the Youden-pair plot, the diagonal line is only shown over
the segment between the points (M - U/?, M • 1.5R) and (M + 15R, M + 15K). Hence, if the
perpendicular projections of points a and b fall on the visible portion of the diagonal line, the
DDRP protocol results are considered to be comparable with those of outside soil laboratories.
11
-------
2.93 Example of a Youden-pair Plot
The data collected in this study for calcium (Ca) extracted by 1M NH4OAc from Bs audit
material are employed in this illustration of Youden-pair plots. Paired results obtained from 14
laboratories are presented in Table 3. The data in this table are ordered by increasing sample
means. In addition, the sample means from the earlier DDRP soil surveys are given along with the
value of 2sp. For this soil parameter and audit material, n = 14 laboratories, the interquartile range
is 0.070 (= 0.225 - 0.155), the median is 0.1925 (=[0.0190 + 0.0195]/2) and the interval defined by
the median plus or minus 1.5 interquartile ranges is 0.0875, 0.2975).
Table 3. Measurements of Calcium Extracted by 1M NI^OAc for Audit Sample Bs
Order No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
DDRP Survey
Data
Laboratory
r
e
k
g
P
d
m
j
1
h
b
a
o
c
1
2
3
4
Precision window, 2sd, = 0.064
*1
0.120
0.140
0.140
0.130
0.160
0.170
0.180
0.18
0.200
0.200
0.180
0.230
0.250
0.470
*2
0.120
0.120
0.140
0.180
0.160
0.160
0.200
0210
0.200
0.220
0270
0260
0250
0.480
X
0.120
0,130
0.140
0.155
0.160
0.165
0.190
0.195
0.200
0.210
0.225
0.245
0.250
0.475
0.203
0.185
0231
0.212
12
-------
It should be noted that the sample means for laboratories a and b, the laboratories that use
the DDRP protocol, are within the interval and therefore the protocol is judged to be comparable
in this instance. The Youden-pair plot for this set of data is shown in Figure 1. In Figure 1, it is
evident that the perpendicular projections of points a and b fall on the diagonal line segment. It
should also be noted that all points fall within the precision window, which would indicate that all
laboratories are using methods of approximately the same, or better, precision as the method
described in the DDRP protocol. It is also noted that the projections of points 1, 2, 3, 4, and of
points a and b, on the diagonal line are near one another and so do not indicate any major change
of calcium in the soil audit material or in the interpretation of the protocol between times of the
soil surveys and of this study.
0.40
0.30-
O
O
0.20]
cr
-------
2.94 Supplemental Statistical Analyses
After reviewing the data from this study it was decided that certain standard tests of equality
of means and variances should be run to further describe the data. Of course, it was assumed at
the beginning of the study that means and variances would be different for different laboratories
that are using different protocols, different procedures, and different personnel; so these tests have
no bearing on the comparability objective of this study. On the basis of the timing of the decision
to make the tests, the differences in the assumptions underlying the tests and underlying the study,
and power considerations, all results should be viewed as descriptive or anecdotal rather than
inferential In particular, any interpretation of stated P-values (e.g., Pr > F) should take these
comments into account. Statistical tests were performed only on results from soil audit materials
A, Bw, Bs, and C, because these were the only audits for which DDRP soil survey data were
available. Except for the "time effect" test, these tests are primarily descriptive comparisons of
earlier results from DDRP laboratories with those from NC laboratories in this study.
2.941 Time Effect
There is an initial question as to whether the composition of the soil audit materials A, Bw,
Bs, and C might have changed in the time between the DDRP soil surveys and this study. The two
DDRP soil surveys were conducted in 1985 and 1986 approximately two years prior to this
comparison study. Two of the four DDRP laboratories, the two C laboratories, were included in
this study as a link over time. Analysis of variance F-tests were performed to determine whether
there were any significant differences in the analytical results over time when comparing the past
and current results of the two C laboratories. Any real differences would be caused by either a
compositional change in the chemical and physical characterization of the soil samples, or a change
in the analysis per se. The former could be the result of drying, microbial action, or contamination
during handling. The latter could be owing to changes in laboratory interpretation of the protocol.
As an example of this test, the information and test results for Ca in 1M NH4OAc are given
in Tables 4a and 4b for all four audit materials for which DDRP data are available. (Tables la and
Ib in Appendix D list the results for all other parameters.) In this case, there are no significant
differences which indicates that it is highly unlikely that there have been any changes over time.
14
-------
Table 4a. Summary Statistics for Time Effect for Calcium Extracted by 1M NH4OAc.
Audit Samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number of Labs
26
28
2
2
14
22
2
2
16
12
2
2 '
14
10
2
2
Mean
0.2689
0.2394
0.2750
0.2900
0.2029
0.1848
0.2450
0.2250
0.2723
0.2089
0.2800
0.2500
0.0830
0.0514
0.0700
0.0350
Standard Deviation
0.0307
0.0457
0.0071
0.0424
0.0427
0.0362
0.0212
0.0636
0.0662
0.0360
0.0000
0.0141
0.0318
0.0243
0.0283
0.0071
Table 4b. Time Effect Analysis of Variance for Calcium Extracted by 1M NH4OAc.
Audit Samples
A
Bs
Bw
C
Source
Lab
Time
Lab* time
Error
Lab
Time
Lab'time
Error
Lab
Time
Lab'time
Error
Lab
Time
Lab*time
Error
df
1
1
1
54
1
1
1
36
1
1
1
28
1
1
1
24
Sum of
Squares
0.0002
0.0030
0.0018
0.0817
0.0013
0.0061
0.0000
0.0558
0.0076
0.0021
0.0010
0.0801
0.0038
0.0007
0.0000
0.0193
Mean
Square
0.0002
0.0030
0.0018
0.0015
0.0013
0.0061
0.0000
0.0015
0.0076
0.0021
0.0010
0.0029
0.0038
0.0007
0.0000
0.0008
F
0.13
1.98
1.22
0.84
3.91
0.00
2.66
0.73
0.34
4.71
0.92
0.01
Pr > F
a - .05*
0.7200
0.1655
0.2743
0.3651
0.0556
0.9649
0.1140
0.4014
0.5643
0.0401
03476
0.9127
* significant difference (Le., there is a time effect) if Pr > F is less than .05
15
-------
2.942 Homogeneity of Laboratory Results
An F-test for laboratory results homogeneity (i.e., equal expected values of parameter
measurements) for all laboratories was performed in a one-way analysis of variance. This test
determines whether any contrast in the sample means is significantly different from zero. Of
particular interest is whether there is a difference between the sample mean of a DDRP laboratory
and an NC laboratory that is significantly different from zero. If the F-test indicates that the results
are significantly different from zero, then there is reason to look for pairs of laboratories that may
have significantly different means.
The results of this homogeneity test for Ca in 1M NH4OAc are given in Table 5 (Table 2a
in Appendix D) and show apparent significant differences among laboratories for all four DDRP
audit materials.
Table 5. Analysis of Variance for Laboratory Result Homogeneity; Calcium Extracted by NH4OAc.
Audit Samples
A
Bs
Bw
C
Source
Lab
Error
Lab
Error
Lab
Error
Lab
Error
df
14
77
15
60
15
48
15
48
Sum of
Squares
0.3156
0.1696
0.2085
0.0714
0.1397
0.1161
0.2769
0.1153
Mean
Square
0.0225
0.0022
0.0139
0.0012
0.0093
0.0024
0.0185
0.0024
F
10.23
11.68
3.85
7.69
Pr > F
a = .05*
0.0001*
0.0001*
0.0002*
0.0001*
' Results are significantly different if less than .05
2.943 Pairwise Comparisons
For cases with a significant F-ratio (a = 0.05) in the above homogeneity tests, the pairwise
differences of all laboratories were examined by using Scheffe's method of contrasts employing a
simultaneous significance level of 0.05. All significant differences between DDRP laboratories and
NC laboratories were identified, and the significant differences and corresponding simultaneous 95
percent confidence intervals are listed. The results for the significant differences of Ca in 1M
NH4OAc are shown in Table 6 (Table 2b in Appendix D). The data suggest that the main
component of the pairwise differences were due to Laboratory c in most cases for this parameter.
16
-------
Table 6. Pairwise Comparison for Significant Difference between DDRP and Non-Contract
Laboratories for Calcium Extracted by 1M NH4OAc.*
Audit Samples
A
Bs
Bw
C
Labs
3 andc
1 andc
1 and j
2 andc
2 and j
3 andc
4 and c
1 and c
2 and c
2 andc
3 and c
1 and c
4 and c
2 andc
Upper Limit
-0.0048
-0.0721
-0.0521
-0.1021
-0.0821
-0.0962
-0.1231
-0.1352
-0.1565
-0,0116
-0.0160
-0.0803
-0.0826
-0.1070
Difference
-0.1840
-02461
-02261
-02756
-02556
-02440
-02634
-02721
-02902
-0.0116
-02285
-02770
-02842
-03086
Lower Limit
-0.3632
-0.4200
-0.4000
-0.4491
-0.4291
-0.3918
-0.4037
-0.4090
-0.4240
-0.4105
-0.4410
-0.4737
-0.4858
-0.5102
• .05 level of significance; Tukey's Studentized Range Test; DDRP labs = 1 - 4; NC labs = c - r
2.944 Group Variability
An analysis of between-group variability compared the sample mean of the DDRP data with
that of the NC laboratory data, whereas the test for sameness of laboratories and pairwise
comparisons compared the difference between the DDRP and NC laboratories on a one-to-one
basis. Two procedures were used to investigate between-group variability. The first test procedure
employed an F-test (a - 0.05) to determine whether the within-group variability is different for the
two groups, and then a t-test (« » 0.05) to determine if the group means are different. The t-test
takes into account whether the within-group variances are equal or unequal as determined by the
F-test. The summary statistics and test results for measurements of Ca in 1M NH4OAc are shown
in Tables 7a and 7b. Results for all other parameters are located in Tables 3a and 3b of Appendix
D. All within-group and between-group comparisons are not significant except for the Bs audit
sample within-group variability. The second comparison of the data from the two sets of
laboratories was performed by using a regression analysis to eliminate the effects of audit materials
and then applying a t-test of the laboratory-effect regression coefficient. These results are given in
Table 8.
17
-------
Table 7a. DDRP and Non-Contract Laboratory Summary Statistics for Ca Extracted by NH4OAc.
Audit
Samples
A
Bs
Bw
C
Group
NC
DDRP
NC
DDRP
NC
DDRP
NC
DDRP
Number
of Labs
12
3
12
4
12
4
12
4
Mean
0.3100
0.2798
0.1992
0.2076
0.2629
0.2496
0.1333
0.0854
Sd
0.0973
0.0468
0.0944
0.0192
0.0675
0.0347
0.0979
0.0336
SE
0.0281
0.0270
0.0273
0.0096
0.0195
0.0173
0.0283
0.0168
Min
0.2050
0.2394
0.1200
0.1848
0.1750
0.2089
0.0400
0.0514
Max
0.5150
0.3310
0.4750
0.2310
0.4200
0.2838
0.3600
0.1315
Table 7b. Within-group and Between-Group Variabilities for DDRP and Non-Contract
Laboratories by Audit Sample for Calcium Extracted by NH4OAc.
Audit
Samples
A
Bs
Bw
C
F
4.33
24.18
3.79
8.51
df
(11,2)
(11,3)
(11,3)
(11,3)
Pr > F
a. » .05
0.4050
0.0237*
03000
0.1042
Variances
Equal
Unequal
Equal
Equal
|T|
0.5127
-0.2909
0.3717
0.9414
df
13.0
13.2
14.0
14.0
Pr > |T|*
a - .05
0.6168
0.7756
0.7157
03624
* Results are significantly different if less than .05
Table 8. Variabilities for DDRP and Non-contract Laboratories for Ca, Mg, K, and Na in
1M NILpAc by Parameter.
Parameter
Ca
Mg
K
Na
Mean
NC
2263
.0963
.1026
.0566
DDRP
.2056
.0965
.0923
.0232
Variance
NC
.00445
.00659
.00894
.00021
DDRP
.00547
.00844
.00900
.00014
t-value
0.415
0.002
0.153
3.562*
critical
t-value *
1.68
* Values greater than 1.68 indicate significant difference
18
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2.945 Combined Parameters
Multivariate analysis of variance (MANOVA) was employed to examine the overall
differences between NC and DDRP results for each parameter group. A multivariate general linear
model regression approach was used to perform the MANOVA because of the inequality in the
number of observations across the different parameters. An F-test was performed on the Hotelling-
Lawley trace statistic. The critical probability (P-value) of the F-test for the parameter group Ca,
Mg, K, and Na in ammonium acetate is given in Table 9, along with the critical probabilities for the
t-tests discussed in the previous paragraph.
Table 9. Critical Probability and t-values for Between-Group Statistical Analysis; DDRP vs.
NC Laboratories for Ca in NH4OAc by Audit, Parameter, and Parameter-Group.
Parameter
Ca, 1M NH4OAc
Mg, 1M NH4OAc
K, 1M NH4OAc
Na, 1M NH4OAc
Audits
Pr>F*
A
.6168
.8921
.6371
.0906
Bs
.7756
.7511
.1127
.0903
Bw
.7157
.6174
.7310
.1461
C
.3624
.2671
.0649
.0667
Parameter
t-value*
0.415
0.002
0.153
3.562*
Parameter
Group
Pr>F*
0.144
* Significantly different if Pr>F is less than .05
* Significantly different if t-value is greater than the critical value
19
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3. RESULTS
The objective of this study was to determine whether the DDRP contract laboratories
provide measurements on soil parameters that are comparable to data that would be obtained by
other soil laboratories in the United States and Canada. To accomplish this objective, data from
the analyses of six soil audit materials by two contract (C) laboratories that used DDRP protocol
were compared with data obtained from the analysis of the same audit materials by other United
States and Canadian (NC) soil laboratories that used their own individual protocols. The
quantitative criterion employed was that if the sample means obtained by the C laboratories for the
measurements of a parameter on a particular audit material were within 1.5 interquartile ranges
of the median of the sample means obtained by both the C and NC laboratories, the DDRP
protocol would be considered to provide comparable results. This criterion was employed for all
parameters and audit materials in which at least six laboratories (C and NC) reported
measurements. A list of the number of laboratories reporting on each parameter for each audit
material is given in Table 10. The results based on the protocol for the C laboratories were found
to be comparable to results from NC laboratories in 122 out of 141 combinations of parameters and
audit materials. A list of the 19 parameters and audit materials where comparable results were not
obtained is given in Table 11. The Youden-pair plots which illustrate the comparability or lack of
comparability are given in Appendix D along with data and the results of the supplementary
statistical tests.
Table 10. Number of Laboratories That Reported Measurements for Each Parameter by Audit
Sample
PARAMETERS
Moisture
Spec Surface
Total Sand
Coarse Sand
Medium Sand
Fine Sand
Very Fine Sand
Total Sflt
Coarse Silt
Clay
pH in DI H2O
pH in 0.01M CaClj
pH in 0.002M CaCl,
A
11
2
10
10
10
10
10
10
4
10
14
14
4
Bs
11
2
10
10
10
10
10
10
4
10
15
15
4
Bw
11
2
10
10
10
10
10
10
4
10
15
15
4
C
9
2
10
10
10
10
10
10
4
6
15
15
4
B
11
2
10
10
10
10
10
10
4
10
15
15
5
O
11
0
3
3
3
3
3
3
1
10
15
15
5
NAT1
S^N
20
-------
Table 10. Continued
PARAMETERS
Ca Exchg in 1M NH4C1
K Exchg in 1M NH4C1
Mg Exchg in 1M NH4C1
Na Exchg in 1M NH4C1
Ca Exchg in 1M NH4OAc
K Exchg in 1M NH4OAc
Mg Exchg in 1M NH4OAc
Na Exchg in 1M NH4OAc
CEC 1M NH4C1
CEC 1M NH4OAc
Exchg Acidity KCL
Exchg Acidity BaQ2
Al Ext. in 1M KCL
Ca Ext. in 0.002 CaClj
Mg Ext. in 0.002M CaClj
K Ext. in 0.002M CaCl,
Na Ext. in 0.002M CaClj
Fe Ext. 0.002M CaClj
Al Ext. 0.002M CaCl2
Fe Ext. in Na PYRO-PO4
Al Ext in Na PYRO-PO4
Fe Ext in Dithionite
Al Ext in Dithionite
SO4 Ext in OI H,O
NO4 Ext in DI H,O
SO4 Adsoip -0 pt
SO4 Adsorp -2 pt
SO4 Adsorp -4 pt
SO4 Adsorp -16 pt
A
6
6
5
5
14
14
14
12
5
11
3
4
6
3
4
4
4
3
4
7
7
6
5
6
4
4
4
4
4
Bs
6
6
5
5
14
14
14
12
5
11
3
4
6
3
4
4
4
4
4
7
7
6
5
6
4
4
4
4
4
Bw
6
6
5
5
14
14
14
12
5
11
3
4
6
3
4
4
4
1
1
7
7
6
5
5
4
4
4
4
4
C
6
6
5
3
14
14
14
.8
5
11
3
4
5
3
4
4
4
1
1
7
7
6
5
5
4
4
4
4
4
B
6
6
5
5
14
14
14
12
5
11
3
6
6
3
4
4
4
1
3
7
7
6
5
5
4
4
4
4
4
O
6
6
5
S
14
14
14
12
S
11
3
6
6
3
4
4
4
3
4
7
7
6
5
6
4
4
4
4
4
NAT1
12
11
12
9
SYN
12
11
12
8
21
-------
Table 10. Continued
PARAMETERS
SO4 Adsorp -32 pt
Total Carbon
Total Nitrogen
Total Sulfur
Inorganic Carbon
A
4
11
10
7
1
Bs
4
11
10
7
1
Bw
4
11
10
7
1
C
4
11
9
2
1
B
4
11
13
7
1
O
4
11
13
7
1
NAT1
SYN
1 A liquid audit sample obtained by extracting a natural soil sample
2 A liquid audit sample obtained by adding pre-determined amounts of Ca, Na, K and Na to a liquid standard
In all 19 failures to meet the comparability criterion, only one, but not always the same one,
of the two contract laboratories had measurements outside the prescribed range. By itself, not too
much should be made of this since the number of laboratories, n, reporting results is less than 8,
and it is impossible for the criterion to indicate that both C laboratories are too large or both too
small. However, a check found only one of the 19 cases where if one C laboratory mean is too
large the other C laboratory had the next smaller mean value, or where one C laboratory mean was
too small the other C laboratory had the next larger mean. That case is "Ai ext. in pyro-PO/ in Bs.
Thus, these 19 cases provide little evidence that the DDRP protocol is causing extreme
measurements. In 9 of these 19 cases, the failure was caused by only one of the two measurements
by the offending C laboratory being outside the prescribed range. The only place where there
seems to be something approaching a consistent pattern of such failures was in the measurement
of sand content. Six of the 19 failures reported in Table 11 are related to the measurement of sand
content, where the failing measurements were all too large.
3.1 Natural and Synthetic Extracts
The purpose of submitting liquid extracts to the analytical laboratories was to differentiate
betweeen instrument and extraction error. If the analytical results for the liquid extracts for the
laboratories are within acceptable limits, then any differences in analytical results among the
laboratories for the audit soil samples could be attributed to differences in soil extraction.
Although liquid extracts could have been submitted for all parameters undergoing extraction
for available nutrients, only cations in ammonium acetate (Ca, Mg, K, and Na) were used to assess
instrument comparability among laboratories. As stated previously, one, liquid audit sample was
extracted from a natural soil sample. The second liquid was a standard solution containing known
amounts of four cations (Ca, Mg, K, and Na) which had been prepared to prescribed naturally-
ocurring soil concentrations. The liquid audits were subjected to replicate analysis by a referee
laboratory to establish a mean and standard deviation for the four cations.
22
-------
Table 11. Parameter, Audit Combinations for which the DDRP Protocol Was Found to Be
Not Comparable
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
Parameter
Moisture
Moisture
Total Sand
Fine Sand
Very fine sand
Very fine sand
Very fine sand
Very fine sand
Total silt
K exchg. NH4C1
K exchg. NH4C1
Ca exchg. NH4OAc
K exchg. NH4OAc
Mg exchg. NH4OAc
Al in pyro-PO4
Fe in dithionite
Total carbon
Total nitrogen
Total nitrogen
Audit
Bs
C
A
Bs
A
Bs
B
C
A
Bs
C
B
Bs
Bs
A
Bs
0
A
Bs
n
11
9
10
10
10
10
10
10
10
6
6
14
14
14
7
6
11
10
10
Cause for Failure to Meet Criterion
Lab b, one measurement too large
Lab a, both measurements too small
Lab b, both measurements too large
Lab b, both measurements too large
Lab b, both measurements too large
Lab b, both measurements too large
Lab b, one measurement too large
Lab a, both measurements too large
Lab b, both measurements too small
Lab b, second measurement too large
Lab b, both measurements too small
Lab a, first measurement too large
Lab b, second measurement too large
Lab b, second measurement too large
Lab a, both measurements too large
Lab a, both measurements too small
Lab b, one measurement too high
Lab a, first measurement too large
Lab a, first measurement too large
Page
No.*
D-5
D-7
D-16
D-49
D-56
D-57
D-60
D-59
D-64
D-125
D-127
D-141
D-162
D-150
D-234
D-245
D-285
D-290
D-291
*Page number of Youden-pair plot for listed parameter and soil audit material
The extract results from this study are given in the tables and figures in the Appendix D.
The figures show several main scenarios: (1) the agreement of all (C and NC) laboratories
compared to the interquartile range, Le. identifying outlier laboratories, (2) a comparison of the C
laboratories with the NC laboratories, and (3) a direct comparison between the two contract
laboratories. The C laboratories are represented in these figures by a triangle (for Lab a) and a
square (for Lab b) and by letters for the NC laboratories.
23
-------
For the natural and synthetic extracts, both C laboratories and most of the NC laboratories
are within the interquartile ranges for all four cations. The NC laboratories that exceeded the range
for the natural extract were c, r, p, j, and h with g being borderline due to low precision. Those that
exceeded the range for the synthetic extract were r, p, and j, with c and h being borderline due to
low precision. These were, generally, the laboratories which also exceeded the interquartile ranges
for the analyses of the audit soil samples. These laboratories were also confirmed in the
supplemental statistical analyses as being significantly different from the DDRP laboratories (Labs/
1, 2, 3, and 4). The C laboratories were generally at the center of the interquartile range and
therefore in the midst of the NC laboratories and also compared very closely with each other. In
fact, in the majority of the cases, the data for the two C laboratories were superimposed. This
indicates identical analytical results and very good precision. However, this would be expected since
the two C laboratories used the same DDRP method for these cations and both laboratories were
experienced with the method.
Overall, the results show that most of the laboratories provided very similar analytical results
for the liquid extracts. This indicates that they were operating under similar calibration procedures,
identical standards, and optimal instrument conditions. Therefore, for these laboratories, any
dissimilarities in analytical results of soil samples could be attributed to differences in laboratory
soil analytical procedures or possibly other idiosyncracies specific to that laboratory. For those NC
laboratories which had results outside the liquid extract interquartile ranges, their soil analytical
results were confounded with instrumentation errors. This makes an assessment of comparability
of C versus NC laboratories more difficult when results from laboratories with
instrument/measurement problems are included. The soil analytical data from these laboratories
should be considered to give outlier results for cations in ammonium acetate.
3.2 Supplemental Statistical Analyses
The results for the supplemental statistical analyses are summarized in Table 12. The
tabular detailed results are located in Appendix D immediately following the Youden-pair plots for
each parameter. These tests differed from the Youden-pair plots in that the plots compared the
contract versus the non-contract laboratory data, and the tests compared the DDRP data to the
non-contract laboratory data. The results from the supplemental tests provide an indication of the
comparability of the DDRP databases to the data generated by other soil characterization
laboratories. While the conclusions which may be drawn from the supplemental tests may be
limited due to the very small degrees of freedom, a brief discussion of the test results are presented
as additional information for the reader.
The supplemental statistics provided in Appendix D test the following items for each
parameter and audit samples A, Bs, Bw, and C: 1) time effect; 2) homogeneity of laboratories; and
3) within-group and between group variability. The DDRP databases do not contain results for the
B and O soil samples nor the liquid extracts and therefore no comparison could be made for these
materials. The F-tests performed to determine whether there was a time effect gave significant
results in 19 cases. For only one type of measurement, air-dry moisture content, were the tests
significant on three audit soil audit materials (A, Bw, Bs, and C was close). In this case, moisture
content increased from the earlier studies to this study by about 0.25% in each material and it is
thought that this is owing to a slight change in audit material storage conditions. The DDRP data
were in agreement with the NC laboratories for these measurements in this study. For four other
measurements, Very Coarse Sand, K exchangeable in 1M NH4C1, Fe in sodium pyrophosphate, and
24 '
-------
Total Carbon, the F-tests were significant for two materials each. The pattern of discrepancy was
not the same across all four materials. All the other significant F-tests involved only one audit
material per type of measurement.
The F-test for homogeneity of all laboratory results were significant for 109 out of the 116
audits for all parameters where six or more laboratories reported results. These results were
anticipated due to the expected variation in laboratory protocol A pairwise comparison was.
performed to determine which non-contract laboratory results differed significantly with the DDRP
data. These results show that in most cases only a few NC laboratories have significantly different
data from the DDRP data. The parameters for which more than four or five NC laboratories were
significantly different were Medium Sand, CEC extracted by 1M NH4OAc, and Total Sulfur. The
Bw audit sample had more than four laboratories with significantly different results for the fine sand
and silt parameters.
The within-group and between-group (DDRP versus NC) comparisons indicated 50 out of
116 and 13 out of 116 significant differences, respectively. The within-group variability may be due
to differences in protocol, standards, and other sources of random error. The between-group
variability shows differences between the DDRP and NC data. Of the 13 between-group significant
differences only two parameters had more than one audit sample, namely Moisture and AL in
Sodium Pyrophosphate. Four of the 13 differences may have been due to large within-group
variability. Table 12 summarizes the results for each audit and parameter, and provides additional
information on overall parameter and parameter-group comparability. Only 4 out of 27 parameters,
Very Coarse Sand, Na Extracted by 1M NH4OAc, and Fe and AL in Sodium Pyrbphosphate, were
significantly different. The parameter group data was all comparable. Overall, the supplemental
tests indicate that the DDRP and NC data are comparable.
Table 12. Critical Probability and t-values for Between-Group Statistical Analysis; DDRP vs.
NC Laboratories for Calcium in 1M NIL^OAc by Audit, Parameter, and Parameter-
Group.
Parameter
Moisture
V. Coarse Sand
Coarse Sand
Medium Sand
Fine Sand
V. Fine Sand
Sand
Audits
Pr>F
A
.0174*
.8523
.3643
.1576
.9472
2067
.2504
Bs
.2037
.2808
.1539
.1537
.2252
.1050
.0477*
Bw
.0092*
.3492
.8473
.2797
.6216
.3071
.6032
C
.5836
.0049*
.0095*
.6487
.0055*
.0033'
.3418
Parameter
t-value*
2.269
2.557*
2263
0.787
1.311
1.631
0.781
Parameter
Group
Pr>F*
—
0.339
25
-------
Table 12. Continued
Parameter
SUt
Clay
pH, H20
pH, .002M CaCl2
pH, .01M CaCl2
Ca, 1M NH4C1
K, 1M NH4C1
Ca, 1M NH4OAc
Mg, 1M NH4OAc
K, 1M NH4OAc
Na, 1M NH4OAc
CEC, 1M NH^l
CEC, 1M NH4OAc
A1,KC1
Fe, pyrophos.
Al, pyrophos.
Fe, dithionite
Al, dithionite
SO* H2O
Total C
Total N
Totals
Audits
Pr>F*
A
.5570
.0850
.2335
.0649
.2978
.9462
.4681
.6168
.8921
.6371
.0906
.6674
.7379
.0653
.0010*
.0008*
.2111
.2465
.9588
.1452
3620
2882
Bs
.6078
.0081*
.3094
.6019
.4048
.9101
.3122
.7756
.7511
.1127
.0903
.6500
.6622
.0748
.4517
.8157
3731
3884
—
3885
.4637
.1582
Bw
.6996
.3828
.3281
.6777
.4400
.5983
.3493
.7157
.6174
.7310
.1461
.6293
.7385
.0591
.0208*
.4810
.2208
.3221
~
.0957
.4428
.0099*
C
.2817
.6812
.3971
.0001*
.3686
.8192
.1372
.3624
.2671
.0649
.0667
.9277
.8746
.1526
.0078
.1897
.5851
.1483
.3921
.0115*
.0934
.6068
Parameter
t-value*
0.173
1.942
0.141
1.931
0.224
0.173
1.005
0.415
0.002
0.153
3.562*
0.781
0.141
~
3.102*
3.808*
0.728
0.583
-
0.141
0387
1363
Parameter
Group
Pr>F"
0.151
0.480
0.614
0.144
0.628
--
0.079
—
0.726
* Significantly different if Pr>F is less than .05
* Significantly different if t-value is greater than the critical value
26
-------
4. CONCLUSIONS
The general conclusion is that the DDRP protocol does provide results comparable to those
results obtained by other soil laboratories for 30 parameters. In 122 of 141 comparisons involving
results from six or more laboratories, the results from the two contract laboratories that used the
DDRP protocol met the comparability criterion. There was never a case in which both contract
laboratories failed to meet the comparability criterion and only one case where one failed and the
other contract laboratory had the next most extreme sample mean. Therefore, it would appear that
the 19 failures to obtain comparability are either a result of random analytical errors in individual
C laboratories, incorrectly reported results, or from the misapplication of the DDRP protocol. In
the case of the sand results, where there is a pattern of measurements by one laboratory that is too
large, it is possible that interpretation or adherence to the protocol may have changed.
27
-------
REFERENCES
1. Byers, G.E., R.D. Van Remortel, I.E. Teberg, MJ. Miah, CJ. Palmer, ML. Papp, W.H.
Cole, A.D. Tansey, D.L. Casseli, and P.W. Shaffer. 1989. Direct/Delayed Response Project:
Quality Assurance Report for Physical and Chemical Analyses of Soils from the Northeastern
United States. U.S. Environmental Protection Agency, Las Vegas, Nevada. EPA/600/4-
89/037.
2. Van Remortel, R.D., G.E. Byers, I.E. Teberg, MJ. Miah, CJ. Palmer, M.L. Papp, M.H.
Bartling, A.D. Tansey, D.L. Casseli and P.W. Shaffer. 1988. Direct/Delayed Response
Project: Quality Assurance Report for Physical and Chemical Analyses of Soils from the
Southern Blue Ridge Province of the United States. U.S. Environmental Protection Agency,
Las Vegas, Nevada. EPA/600/8-88/100.
3. Bartz, J.K., S.K. Drouse, KA. Cappo, M.L. Papp, GA. Raab, MA. Stapanian, F.C. Garner,
D.S. Coffey, and K. Thornton. 1987. Direct/Delayed Response Project: Quality Assurance
Plan for Soil Sampling, Preparation, and Analysis. U.S. Environmental Protection Agency,
Las Vegas, Nevada. EPA/600/8-87/021.
4. Cappo, KA., LJ. Blume, GA. Raab, J.K. Bartz, and J.L. Engels. 1987. Analytical Methods
Manual for the Direct/Delayed Response Project Soil Survey. U.S. Environmental Protection
Agency, Las Vegas, Nevada. EPA 600/8-87/020.
5. Gray, C, and F. Cox. 1985. Survey of State Soil Testing Laboratories in the United States.
Soil Testing and Plant Analysis Committee - S877 of the Soil Science Society of America.
6. Manual of Soil Sampling and Methods of Soil Analysis. 1978. J A. Mckeague, Ed. Soil
Survey Committee, Canadian Society of Soil Science, Ottawa, Ontario.
7. Methods of Soil Analysis, Parts 1 & 2. 1982. A.L. Page, ed. Agronomy 9 monograph,
American Society of Agronomy, Madison, Wisconsin.
8. Soil Survey Laboratory Methods and Procedures For Collecting Soil Samples. 1972. Soil
Survey Investigations Report No. 1. Soil Conservation Service, U.S. Department of
Agriculture. Washington, DC 20402.
9. Analytical Methods Manual. 1984. B.H. Sheldrick, Ed. Land Resource Research Institute,
Ottawa, Ontario. LLRI Contribution No. 8430.
10. Youden, WJ., and E.H. Steiner. 1975. Statistical Manual of the Association of Official
Analytical Chemists. Association of Official Analytical Chemists, Arlington, VA, 87 pp.
11. Tukey, J.W. 1977. Exploratory Data Analysis. Addison-Wesley, Reading, MA
12. SAS Institute, Inc. 1988. SAS Procedures Guide, Release 6.03 Edition. SAS Institute, Inc.,
Gary, NC, 441 pp.
28
-------
APPENDIX A
SUMMARY OF THE NE AND SBRP
AUDIT SOIL RESULTS
A-l
-------
A-2
-------
Audit Sample?
A Bs Bw C
Lab x SD d x SD d x SD d x SD
Moisture % dry wt
{ME;
i
2
3
4
ALL
\
1.89
1.81
.._
.._
1.85
0.08
0.15
-.—
-.—
0.13
0.04
0.04
-.—
-.—
161
2.63
2.25
2.83
2.62
0.10
0.15
0.18
0.29
0.29
0.00
0.01
037»
0.21*
1.94
128
2.05
2.25
112
0.10
0.18
0.05
0.06
0.20
0.19**
0.16*
0.07
0.13«
0.13 0.04
0.16 0.03
-.— -.—
0.15 0.04
0.14 0.04
0.02
0.02
.._
0.01
{ SBRP }
1
2
3
ALL
1.95 0.13
1.87 0.28
1.82 0.20
1.89 0.22
0.06
-0.01
•0.06
179
2.81
-.—
180
0.31
0.72
-.—
0.56
•0.01
0.01
-.—
136
234
128
133
0.12
0.04
0.15
0.11
0.03
0.01
-0.05
0.14
0.15
0.15
0.15
0.01
0.00
0.01
0.01
•0.01
0.00
0.00
Specific Surface m2/g
{NE}
1 84.6 15.4 21.0» 19.0 1.13 14.4* 30.5 8.67 1.40 1.43 1.43 1.50*
2 413 152 21.1» 35.0 5.43 1.60 36.7 7.15 4.90* 104 0.66 0.89*
3 .._ .._ .._ 416 6.74 9.20* 33.5 0.75 1.60 -.- -.-
4 -.- -.- -.- 310 9.30 1.40 27.2 651 4.70* 5.28 121 230*
ALL 63.4108. 33.4 9.56 31.9 7.99 194 140
{SBRP}
1 403 4.56 3.40 26.0 6.59 -0.63 40.1 1.98 3.9 121 0.15 -0.24
2 28.2 9.31 -8.64 27.1 8.23 0.52 253 7.28 -10.9 158 0.40 -0.87
3 44.8 4.98 7.90 -.- -.- -.- 41.4 1.47 5.1 3.11 1.19 0.66
ALL 36.9 9.81 . 26.6 738 . 36.3 8.11 . 145 1.10
Total Sand (10 - 0.5 nun) % dry wt
{NE}
1 54.4 037 140 83.4 0.80 0.63 24.0 0.51 4.10* 95.1 1.11 037
2 59.2 0.59 140 83.4 0.93 0.60 333 232 5.20* 95.9 1.64 0.47
3 .._ .._ -._ 84.7 1.13 0.68 26.2 0.28 1.90* -.- -.-
4 ..- -._ -.- 84^ 0.97 0.45 28.7 3.84 0.60 95.6 0.82 0.16
ALL 56* 152 84.1 1.09 28.1 4.52 95J 1.16
{SBRP}
1 54.1 4.00 -140 85.6 1.14 0.18 243 0.44 -181 93.6 134 -1.74
2 59.2 1.18 170 853 136 -0.15 315 3.65 5.40 973 100 1.90
3 55.6 0.61 -0.82 -.- -.- --- 25* 1.47 -121 94.7 133 -0.67
ALL 56.5 333 85.5 1.25 27.1 4.10 95.4 2.04
A-3
-------
Audit Sample"
A Bs Bw C
Lab x SD d x SD d i" SD d x SD
Very Coarse Sand (2.0 -1.0 mm) % diy wt
{NE}
1 0.84 0.19 0.01 7.17 0.93 0.21 2.95 0.40 0.07 4.96 1.04 0.00
2 0.85 0.16 0.01 7.28 122 031 3.17 1.01 0.16 4.57 1.82 039*
3 .._ .._ .._ 7.18 2.11 021 3.15 0.07 0.13 -.- -.-
4 .... .._ .._ 6.45 1.97 0.52* 2£8 0.79 0.14 5.20 0.97 0.24
ALL 0.84 0.17 6.97 1.63 3.02 0.70 4.96 1.19
{ SBRP }
1 0.79 0.22 -0.18 10.6 1.03 0.77 2.77 036 0.15 3.45 0.78 0.01
2 1.00 0.22 0.03 9.15 2.17 -0.65 235 0.47 -0.27 4.47 2J8 1.03
3 1.15 0.45 0.18 -.- -.- -.- 2.67 0.64 0.05 2.75 0.88 -0.69
ALL 0.97 033 9.80 1.86 2.62 0.48 3.44 1.69
Coarse Sand (1.0 - 0.5 nun) % dry wt
{NE}
1 3.10 0.15 0.03 152 1.27 1.50* 430 0.24 0.23* 15S 2.10 028
2 3.04 027 0.03 ' 15.9 0.94 0.80* 3.82 0.47 025* 14.6 2.74 0.58
3 -._ .._ .._ 18.4 329 1.70* 430 0.00 023* -.- -.-
4 .._ .._ .._ 17.1 2.40 0.40 3.95 0.47 0.12 152 2.94 0.01
ALL 3.07 021 16.7 230 4.07 0.42 152 2.49
{SBRP}
1 3.13 034
2 3.14 021
3 3.00 0.44
ALL 3.10 033
Medium Sand (0.5 - 025 mm) % dry wt
{NE}
1
2
3
4
ALL
{SBRP}
1 8.09 0.62 -0.18 263 0.71 0.10 3.50 0.09 -0.01 29.6 2.90 -1.94
2 834 029 0.08 26.1 122 -0.08 335 0.13 -0.16 31.0 231 -032
3 838 0.54 0.11 -.- -.- -.- 3.70 0.12 0.19 32S 134 0.99
ALL 827 0.50 262 1.00 351 0.17 31.5 229
0.03
0.04
-0.10
20.8
19.0
.._
19.8
1.44 1.00
2.48 -0.85
-.— -.—
224
4.18
3.42
4.42
4.04
028 0.15
0.43 -0.61
030 039
0.52
132
133
11.0
12.1
3.04
4.44
1.56
2.95
1.00
120
-1.13
7.95
839
.._
-._
8.17
0.13
037
.._
..—
035
022
022
.._
-._
263
253
28.0
282
26.9
0.61
0.90
0.85
0.81
1.55
0.60
1.60*
1.10
,130
3.46
3.60
3.65
3.92
3.62
0.08
0.15
021
0.66
036
0.16
0.02
0.03
029*
31.7
29.4
-.—
32£
31.6
156
134
...
230
2.16
0.10
220*
-.—
120
A-4
-------
Audit Sample*
Lab
X
A
SD
d
X
Bs
SD
d
Fine Sand (025 - 0
{ NE
1
2
3
4
ALL
}
215
24.9
-.—
-.—
23.2
0.98
033
-.—
-.—
1.87
1.70*
1.70*
..—
-.—
252
25.6
23.7
243
24.7
1.08
057
3.64
238
220
0.48
0.87
1.05
0.43
Bw
x SD
.1 mm) %
357 0.19
420 0.21
4.00 0.00
5.02 1.85
4.13 1.01
d
dry wt
056*
0.07
0.13
0.89*
X
32.2
35.4
-._
32.7
33.0
C
SD
1.68
2.06
.._
2.64
2.42
d
0.80
230*
.._
030
{ SBRP }
1
2
3
ALL
21.6
24.7
243
235
2.09
0.51
0.67
1.92
-1.92
120
0.75
20.8
235
-.—
223
151
105
-.—
125
-1.48
120
-.—
Very Fine Sand (0.1 -
{ME
1
2
3
4
ALL
}
21.0
22.1
-.—
-.—
21.5
0.89
0.66
..—
-.—
0.94
054*
054*
..—
..—
9.47
9.45
7.47
8.44
8.72
0.71
054
1.04
155
130
0.76*
0.73*
125*
028*
357 0.12
4.15 0.13
4.17 0.15
3.91 033
0.05 nun)
9.69 029
185 141
11.0 0.07
13.0 1.61
133 4.05
-034
024
0.27
% dry wt
357*
520*
221*
029
343
36.6
37.7
36.7
10.8
11.6
.._
9.79
10.6
3.89
433
1.94
3.13
1.98
256
.._
170
140
-2.50
-0.12
0.92
020
0.99*
.._
0.84*
{ SBRP}
1
2
3
ALL
205
22.0
18.8
20.6
1.78
1.05
0.74
1.80
-0.17
1.40
-1.77
7.15
758
.._
739
0.91
1.05
.._
0.99
Total Silt
{NE
1
2
3
4
ALL
}
26.6
216
....
.._
24.6
1.04
0.82
.,_
..-
130
100*
100*
.._
-.—
100
15.9
14.8
143
14.8
14.9
1.09
123
1.43
1.00
121
•024
020
.._
103 0.12
193 188
10.9 0.43
13.0 433
-2.76
630
-2.09
133
11.9
10.8
11.6
1.48
3.06
120
106
1.70
032
-0.76
(0.05.0.002mm) %drywt
1.00
0.01
052
0.09
027
68.8 0.42
59.0 1.94
65.0 057
66.1 3.15
64.9 452
3.90*
5.90*
0.10
120
4.71
182
..—
3.80
3.98
1.11
1.74
-.—
122
1.45
0.73*
1.16*
..—
0.18
{SBRP}
1
2
3
ALL
28.0
217
265
25.6
526
143
0.67
4.15
140
-189
QS5
119
118
..—
118
1.05
1.45
..—
125
0.04
-0.03
-.—
685 0.96
60.0 3.78
663 125
65.4 422
3.10
-5.47
0.90
6.00
230
527
4.40
127
1.97
129
111
1.60
-110
0.87
A-5
-------
Audit Sample*
Lab
X
A
SD
d
Bs
x SD
d
Coarse Silt (0.05 -
{ME
1
2
3
4
ALL
}
113
8.90
-.— "
-.—
1.60
0.95
1.08
-.—
-.—
1.20
120*
120*
..—
-.—
10.1
11.0 0.70
9.79 0.90
9.73 1.22
102 0.69
0.94 034
0.91
030
036
0.15
31.1
X
Bw
SD
0.02 mm) V
35.0
24.9
32.6
323
4.83
033
186
127
330
330
d
» dry wt
3.90*
620*
130
120
337
X
431
2.43
-._
336
137
C
SD
0.95
1.58
.._
123
0.63
d
0.74»
1.13*
.._
0.21*
{ SBRP }
1
2
3
ALL
{NE
1
2
3
4
ALL
12.9
10.4
113
11.6
}
153
13.7
-.—
-.—
132
6.40
4.12
0.49
4.61
031
1.45
-.—
.._
0.82
130
-128
0.17
032»
032*
-.—
-.—
4.77
8.69 0.66
8.85 1.24
-.— -.—
8.78 1.00
Fine Silt
4.85 0.45
5.07 1.15
4.62 037
4.52 034
038 022
-0.09
0.07
-.—
34.6
31.1
35.1
33.7
031
195
0.78
231
(0.02 - 0.005 mm) %
0.08
030
0.15
025
333
333
34.1
323
333
1.75
0.60
119
0.64
164
022
0.84
-239
130
dry wt
0.02
032
1.40
0.01
0.40
5.40
1.97
5.02
4.07
0.41
033
-.—
0.44
020
1.13
117
121
111
0.19
031
-.—
0.14
0.03
137
-109
0.95
0.00
0.07
.._
0.04
{SBRP}
1
2
3
ALL
15.1
123
14.7
13.9
1.17
1.82
036
134
120
-1.61
0.77
421 038
3.97 0.71
-.— -.—
4.08 0.78
0.13
-0.11
-.—
33.9
283
313
31.7
034
1.46
0.83
236
Total Clay (< 0.002 mm) %
{ME
1
2
3
4
ALL
}
19.0
182
.._
.._
032
030
0.71
.._
.._
036
036
036
.._
.._
1.08
0.70 036
1.69 036
055 0.40
0.71 025
0.70 0.40
038
0.61
0.13
037
727
7.70
835
520
7.05
036
1.43
0.92
138
131
220
-188
•0.43
035
dry wt
022
0.65-
130»
135*
0.60
035
027
021
0.17
122
-._
0.67
037
0.14
026
0.14
0.13
0.95
-.—
034
0.76
025
0.00
-0.08
0.40*
0.65»
-._
0.10*
{ SBRP }
1
2
3
ALL
175
18.1
173
17.9
1.42
121
034
1.61
-0.07
0.15
-0.12
1.46 0.76
138 038
-.— -.—
1.69 034
4)23
0.19
..—
725
732
7.77
7.48
037
029
039
0.63
-023
0.05
030
035
0.42
0.00
020
0.07
0.05
0.00
021
0.15
023
-020
A-6
-------
Audit Sample8
Lab
X
A
SD d
8s
x SD
d
X
Bw
SD d
C
x SD
d
pH in HjO
{NE}
1 4.53 0.04 0.00 436 0.09 0.13 5.02 0.04 0.06 5.19 0.27 0.14
2 432 0.03 0.00 4.52 0.04 0.03 5.14 0.03 0.06 536 0.08 0.24
3 .._ .._ .._ 4.50 0.04 0.01 5.15 0.01 0.06 -.- -.-
4 .._ .._ .._ 4.50 0.03 0.01 5.09 0.06 0.00 534 0.09 0.02
ALL 0.04 -.- 4.49 0.07 -.- 5.08 0.06 -.- 532 0.24 -.-
{SBRP}
1 4.50 0.04 -0.02 4.53 0.05 -0.02 5.10 0.04 -0.03 5.21 0.08 -0.27
2 4.51 0.03 -0.01 436 0.19 0.01 5.12 0.03 -0.01 5.49 0.03 0.01
3 4.56 0.04 0.04 -.- -.- -.- 5.18 0.02 0.05 537 0.07 0.08
ALL 432 0.04 435 0.14 5.13 0.05 5.48 0.14
pH in 0.002M CaClj
{NE}
1 423 0.03 0.01 4.13 0.01 0.02 4.65 0.10 0.06 4.91 0.06 0.05
2 4.21 0.01 0.01 4.14 0.02 0.00 4.72 0.02 0.02 4.97 0.12 0.01
3 .._ -._ ... 4.14 0.03 0.00 4.75 0.02 0.04 -.- -.-
4 -.- .._ -.- 4.15 0.04 0.01 4.77 0.07 0.06 5.01 0.05 0.05
All 4.22 0.02 4.14 0.03 4.71 0.09 4.96 0.08
{ SBRP }
1 423 0.03 -0.02 4.19 0.03 0.06 4.72 0.03 -0.00 4.75 0.02 430
2 4.21 0.02 -0.04 4.08 0.03 -0.05 4.67 0.03 -0.05 4.99 0.06 -0.05
3 434 0.09 0.09 -.- -.- -.- 4.78 0.03 0.06 5.17 0.08 0.13
ALL 4.25 0.07 4.13 0.06 4.72 0.05 5.04 0.17
pHinO.OlMCaClj
{NE}
1 4.02 0.04 0.04 336 0.03 0.03 437 0.03 0.04 4.72 0.12 0.04
2 3.95 0.02 0.03 3.93 0.02 0.01 4.46 032 0.07 4.87 0.03 0.12
3 -.- -.- -.- 334 0.03 0.00 438 0.05 0.04 -.- -.-
4 -.- -.- -.- 333 0.07 0.01 436 0.07 0.02 4.73 0.11 0.03
ALL 339 0.05 3.94 0.05 434 0.28 4.76 0.12
{SBRP}
1 4.01 0.04 -0.01 4.00 0.07 0.04 4.61 0.01 -0.01 4.71 0.02 -0.14
2 358 0.04 -0.04 332 0.03 -0.03 437 0.02 -0.04 4.79 0.02 -0.05
3 4.09 0.02 0.07 -.- -.- -.- 4.67 0.03 0.06 4.92 0.07 0.08
ALL 4.02 0.06 3.96 0.07 4.62 0.04 434 0.10
A-7
-------
Audit Sample?
Lab
{NE}
1
2
3
4
ALL
{ SBRP
1
2
3
ALL
1
2
3
4
ALL
{SBRP
1
2
3
All
X
0.29
0.25
-.—
..—
027
}
030
025
033
029
022
022
-.—
-._
022
}
023
022
020
021
A
SD
0.04
0.02
-.—
-.—
0.04
0.04
0.06
0.06
0.06
0.03
0.01
..—
-.—
0.02
0.02
0.01
0.01
0.02
d
0.02
0.02
-.—
-.—
0.01
4.04
0.04
0.00
0.00
..— .
-.—
0.01
0.00
4.02
X
032
025
027
030
028
030
022
-.—
025
0.06
0.05
0.05
0.06
0.05
0.06
0.05
.._
0.05
Bs
SD
Ca
0.03
0.06
0.04
0.10
0.07
0.04
0.03
-.—
0.05
Mg
0.00
0.01
0.01
0.01
0.01
0.01
0.01
.._
0.01
d
inNH4Cl
0.04*
0.03»
0.01
0.02
0.05
4.04
-.—
inNH4Cl
0.01
0.00
0.00
0.01
0.01
4.01
.._
KinNH^Cl
{NE}
1
2
3
4
ALL
024
024
.._
.._
024
0.02
0.02
.._
.._
0.02
0.00
0.00
.._
.._
0.02
0.04
0.03
0.03
0.03
0.01
0.02
0.01
0.00
0.02
0.02
0.01
0.00
0.00
Bw
x SD
meq/lOOg
029 0.05
024 0.05
0.29 0.00
0.28 0.03
027 0.05
030 0.05
0.23 0.02
031 0.05
028 0.05
meq/lOOg
0.05 0.05
0.05 0.01
0.04 0.01
0.06 0.01
0.05 0.03
0.05 0.01
0.06 0.01
0.05 0.01
0.05 0.01
meq/lOOg
0.06 0.01
0.06 0.01
0.07 0.00
0.06 0.00
0.06 0.01
d
0.02
0.03*
0.02
0.01
0.02
4.05
0.03
0.00
0.00
0.01
0.01
4.00
0.00
4.00
0.00
0.00
0.01
0.00
X
0.08
0.08
-.—
0.08
0.07
0.11
0.09
0.13
0.11
0.03
0.03
.._
0.03
0.03
0.03
0.03
0.04
0.03
0.03
0.03
-.—
0.03
0.03
C
SD
0.02
0.03
-.—
0.01
0.02
0.05
0.02
0.04
0.04
0.02
0.01
-._
0.00
0.01
0.02
0.01
0.01
0.01
0.02
0.01
..—
0.00
0.01
d
0.01
0.02
.._
0.00
4.00
4.02
0.02
0.00
0.00
.._
0.00
4.00
4.01
0.01
0.00
0.00
..—
0.00
{ SBRP }
1
2
3
ALL
029
025
024
026
0.15
0.02
0.02
0.09
0.02
4.01
4.02
0.02
0.02
.._
0.02
0.03
0.00
-._
0.02
4.00
0.00
-.—
0.06 0.01
0.06 0.01
0.05 0.01
0.06 0.01
0.00
0.00
4.01
0.02
0.02
0.03
0.03
0.00
0.01
0.01
0.01
4.00
4.00
0.00
A-8
-------
Audit Sample*
Lab
X
A
SD d
X
Bs
SD d
Bw
x SD d
C
x SD
d
Na in NH4C1 meq/lOOg
{NE}
1 0.04 0.01 0.01 0.00 0.03 0.02 0.06 0.06 0.02 0.01 0.03 0.01
2 0.02 0.01 0.01 0.01 0.00 0.00 0.02 0.00 0.02 0.00 0.01 0.01
3 .._ .._ .._ 0.03 0.01 0.01 0.02 0.02 0.02 -.- -.-
4 .._ .._ .._ 0.02 0.00 0.00 0.04 0.01 0.00 0.01 0.00 0.01
ALL 0.03 0.02 0.02 0.01 0.04 0.04 0.00 0.02
{ SBRP }
1 0.05 0.03 0.01 0.03 0.03 0.01 0.02 0.03 0.00 0.01 0.01 -0.00
2 0.04 0.01 0.00 0.02 0.01 -0.01 0.02 0.02 0.00 0.00 0.00 -0.01
3 0.03 0.02 -0.01 -.- -.- -.- 0.02 0.01 0.00 0.02 0.02 0.01
ALL 0.04 0.02 0.02 0.02 0.02 0.02 0.01 0.02
Ca in NH4OAC meq/lOOg
{NE}
1 027 0.03 0.01 0.24 0.04 0.03* 039 0.07 0.04* 0.08 0.03 0.01
2 026 0.02 0.01 020 0.02 0.02 022 0.04 0.03* O.OS 0.02 0.02
3 .._ .._ .> 023 0.05 0.02 026 0.02 0.01 -.- -.-
4 .._ ... ... 021 0.02 0.00 023 0.02 0.02 0.08 0.01 0.00
ALL 027 0.03 021 0.03 025 0.06 0.07 0.03
{ SBRP }
1 027 0.03 0.00 0.19 0.03 0.01 024 0.04 0.00 0.08 0.03 -0.01
2 023 0.05 -0.04 0.17 0.04 -0.01 0.18 0.01 -0.06 0.05 0.03 -0.05
3 0.33 0.05 0.06 -.- -.- -.- 029 0.05 0.05 0.13 0.05 0.04
ALL 027 0.06 0.18 0.04 024 0.06 0.09 0.06
Mg in NH«OAC meq/lOOg
{NE}
1 024 0.03 0.01 0.06 0.02 0.01 0.05 0.02 0.00 0.02 0.02 0.00
2 022 0.02 0.01 0.04 0.01 0.01 0.05 0.01 0.00 0.03 0.01 0.00
3 .._ ... .._ 0.05 0.01 0.00 0.06 0.01 0.01 -.- -.-
4 -.- -.- -.- 0.05 0.00 0.00 0.05 0.00 0.00 0.03 0.01 0.01
ALL 023 0.03 0.05 0.01 0.05 0.01 0.03 0.02
{ SBRP}
1 025 0.02 0.01 0.05 0.02 0.00 0.07 0.01 0.01 0.04 0.00 0.01
2 022 0.02 -0.01 0.05 0.01 0.00 0.04 0.00 -0.01 0.03 0.01 -0.01
3 023 0.02 0.00 -.- -.- -.- 0.06 0.01 0.00 0.04 0.01 0.00
ALL 023 0.02 0.05 0.01 0.06 0.01 0.04 0.01
A-9
-------
Audit Sample"
Lab
{NE}
1
2
3
4
ALL
{SBRP
1
2
3
ALL
X
0.26
0.24
-.—
-.—
0.25
}
021
0.26
0.25
026
A
SD
0.01
0.02
-.—
..—
0.02
0.06
0.01
0.01
0.04
d
0.01
0.01
-.—
-.—
0.01
0.00
-0.01
X
0.02
0.02
0.04
0.03
0.03
0.03
0.03
-,—
0.03
Bs
SD
Kin
0.01
0.01
0.01
0.00
0.01
0.02
0.00
.._
0.01
d
NH4OAC
0.00
0.00
0.01
0.00
0.00
0.00
..—
Bw
x SD
meq/lOOg
0.07 0.04
0.04 0.01
0.07 0.00
0.06 0.00
0.06 0.02
0.06 0.02
0.06 0.01
0.06 0.01
0.06 0.01
d
0.01
0.02
0.01
0.00
0.00
0.00
0.00
X
0.02
0.02
-.—
0.03
0.02
0.05
0.02
0.03
0.03
C
SD
0.01
0.01
-.—
0.00
0.01
0.00
0.00
0.01
0.01
d
0.00
0.00
.._
0.01
0.02
0.01
0.00
Na in NH4OAC meq/lOOg
{NE}
1
2
3
4
ALL
0.03
0.04
-.—
-.—
0.03
0.01
0.01
-.—
-.—
0.01
0.00
0.00
-.—
-.—
0.04
0.01
0.02
0.02
0.02
0.07
0.00
0.01
0.00
0.02
0.02
0.01
0.00
0.00
0.04 0.07
0.02 0.01
0.08 0.08
0.02 0.01
0.03 0.05
0.01
0.01
0.05
0.01
0.01
0.00
-.-
0.00
0.00
0.01
0.00
-.—
0.00
0.01
0.00
0.00
-._
0.00
{SBRP}
1-
2
3
All
0.05
0.04
0.03
0.04
0.03
0.01
0.01
0.02
0.01
0.00
-0.01
0.02
0.02
-._
0.02
0.03
0.01
.._
0.02
0.00
0.00
.._
CEC in NH,Q
{NE}
1
2
3
4
ALL
8.0
73
-.—
.._
7.7
0.25
0.46
-.—
.._
0.49
032
032
..—
.._
75
75
12.9
8.4
8.9
1.16
038
1.40
0.85
225
136*
137*
4.00*
050*
0.03 0.01
0.03 0.01
0.02 0.01
0.02 0.01
0.00
0.00
•0.01
0.01
0.00
0.01
0.01
0.00
0.01
0.01
0.01
0.00
-0.01
0.00
meq/lOOg
6.0 0.67
3.7 0.12
9.6 059
43 039
52 1.71
0.81»
1.44*
4.40*
0.91»
054
052
-.—
0.63
057
028
0.14
-.—
037
0.29
0.03
0.05*
-.—
0.06»
{SBRP}
1
2
8.05
7.11
3 10.9
ALL
8.47
1.08
051
L59
1.90
-0.42
-136
2.43
624
7.20
...
7.67
056
0.92
>.—
0.93
057
-0.48
.._
4.82 0.82
4.01 0.77
9.01 0.64
5.79 236
-0.97
-1.77
3.22
0.77
0.84
- 1.47
1.14
0.03
058
038
052
-037
•031
033
A-10
-------
Audit Sample"
A Bs Bw C
Lab x SD d x SD d x SD d x SD
CEC in NH4OAC meq/lOOg
{NE}
1 18.7 0.40 1.69* 273 0.82 2.65* 13.9 1.18 135* 1.26 0.12 0.25*
2 15.4 0.74 1.62* 22.0 122 2.64* 10.4 1.41 2.14* 0.76 034 0.25*
3 .._ .._ .._ 26.5 2.01 1.80* 16.4 1.15 3.85* -.- -.-
4 .._ .._ .._ 252 2.16 0.52 11.9 0.82 0.65* 0.85 0.15 0.16*
ALL 17.0 1.77 24.7 180 1.46 12.5 117 1.00 029
{SBRP }
1 18.8 0.76 0.73 23.2 121 1.00 13.8 151 0.66 134 0.18 -0.09
2 15.5 1.19 -2.62 213 127 0.86 9.64 0.64 3.48 0.94 0.12 -0.49
3 20.9 1.61 2.80 -.- -.- -.- 15.6 1.45 -150 1.79 033 036
ALL 18.1 2.53 22.2 1.55 13.1 197 1.43 0.46
KCL Acidity meq/lOOg
{NE}
1 3.01 0.11 032* 4.24 0.27 0.43* 1.59 0.14 0.03 0.14 0.07 0.03
2 3.64 0.19 032' 4.82 030 0.14 1.65 0.17 0.03 0.23 0.08 0.06
3 .._ .._ .._ 3.99 0.54 0.68* 1.67 0.07 0.05 -.- -.-
4 .._ .._ .._ 5.12 0.61 0.44* 1.62 021 0.00 0.17 0.05 0.00
ALL 333 036 4.68 0.63 1.62 0.16 0.17 0.07
{SBRP}
1 3.19 026 -0.28 4.10 0.40 0.09 1.42 0.07 -032 0.02 0.05 -029
2 3.50 033 0.02 3.94 1.19 -0.07 139 0.08 -0.15 0.17 0.07 -0.15
3 3.80 0.76 033 -.- -.- -.- 238 0.59 0.63 0.52 036 0.20
ALL 3.47 0.52 4.01 0.90 1.74 0.51 032 033
BaClj Acidity meq/lOOg
{NE}
1 20.6 3.59 0.66 39.1 0.10 0.55 172 1.76 0.14 039 1.40 034*
2 192 103 0.66 39.7 428 0.07 182 1.06 0.83 1.07 0.56 0.14*
3 -.- -.- ..- 342 621 5.40* 153 0.15 103* -.- -.-
4 -.- -.- -.- 43.0 4.69 3.40' 17.1 134 020 125 0.88 032*
ALL 19.9 190 39.6 5.40 173 1.54 0.93 1.10
{ SBRP }
1 18.6 1.45 0.00 34.8 114 -0.13 17.4 129 0.13 0.44 0.07 -0.55
2 19.4 145 0.73 35.0 189 0.11 183 1.80 1.10 1.69 0.88 0.70
3 17.6 4.99 -1.05 -.- -.- -.- 16.0 0.79 -124 0.71 0.62 -028
ALL 18.6 3.13 34.9 152 172 1.53 0.99 0.81
A-ll
-------
Audit Sample?
Lab
X
A
SD
d
Bs
x SD
d
X
KCL Extractable Al
{NE}
1
2
3
4
ALL
{ SBRP
1
2
3
ALL
{NE}
1
2
3
4
ALL
{SBRP
1
2
3
ALL
2.46
320
..—
-.—
2.83
}
2.72
3.12
3.07
2.97
0.41
0.45
-.—
..—
0.43
}
035
0.46
035
0.40
0.14
035
-.—
-.—
0.46
0.21
0.29
0.18
030
0.04
0.03
-.—
..—
0.04
0.05
0.06
0.12
0.09
037*
037*
-.—
-.—
-025
0.15
0.10
•
0.02
0.02
-.—
-.-
-0.04
0.07
-0.04
3.72 0.16
3.92 0.40
3.63 0.24
4.78 1.50
4.12 1.00
3.72 0.62
3.93 0.70
-.— -.—
3.84 0.66
Ca in
035 0.02
0.51 0.04
034 0.02
0.51 0.06
0.45 0.09
0.49 0.05
0.55 0.04
-.— -.—
0.52 0.06
0.40*
024*
0.49*
0.66*
•0.12
0.10
-.—
0.002M
0.10*
0.06*
0.12*
0.05*
4.03
0.03
-.—
Mgin0.002M
{NE}
1
2
3
4
ALL
0.10
0.14
.._
.._
0.12
0.07
0.01
..—
.._
0.05
0.02
0.02
-.—
-._.
0.03 0.01
0.05 0.01
0.03 0.00
0.04 0.01
0.04 0.01
0.00
0.01
0.01
0.00
1.53
1.22
1.71
1.88
1.53
129
1.50
1.54
1.42
Cad,
038
0.60
038
0.63
0.51
0.61
0.64
0.55
0.60
Cad,
0.03
0.04
0.03
0.04
0.03
Bw
SD
d
X
C
SD
d
meq/lOOg
0.17
0.15
0.08
0.10
029
0.09
023
0.10
0.18
0.00
031*
0.18*
035*
-0.13
0.08
0.12
0.05
0.10
-._
0.14
0.10
0.06
0.14
0.18
0.15
0.04
0.04
.._
0.04
0.06
0.00
0.03
0.05
0.06
0.04*
0.01
.._
0.05*
-0.09
-0.01
0.04
meq/lOOg
0.04
0.03
0.06
0.02
0.12
0.04
0.01
0.12
0.07
0.13*
0.09*
0.13*
0.13*
0.01
0.04
-0.05
0.55
0.73
.._
0.80
0.68
0.71
059
059
0.61
0.07
0.05
.._
0.03
0.13
0.04
039
0.03
021
0.13*
0.05*
.._
0.12*
0.11
-0.02
-0.02
meq/lOOg
0.00
0.01
0.01
0.01
0.01
0.01
0.01
0.00
0.00
0.01
0.01
..-
0.03
0.02
0.00
0.00
-.-
0.05
0.03
0.01
0.01
-.—
0.01
{ SBRP }
1
2
3
All
0.14
0.12
0.11
0.13
0.03
0.01
0.02
0.02
0.02
0.00
-0.02
0.04 0.00
0.03 0.00
-.- -.—
0.04 0.01
0.00
0.00
-.—
0.04
0.04
0.03
0.04
0.00
0.00
0.01
0.01
0.00
0.00
-0.01
0.02
0.01
0.02
0.01
0.00
0.01
0.00
0.01
0.00
0.00
0.00
A-12
-------
Audit Sample3
A Bs Bw C
Lab x SD d x SD d x SD d x SD
K in 0.002M CaCl, meq/lOOg
{NE}
1 0.06 0.00 0.00 0.01 0.00 0.00 0.01 0.00 0.00 0.01 0.00 0.00
2 0.06 0.01 0.00 0.02 0.00 0.00 0.01 0.00 0.00 0.01 0.00 0.00
3 .._ .._ .._ 0.01 0.00 0.00 0.01 0.00 0.00 -.- -.-
4 .._ .._ .._ 0.01 0.00 0.00 0.01 0.00 0.00 0.01 0.00 0.00
ALL 0.06 0.01 0.01 0.00 0.01 0.00 0.01 0.00
{SBRP }
1 0.07 0.01 0.01 0.02 0.01 0.00 0.01 0.00 0.00 0.01 0.00 0.00
2 0.06 0.01 0.00 0.01 0.00 0.00 0.01 0.00 0.00 0.01 0.01 0.00
3 0.06 0.01 -0.01 ..- ..- -.- 0.01 0.00 0.00 0.01 0.00 0.00
All 0.06 0.01 0.01 0.00 0.01 0.00 0.01 0.00
Na in 0.002M CaClj meq/lOOg
{NE}
1 0.03 0.00 0.00 0.02 0.00 0.00 0.02 0.00 0.00 0.00 0.00 0.00
2 0.03 0.00 0.00 0.02 0.00 0.00 0.02 0.00 0.00 0.00 0.00 0.00
3 .._ .._ .._ 0.01 0.00 0.00 0.02 0.01 0.00 -.- -.-
4 .._ ... ... 0.02 0.00 0.00 0.02 0.00 0.00 0.00 0.00 0.00
ALL 0.03 0.00 0.02 0.00 0.02 0.00 0.00 0.00
{ SBRP}
1 0.04 0.01 0.00 0.02 0.01 0.00 0.02 0.01 0.00 0.00 0.00 0.00
2 0.03 0.00 0.00 0.02 0.00 0.00 0.02 0.00 0.00 0.00 0.00 0.00
3 0.03 0.00 0.00 -.- -.- -.- 0.02 0.00 0.00 0.01 0.00 0.00
All 0.03 0.01 0.02 0.01 0.02 0.00 0.00 0.00
Fe in 0.002M CaCl, meq/lOOg
{NE}
1 0.02 0.01 0.00 0.03 0.00 0.02 0.00 0.00 0.00 0.00 0.01 0.00
2 0.02 0.01 0.00 0.06 0.01 0.01 0.00 0.00 0.00 0.00 0.00 0.00
3 ... .._ .._ 0.04 0.01 0.00 0.00 0.00 0.00 -.- -.-
4 -.- -.- -.- 0.04 0.01 0.01 0.00 0.00 0.00 0.00 0.00 0.00
ALL 0.02 0.01 0.04 0.01 0.00 0.00 0.00 0.00
{ SBRP}
1 0.02 0.01 0.00 0.05 0.01 0.01 0.00 0.00 0.00 0.00 0.00 0.00
2 0.02 0.01 0.00 0.04 0.01 -0.01 0.00 0.00 0.00 0.00 0.00 0.00
3 0.02 0.00 0.00 -.- -.- -.- 0.00 0.00 0.00 0.00 0.00 0.00
ALL 0.02 0.01 0.04 0.01 0.00 0.00 0.00 0.00
A-13
-------
Audit Sample*
A Bs Bw C
Lab x SD d x SD d x SD d x SD
Al in 0.002M CaCl, meq/lOOg
{NE}
1 0.09 0.01 0.01 0.10 0.03 0.06 0.00 0.01 0.00 0.00 0.02 0.00
I 0.08 0.01 0.01 0.17 0.01 0.01 0.01 0.00 0.00 0.00 0.00 0.00
3 .._ .._ .._ 0.14 0.02 0.02 0.00 0.00 0.00 -.- -.-
4 .._ .._ .._ 0.19 0.03 0.03 0.01 0.00 0.01 0.01 0.00 0.00
ALL 0.09 0.01 0.16 0.04 0.00 0.01 0.00 0.01
{SBRP }
1 0.10 0.03 0.02 0.19 0.02 0.02 0.00 0.00 0.00 0.00 0.00 0.00
2 0.08 0.02 0.01 0.1S 0.04 -0.02 0.00 0.00 0.00 0.00 0.00 0.00
3 0.07 0.02 -0.01 -.- -.- -.- 0.01 0.00 -.00 0.01 0.00 -.00
ALL 6.08 0.03 0.17 0.03 0.00 0.00 0.00 0.00
Fe in Pyrophosphate % diy wt
{NE}
1 0.68 0.08 0.03 0.63 0.06 0.01 0.82 0.08 0.01 0.04 0.01 0.00
2 0.62 0.06 0.03 0.61 0.08 0.03 0.81 0.15 0.01 0.03 0.01 0.00
3 .._ -._ .._ 0.65 0.09 0.01 0.95 0.02 0.14* -.- -.-
4 ... .._ .._ 0.67 0.06 0.03 0.73 0.06 0.07* 0.04 0.01 0.00
ALL 0.65 0.07 0.64 0.07 0.80 0.11 0.04 0.01
{SBRP}
1 0.60 0.05 -0.04 0.58 0.04 0.00 0.80 0.06 -0.05 0.05 0.01 0.01
2 0.65 0.06 0.01 038 0.10 0.00 0.84 0.08 -0.01 0.03 0.00 -0.01
3 0.66 0.08 0.03 -.- -.- -.- 0.94 0.12 0.09 0.04 0.01 0.00
ALL 0.63 0.07 0.58 0.07 0.85 0.10 0.04 0.01
Al in Pyrophosphate % dry wt
{NE}
1 0.77 0.14 0.05 0.78 0.09 0.06* 0.62 0.10 0.04* 0.06 0.01 0.00
2 0.66 0.07 0.05 0.84 0.05 0.00 0.55 0.06 0.03 0.05 0.01 0.01
3 -.- -.- -.- 0.83 0.10 0.01 038 0.02 0.00 -.- -.-
4 ... .... .._ 0.88 0.12 0.03 034 0.09 0.04 0.06 0.01 0.00
ALL 0.71 0.12 0.84 0.09 037 0.09 0.06 0.01
{ SBRP}
1 0.60 0.09 0.00 0.79 0.05 0.02 0.60 0.02 0.02 0.06 0.00 0.01
2 0.63 0.12 0.04 0.75 0.13 -0.02 034 0.07 -0.04 0.04 0.01 -0.02
3 0.54 0.06 -0.06 -.- -.- -.- 039 0.06 0.01 0.06 0.01 0.01
ALL 039 0.10 0.77 0.10 038 0.05 0.06 0.01
A-14
-------
Audit Sample8
Lab
{NE}
1
2
3
4
ALL
{ SBRP
1
2
3
ALL
{NE}
1
2
3
4
ALL
{SBRP
1
2
3
ALL
A
x SD
039 0.03
0.48 0.02
-.— -.—
-.— -.—
0.44 0.05
}
039 0.05
0.45 0.04
039 0.02
0.41 0.05
038 0.03
0.55 0.03
-.— -.—
-.— -.—
0.46 0.09
}
0.40 0.06
0.48 0.07
038 0.04
0.42 0.07
d
0.04*
0.04»
-.—
-.—
-0.02
0.04
-0.02
0.08*
0.08*
'-.—
-.—
-0.03
0.06
-0.05
X
0.79
1.07
1.10
0.97
1.00
0.84
0.99
-.—
0.93
1.01
128
0.98
1.08
1.12
0.95
0.98
.,_
0.97
Bs
SD
Fe in
0.07
0.16
0.27
029
0.24
0.23
031
-.—
0.28
Alin
0.09
0.09
0.07
0.12
0.15
0.12
0.13
.._
0.12
d
X
Acid Oxalate
0.22*
0.06»
0.10*
0.03
-0.08 •
0.07
-.—
1.01
1.09
1.05
0.97
1.03
0.99
120
0.91
1.03
Acid Oxalate
0.11*
0.16*
0.14*
0.04
-0.01
0.01
.._
0.90
0.93
0.86
0.92
0.91
0.87
1.01
0.75
0.88
Bw
SD
d
X
C
SD
d
% diy wt
0.18
0.18
0.07
0.09
0.16
0.16
0.09
0.06
0.16
0.02
0.06*
0.02
0.06*
-0.04
0.17
-0.11
0.06
0.10
-._
0.08
0.07
0.11
0.04
0.10
0.08
0.01
0.07
.._
0.10
0.07
0.07
0.01
0.07
0.06
0.02*
0.03*
.._
0.00
0.03
-0.04
0.02
% dry wt
0.09
0.10
0.05
0.04
0.08
0.06
0.04
0.08
0.11
Fe in Citrate Dithionite %
{NE}
1
2
3
4
ALL
{SBRP
1
2
3
ALL
1.74 024
1.17 0.72
-.— -.—
-.— -.—
1.45 0.59
}
1.68 021
1.73 0.15
223 0.14
1.85 029
028»
028*
.._
-._.
-0.17
-0.12
038
1.03
0.98
126
1.01
1.06
0.93
1.05
.._
0.99
0.03
0.17
021
0.11
0.18
0.06
0.14
.._
0.12
0.02
0.07*
021*
0.04
-0.06
0.05
-.—
1.50
1.43
2.15
1.61
1.55
1.77
1.83
2.10
1.88
0.15
025
0.00
0.08
025
0.55
0.08
0.13
038
0.01
0.02
0.05
0.01
•0.01
0.13
-0.12
dry wt
0.05
0.12*
0.60*
0.05
-0.11
-0.06
022
0.08
0.08
-.—
0.08
0.08
0.07
0.05
0.07
0.06
0.18
0.17
-.—
0.15
0.17
0.17
0.12
023
0.19
0.02
0.02
..—
0.02
0.02
0.01
0.00
0.01
0.01
0.04
0.05
-.—
0.02
0.03
0.01
0.03
0.04
0.06
0.00
0.00
-._
0.00
0.01
-0.01
0.01
0.01
0.00
-.—
0.02
-0.01
-0.06
0.05
A-15
-------
Audit Sample"
Lab x
{NE}
1 0.46
2 0.44
3
4
ALL 0.45
{ SBRP }
1 0.45
2 051
3 0.56
ALL 0.50
A
SD
0.04
0.14
..—
-.—
0.10
0.03
0.05
0.04
0.06
d
0.01
0.01
-.—
-.—
-0.05
0.01
0.06
X
Al
0.83
0.85
0.92
0.99
0.91
0.73
0.83
-.—
0.78
Bs
SD
d
X
in Citrate Dithionite
0.02
0.16
0.19
0.08
0.14
0.05
0.07
-.—
0.08
0.07*
0.06*
0.01
0.08*
-0.05
0.05
-.—
0.52
0.68
0£6
0.62
0.62
0.60
0.67
0.78
0.67
Bw
SD
d
X
C
SD
d
% diy wt
0.06
0.11
0.03
0.04
0.12
020
0.03
0.09
0.15
0.10*
0.06*
024*
0.00
-0.07
0.00
0.11
0.05
0.07
.._
0.06
0.06
0.05
0.04
0.07
0.05
0.01
0.02
.._
0.01
0.01
0.00
0.01
0.01
0.01
0.01
0.01
.._
0.00
0.00
•0.02
0.01
Sulfate in H2O tng S/kg
{NE}
1 31.1
2 32.9
3
4
ALL 32.0
{SBRP }
1 31.6
2 29.9
3 26.9
ALL 29.7
3.15
2.55
-._
..—
2.92
1.20
1.45
225
2.44
0.88
0.88
-._
..—
1.90
021
-176
725
922
757
9.28
8.63
838
8.01
.._
8.18
031
1.25
0.87
1.81
154
153
2.16
.._
137
1.38*
059*
1.05*
0.65*
020
-0.17
_._
20.1
203
215
20.9
205
23A
22.7
21.7
22,9
Total Carbon %
{NE}
1 4.57
2 4.95
3
4
ALL 4.76
{SBRP}
1 4.62
2 4.64
3 4.7S
ALL 4.66
029
051
-.—
.._
0.45
020
0.17
052
0.31
0.19
0.19
-.—
....
•
-0.04
-0.02
0.09
6.08
3.88
351
358
4.00
4.19
3.49
-.—
3.81
0.28
033
0.45
0.49
0.93
0.80
0.31
-.—
0.67
2.08*
0.12
0.49*
0.42*
038
-032
-.—
158
153
1.48
157
156
155
1.41
154
151
126
0.99
059
153
124
1.40
0.68
3.98
233
diy wt
0.03
0.05
0.09
0.06
0.06
0.04
0.02
0.14
0.10
038
0.16
1.05*
0.48
0.96
-021
-123
0.02
0.02
0.07
0.02
0.05
-0.10
0.03
2.81
250
.._
2.00
2.45
2.74
175
3.65
320
0.16
0.13
-.—
0.13
0.14
0.13
0.14
0.15
0.14
058
0.72
.._
0.71
0.73
034
1.68
0.84
1.15
0.03
0.01
-.—
0.03
0.03
0.01
0.02
0.04
0.03
036*
0.05
.._
0.46*
-0.46
-0.45
0.45
0.02
0.02
-.—
0.01
-0.01
0.00
0.00
A-16
-------
Audit Sample*
Lab
A
SD
Bs
SD
Bw
SD
C
SD
Total Nitrogen % dry wt
1
2
3
4
ALL
0.18
0.16
-.—
.._
0.17
0.05
0.01
..—
..—
0.04
0.01
0.01
-.—
-.—
0.18
0.12
0.12
0.12
0.13
0.02
0.01
0.01
0.01
0.02
0.05*
0.01
0.01
0.01
0.13 0.03
0.11 0.00
0.11 0.01
0.13 0.01
0.12 0.02
0.00
0.01
0.01
0.01
0.00
0.00
..—
0.00
0.00
0.00
0.00
-.—
0.00
0.00
0.00
0.00
.._
0.00
{SBRP}
1
2
3
ALL
0.15
0.15
0.17
0.16
0.02
0.01
0.02
0.02
0.00
0.00
0.01
0.14 0.04
0.11 0.01
-.— -.—
0.12 0.03
0.01
-0.01
-.-
0.11
0.10
0.12
0.11
0.02
0.01
0.01
0.02
0.00
-0.01
0.01
0.02
0.00
0.01
0.01
0.00
0.00
0.00
0.01
0.01
0.00
0.00
{NE}
1 0.0240.01 0.003
2 0.0300.00 0.003
3 .._ .._
4 .._ .._
ALL 0.0270.01
{SBRP}
1 0.0230.001 -0.002
2 0.0270.002 0.002
3 0.0230.002 -0.002
ALL 0.0250.002
Total Sulfur % dry vrt
0.0300.00 0.012
0.0190.00 0.001
0.0170.01 0.001
0.0120.01 0.006
0.0180.01
0.0150.002 -0.002
0.0180.001 0.001
0.0170.001
0.020 0.01 0.001
0.0170.01 0.002
0.020 0.00 0.001
0.0210.00 0.002
0.0190.01
0.0200.001 0.001
0.0200.000 0.001
0.0180.002 -0.001
0.0190.001
0.0020.00
0.0060.00
0.0020.00
0.0010.00
0.001
0.005
0.001
0.0000.004 -0.004
0.0030.001 -0.001
0.0050.002 0.001
0.0040.002
SD is standard deviation; d is difference from the interlaboratoiy mean.
Relative difference greater than 5 percent
Not analyzed by laboratory.
A-17
-------
APPENDIX B
PREPARATION OF
LIQUID AUDIT SAMPLES
B-l
-------
B-2
-------
A liquid synthetic audit sample and a liquid extract from an audit soil sample were prepared
for the DDRP U.S./Canadian Soil Characterization Comparison study. These samples were
included with the other soil audit samples distributed to all laboratories participating in this study.
The purpose of the liquid audit samples was to provide some assessment of the extraction versus
measurement error. Individual sample volumes were 125 mL, and the samples were contained in
amber plastic seal-capped bottles.
Preparation of the liquid synthetic audit samples was performed accordingly:
1. The audit sample was designed to contain specified concentrations of calcium (Ca),
magnesium (Mg), potassium (K), and sodium (Na) in neutral (pH 7.0) NH4OAc.
2. Concentrations specified are: 2.0 mg/L Ca, 1.0 mg/L Mg, 0.80 mg/L K, and 0.50 mg/L Na.
3. These ions were added to an ammonium acetate solution.
4. The detection limits for Ca, Mg, K, and Na in ammonium acetate are 0.05 mg/L.
5. Volume of the final bulk solution was 3.0 liters, and two 3.0 liter samples were prepared,
one for each batch shipment.
6. The analyte concentrations in each 3.0 liter bulk sample were analytically verified prior to
subsampling and shipment to the participating laboratories.
7. The subsamples consisted of 125 mL portions of the 3.0 liter bulk solution, and were placed
in 125 mL amber plastic bottles.
Preparation of the natural liquid audit sample by extracting an existing soil audit sample was
performed according to the summary below.
1. The sample was extracted with neutral (pH 7.0) ammonium acetate. A bulk soil sample
weighing 160 grams was extracted with 4.0 liters of NH4OAc, i.e., a 1:25 extraction ratio.
2. Since high clay content soils retain proportionally more extracting solution, the above sample
weight to volume ratio of 160g soil to 4.0 L NH4OAc was suggested merely to ensure a final
extraction solution volume of at least 3.0 L.
3. The extract was agitated for 8 hours, let stand overnight, decanted, and filtered until clear.
4. The final bulk extract was analyzed for Ca, Mg, K, and Na, subsampled and prepared for
shipment.
5. The subsamples consisted of 125 mL portions of the bulk extract, and were placed in 125
mL amber plastic bottles.
Analytical results for four subsamples of the synthetic and natural liquid audits are listed
below. The calcium concentration for the synthetic liquid audit is higher than would be expected
from preparation. This higher concentration is due to contamination during preparation, but does
not effect the utility and quality of the audit.
Sample Sodium Calcium Magnesium Potassium
Synthetic
Average 0.503 mg/L 2.275 mg/L 1.025 mg/L 0.768 mg/L
Std. Deviation 0.0098 0.0092 0.0104 0.0029
Natural
Average 0.571 mg/L 1.433 mg/L 0.376 mg/L 1.274 mg/L
Std. Deviation 0.0055 0.0131 0.0052 0.0053
B-3
-------
APPENDIX C
COMPARISON STUDY
WORKSHOP
C-l
-------
C-2
-------
TABLE Cl. AGENDA FOR THE COMPARISON WORKSHOP
8:00 Registration, coffee, and get acquainted
8:30 Welcome and introductions: G. Pearson and G. Byers
8:45 Description of DDRP comparison study
Objectives of the study: C. Palmer
Study procedures
Selection of laboratories: L. Fenstermaker
Reporting and collection of data: K. Lauckner
Evaluation of data: T. Starks
Objectives of the workshop:, C. Palmer
9:15 Statements by the participating laboratories (5 minutes each)
• Description of laboratories and comments on the study
10:45 Presentation/evaluation of study results and discussion of comparability by
parameter: C. Palmer
SoilpH
Soil texture
Cation exchange capacity and basic cations
soil audits
liquid audits
Total C, N, and S
Extractable Fe, Al, and exchangeable acidity
Extractable sulfate and isotherm
1:00 Continuation of presentation and discussion of study results
3:15 Continuation of presentation and discussion of study results
4:30 Description of the DDRP QA program: L. Blume
QA requirements of EPA
What is the Direct/Delayed Response Project (DDRP)
Overview of DDRP QA program
Data verification process
Data quality assessment
Lessons learned
5:00 Summary of the workshop: R. Holdren
C-3
-------
TABLE C2. LIST OF WORKSHOP ATTENDEES
UNITED STATES
NORTH CENTRAL REGION
Dr. Thomas Fenton
105 Agronomy Laboratory
Iowa State University
Ames, IA 50011
515-294-2414
Jeff Phillips
Soil Testing Laboratory
Agronomy Department, Purdue Univ.
West Lafayette, IN 47905
317-494-8080
WESTERN REGION
Andy Bristol
Agronomy & Horticulture
Dept. 3Q, Box 30003
New Mexico State University
Las Cruces, NM 88003-0003
505-646-1139
Karl Topper
Soil, Plant, and Water Analysis
Utah State University
Logan, UT 84322-4830
801-750-2217
CANADA
WESTERN REGION
Dr. Douglas G. Maynard
Canadian Forestry Service
Northern Forestry Centre
5320 - 122nd Street
Edmonton, Alberta T6H 3S5
Canada 403-435-7210
Gerry Lutwick
Alberta Environment, Earth Sciences Div.
3rd Floor, Cousins Building
Lethbridge, Alberta T1H 4V4
Canada 403-381-5322
Dr. Salim Abboud
Alberta Research Council
Terrain Sciences Department
Box 8330-Postal Station F
Edmonton, Alberta T6H 5X2
Canada 403-450-5470
NORTHEAST REGION
Dr. Edward Ciolkosz
Department of Agronomy
119 Tyson Building
Pennsylvania State University
University Park, PA 16802
814-865-1530
SOUTHERN REGION
Frank Sodek m
Soil Characterization Laboratory
G-159 McCarty Hall
University of Florida
Gainesville, FL 32611
904-392-1951
EASTERN REGION
Earl Gagnon
Dept of Land Resource Science
University of Guelph
Guelph, Ontario NIG 2W1
Canada 519-824-4120, ext. 2494
C-4
-------
TABLE C2. LIST OF WORKSHOP ATTENDEES CONT.
CONTRACT LABORATORIES
Dale Raines 303-278-4455
Huffman Laboratories
4630 Indiana Street
Golden, CO 80403
U.S. ENVIRONMENTAL PROTECTION AGENCY
Environmental Monitoring Systems Labs
P. O. Box 93478
Las Vegas, NV 89193-3478
Louis Blume 702-798-2213
BobSchonbrod 702-798-2229
Kevin Shields 402-476-2811
Harris Laboratories
624 Peach Street
Lincoln, NE 68502
Dr. Jeff Lee 503-757-4666
Environmental Research Lab
200 SW 35th Street
Corvallis,OR 97333
U.S. EPA CONTRACTORS/COOPERATQRS
ENVIRONMENTAL RESEARCH CENTER
University of Nevada at Las Vegas
4505 Maryland Parkway
Las Vegas, NV 89154
Dr. Craig Palmer
Lynn Fenstermaker
Marie Schnell
Kathy Lauckner
Dr. Tom Starks
702-739-0849
702-739-3742
702-798-2285
702-739-3742
702-739-0826
LOCKHEED ESC
1050 E. Flamingo Road, Suite 301
Las Vegas, NV 89119
Dr. Jerry Byers 702-734-3327
Rob Tidwell 702-734-3232
Tun Lewis 702-798-2676
Judy Burton 702-734-3294
Joan Bartz 702-734-3326
ENVIRONMENTAL RESEARCH LABORATORY
Northrop Services, Inc.
200 SW 35th Street
Corvallis,OR 97333
Dr. Rich Holdren
Paul Shaffer
Mark Johnson
Jeffrey Kern
503-757-4666, exL 352
503-757-4666, ext 350
503-757-4666, tost. 362
503-757-4666, exL 303
C-5
-------
APPENDIX D
COMPARISON STUDY
RESULTS
D-l
-------
D-2
-------
AUDIT
SOIL X
{A} 1.926
{
2.301
2.210
1.940
2.500
2.310
2.250
2.150
2.010
1.800
1.970
2.060
2.150
s) 2.315
3.215
2.820
4.050
2.830
2.660
3.090
2.560
2.850
2.860
3.210
2.740
2.600
{Bw} 1.938
2.881
2.410
2.670
2.690
2.590
2.770
2.350
2.350
2.340
2.480
2.420
2.380
1.926
2
2
2
2,
2,
2.
2.
2.
1.
2.
2.
2.
301
020
240
450
120
150
040
190
940
090
250
360
2.315
3
2
2,
2,
2,
2.
2.
2.
2.
2.
3.
0.
215
710
670
600
780
880
990
020
420
630
140
140
1.938
2
2
2
0
2,
2,
2,
2.
2.
2.
2.
,881
,310
990
190
230
560
350
540
010
370
330
4.900
LAB
*
*
a
b
c
d
e
9
j
k
1
P
r
*
*
a
b
c
d
e
9
j
k
1
P
r
*
*
a
b
c
d
e
g
j
k
1
P
r
MOISTURE
(by wt %)
AUDIT
SOIL X
{C} 0.110
{
0.200
0.080
0.100
0.160
0.500
0.110
0.120
0.190
0.170
0.130
B} 4.252
5.826
4.970
5.590
0.730
5.130
5.600
5.150
5.190
4.650
4.980
4.970
5.100
{0} 4.786
12.361
6.440
8.440
11.370
9.320
8.340
8.230
10.100
8.060
10.870
10.590
9.780
0.110
0.200
0.090
0.200
0.190
0.400
0,190
0.140
0.170
140
000
252
826
070
470
470
050
490
150
390
880
870
110
220
786
12.361
6.980
8.710
11.340
9.410
7.870
8.580
10.390
7.590
9.830
10.400
2.550
LAB
*
*
a
b
d
e
j
k
1
P
r
*
*
a
b
c
d
e
?
j
k
1
P
r
a
b
c
d
e
9
j
k
1
P
r
D-3
-------
Moisture
A
3.CM
2.5-
2.0-
1.5-
1.0-
1.0
D .P
1
32k
N 11
Mean 2.145
Sa 0.130
Median 2.115
1.5
2.0
weight %
2.5
3.0
-------
Moisture
Bs
9
en
4.5-f
3.5-
2.5-
1.5-
4 P
1.5
Lab r not shown
2.5 3.5
weight %
a
N 11
Mean 1.693
Sd 0.498
Median 2.765
4.5
-------
Moisture
Bw
4.0
3.0
C7>
'(U
2.0
1.0-
1.0
2.0 . 3.0
weight %
N 11
Mean 2.465
Sd OJ22
Median 2.410
I
4.0
Lab c not shown
-------
0.60-
0.50-
0.40-
* 0.30-
!c
en
£ 0.20-
0.10-
0.00-
-.10-
Moisture
C
•^
A /
N 9
Mean 0.671
Sd 1.464
MedUn 0.155
.10 0.00 0.10 0.20 0.30 0.40 0.50 0.60
weight %
Lab r not shown
-------
e.o-r
Moisture
B
5.0-
4.0-
3.0-
3.0
4.0
weight
5.0
N 11
Mean 4.829
Sd 0.764
Median 5.040
T
6.0
-------
15-
Moisture
0
5-
0-
N 11
Mean 8.872
Sd 1.646
Median 8J75
I
0
I
5
I
10
weight
15
Lab o not shown
-------
Air-Dry Moisture
wt %
Table 1a. Summary Statistics for Tim*
Effect
Table 1b. Analyala of Variance for Time Effact
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs
26
28
2
2
14
22
1
1
16
12
1
1
14
10
1
1
Mean
1.8309
1.8540
2.1150
2.0900
£7393
2.7280
2.8200
4.0500
2.0949
2.3018
2.4100
2.6700
0.1276
0.1582
0.0800
0.1000
Standard
deviation
0.1175
0.2505
0.1344
0.2121
0.2777
0.5358
p
•
0.2352
0.1471
t
•
0.0409
0.0239
f
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 34
Lab 1
Time 1
Lab'time 1
Error 26
Lab 1
Time 1
Labnime 1
Error 22
Sum of
squares
0.0097
0.1643
0.0025
2.1030
0.7016
0.9295
0.7279
7.0300
0.1016
0.2176
0.0013
1.0680
0.0012
0.0052
0.0001
0.0269
Mean
square
0.0097
0.1643
0.0025
0.0389
0.7016
0.9295
0.7279
0.2068
0.1016
0.2176
0.0013
0.0411
0.0012
0.0052
0.0001
0.0012
F
0.25
4.22
0.06
3.39
4.50
3.52
2.47
5.30
0.03
0.96
4.21
0.04
Pr> F
o - .05
0.6202
0.0448
0.8004
0.0742
0.0414
0.0692
0.1280
0.0296
0.8592
0.3367
0.0523
0.8385
Tabla 2a. Analyala of Varlanca for Homoganalty of
Laboratorlaa
Audit Sum of Mean Pr > F
samples Source df squares square F o - .05
A Lab 11 1.6816 0.1529 4.27 00001*
Error 74 2.6471 0.0356
Bs Lab 12 1.9262 0.1605 0.97 0.4914
Error 48 7.9592 0.1656
Bw Lab 12 1.1380 0.0948 2.79 00086*
Error 36 1.2248 0.0340
C Lab 12 0.1596 0.0133 10.66 OjOOOl*
Error 36 0.0449 0.0012
Tabla 2b. Palrwlae Comparlaon for Significant Difference Between DORP and Non-Contract Laboratorlaa
Bs
Bw
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
2 and a -0.1588 -0.3418 -0.5248
4 and a -0.1620 -0.3450 -0.5280
3 and a -0.1586 -0.3470 -0.5354
land a -0.1919 -0.5530 -0.3724
' .05 level of significance; Tukey'e Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistic* for DDRP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean Sd
NC 8 2.1550 0.1664
DORP 3 1.8685 0.0566
NC 0 2.8222 0.2167
DDRP 4 £6354 03623
NC 9 2.4856 0.1609
DDRP 4 22115 0.0881
NC 9 0.1744 0.1352
DORP 4 0.1484 0.0141
SE
0.0555
0.0327
0.0722
0.1311
0.0536
0.0440
0.0451
0.0070
Min
1.8700
1.8208
2.5600
22477
2.3400
2.0949
0.0000
0.1276
Max
2.4750
1.9309
32100
2.8268
2.7700
2.3018
0.5000
0.1582
Wlthln-Group and Between-Oroup Varlabllltlee for ODRP
•nd Non-Contract Laboratories
Pr>F*
F df a - .05 Variances |T|
8.65 (8.2) 0.2153 Equal 2.8466
1.47 (3.8) 0.5907 Equal 1.3515
3.34 (8.3) 0.3504 Equal 3.1513
9222 (8.3) 0.0034* Unequal 0.5701
df
10.0
11.0
11.0
8.4
Pr>|T|
a- .05
0.0174*
02037
0.0092*
0.5836
* If Pr > F Is less than 0.05. there Is a significant difference within groups.
* If Pr > |T| Is less than 0.05, there is a significant difference between
groups.
-------
D-12
-------
SPECIFIC SURFACE
AUDIT
SOIL^ X Y LAB
(A) 42.630 40.020 a
| 42.680 20.360 b
{Bs} 30.380 28.410 a
| 19.030 21.640 b
{Bw} 35.790 36.210 a
| 23.040 22.840 b
{C} 0.230 2.140 a
| -0.360 -0.910 b
{B} 49.350 48.840 a
I 30.160 23.180 b
D-13
-------
D-14
-------
TOTAL SAND
AUDIT
SOIL X
(A) 47.275
60.175
52.800
64.100
53.600
60.100
51.100
49.000
52.700
57.500
51.200
54.200
{Bs} 73.725
92.325
86.600
85.200
84.400
85.100
82.800
72.000
83.000
82.300
78.100
77.800
{Bw} 15.200
36.050
21.300
31.900
29.800
30.600
23.200
24.000
24.200
26.600
24.000
27.500
LAB
47.275
60.175
54.100
60.600
56.700
59.400
50.800
50.000
53.000 -
54.600
52.300
53.800
73.725
92.325
84.300
84.100
86.200
85.000
81.500
73.000
84.100
82.700
78.800
79.900
15.200
36.050
21.600
31.000
33.900
31.900
23.800
26.000
24.400
29.300
24.800
25.000
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL X
{C} 92.550
(I
100.800
94.500
97.300
98.000
96.000
93.000
95.000
97.000
99.000
98.000
96.200
J} 32.375
57.125
47.200
58.900
50.900
52.500
42.400
43.000
45.300
45.300
44.300
44.900
92.550
100.800
93.700
98.200
99.600
96.900
93.000
95.000
94.900
94.800
98.000
97.900
32.375
57.125
45.100
53.000
53.600
51.900
42.300
44.000
43.800
43.900
43.600
44.900
LAB
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
D-15
-------
Total Sand
A
a
»-»
ON
65-T
60-
55-
0)
50-
45-
45
N 10
Mean S4.580
Sd 3.961
Median 53.725
50
55
weight %
60
65
-------
Total Sand
Bs
95-
90-
85 H
(D
80-
75-
70-
h
70 75 80 85
weight x
N 10
Mean UJMS
Sd 4.141
Median 83.025
90
95
-------
Total Sand
Bw
a
55
45
35-
15-
5-
15
25
weight %
N 10
Mean 26.740
Sd 3.701
Median 25.625
35
45
-------
Total Sand
C
105-T
100-
>
95-
90-
90
95
100
N 10
Mean 96.300
Sd 1.818
Median 96.675
105
weight
-------
Total Sand
B
to
o
60-1
55-
50-
40-
35-
30-
30 35
a
N 10
Mean 47.040
Sd 4.652
Median 44.730
I
40 45 50
weight %
55 60
-------
Tab)* 1c. Summary Statistic* lor Tim*
Effect
Audit Number Standard
samples Lab of labs Mean deviation
Total Sand
wt %
Tabl* 1b. Analy*!* of Variance for Tim* Effect
A
BS
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
54.1692
59.2071
53.4500
62.3500
85.0071
84.4636
85.4500
84.6500
24.0688
33.0417
21.4500
31.4500
94.9000
96.4800
94.1000
97.7500
3.3056
1.0331
0.9192
2.4749
1.4568
1.4956
1.6264
0.7778
0.4909
2.6851
0.2121
0.6364
1.2070
1.8146
0.5657
0.6364
Audit
samples
A
Bs
Bw
C
Source
Lab
Time
Lab'time
Error
Lab
Time
Lab'time
Error
Lab
Time
LabMime
Error
Lab
Time
Lab*time
Error
df
1
1
1
54
1
1
1
36
1
1
1
28
1
1
1
24
Sum of
squares
Mean
square
180.8506 160.8506
5.4683
13.8857
308.9640
1.6161
0.3545
0.0589
77.8102
5.4683
13.8857
5.7216
1.6161
0.3545
0.0589
2.1614
314.1570 314.1570
15.4714
0.9206
83.3735
23.3500
0.1886
3.6578
49.3010
15.4714
0.9206
2.9776
23.3500
0.1886
3.6578
2.0542
F
31.61
0.96
2.43
0.75
0.16
0.03
105.51
5.20
0.31
11.37
0.09
1.78
Pr > F
a = .05
0.0001*
0.3326
0.1251
0.3929
0.6879
0.8698
0.0001*
0.0305*
0.5826
0.0025*
0.7645
0.1946
Tabl* 2a. Analy*)* of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 10 605.8909 60.5891 13.94 00001*
Error 73 317.3390 4.3471
Bs Lab 11 418.4215 38.0383 22.30 00001*
Error 56 95.5185 1.7057
Bw Lab 11 733.3081 66.6644 16.14 00001*
Error 44 181.7569 4.1308
Lab 11 73.9910 6.7265 3.81 00007*
Error 44 77.6433 1.7646
Table 2fa. Palrwlee Comparison for Significant Difference Between DORP end Non-Contract Laboratories
Bs
Bw
Upper Lower
Labs limit Difference limit
2 and I 14.218 7.457 0.696
2ande 15.018 8.257 1.496
2 and h 16.468 9.707 2.946
Labs
1
1
1
3
3
3
4
4
4
2
2
2
and
and
and
and
and
and
and
and
and
and
and
and
m
I
h
m
1
h
m
1
h
m
1
h
Upper
limit
10.746
11.146
17.096
10.840
11.240
17.190
10.352
10.752
16.702
10.097
10.497
16.447
Difference
6.157
6.557
12.507
5.883
6.283
12.233
5.650
6.050
12.000
5.614
6.014
11.964
Lower
limit
1.568
1.968
7.918
0.927
1.327
7.277
0.948
1.348
7298
1.130
1.530
7.480
2
2
2
2
1
1
Labs
andh
and 1
andj
and e
and c
and d
Upper
limit
15.348"
15.948
16.048
16.848
•0.606
-0.006
Difference
8.042
8.642
8.742
9.542
-7.781
-7.181
Lower Upper Lower
limit Labs limit Difference limit
0.735
1.335
1.435
2.235
-14.956
-14.356
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistics for DDRP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean Sd SE
NC 8 53.7500 3.2519 1.1497
DORP 3 56.3421 2.5893 1.4949
NC 8 81.0438 4.2816 1.5138
DORP 4 84.6760 0.2510 0.1255
NC 8 26.8125 3.2309 1.1423
DDRP 4 27.9443 3.8938 1.9469
NC 8 96.3938 1.8015 0.6369
DORP 4 95.4342 0.8034 0.4017
Min
49.5000
54.1692
72.5000
84.4636
23.5000
24.0688
93.0000
94.7167
Max
59.7500
59.2071
85.3000
85.0071
31.8500
33.0417
98.8000
96.4800
Wlthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
Pr > F'
F df a - .05 Variances |T| df
1.58 (7.2) 0.8832 Equal -1.2284 9.0
290.97 (7.3) 0.0006* Unequal -2.3913 7.1
1.45 (3.7) 0.6144 Equal -0.5368 10.0
5.03 (7.3) 0.2121 Equal 0.9980 10.0
Pr> |T|
a = .05
0.2504
0.0477*
0.6032
0.3418
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| is less than 0.05. there is a significant difference between
groups.
-------
VERY COARSE SAND
AUDIT
SOIL X
{A} 0.340
1.660
1.100
1.500
1.100
1.830
0.600
1.700
0.200
0.960
0.800
{Bs} 3.325
14.425
8.200
5.800
11.300
11.130
11.500
12.300
6.500
5.840
8.100
5.700
(Bw> 0.661
5.072
2.400
1.600
3.000
3.850
1.610
6.500
3.400
2.140
2.800
LAB
3.100
0.340
1.660
0.900
1.100
0.800
1.530
0.400
1.000 .
0.500
0.860
1.900
3.325
14.425
9.100
6.100
17.000
11.600
8.260
9.300
11.300
4.790
9.600
8.500
0.661
5.072
1.500
1.800
3.000
4.130
2.550
2.900
3.700
3.330
3.300
1.600
*
*
a
b
c
d
e
h
j
k
1
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL X
{C} 2.125
12.775
6.700
4.900
4.900
15.100
6.790
6.000
7.000
10.790
8.900
7.200
(B) 2.200
8.950
6.800
3.900
4.700
7.600
3.880
6.800
7.200
4.910
7.400
3.900
4,
5,
2.125
12.775
.200
.100
17.600
11.570
6.710
13.200
5.600
3.810
10.800
8.000
2.200
8.950
,700
,900
.500
.500
.080
.900
.500
.390
.400
4.300
LAB
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
D-23
-------
3.0
Very Coarse Sand
A
2.0-
0.0-
-1.0-
-1.0
N 9
MCM 1.043
Sd 0.428
Median 1.000
0.0
1.0
weight %
2.0
3.0
-------
Very Coarse Sand
Bs
184
a
fe
14-
•& 10-1
6-
2-
i
10
N 10
Mean 9.096
Sd 2.639
Median
14
18
weight
-------
8-f
Very Coarse Sand
Bw
si
cr>
2-
0-
-2-
-2
0
i
2
i
4
h •
N 10
Mean 1910
Sd 0.956
Median 1867
6
i
8
weight %
-------
Very Coarse Sand
C
18-
16-
14-
12-
.c
a>
8-
6-
4-
2-
0-
0
I
2
N 10
Mean 6242
Sd 2.688
Median 7.450
I ' I ' I ' I
6 8 10 12
i
14 16 18
weight
-------
10-f
Very Coarse Sand
B
8-
6-
D
JZ
en
'(D
4-
ck
2-
0-
0
4
^T
weight
N 10
Mean 5.563
Sd 1.229
Median 5^75
8
10
-------
Very Coarse Sand
wt %
Table 1a. Summary Statistic* for Tim*
Effect
Audit Number Standard
samples Lab of labs Mean deviation
Table 1b. Analyal* of Variance for Time Effect
o
to
A
Bs
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
0.8077
0.9607
1.0000
1.3000
9.6000
8.3000
8.6500
5.9500
2.8813
2.9000
1.9500
1.7000
4.7429
4.5300
5.4500
5.0000
0.2096
0.2132
0.1414
0.2828
1.6605
2.0036
0.6364
0.2121
0.3834
0.9352
0.6364
0.1414
1.1230
2.0155
1.7678
0.1414
Audit
samples
A
Bs
Source df
Lab 1
Time 1
Lab'time 1
Error 54
Lab 1
Time 1
Lab*time 1
Sum of
squares
0.1911
0.2631
0.0201
2.4252
14.3256
9.7503
1.7549
Error 36 129.7500
Bw
C
Lab 1
Time 1
Lab'time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
0.0467
3.9641
0.0630
12.2494
0.3751
1.1829
0.0480
56.1003
Mean
square
0.1911
0.2631
0.0201
0.0449
14.3256
9.7503
1.7549
3.6042
0.0467
3.9641
0.0630
0.4375
0.3751
1.1829
0.0480
2.3375
F
4.25
5.86
0.45
3.97
2.71
0.49
0.11
9.06
0.14
0.16
0.51
0.02
Pr > F
a = .05
0.0440
0.0189*
0.5062
0.0538
0.1087
0.4898
0.7464
0.0055*
0.7071
0.6923
0.4837
0.8872
Table 2a. Analyale of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 10 5.0310 0.5031 6.07 04001*
Error 73 6.0502 0.0829
Bs Lab 11 189.6636 17.2421 4.20 00)02*
Error 56 229.8338 4.1042
Bw Lab 11 11.5586 1.0508 1.81 0.0805*
Error 44 25.4901 0.5793
C Lab 11 339.1101 30.8282 6.60 00301*
Error 44 205.5741 4.6721
Table 2b. Palrwlse Comparison for Significant Difference Between DORP and Non-Contract Laboratories
Bs
Bw
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Labs
Upper Lower
limit Difference limit
4 and c -0.4060 -7.7000 -14.994
4
1
2
3
3
and
and
and
and
and
d
d
d
d
c
-0.2540
-0.9010
-0.9240
-2.2780
-0.1930
-8.1350
-8.5920
-8.8050
-10.5850
-8.5000
-16.0160
-16.2830
-16.6860
-18.8920
-16.8070
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistics for DORP and Non-Contract Laboratories
O
&
o
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group
NC
DDRP
NC
DORP
NC
DDRP
NC
DDRP
of labs Mean
8 0.9113
3 0.9728
8 9.5450
4 7.8833
8 3.1819
4 Z8745
8 8.9981
4 4.3057
Sd
0.5302
0.1715
2.6986
1.3742
0.8660
0.0287
2.4536
1.0741
SE
0.1874
0.0990
0.9541
0.6871
0.3062
0.0143
0.8675
0.5371
Min
0.2000
0.8077
5.3150
6.4500
2.0800
2.8333
6.3000
2.7500
Max
1.6800
1.1500
14.1500
9.6000
4.7000
2.9000
13.3350
5.2000
Wlthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
F
9.56
3.86
911.40
5.22
df
(7.2)
(7.3)
(7.3)
(7.3)
Pr > F*
a - .05
0.1959
0.2948
0.0001*
0.2024*
Variances |T|
Equal -0.1916
Equal 1.1402
Unequal 1.0029
Equal 3.5883
df
9.0
10.0
7.0
10.0
Pr > |T|
a *> .05
0.8523
0.2808
0.3492
0.0049*
' If Pr > F is less than 0.05. there is a significant difference within groups.
" If Pr > |T| is less than 0.05. there is a significant difference between
groups.
-------
COARSE SAND
AUDIT
SOIL
LAB
{A} 2.086
3.661
3.000
3.000
2.600
8.530
2.180
6.600
2.400
3.620
2.600
2.800
{ s) 12.415
26.515
24.400
15.500
26.000
27.330
19.530
20.700
17.400
20.270
17.200
14.000
{Bw} 2.765
5.015
3.900
3.100
4.500
5.250
4.050
4.600
4.500
4.530
3.600
4.100
2.086
3.661
2.900
3.300
2.900
9.630
2.120
5.500
2.900
2.730
3.000
2.400
12.415
26.515
17.600
12.900
23.600
25.500
20.130
17.500
20.200
21.720
15.400
17.800
2.765
5.015
3.800
3.400
4.200
5.300
4.110
3.100
4.200
3.330
3.600
3.100
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL X
(C) 9.438
27.813
16.400
17.800
15.500
27.670
15.160
18.600
17.600
30.830
15.800
16.400
{B} 5.760
8.790
7.700
7.300
7.400
11.700
8.280
6.500
7.100
7.980
7.600
6.500
9.438
27.813
13.100
14.700
29.300
29.930
17.890
26.700
16.300
18.790
22.500
19.800
5.760
8.790
7
6,
6,
9,
7.
6.
7.
7.
7.
200
400
800
870
440
900
100
890
400
6.200
LAB
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
J
k
1
m
D-31
-------
«*»
K>
5-
Coarse Sand
A
i
3
weight %
N 10
Mean 3.736
Sd 2.161
Median 2.875
I
Labs d and h not shown
-------
Coarse Sand
Bs
Ui
U)
30-r
25-
20-
(D
15-
10-
10
I
15
i
20
N 10
Mean 19.734
Sd 3^28
Median 19.465
25
30
weight %
-------
Coarse Sand
Bw
o
U)
' 7
5
'» 4-1
"a)
2
1
4
5
N 10
Memo 4.014
Sd OA59
Median 1890
6
7
weight
-------
40-f
Coarse Sand
C
30-
>
20-
10
0-
0
I
10
1
20
N 10
MCM 20.039
Sd 4.ai
McdUn 1&&2S
30
40
weight
-------
Coarse Sand
B
s
ON
12-
10-
01 8-
6-
4-
6
8
weight %
N 10
Mean 7.563
Sd 1.237
Median 7J75
10
12
-------
o
i>
Table 1a. Summary Statistics for Time
Effect
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs Mean
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
3.1231
3.1107
2.9500
3.1500
19.2357
17.5591
21.0000
14.2000
4.2563
3.6917
3.8500
3.2500
15.1286
14.0800
14.7500
16.2500
Standard
deviation
0.2930
0.2250
0.0707
0.2121
2.9705
2.4736
4.8083
1.8385
0.2503
0.4833
0.0707
0.2121
2.2710
3.3462
2.3335
2.1920
Coarse Sand
wt %
Table 1b. Analytic of Variance lor Tlm« Effect
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab'tlme 1
Error 36
Lab 1
Time 1
Lab'time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
Sum of
squares
0.0328
0.0167
0.0420
3.5630
64.3336
2.2772
23.5020
269.7053
1.1836
0.6275
0.0011
3.5585
0.1740
2.7386
5.5447
178.0746
Mean
square
0.0328
0.0167
0.0420
0.0660
64.3336
2.2772
23.5020
7.4918
1.1836
0.6275
0.0011
0.1271
0.1740
2.7396
5.5447
7.4198
F
0.50
0.25
0.64
8.59
6.30
3.14
9.31
4.94
0.01
0.02
0.37
0.75
Pr > F
a = .05
0.4840
0.6173
0.4285
0.0058*
0.5848
0.0850
0.0049*
0.0345*
0.9267
0.8796
0.5491
0.3959
Table 2a. Analytic of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a •> .05
A Lab 10 90.3957 9.0396 82.37 00001*
Error 73 8.0108 0.1097
Bs Lab 11 291.5814 26.5074 3.98 00003*
Error 56 372.5464 6.6526
Bw Lab 11 7.1802 0.6527 3.92 00006*
Error 44 7.3300 0.1666
C Lab 11 885.2104 80.4737 7.17 00001*
Error 44 493.7496 11.2216
Table 2b. Palrwlee Comparison for Significant Difference Between DDRP and Non-Contract Laboratories
Labs
1
1
2
2
3
3
and
and
and
and
and
and
d
h
d
h
d
h
Upper
limit
-4.8799
-1.8499
-4.8950
-1.8650
-4.9705
-1.9405
A'
Difference
-5.9569
-2.9269
•5.9693
-2.9393
-6.0800
-3.0500
Bs Bw
Lower Upper Lower Upper Lower
limit Labs limit Difference limit Labs limit Difference limit
-7.0339 2andd -0.0010 -8.8560 -17.7110 2 and d -0.1160 -1.5830 -3.0510
-4.0039 4 and d -0.0380 -9.3250 -18.6120
-7.0435
-4.0135
-7.1895
-4.1595
Labs
4
1
2
3
3
and
and
and
and
and
d
d
d
d
k
Upper
limit
-1.3970
-1.7520
-2.5070
-4.9260
-0.9360
C
Difference
-13.6100
-13.6710
-14.7200
-17.8000
-13.8100
Lower
limit
-25.6230
-25.5900
-26.9330
-30.6740
-26.6840
' .05 level of significance; Tukey'e Studentized Range Test; DDRP labs - 1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistics for DORP and Non-Contract Laboratories
d
fe
Audit
samples
A
Bo
Bw
C
Table 3b.
Audit
samples
Group
NC
DDRP
NC
ODRP
NC
DORP
NC
DORP
Number
of labs Mean
8
3
8
4
8
4
8
4
3.9069
3.0779
20.2675
18.0754
4.1294
4.0703
21.1731
13.8496
Sd
2.4151
0.0678
3.7300
0.9488
0.5465
0.3111
4.2772
1.9669
SE
0.8539
0.0391
1.3187
0.4744
0.1932
0.1556
1.5122
0.9834
Min
2.1500
3.0000
15.9000
17.0900
3.6000
3.6917
16.5250
11.0000
Max
9.0800
3.1231
26.4150
19.2357
5.2750
4.3833
28.8000
15.1900
Wlthln-Group and Between-Group Varlabllltlee for DDRP
and Non-Contract Laboratories
F
A 1269.85
Bs 15.46
Bw 3.09
C 4.73
df
(7.2)
(7.3)
(7.3)
(7.3)
Pr > F*
a - .05
0.0016*
0.0462*
0.3836
0.2292
Variances |T|
Unequal 0.9698
Unequal 1.5642
Equal 0.1977
Equal 3.2001
df
7.0
8.6
10.0
10.0
Pr > |T|
a - .05
0.3643
0.1539
0.8473
0.0095*
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| is less than 0.05, there is a significant difference between
groups.
-------
MEDIUM SAND
AUDIT
SOIL
LAB
AUDIT
SOIL
LAB
{A} 5.118
10.533
7.500
8.300
8.300
5.600
6.550
9.300
7.800
6.540
8.900
8.100
(Bs) 17.695
32.920
27.800
25.800
27.200
17.570
25.270
18.800
28.600
22.030
27.900
24.400
{Bw} 2.790
4.410
3.200
3.600
4.500
1.800
3.880
2.700
3.800
3.060
3.900
3.900
5.118
10.533
7.500
8.600
7.000
5.630
6.740
8.100
8.500
6.040
9.700
7.900
17.695
32.920
26.600
23.700
26.100
17.800
25.860
18.700
27.300
22.220
26.500
25.700
2.790
4.410
3.400
3.500
2.800
1.870
3.760
2.200
3.800
3.460
3.900
3.700
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
{C> 21.455
42.575
30.000
31.300
35.200
22.570
31.640
23.900
34.400
28.170
36.700
32.000
{B} 4.860
9.990
7.800
8.400
8.900
4.030
7.530
5.500
7.100
5.820
7.700
7.400
21.455
42.575
29.700
34.200
37.100
24.400
30.920
24.300
34.000
26.150
35.800
34.800
4.860
9.990
7.100
7.000
9.000
4.030
7.530
6.100
7.700
5.860
7.400
7.300
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
D-39
-------
Medium Sand
A
12-
10-
8-
6-
4-
2-
"T"
4
8
N 10
Mean 7.630
Sd 1.148
Medium 7.825
I
10
r
12
weight
-------
Medium Sand
Bs
35-
30-
20-
15-
10
14.293
Sd 3.610
Median 25.306
15 20
25
weight %
30 35
-------
Medium Sand
Bw
5-f
a
V
K>
4-
cr>
2-
1 -
N 10
Mean 3.337
Sd 0.681
Median 3.600
2 3
weight
-------
Medium Sand
C
2
45-f
40-
35-
30-
25-
20-
15-
15 20
i
25
30 35
weight %
N 10
Mun 30.861
Sd 4.633
Median 32.015
I
I
40 45
-------
12-f
Medium Sand
B
10
8-
6-
4-
D
2-
N 10
Mean 6.960
Sd 1.37J
Median 7.425
6 8
weight %
i
10
i
12
-------
d
.u
in
Table 1a. Summary Statistics for Time
Effect
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs Mean
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
8.0462
8.3571
7.5000
8.4500
26.2857
25.7045
27.2000
24.7500
3.4750
3.5167
3.3000
3.5500
31.3786
30.0400
29.8500
32.7500
Standard
deviation
0.5171
0.3096
0.0000
0.2121
0.6608
1.1412
0.8485
1.4849
0.0856
0.1851
0.1414
0.0707
1.8158
1.8488
0.2121
2.0506
Medium Sand
wt %
Table 1b. Analysis
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab'time 1
Error 54
Lab 1
Time 1
Lab'tlme 1
Error 36
Lab 1
Time 1
Lab'time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
of Variance for Time Effect
Sum of
squares
1.4803
0.1913
0.3801
9.3182
8.2265
0.0015
3.1270
35.9517
0.0742
0.0175
0.0379
0.5117
2.0813
1.1915
15.3364
77.8776
Mean
square
1.4803
0.1913
0.3801
0.1726
8.2265
0.0015
3.1270
0.9987
0.0742
0.0175
0.0379
0.0183
2.0813
1.1915
15.3364
3.2449
F
8.58
1.11
2.20
8.24
0.00
3.13
4.06
0.96
2.07
0.64
0.37
4.73
Pr > F
a = .05
0.0050*
0.2971
0.1436
0.0068*
0.9698
0.0853
0.0535
0.3360
0.1610
0.4311
0.5502
0.0398*
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a •» .05
A Lab 10 30.1723 3.0172 14.33
Error 73 15.3703 0.2106
Bs Lab 11 360.1703 32.7428 39.76 OJOOOI*
Error 56 46.1196 0.8236
Bw Lab 11 10.0478 0.9134 9.01 00001*
Error 44 4.4630 0.1014
C Lab 11 427.7286 38.8844 11.39 0.0001*
Error 44 150.2008 3.4137
Table 2b. Palrwlse Comparison for Significant Difference Between DORP and Non-Contract Laboratories
Labs
3 and e
3 and k
3 andd
2 and e
2 and k
2 andd
1 andk
1 and d
Upper
limit
3.2700
3.6250
4.3000
3.2000
3.5550
4.2300
3.2480
3.9230
A*
Difference
1.7340
2.0890
2.7640
1.7120
2.0670
2.7420
1.7560
2.4310
Lower
limit
0.1970
0.5520
1.2270
0.2240
0.5790
1.2540
0.2640
0.9390
Labs
4 and k
4 and h
4 and d
3 and k
3 and h
3 andd
1 and k
1 and h
Upper
limit
9.3130
12.6880
13.7530
9.2860
12.6610
13.7260
7.3490
10.7240
BS
Difference
6.0450
9.4200
10.4850
5.8420
9.2170
10.2820
4.1610
7.5360
Lower
limit
2.7770
6.1520
7.2170
2.3970
5.7720
6.8370
0.9720
4.3470
Labs
4 and h
4 and d
3 and h
3 and d
2 and d
1 and d
Upper
limit
2.6910
3.3060
2.4570
3.0720
2.8270
2.7640
Bw
Difference
1.4670
2.0820
1.2330
1.8480
1.6820
1.6400
Lower
limit
0.2430
0.8580
0.0090
0.6240
0.5370
0.5160
Labs
4 and h
4 and d
3 and h
3 and d
1 and h
1 and d
Upper
limit
15.4060
16.0210
15.4840
16.0990
13.8520
14.4670
C
Difference
8.6700
9.2850
8.3830
6.9980
7.2790
7.8940
Lower
limit
1.9340
2.5490
1.2030
1.8960
0.7050
1.3200
(Continued)
-------
Table 2b. Continued
Bs
Upper Lower
Labs limit Difference limit
Labs
Upper . Lower
limit Difference limit
1 and d 11.7890
2 and k 6.6950
2andh 10.0700
2andd 11.1350
8.6010 5.4120
3.5800 0.4640
6.9550 3.8390
8.0200 4.9040
Bw
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
* .05 level of significance; Tukey's Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
Table 3a. Summary Statistics for DDRP and Non-Contract Laboratories
Audit Number
samples Group of labs Mean Sd
SE
Min
Max
0
-U
A
Bs
Bw
NC
DDRP
NC
DDRP
NC
DDRP
8
3
7.5438
8.2606
8 23.8719
4 27.0317
3.3144
3.6479
1.2597
0.1860
3.9141
1.2231
0.7673
0.2005
0.4454
0.1074
1.3839
0.6115
0.2713
0.1003
5.6150
8.0462
17.6850
25.7045
1.8350
3.4750
9.3000
8.3786
27.9500
28.1700
3.9000
3.9167
c
NC
DDRP
8
4
30.7531
31.6660
5.1894
1.2401
1.8347
0.6200
23.4850
30.0400
36.2500
32.7700
Table 3b. Wlthln-Group and Between-Group Variabilities for ODRP
and Non-Contract Laboratories
Audit
samples
df
Pr > F*
a - .05
Variances
|T|
Pr > |T|
df a - .05
A 45.85 (7.2)
Bs 10.24 (7.3)
Bw 14.65 (7.3)
C 17.51 (7.3)
0.0430*
0.0823
0.0499
0.0387*
Unequal -1.5647 7.7 0.1576
Equal -1.5437 10.0 0.1537
Unequal -1.1532 8.7 0.2797
Unequal -0.4724 8.4 0.6487
* If Pr > F is less than 0.05. there is a significant difference within groups.
* If Pr > |T| is less than 0.05. there is a significant difference between
groups.
-------
FINE SAND
AUDIT
SOIL X
(A) 19.921
27.573
22.300
25.300
24.000
24.530
23.880
23.300
23.300
28.200
15.400
23.200
{Bs} 19.410
24.390
20.300
27.500
16.600
22.570
21.230
20.800
23.200
26.890
15.700
25.000
(Bw) 2.175
6.825
3.100
4.500
5.200
5.600
4.710
4.000
3.900
5.180
2.500
4.500
Y
19.921
27.573
22.700
25.600
26.600
26.870
23.610
24.200
22.500
26.270
15.500
22.900
19.410
24.390
23.000
29.400
15.100
23.200
21.650
23.500
19.700
26.360
17.600
21.200
2.175
6.825
4.000
4.500
6.600
5.200
4.600
4.000
3.800
5.760
2.400
4.500
LAB
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL X
(C) 23.241
37.206
31.300
33.300
36.400
25.600
31.790
35.000
30.300
24.100
23.400
31.800
{B} 9.125
15.275
10.900
13.600
13.500
13.900
11.600
11.500
11.200
13.210
7.000
11.700
23.241
37.206
34.900
36.800
13.500
26.800
29.920
25.600
30.300
35.190
20.500
28.500
9.125
15.275
10.600
12.800
13.500
12.900
11.630
13.800
11.100
12.690
7.100
11.800
LAB
*
*
a
b
c
d
e
h
j
k
1
m
a
b
c
d
e
h
j
k
1
m
D-47
-------
Fine Sand
A
32-
28,
24-
JI
cn
"(D
20-
16-
12-
12 16 20 24
weight %
N 10
Mean 23308
Sd 3.203
Median 23.746
I
28
32
-------
16-
Fine Sand
Bs
32-r
28-
24-
20-
D
12-
N 10
Mean 22.025
Sd 3^32
Median 21.900
12 16
20 24
weight %
28 32
-------
Fine Sand
Bw
10
8
6
Ol
o
JZ
CT>
4
2
0
N 10
Mean 4.428
&J 1.02S
Median 4300
0
2
4
nr
6
8
-r
10
weight %
-------
Fine Sand
C
50 4
40-
•g, 30-1
20-
10-
10
20
N 10
MCM 29.250
Sd 3877
MedUn 30J25
30
weight
40
50
-------
Fine Sand
B
204
d
to
15-
C7»
10-
ad
5-
N 10
Mean 11.800
Sd 1.932
Median 12.200
I
5
10 15
weight %
20
-------
9
Ul
Table 1a. Summary Statistics for Time
Effect
Audit
samples
A
Be
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs Mean
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
21.5731
24.7679
22.5000
25.4500
22.0714
24.4727
21.6500
28.4500
3.5688
4.1833
3.5500
4.5000
32.4571
35.8700
33.1000
35.0500
Standard
deviation
1.7990
0.4603
0.2828
0.2121
2.4771
1.8665
1.9092
1.3435
0.1622
0.1851
0.6364
0.0000
2.0350
3.0019
2.S4S6
2.4749
Table 1b. Analysis
Audit
samples
A
Be
Bw
C
Source
Lab
Time
Lab*time
Error
Lab
Time
Lab*tlme
Error
Lab
Time
Lab*time
Error
Lab
Time
Lab*time
Error
df
1
1
1
54
1
1
1
Fine Sand
wt %
of Variance lor Tim* Effect
Sum of
squares
35.1510
2.4103
0.0558
86.7572
75.8037
11.3208
17.3237
36158.3822
1
1
1
26
1
1
1
2.1364
0.0775
0.0982
1.1760
24.5514
0.0268
1.6268
24 147.5403
Mean
square
35.1510
2.4103
0.0558
1.6066
75.8037
11.3208
17.3237
4.3995
2.1364
0.0775
0.0982
0.0420
24.5514
0.0268
1.8268
6.1475
F
21.88
1.50
0.03
17.23
2.57
3.94
50.86
1.84
2.34
3.99
0.00
0.30
Pr > F
a - .05
0.0001*
02260
0.8529
0.0002*
0.1174
0.0549
0.0001*
0.1853
0.1375
0.0571
0.9479
0.5907
Table 2a. Analyal* of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F o - .05
A Lab 10 324.7174 32.4717 23.41 00001*
Error 73 101.2475 1.3870
Bs Lab 11 299.2689 27.2063 5.25 00301*
Error 56 290.3153 5.1842
Bw Lab 11 29.3446 2.6677 6.12 00001*
Error 44 19.1920 0.4362
C Lab 11 741.6738 67.4249 4.98 04001*
Error 44 596.2821 13.5519
Table 2b. Palrwlee Comparleon for Significant Difference Between DORP and Non-Contract Laboratories
Labs
2 and I
3 and I
1 and k
1 and d
1 and I
Upper
limit
13.1370
12.7730
-1.8330
-0.2980
9.9520
A'
Difference
9.3180
6.8290
-5.6620
-4.1270
6.1230
Lower
limit
5.4990
4.8840
-9.4910
-7.9560
2.2940
Labs
2 and I
2 andc
4 and c
Upper
limit
15.6390
16.4390
16.6680
Bs
Difference
7.8230
8.6230
8.4700
Lower
limit
0.0060
0.8060
0.2720
Bw C
Upper Lower Upper Lower
Labs limit Difference limit Labs limit Difference limit
4 and I 5.1050 2.5670 0.0290 3 and 1 29.864015.7170 1.5690
2 and 1 27.342013.9200 0.4980
* .05 level of significance; Tukey's Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistics lor DDRP and Non-Contract Laboratories
O
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
"If Pr >
"If Pr >
Number
Group of labs Mean Sd SE Min
NC 8 23.3913 3.5340 1.2495 15.4500
DORP 3 23.5398 1.7207 0.9935 21.5731
NC 8 21.2688 3.5090 1.2406 15.8500
OORP 4 23.6410 1.0985 0.5492 22.0714
NC 8 4.5281 1.1086 0.3920 2.4500
DDRP 4 4.2214 0.5974 0.2987 3.5688
NC 8 28.0438 3.2774 1.1587 21.9500
DDRP 4 34.6685 2.5349 1.2674 32.4571
Wlthln-Group and Between-Group Variabilities for DDRP
and Non-Contract Laboratories
Pr > F' Pr > |T|
F df a - .05 Variances |T| df a - .05
4.22 (7.2) 0.4100 Equal -0.0681 9.0 0.9472
10.20 (7.3) 0.0827 Equal -1.2927 10.0 0.2252
3.44 (7.3) 0.3376 Equal 0.5093 10.0 0.6216
, 1.67 (7.3) 0.7276 Equal -3.5198 10.0 0.0055*
F is less than 0.05. there is a significant difference within groups.
|T| is less than 0.05. there Is a significant difference between
Max
27.2350
24.7679
26.6250
24.4727
5.9000
5.0167
30.8550
37.6667
groups.
-------
VERY FINE SAND
AUDIT
SOIL X
{A} 15.370
21.880
18.800
26.100
17.700
19.630
17.890
13.100
18.800
18.190
22.500
20.100
{Bs} 4.758
8.806
5.800
10.600
3.400
6.530
5.260
5.700
7.300
7.280
8.200
8.700
{Bw} 2.645
19.745
8.700
19.200
11.900
14.100
8.910
6.400
8.600
11.740
10.400
11.900
15.370
21.880
20.000
21.900
19.400
15.740
17.970
14.200
18.600
18.710
22.000
20.100
4.758
8.806
7.900
12.000
4.
6.
5.
7.
5.
7.
9.
6.
2.
.400
.900
.600
,100
.600
.630
.600
.800
.645
19.745
8.900
17.900
17.100
15.430
8.810
8.700
8.900
11.540
11.100
12.100
LAB
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL
LAB
(C) 6.126
9.773
10.000
10.100
5.900
5.030
7.620
10.800
7.600
4.110
10.800
8.800
(B) 7.700
20.900
13.900
25.700
16.500
15.300
11.100
9.700
12.800
13.380
13.800
15.400
6.126
9.773
11.800
7.300
2.100
4.570
7.540
5.400
8.600
10.860
8.100
6.800
7.700
20.900
14.400
21.000
19.800
18.700
11.600
11.700
12.400
13.030
15.100
15.300
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
D-55
-------
Very Fine Sand
A
28-T
Ul
o\
24-
20-
16-
12-
a
8-
8 12
\
16
\
20
N 10
Mean 19.072
Sd 2.768
Median 18.625
T
24 28
weight
-------
14-f
Very Fine Sand
Bs
12-
10-
.. Q
SI
en
6-
4-
2-
0-
0 2
a
6 8
weight %
N 10
Mean 7.115
&J 1.968
Median 6.781
I
10 12 14
-------
Very Fine Sand
Bw
o
oo
24-
20-
16-
12-
8-
4-
0-
i ^ r
0 4
i
8
12 16
weight %
N 10
Mean 11.617
Sd 3.456
Median 11.195
T
20
24
-------
Very Fine Sand
C
16-f
14
12
10
cn
6
4
2-
0-
0
m
6 810
weight %
N 10
Mun 7.692
Sd 2.022
Median 7.950
T
12 14 16
-------
Very Fine Sand
B
25 4
20,
cr>
15-
10-
5-
i • i
10 15
N 10
Mean 15.031
Sd 3.735
Median 14.300
20 25
weight %
-------
Very Fine Sand
wt %
Table 1a. Summary Statistic* for Tim*
Effect
Table 1b. Analyst* of Variance for Tim* Effect
o
o\
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number Standard
of labs Mean deviation
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
20.6231
22.0321
19.4000
24.0000
7.8143
8.4318
6.8500
11.3000
9.9000
18.7417
8.8000
18.5500
11.1786
11.7400
10.9000
8.7000
1.5591
0.9436
0.8485
2.9699
1.3688
1.2711
1.4849
0.9900
0.3670
2.4707
0.1414
0.9192
2.0633
2.6056
1.2728
1.9799
Audit
samples
A
Bs
Bw
C
Source
Lab
Time
Lab* time
Error
Lab
Time
Lab'time
Error
Lab
Time
Lab*time
Error
Lab
Time
Lab'time
Error
df
1
1
1
54
1
1
1
36
Sum of
squares
33.6154
0.5164
9.4790
94.3472
22.9925
3.2455
13.1507
61.4699
1 301.6582
1
1
28
1
1
1
24
1.4561
0.7201
70.0342
2.2920
9.4013
6.5096
121.9876
Mean
square
33.6154
0.5164
9.4790
1.7472
22.9925
3.2455
13.1507
1.7075
301.6582
1.4561
0.7201
2.5012
2.2920
9.4013
6.5096
5.0828
F
19.24
0.30
5.43
13.47
1.90
7.70
120.60
0.58
0.29
0.45
1.85
1.28
Pr > F
a - .05
0.0001*
0.5889
0.0236*
0.0008*
0.1765
0.0087*
0.0001*
0.4519
0.5958
0.5083
0.1865
0.2690
Tabl* 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 10 254.7958 25.4796 18.28 00001*
Error 73 101.7417 1.3937
Bs Lab 11 67.7828 6.1621 3.78 OXM04*
Error 56 91.1797 1.6282
Bw Lab 11 720.7016 65.5183 28.82 00)01*
Error 44 100.0403 2.2736
C Lab 11 228.3856 20.7623 3.80 00007*
Error 44 240.3466 5.4624
Table 2b. Palrwlee Comparison for Significant Difference Between DORP and Non-Contract Laboratories
2
2
2
1
3
Labs
and
and
and
and
and
e
d
h
h
h
Upper
limit
7.9310
8.1760
12.2110
10.8110
9.1540
A*
Difference
4.1020
4.3470
8.3820
6.9730
5.2000
Bs
Lower Upper Lower
limit Labs limit Difference limit
0.2740 2 and c 8.9120 4.5320 0.1510
0.5190
4.5540
3.1350
1.2460
2
2
2
2
2
2
Labs
and
and
and
and
and
and
m
k
1
e
i
h
Upper
limit
12.1620
12.5220
13.4120
15.3020
15.4120
16.6120
Bw
Difference
6.7420
7.1020
7.9920
9.8820
9.9920
11.1920
C
Lower Upper Lower
limit Labs limit Difference limit
1.3210
1.6810
2.5710
4.4610
4.5710
5.7710
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs • 1 to 4; NC labs • c to r.
-------
Table 3a. Summary Statistics for DORP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean Sd SE
NC 8 18.4144 2.4237 0.8569
DDRP 3 20.5017 1.5945 0.9208
NC 8 6.6250 1.5153 0.5357
DDRP 4 8.0382 0.4807 0.2403
NC 8 11.1019 2.6554 0.9388
DDRP 4 13.1438 3.9425 1.9712
NC 8 7.1644 1.8228 0.6445
DDRP 4 10.8896 0.8200 0.4100
Min
13.6500
18.8500
3.9000
7.4667
7.5500
9.9000
4.0000
9.7900
Max
22.2500
22.0321
8.9000
8.4400
14.7650
18.7417
9.4500
11.7400
Wlthln-Group and Between-Group Variabilities for DDRP
and Non-Contract Laboratories
Pr > F*
F df a - .05 Variances |T| df
2.31 (7.2) 0.6701 Equal -1.3608 9.0
9.94 (7.3) 0.0858 Equal -1.7822 10.0
2.20 (3.7) 0.3507 Equal -1.0762 10.0
4.94 (7.3) 0.2169 Equal -3.8264 10.0
Pr > |T|
a - .05
0.2067
0.1050
0.3071
0.0033*
* If Pr > F is less than 0.05. there is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there is a significant difference between
groups.
-------
TOTAL SILT
AUDIT
SOIL X
.{A} 21.000
33.900
28.400
18.900
27.900
24.100
29.200
29.000
29.400
21.500
28.200
24.600
(Bs) 10.275
{
17.625
11.500
14.300
11.300
13.200
14.800
20.000
16.700
12.700
13.900
16.100
Jw) 56.125
73.525
70.500
60.900
67.000
64.500
63.900
61.000
67.900
59.900
66.600
65.000
LAB
21.000
33.900
27.300
20.600
26.200
24.900
28.400
29.000
28.500
22.600
28.600
24.700
10.275
17.625
14.100
12.800
10.400
13.500
14.800
20.000
14.100
13.200
14.800
15.100
56.125
73.525
70.300
61.000
63.100
64.700
63.500
61.000
68.000
55.900
65.700
68.600
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL X
{C} -0.850
6.200
4.700
2.300
1.200
3.500
6.800
2.000
3.200
1.000
1.300
3.700
.{B} 35.000
55.250
48.500
37.200
43.900
44.800
49.500
45.000
51.700
44.200
45.800
29.900
-0.850
6.
5,
0,
200
800
900
0.400
2.
6.
3.
4.
4.
1.
2.
.700
.700
.000
.700
.000
.900
.000
35.000
55.250
50.100
42.400
41.200
45.700
49.400
45.000
51.300
45.800
48.100
30.300
LAB
*
*
a
b
c
d
e
h
j
k
1
m
*'
*
a
b
c
d
e
h
j
k
1
m
D-63
-------
Total Silt
A
d
4
40-r
35-
30-
cr>
*a>
25-
20-
15-
I
15
20
25 30
weight %
N 10
Mean 26.100
Sd 3.240
Median 27.450
35
r
40
-------
Total Silt
Bs
o
o\
20-f
15-
10-
5-
10
15
N 10
MUD 14.365
Sd 2.428
Median 13.950
T
20
weight
-------
Total Silt
Bw
80-
75-
70-
60-
55-
50-
N 10
Meia 64.450
Sd 3.713
Mcdua 64A2S
50 55
60 65 70
weight %
75 80
-------
Total Silt
C
a
CA
-4
10-
8
6-
2
0
-4-
T ' I ' ^ ' I ' I
-4-20 2 4
N 10
Me«n 3.090
Sd 1.802
Median 2.675
8 10
weight
-------
Total Silt
B
60 4
50
30
20-1^
20
m
N 10
Mean 44.490
Sd 6.118
Median 45.125
—r
60
40
50
weight %
-------
Total Silt
wt %
TabU 1a. Summary Statistics for Tim*
Effect
Table 1b. Analysis of Variance for Time Effect
d
Ax
o
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs Mean
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
27.6115
22.6464
27.8500
19.7500
13.7357
13.7364
12.8000
13.5500
68.6625
59.3417
70.4000
60.9500
4.8929
2.6100
5.2500
1.6000
Standard
deviation
4.4185
2.0835
0.7778
1.2021
1.7332
1.6817
1.8385
1.0607
0.6551
2.5536
0.1414
0.0707
1.1777
1.7419
0.7778
0.9900
Audit
samples
A
Bs
Bw
C
Source
Lab
Time
Lab'timo
Error
Lab
Time
Lab'time
Error
Lab
Time
Lab*time
Error
Lab
Time
LabMime
Error
df
1
1
1
54
1
1
1
36
1
1
1
28
1
1
1
24
Sum of
squares
Mu an
square
158.9098 158.9098
6.5769
9.1489
607.3262
0.5045
1.1273
0.5028
102.9481
6.5769
9.1489
11.2468
0.5045
1.1273
0.5028
2.8597
307.5004307.5004
9.7698
0.0146
78.1917
30.0478
0.3638
1.5956
46.9233
9.7698
0.0146
2.7926
30.0478
0.3638
1.5956
1.9551
F
14.13
0.58
0.81
0.18
6.39
0.18
110.11
3.50
0.01
15.37
0.19
0.82
FT > F
a = .05
0.0004*
0.4478
0.3711
0.6770
0.5341
0.6775
0.0001*
0.0719
0.9429
0.0006*
0.6700
0.3753
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Ft > F
samples Source df squares square F a - .05
A Lab 10 476.5248 47.6525 5.66 00001*
Error 73 614.2733 8.4147
Bs Lab 11 112.8473 10.2588 4.69 00001*
Error 56 122.5974 2.1892
Bw Lab 11 771.5798 70.143619.56 00001*
Error 44 157.7700 3.5857
C Lab 11 98.4589 8.9508 5.21 00001*
Error 44 75.5266 1.7165
Table 2b. Palrwlse Comparison for Significant Difference Between DORP and Non-Contract Laboratories
A* Bs
Upper Lower Upper Lower
Labs limit Difference limit Labs limit Difference limit
3 and h -0.051 -5.667 -11.282
2 and h -1.184 -6.264 -11.343
1 and h -1.065 -6.264 -11.463
Labs
1 and h
1 and k
4 and k
3andk
2 and j
2 and m
2 and 1
Upper
limit
14.347
17.447
15.461
15.277
-1.801
-0.651
-0.001
Bw
C
Lower Upper Lower
Difference limit Labs limit Difference limit
7.662
10.762
8.183
8.000
-8.608
-7.458
-6.808
0.978
4.078
0.906
0.723
-15.416
-14.266
-13.616
* .05 level of significance; Tukey's Studentized Range Test; DORP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistic* for DDRP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group
NC
DDRP
NC
DDRP
NC
DDRP
NC
DDRP
of labs Mean
8 26.6750
3 25.5908
8 14.6625
4 14.1439
8 64.1438
4 64.9969
8 3.0063
4 4.1424
Sd
2.6305
2.6082
2.6517
0.5035
3.2877
3.9755
1.7847
1.1962
SE
0.9300
1.5059
0.9375
0.2518
1.1624
1.9878
0.6310
0.5981
Min
22.0500
22.6464
10.8500
13.7357
57.9000
59.3417
0.8000
2.6100
Max
29.0000
27.6115
20.0000
14.7700
67.9500
68.6625
6.7500
5.2667
Wlthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
F
1.02
27.73
1.46
2.23
df
(7.2)
(7.3)
(3.7)
(7.3)
Pr > F"
o - .05
1.0000
0.0199*
0.6096
0.5485
Variances |T|
Equal 0.6100
Unequal 0.5343
Equal -0.3971
Equal -1.1378
df
9.0
7.9
10.0
10.0
Pr>|T|
o - .05
0.5570
0.6078
0.6996
0.2817
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there is a significant difference between
groups.
-------
COARSE SILT
AUDIT
SOIL X Y LAB
(A)
(Bs)
{Bw>
(C)
{8}
{0}
13.
6.
12.
12.
7.
9.
11.
10.
36.
31.
34.
32.
4.
2.
1.
1.
24.
18.
25.
22.
8.
700
400
600
800
700
800
500
000
900
500
000
400
400
300
900
200
600
900
200
200
100
12
7
12
13
9
10
9
11
36
32
34
33
5
0
4
1
27
23
26
24
33
.200
.900
.700
.900
.400
.100
.900
.700
.800
.600
.100
.200
.300
.700
.200
.400
.400
.300
.300
.700
.900
a
b
j
1
a
b
j
1
a
b
j
1
a
b
j
1
a
b
j
1
j
D-71
-------
D-72
-------
CLAY
AUDIT
SOIL X
(A) 14.150.
24.500
18.900
17.000
18.500
15.800
19.700
22.000
18.000
21.000
20.600
21.200
{Bs} -2.300
9.100
1.900
0.500
4.200
1.700
2.400
8.000
0.200
5.000
8.000
6.100
(Bw) -0.775
16.775
8.200
7.200
3.800
4.900
12.900
15.000
8.000
13.500
9.400
7.500
Y
14.150
24.500
18.700
18.800
17.100
15.700
20.800
21.000
18.600
22.900
19.100
21.500
-2.300
9.100
1.600
3.000
3.300
1.500
3.700
7.000
1.700
4.000
6.400
5.000
-0.775
16.775
8.200
8.000
3.000
3.400
12.700
13.000
7.600
14.800
9.500
6.400
LA
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
*
*
a
b
c
d
e
h
j
k
1
m
AUDIT
SOIL X
(C) -0.175
1.025
0.400
0.500
0.200
3.000
0.700
0.100
{B} -2.450
15.850
4.300
4.000
5.200
2.700
8.100
12.000
3.000
10.500
9.900
25.200
Y
-0.175
1.025
0.900
0.400
0.300
2.000
0.100
0.100
-2.450
15.850
4.800
4.600
5.200
2.400
8.300
11.000
4.900
10.300
8.300
24.800
LAB
*
b
d
e
h
1
m
*
*
a
b
c
d
e
h
j
k
1
m
D-73
-------
Total Clay
A
28-r
24-
20-
(U
16-
12-
12
16
20
weight
N 10
Mean 19.345
Sd 1.961
MedUn 19J25
r
24
28
-------
Total Clay
Bs
10-
5-
0-
Q
N 10
Mean 1760
Sd 2.374
Medun 3.400
-5
0
weight
10
15
-------
Total Clay
Bw
25-f
20-
15-
> 10-1
5-
0-
\ ' I
-5 0
\
5
I
10
N 10
Mean 8.850
Sd 3.787
Median 8.000
I
15 20 25
weight
-------
C7»
3.5-f
2.5-
1.5-
0.5-
-0.5-
-1.5-
Total Clay
C
D
-2.5-
1 i ' i r i
2.5 -1.5 -0.5 0.5
weight
N 6
Mean 0.72S
Sd 0.889
Median 0.425
I ' I
1.5 2.5 3.5
-------
Total Clay
B
30
25
20
K 15
10-
5
0-
-5-
-5 0
i
5
10 15
weight %
m
N 10
Mean 8.47S
Sd 6.S4S
Median 6.100
I
20 25 30
-------
Table 1a. Summery Statistics for Tim*
Effect Table 1b. Analyst*
Audit Number
samples Lab of labs Mean
A 1
2
a
b
Bs 1
2
a
b
Bw 1
2
a
b
C 1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
Table 2b. Palrwlse
182115
18.1393
18.8000
17.9000
1.2429
1.7955
1.7500
1.7500
7.2625
7.6417
8.2000
7.6000
0.1929
0.9000
0.4000
0.6500
Standard Audit
deviation
1.3417
1.8908
0.1414
1.2728
0.7460
0.8577
02121
1.7678
0.5726
1.1517
0.0000
0.5657
0.1385
0.8165
0.5657
0.3536
samples Source df
A Lab 1
Time 1
Lab*time 1
Total Clay
wt %
Table 2a. Analysis of Variance for Homogeneity of
of Variance for Time Effect Laboratories
Sum of
squares
0.8800
0.1135
0.6379
Error 54 143.1733
Bs Lab 1
Time 1
Lab'time 1
Error 36
Bw Lab 1
Time 1
Lab'time 1
Error 28
C Lab 1
Time 1
Lab'time 1
Error 24
0.2734
0.1908
0.2734
25.8538
0.0426
0.7004
0.8367
19.8267
0.7821
0.0016
0.1784
6.6943
Mean Pr > F Audit
Sum of
square F a = .05 samples Source df squares
0.8800 0.33 0.5669
0.1135 0.04 0.8369
0.6379 0.24 0.6258
2.6514
0.2734 0.38 0.5411
0.1908 0.27 0.6094
0.2734 0.38 0.5411
0.7182
0.0426 0.06 0.8081
0.7004 0.99 0.3285
0.8367 1.18 0.2863
0.7081
0.7821 2.80 0.1070
0.0016 0.01 0.9409
0.1784 0.64 0.4317
0.2789
A Lab
Error
Bs Lab
Error
Bw Lab
Error
C Lab
Error
10 95.0487
73 150.6069
11 195.2891
56 29.3278
Mean
square
9.5049
2.0631
17.7536
0.5237
11 325.7113 29.6101
44 36.9200
11 13.3431
44 14.4653
0.8391
1.2130
0.3288
Pr > F
F a = .05
4.61 00001*
33.90 0X5001*
35.29 00001*
3.69 00309*
Comparison for Significant Difference Between DORP and Non-Contract Laboratories
A*
Upper
Labs limit
Difference
Lower
limit
Labs
2andh
2 and 1
2 and m
2andk
1 andh
1 and I
1 and m
1 and k
3 andh
3 and I
Bs
Upper
Lower
limit Difference limit
-3.220 -5.705
-2.920 -5.405
-1.270 -3.755
-0.220 -2.705
-3.714 -6.257
-3.414 -5.957
-1.764 -4.307
-0.714 -3.257
-3.803 -6.550
-3.503 -6.250
-8.189
-7.889
-6.239
-5.189
-8.800
-8.500
-6.850
-5.800
-9.297
-8.997
Bw
Upper
Labs limit Difference
3 and k -2.496 -6.017
3 and h -2.346 -5.867
3 and e -1.146 -4.667
3 and d 7.504 3.983
3 and c 8.254 4.733
2 and k -3.215 -6.508
2 and h -3.065 -6.358
2 and e -1.865 -5.158
2 and d 6.785 3.492
2 and c 7.535 4.242
Lower
limit
-9.537
-9.387
-8.187
0.463
1.213
-9.801
-9.651
-8.451
0.199
0.949
Upper
Labs limit
1 and h -0.267
3 and h -0.296
C
Lower
Difference limit
-2.307
-2.500
-4.347
-4.704
(Continued)
-------
Table 2b. Continued
Bs
Bw
Labs
Upper Lower
limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
3 and m -1.853 -4.600
3 and k -0.803 -3.550
3 and c -0.053 -2.800
4 and h -4.184 -6.790
4 and I -3.884 -6.490
4 and m -2.234 -4.840
4 and k -1.184 -3.790
4 and c -0.434 -3.040
1 .05 level
Table 3a.
Audit
camples
A
Bs
Bw
C
-7.347
-6.297
-5.547
-9.396
-9.096
-7.446
-6.396
-5.646
1andk -3.654 -6.888 -10.121
1 and h -3.504 -6.738 -9.971
1 and e -2.304 -5.538 -8.771
1 and c 7.096 3.862 0.629
4 and k -5.430 -8.950 -12.470
4 and h -5.280 -8.800 -12.320
4 and e -4.080 -7.600 -11.120
4 and I -0.730 -4.250 -7.770
of significance; Tuke/s Studentlzed Range Test; DDRP labs - 1 to 4; NC labs - c to r.
Summary Statistic* for DORP and Non-Contract Laboratories
Group
NC
DDRP
NC
DDRP
NC
DDRP
NC
DDRP
Number
of labs
8
3
8
4
6
4
8
4
Mean
19.5938
18.0598
4.2625
1.1746
9.0875
7.0594
0.6188
0.4407
Sd
2.1525
0.2035
2.4089
0.4678
4.2532
1.2898
0.7750
0.4160
SE
0.7610
0.1175
0.8517
0.2339
1.5037
0.6449
0.2740
0.2080
Win
15.7500
17.8286
0.9500
0.7100
3.4000
5.2000
0.1000
0.0000
Max
21.9500
18.2115
7.5000
1.7955
14.1500
8.1333
2.5000
0.9000
Table 3b. Wlthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
F
111.90
26.52
10.87
3.47
Pr > F*
df 0 « .05
(7.2
(7.3
(7.3
(7.3
0.0178
0.0213*
0.0758
0.3344
Variances
Unequal
Unequal
Equal
Equal
m
1.9921
3.4963
0.9129
0.4230
df
7.3
8.0
10.0
10.0
Pr > |T|
a - .05
0.0850
0.0081*
0.3828
0.6812
* If Pr > F is less than 0.05. there is a significant difference within groups.
* If Pr > |T| is less than 0.05. there is a significant difference between
groups.
-------
AUDIT
SOIL
pH IN DEIONIZED WATER
;UDIT
LAB SOIL X
LAB
(A) 4.200
4.800
4.500
4.500
4.400
4.300
4.600
4.600
4.600
4.600
4.400
4.500
4.000
4.600
4.700
4.400
(Bs) 4.200
4.800
4.500
4.500
4.300
4.300
4.600
4.500
4.600
4.500
4.700
4.400
4.500
4.400
4.600
4.700
4.300
{Bw} 4.875
5.325
5.300
5.000
5.000
4.800
5.200
5.200
5.200
5.100
5.300
5.000
5.000
4.600
5.200
5.300
5.200
4.200
4.800
4.500
4.500
4.300
4.200
4.600
4.400
4.600
4.600
4.400
4.500
4.000
4.600
4.600
4.500
4.200
4.800
4.400
4.500
4.300
4.200
4.600
4.400
4.600
4.600
4.600
4.500
4.500
4.400
4.500
4.600
4.500
4.875
5.325
5.100
5.100
5.000
4.900
5.200
5.000
5.200
5.100
5.300
5.100
5.100
4.700
5.300
5.200
5.200
*
*
a
b
c
d
e
g
h
J
k
1
m
n
0
P
*
*
a
.b
c
d
e
g
h
1
j
k
1
m
n
0
P
*
*
a
b
c
d
e
g
h
1
j
k
1
m
n
0
P
{C} 5.125
5.875
5.200
5.400
5.200
5.300
5.900
5.700
5.600
5.300
5.500
5.600
5.500
4.900
5.500
5.500
5.700
{B} 4.675
5.125
5.100
4.900
4.700
4.800
5.000
4.900
5.000
4.800
5.000
4.800
4.900
4.400
5.000
5.000
4.900
{0} 3.850
4.450
4.200
4.200
4.200
4.100
4.200
4.200
4.000
4.100
4.100
4.100
3.900
3.700
4.200
4.000
4.100
5.125
5.875
5.100
5.500
5.200
5.400
5.700
5.600
5.600
5.400
5.500
5.500
5.300
5.000
5.500
5.500
5.600
4.675
5.125
4.800
4.900
4.700
4.300
5.000
4.900
4.900
4.900
5.000
5.400
4.900
4.400
5.000
5.000
4.900
3.850
4.450
4.200
4.200
4.200
3.900
4.200
4.100
4.000
4.000
4.100
4.300
4.000
3.600
4.100
4.400
4.000
*
*
a
b
c
d
e
g
h
i
j
k
1
m
n
0
P
*
*
a
b
c
d
e
g
h
1
j
k
1
m
n
o
P
*
*
a
b
c
d
e
g
h
i
j
k
1
m
n
0
P
D-81
-------
pH in Water
A
4.9-
4.7-
4.5-
c
D
I
a.
4.3-
4.1 -
3.9-
3
no
.9
i
4.1
N 14
Mean 4.464
Sd 0.174
Median 4JOO
4.3 4.5
pH units
4.7 4.9
-------
pH in Water
Bs
oo
U)
4.9-f
4.7-
4.5-
I
Q-
4.3-
4.1 -
4.1
4.3
15
4.487
0.119
Median 4.500
N
Mean
Sd
4.5
pH units
4.7
4.9
-------
pH in Water
Bw
5.5-
5.3-
5.1 H
c
D
I
a.
4.9-
4.7-
4.5-
m
N 15
Mcaa 5.098
Sd 0.171
Median 5.100
I ' I ' I ' I
4.5 4.7 4.9 5.1
5.3 5.5
pH units
-------
pH in Water
C
o
00
6.0-
5.8-
5.6-
cn
•4-J
"c
D
X
CL
5.4-
5.2^
5.0-
4.8-
m
a
N IS
Mean 5.440
Sit 0.218
Median 5-500
I ' I ' I ' I ' I
4.8 5.0 5.2 5.4 5.6
T
I
5.8 6.0
pH units
-------
pH in Water
B
o
fe
5.5-
5.3-
5.1-
§4.9J
'I
Q.
4.7-
4.5-
4.3-
4
m
.2 4.4
N 15
Mean 4.873
Sa 0.187
Median 4.900
I
4.6 4.8 5.0
pH units
5.2 5.4
-------
pH in Water
0
4.7-
4.5-
4.3
§4.H
I
CL
3.9-
3.7-
3.5-
m
3.5 3.7
3.9 4.1 4.3
pH units
N 15
Mean 4.067
Sd 0.149
Median 4.150
T
4.5 4.7
-------
Table 1a.
Audit
samples
A
Bs
Bw
C
Table
2b.
Labs
3
3
3
3
3
3
2
2
2
2
1
1
1
1
and
and
and
and
and
and
and
and
and
and
and
and
and
and
k
g
c
d
m
q
c
d
m
q
c
d
m
q
pH in Water
pH units
Summary Statistics for Time Table 2s. Analysis of Varlancs for Homogeneity of
Effect Table 1b. Analysis of Variance for Time Effect Laboratories
Number
Lab of labs Mean
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26 4.5115
28 4.5164
1 4.5000
1 4.5000
14 4.4600
22 4.5409
1 4.4000
1 4.5000
16 5.0513
12 5.1308
1 5.1000
1 5.1000
14 5.1800
10 5.5350
1 5.1000
1 5.5000
Standard Audit Sum of
deviation samples Source df squares
0.0451
0.02S7
0.0999
0.1388
0.0554
0.0268
0.2495
0.0746
Palrwlse Comparison for Significant
Upper
limit
02978
02978
0.3978
0.4978
0.6878
4.6978
0.3491
0.4491
0.6491
4.6491
0.3444
0.4444
0.6444
4.6444
A*
Difference
0.1629
0.1629
02629
0.3629
0.5629
4.5629
02164
0.3164
0.5164
4.5164
02115
0.3115
0.5115
4.5115
Lower
limit Labs
0.0279 2 and q
0.0279 3 and q
0.1279 4 and q
0.2279 1 and q
0.4279
4.4279
0.0838
0.1838
0.3838
4.3838
0.0787
0.1787
0.3787
4.3787
A Lab 1
Time 1
Labxtime 1
Error 52
Bs Lab 1
Time 1
Labxtime 1
Error 34
Bw Lab 1
Time 1
Labxtime 1
Error 26
C Lab 1
Time 1
Labxtime 1
Error 22
Difference Between
Bs
Upper
limit Difference
4.5409 4.9440
4.5017 4.9275
4.4960 4.9115
4.4800 4.8881
0.0000
0.0004
0.0000
0.0688
0.0122
0.0069
0.0007
0.5346
0.0030
0.0001
0.0030
0.0539
02556
0.0072
0.0014
0.8595
Mean Pr > F Audit
square F a - .05 samples Source df
0.0000 0.01 0.9260
0.0004 0.29 0.5957
0.0000 0.01 0.9260
0.0013
0.0122 0.78 0.3840
0.0069 0.44 0.5120
0.0007 0.05 0.6316
0.0157
0.0030 1.42 0.2434
0.0001 0.07 0.7803
0.0030 1.42 02434
0.0021
02556 6.54 0.0179*
0.0072 0.18 0.6720
0.0014 0.04 0.8520
0.0391
A Lab
Error
Bs Lab
Error
Bw Lqb
Error
C Lab
Error
16
65
17
48
17
36
17
36
Sum of Mean Pr > F
squares square F a - .05
20.6118 12682 982.04 04001*
0.0853 0.0013
20.2390 1.1905 103.97 00001*
0.5496 0.0115
25.9316 1.5254 747.30 00001*
0.0735 0.0020
28.8624 1.7625 65.51 OXJ001*
0.8686 0.0269
DDRP and Non-Contract Laboratories
Lower
limit
4.1378
4.0759
4.0645
4.0719
Bw
Upper
Labs limit Difference
3andd 0.2683 0.4513
3 and m 0.4683 0.6513
3andq 5.1683 5.3513
2andd 02308 0.4072
2 and m 0.4308 0.6072
2andq 5.1308 5.3072
4 and n -0.0303 -02133
4 and] -0.0303 -0.2133
4 and d 0.1867 0.3697
4 and m 0.3867 0.5697
4 and q 5.0867 5.2687
1 and n -0.0741 -02487
1 and j -0.0741 -0.2487
1 and m 0.3513 0.5258
1 and q 5.0513 5.2258
Lower
limit
0.0853
02853
4.9853
0.0545
0.2545
4.9545
-0.3863
•0.3963
0.0037
02037
4.8037
-0.4234
-0.4234
0.1766
4.8766
C
Upper Lower
Labs limit Difference limit
3 and
2 and
4 and
land
q 5.5683 6.2326 4.8039
q 5.5350 6.1802 4.8888
q 5.3390 5.9842 4.6938
q 5.1900 15.8268 4.5532
.05 level of significance; Tukey's Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3«. Summary Statistics for DORP and Non-Contract Laboratories
oo
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean
NC
DORP
NC
DORP
NC
DORP
NC
DORP
14
3
14
4
14
4
14
4
4.1286
4.5303
4.1643
4.5051
4.7357
5.1093
5.0571
5.4081
Sd
1.2016
0.0283
1.2049
0.0257
1.3726
0.0511
1.4669
0.1771
SE
0.3211
0.0164
0.3220
0.0128
0.3668
0.0255
0.3921
04886
Min
0.0000
4.5115
0.0000
4.4800
0.0000
5.0513
0.0000
5.1900
Max
4.6000
4.5629
4.6000
4.5409
5.3000
5.1683
5.7000
5.5683
Table 3b. Wlthln-Group and BetweeivOroup Variabilities for DORP and
Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
F
1789.75
2205.69
721.78
68.59
df
03.2)
(13,3)
(13.3)
(13.3)
Pr > F'
o - .05 Variances |T|
0.0011*
0.0000*
0.0001*
0.0051*
Unequal -12493
Unequal -1.0577
Unequal -1.0158
Unequal -0.8731
df
13.1
13.0
13.1
14.2
Pr>|T|
a - .05
02335
0.3094
0.3281
0.3971
• If Pr > F Is less than 0.05. there Is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there la a significant difference between
groups.
-------
D-90
-------
pH IN 0.002M CaCl.
AUDIT
SOIL X
{A} 4.063
4.437
4.300
4.200
4.300
4.200
{Bs} 4.075
4.225
4.100
4.000
4.100
4.100
{Bw} 4.488
4.863
4.700
4.600
4.800
4.700
4.
4.
4.
4.
4.
4.
063
437
300
200
300
100
4.075
4.225
200
100
200
200
488
863
500
700
800
4.700
LAB
a
b
e
k
a
b
e
k
*
*
a
b
e
k
AUDIT
SOIL X
{C} 4.600
5.350
5.000
4.900
5.400
4.900
{B} 4.350
4.650
4.500
4.400
4.500
4.400
4.400
{0} 3.600
3.900
3.700
3.700
3.800
3.700
3.800
4
5
4
5
5
5
4
4
4
4
4,
4,
4,
3.
3.
3.
3.
3.
3.
.600
.350
,700
,000
,200
100
350
650
500
400
500
400
700
600
900
700
800
800
700
3.900
LAB
*
*
a
b
e
k
*
*
a
b
e
i
k
*
*
a
b
e
i
.k
D-91
-------
pH in 0.002M Calcium Chloride
A
4.6-
4.5-
4.4-
4.3-
4.1 -
4.0-
3.9-
r ' i • i
3.9 4.0 4.1
4.2 4.3
pH units
N 4
Mean 4.238
Sd 0.075
Median 4.250
I
4.4 4.5 4.6
-------
4.4-f
pH in 0.002M Calcium Chloride
Bs
4.3-
-4.2-
c
D
I
O_
4.1 -
4.0-
3.9-
3
.9 4.0
I
4.1
4.2
pH units
N 5
Mean 4.120
Sd 0045
Median 4.130
4.3 4.4
-------
pH in 0.002M Calcium Chloride
Bw
d
fc
5.0
4.9
4.8
4.7-
4.5-
4.4-
4.3-
4.3 4.4
i • i • i
4.5 4.6 4.7
N 5
Me«n 4.680
Sd 0.076
Median 4.650
I ' I
4.8 4.9 5.0
pH units
-------
pH in 0.002M Calcium Chloride
C
5.5-f
5.3-
Cfl
-t-J
'c
D
CL
5.1 -
4.9-
4.7-
4.5-
i • i • i • I
4.5 4.7 4.9 5.1
N 5
Mean 3.000
Sd 0.177
Median 4.950
5.3 5.5
pH units
-------
pH in 0.002M Calcium Chloride
B
4.7-
VO
O\
4.6-
c
D
I
CL
4.5-
4.4-
4.3-
4
.3 4.4
4.5 4.6
pH units
N 5
Mean 4.4TO
Sd 0.067
Mediaa 4^00
4.8
-------
4.0-f
pH in 0.002M Calcium Chloride
0
3.9-
3.8-
X
Q.
3.7-
3.6-
3.5-
3.5 3.6
3.7 3.8
pH units
N S
Mean 3.760
Sd 0.065
Median 3.750
T
3.9 4.0
-------
pH In 0.002M CaCI,
Table 1a. Summary Statistic* for Tim*
Effect
Audit Number Standard
samples Lab of labs Mean deviation
Table 1b. Analysis of Variance for Time Effect
O
^
oo
A
Be
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
a
22
2
2
16
12
2
2
14
10
2
2
42289
42071
4.3000
42000
4.1700
4.1077
4.1500
4.0500
4.6750
4.7050
4.6000
4.6500
4.8879
4.9780
4.8500
4.9500
0.0324
0.0188
0.0000
0.0000
0.0384
0.0428
0.0707
0.0707
0.0889
0.0332
0.1414
0.0707
0.0817
0.0938
02121
0.0707
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab*time 1
Error 24
Sum of
squares
0.0138
0.0038
0.0057
0.0358
0.0236
0.0054
0.0013
0.0676
0.0056
0.0147
0.0003
0.1557
0.0309
0.0037
0.0001
0.2160
Mean
square
0.0138
0.0036
0.0057
0.0007
0.0236
0.0054
0.0013
0.0019
0.0056
0.0147
0.0003
0.0056
0.0309
0.0037
0.0001
0.0090
F
20.78
5.75
8.60
1Z56
2.88
0.66
1.00
2.65
0.06
3.43
0.41
0.01
Pr>F
a- .05
0.0001
0.0200*
0.0049
0.0011
0.0982
0.4154
0.3248
0.1146
0.8040
0.0764
0.5273
0.9243
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab S 0.1964 0.0383 18.91 04001*
Error 67 0.1391 0.0021
Bs Lab 6 0.0396 0.0066 4.04 00022*
Error 51 0.0834 0.0016
Bw Lab 6 0.0829 0.0138 3.26 OX>107*
Error 39 0.1651 0.0042
C Lab 7 4.4556 0.6365 87.90 OXXK>1*
Error 39 0.2824 0.0072
Table 2b. Palrwlee Comparison for Significant Difference Between ODRP and Non-Contract Laboratories
Bs
Bw
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Labs
Upper Lower
limit Difference limit
3andk 0-3074 0.1893 0.0712
3 and c 2.5388 2.1733
4 and e -0.0271 -0.2890
4 and c 2.3656 2.0110
2 and a -0.0601 -0.3220
2 and C 2.3326 1.9780
1 and e -0.1565 -0.4121
1 and c 2.2379 1.8879
1.8081
-0.5509
1.6564
•0.5839
1.6234
•0.6677
1.5379
* .05 level of significance; Tuke/s Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistic* for DORP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Group
NC
DORP
NC
ODRP
NC
DORP
NC
DORP
Number
of lab* Mean
3 4.2167
3 4.2584
3 4.1333
4 4.1426
3 4.7167
4 4.7268
4 4.5500
4 6.0125
Sd
0.0764
0.0709
0.0289
0.0261
0.0764
0.0464
1.0472
0.1192
SE
0.0441
0.0409
0.0167
0.0130
0.0441
0.0232
0.5236
0.0596
Min
4.1500
4.2071
4.1000
4.1077
4.6500
4.6750
3.0000
4.8879
Max
4.3000
4.3393
4.1500
4.1700
4.8000
4.7683
5.3000
5.1733
Wlthln-Qroup and Between-Group Variabllltlee lor DDRP
and Non-Contract Laboratoriee
F
1.16
1.23
2.71
77.24
df
(2.2)
(2.3)
(2.3)
(3.3)
Pr >F*
a- .05
0.9252
0.6161
0.4254
0.0049*
Variances |T|
Equal -0.6942
Equal -0.4456
Equal -0.2628
Unequal -0.8777
df
4.0
5.0
5.0
3.1
Pr>|T|
a - .05
0.5258
0.6745
0.8032
0.4435
' If Pr > F is less than 0.05. there is a significant difference within groups.
6 If Pr > |T| Is less than 0.05. there le a significant difference between
groups.
-------
D-100
-------
pH IN 0.01M CaCl.
AUDIT
SOIL
LAB
AUDIT
SOIL
LAB
{A} 3.800
4.250
4.200
4.000
4.000
3.700
3.900
4.100
4.100
3.900
4.000
3.700
4.100
4.100
4.100
4.000
(Bs) 3.775
4.225
4.100
3.900
3.900
3.900
3.900
3.900
3.900
4.100
4.000
4.000
3.700
4.100
4.100
4.000
4.000
{Bw} 4.175
4.925
4.700
4.500
4.600
4.400
4.500
4.600
4.500
4.700
4.500
4.500
4.300
4.700
4.700
4.700
4.400
3.800
4.250
4.100
4.000
4.000
3.800
4.000
4.000
4.100
4.000
4.100
3.900
4.100
4.000
4.100
3.900
3.775
4.225
4.100
3.900
3.900
3.900
3.900
3.900
3.900
4.100
4.100
4.000
3.900
4.000
4.100
4.100
4.000
4.1,75
4.925
4.700
4.500
4.600
4.500
4.400
4.600
4.500
4.700
4.600
4.600
4.400
4.700
4.500
5.700
4.400
*
*
a
b
c
d
e
g
j
k
1
m
n
0
P
q
*
*
a
b
c
d
e
9
i
j
k
1
m
n
0
P
q
*
*
a
b
c
d
e
9
i
j
k
1
m
n
0
P
q
{C} 4.675
5.125
4.900
4.800
4.800
4.900
5.000
4.900
4.800
4.800
4.800
5.000
4.800
5.000
4.800
5.100
{8} 4.800
4.000
4.600
4.400
4.200
4.300
4.200
4.200
4.300
4.200
4.400
4.300
4.300
4.100
4.400
4.400
4.400
{0} 4.200
3.100
3.700
3.500
3.300
3.300
3.300
3.500
3.400
3.300
3.500
3.400
3.400
3.300
3.400
3.500
3.500
3.400
4.675
5.125
4.900
4.800
4.900
5.000
4.900
4.900
4.700
4.900
5.000
4.900
3.900
4.900
4.700
5.100
4.800
4.000
4.600
4.400
4.200
4.200
3.900
4.200
4.300
4.200
4.400
4.300
4.300
4.200
4.400
4.200
4.400
4.100
3.100
3.700
3.500
3.300
3.300
3.200
3.500
3.300
3.300
3.600
3.500
3.400
3.400
3.400
3.500
3.400
3.400
*
*
a
b
c
d
e
g
i
j
k
1
m
n
0
p
q
*
*
a
b
c
d
e
g
i
j
k
1
m
n
0
p
q
*
*
a
b
c
d
e
g
i
j
k
1
m
n
0
P
q
D-101
-------
pH in 0.01M Calcium Chloride
A
8
4.4
4.2
§ 4.0
i
Q.
3.8-
3.6-
3.6
m
N M
Mean 4.000
Sd 0.114
Median 4.025
3.8 4.0
pH units
4.2
4.4
-------
pH in 0.01 M Calcium Chloride
Bs"
A-A 4
O
§
4.2-
(Tt
-«-j
'c
D
I
Q.
4.0-
3.8-
3.6-
3
.6
m
N 15
Mua 3.977
Sd 0.096
MedUo 4.000
3.8 4.0
pH units
4.2.
4.4
-------
pH in 0.01 M Calcium Chloride
Bw
O
»—>
£
5.8
5.6
5.2-
5.0-
V)
-^_
§ 4.8-
O.
4.6-
4.4-
4.2-
4.0-
3.8-
N 15
Meu 4S90
Sd 0.200
Median 4550
' i • i ' i ' i ' i ' i ' i • r ^ i • \
3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4 5.6 5.8
pH units
-------
pH in 0.01 M Calcium Chloride
C
o
I
H-»
o
5.4-
5.2-
5.0-
I
a_
4.8-
4.6-
4.4-
' i ' i • i
4.4 4.6 4.8 5.0
N 15
Mean 4J50
Sd 0.166
Median 4.900
5,2 5.4
pH units
-------
4.8-f
pH in 0.01 M Calcium Chloride
B
4.6
4.4
c
D
I
Q.
4.2-
m
c o
4.0-
3.8-
3
.8 4.0
4.2 4.4
pH units
N 15
Mean 4067
Sd 0.108
Median 4.300
4.6 4.8
-------
3.8-f
pH in 0.01M Calcium Chloride
0
3.6
(fl
-«-J
'c
n
I
0.
3.4-
m
3.2-
3.0-
N 15
Mean 1400
Sd 0.091
Median 3.400
3.0 3.2
3.4
pH units
3.6 3.8
-------
o
00
Table la. Summary Statistics for Time
Effect
pH In 0.01M CaCI,
pH unite
Table 1b. Analysis of Variance for Time Effect
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit
samples
A
Bs
Bw
C
Number Standard Audit Sum of Mean Pr >
Lab of labs Mean deviation samples Source df squares square F a -
1 26 4.0123 0.0364 A Lab 1
2 28 3.9750 0.0346 Time 1
a 1 4.1000 Lab*time 1
b 1 4.0000 Error 52
1 14 3.8893 0.0632 Bw Lab 1
2 22 3.9255 0.0286 Time 1
a 1 4.1000 Lab*time 1
b 1 3.9000 Error 34
1 16 4.5881 0.0290 Bw Lab 1
2 12 4.5017 0.4162 Time 1
a 1 4.7000 Lab'time 1
b 1 4.5000 Error 26
1 14 4.7164 0.1105 C Lab 1
2 10 4.8430 0.0506 Time 1
a 1 4.9000 Lab*tlme 1
b 1 4.8000 Error 22
F Audit Sum of Mean
.05 samples Source df squares square
0.0091 0.0091 7.23 0.0096*
0.0061 0.0061 4.67 0.0317*
0.0019 0.0019 1.51 0.2250
0.0654 0.0013
0.0329 0.0329 16.19 0.0003*
0.0034 0.0034 1.69 0.2022
0.0088 0.0088 4.31 0.0454*
0.0690 0.0020
0.0382 0.0382 0.52 0.4780
0.0057 0.0057 0.08 0.7840
0.0060 0.0060 0.08 0.7776
1.9184 0.0738
0.0003 0.0003 0.04 0.8446
0.0091 0.0091 1.10 0.3053
0.0236 0.0236 £66 0.1048
0.1817 0.0083
Pr > F
F a -.05
A Lab 16 16.1317 1.0082 92457 00001*
Error 65 0.0709 0.0011
Bs Lab 17 15.5414 0.9142 364.96 00001*
Error 48 0.1202 0.0025
Bw Lab 17 22.1071 1.3004 23.88 0X1001*
Error 36 1.9608 0.0545
C Lab 17 23.8238 1.4014 155.85 00001*
Error 36 0.3237 0.0090
Table 2b. Palrwlae Comparison for Significant Difference Between DORP and Non-Contract Laboratories
Labs
3 and q
3 and m
3andd
3andh
1 andd
1 and h
2andl
2 and n
2 and p
2andj
2 andd
2andh
Upper
limit
0.3173
0.3173
0.4173
45173
0.3334
4.1334
•0.0040
•0.0040
-0.0040
•0.0040
05960
4.0960
A'
Difference
0.1943
0.1943
05943
4.0943
05123
4.0123
•0.1250
•0.1250
-0.1250
•0.1250
0.1750
3.9750
Bs
Lower Upper
limit Labs limit Difference
0.0713 1 and h 4.1801 3.9893
0.0713 3 and h 4.1392 3.9400
0.1713 4 and h 4.1234 3.9300
3.9713 2andh 4.1140 3.9255
0.0912
3.8912
•0.2460
•0.2460
•0.2460
-0.2460
0.0540
3.8540
Lower
limit
3.7984
3.7408
3.7366
3.7369
Upper
Labs limit
3 and p -0.1130
3 and h 5.5870
1 and p -05097
1 and h 5.4903
4andp -0.1930
4andh 5.5070
2 and p -05873
2andh 5.4127
Bw
Lower
Difference limit
-1.0583
4.6417
-1.1119
4.5881
-1.1383
4.5617
-1.1983
4.5017
-2.0037
3.6963
-2.0141
3.6859
-2.0837
3.6163
-2.1093
3.5907
Labs
3 and m
Sandh
2 and m
2andh
4 and m
4andh
1 andp
1 and m
landh
Upper
limit
1.4025
5.3025
1.3160
5.2160
1.2040
5.1040
•0.0155
1.1845
5.0845
C
Difference
1.0183
4.9183
0.9430
4.8430
0.8310
4.7310
•0.3836
0.8164
4.7164
Lower
limit
0.6342
4.5342
0.5700
4.4700
0.4580
4.3580
-0.7517
0.4483
4.3483
* .05 level of significance; Tukey's Studentized Range Test; DORP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summery Statistics for DDRP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Group
NC
DORP
NC
DORP
NC
ODRP
NC
ODRP
Number
of labs
14
3
14
4
14
4
14
4
Mean
3.7143
4.0272
3.7000
3.9462
4.3000
4.5733
4.4714
4.8022
Sd
1.0726
0.0610
1.0684
0.0284
1.2784
0.0582
1.3182
0.0858
SE
0.2867
0.0352
0.2855
0.0147
0.3418
0.0281
0.3523
0.0478
Min
0.0000
3.8750
0.0000
3.8255
0.0000
4.5017
0.0000
4.7164
Max
4.1000
4.0843
4.1000
3.8883
5.7000
4.6417
5.1000
4.8183
Table 3b. Wlthln-Ctraup and Between-Graup Variabilities for DDRP
and Non-Contract Laboratories
Audit
samples F
A 308.88
Bs 1323.46
Bw 483.32
C 188.02
df
(13.2)
(13,3)
(13.3)
(13.3)
Pr > F*
a - .05
0.0065*
0.0000*
0.0003*
0.0011*
Variances
Unequal
Unequal
Unequal
Unequal
m
-1.0834
-0.8610
-0.7863
-0.9303
df
13.4
13.1
13.2
13.5
Pr> |T|
o - .05
0.2878
0.4048
0.4400
0.3666
• If Pr > F is less than 0.05. there is a significant difference within groups.
" If Pr > |T| Is less than 0.05. there is a significant difference between
groups.
-------
D-110
-------
CALCIUM EXCHANGEABLE IN 1M NH4CL
AUDIT
SOIL X
{A} 0.158
0.381
0.270
0.240
0.650
0.330
0.290
0.040
(Bs) 0.210
0.330
0.280
0.250
0.510
0.290
0.270
0.010
{Bw} 0.185
0.350
0.240
0.230
0.390
0.270
0.270
0.010
Y
0.158
0.381
0.270
0.230
0.500
0.290
0.260
0.050
0.210
0.330
0.240
0.230
0.460
0.270
0.290
0.010
0.185
0.350
0.330
0.230
0.370
0.270
0.260
0.020
LA
*
*
a
b
c
i
k
p
*
*
a
b
c
i
k
p
*
*
a
b
c
i
k
P
AUDIT
SOIL X
(C) - 0.040
0.185
0.140
0.020
0.210
0.050
0.070
0.030
{B} 0.201
0.441
0.310
0.300
0.490
0.400
0.340
0.010
{0} 2.495
13.535
9.700
6.400
6.600
14.860
9.690
5.370
Y
-0.040
0.185
0.070
0.010
0.250
0.060
0.110
0.030
0.201
0.441
0.310
0.310
0.440
0.370
0.330
0.030
2.495
13.535
10.260
6.420
6.000
14.030
9.550
5.510
LA
*
*
a
b
c
i
k
p
r
*
*
a
b
c
1
k
p
r
*
*
a
b
c
i
k
P
D-lll
-------
Exchangeable Calcium in Ammonium Chloride
A
O
i-^
to
0.7-
0.6-
0.5-
cn
0
£0.3-1
0.2-
0.1 -
0.0-
0
N 6
Moo 0.285
Sd 0.170
Median 0.273
I
0 0.1 0.2 0.3 0.4 0.5
meq/100g
0.6 0.7
-------
Exchangeable Calcium in Ammonium Chloride
Bs
0.64
0.5-
0.4:
cr>
o
o
0.3-
cr
a>
E
0.2-
0.1 -
0.0-
I ' I
0.0 0.1
2 / ,
'D A
I r I
0.2 0.3 0.4
meq/100g
N 6
Mcao 0.259
Sd 0.151
Median 0.270
I
0.5 0.6
-------
Exchangeable Calcium in Ammonium Chloride
Bw
0.4-
0.3
en
O
O
0.2-
cr
0)
E
0.1-
0.0-
0.0
N
MCM
Sd 0.122
MedUn 0.266
T
0.1 0.2
meq/100g
0.3
0.4
-------
Exchangeable Calcium in Ammonium Chloride
C
d
0.25-f
0.20-
0.15-
5" 0.05-I
0.00-
-.05-
-.10-
N 6
MUD 0.086
Sd 0.078
Median 0.073
-.10 -.05 0.00 0.05 0.10 0.15 0.20 0.25
meq/1 OOg
-------
Exchangeable Calcium in Ammonium Chloride
B
o\
0.604
0.50
0.40-
cn
O
O
0.30-
cr
(U
E
0.20
0.10-
0.00-
T ' I
0.00 0.10
N 6
Mean 0305
Sd 0.151
Median 0.328
I
0.20 0.30 0.40
meq/100g
0.50 0.60
-------
Exchangeable Calcium in Ammonium Chloride
0
cr>
O
O
cr
0)
E
10-
5-
0-
0
5 10
meq/100g
N 6
Mean 8.699
Sd 3.380
Median 8.015
15
-------
Table 1a. Summary Statistic* for Tim*
Effect
Calcium Exchangeable in 1M NH4CI
meq/100g
Table 16. Analysis of Variance for Time Effect
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
oo
Audit
samples
A
Bs
Bw
C
Number Standard Audit Sum of
Lab of labs Mean deviation samples Source df squares
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
02050 0.0422
0.2525 0.0487
02700 0.0000
02350 0.0071
0.3046 0.0389
02337 0.0454
02600 0.0283
02400 0.0141
0.2834 0.0486
02381 0.0378
02850 0.0636
02300 0.0000
0.0867 0.0274
0.0664 0.0344
0.1050 0.0485
0.0150 0.0071
Table 2b. Palrwlae Comparison for Significant
Labs
3 and c
3 and p
1 and c
1 and p
2 and c
2 and p
Upper
limit
•0.1340
0.3860
-0.1710
0.3580
•0.2137
0.3163
A-
Lower
Difference limit Labs
•0.2464 -0.3587 1 and c
0.2836 0.1713 1 and p
-0.2800 -0.3881 4 and c
0.2500 0.1408 4 and p
•0.3225 -0.4313 3 and c
0.2075 0.0887 3 and p
A Lab 1
Time 1
Lab*time 1
Error 54
Bs Lab 1
Time 1
Lab*tlme 1
Error 36
Bw Lab 1
Time 1
Lab*tlme 1
Error 26
C Lab 1
Time 1
Lab*tlme 1
Error 24
Difference Between
Bs
Upper
limit Difference
-0.0458 -0.1804
0.4282 0.2846
-O.0500 -0.1878
0.4250 0.2871
-0.0718 -02172
0.4032 02578
0.0056
0.0017
0.0001
0.1087
0.0074
0.0013
0.0023
0.0851
0.0106
0.0002
0.0000
0.0567
0.0104
0.0008
0.0041
0.0230
Mean Pr > F Audit
square F a - .05 samples Source df
0.0056 2.77 0.1016
0.0017 0.84 0.3647
0.0001 0.03 0.8737
0.0020
0.0074 4.08 0.0505
0.0013 0.73 0.3888
0.0023 1.28 0.2648
0.0018
0.0106 5.25 0.0287*
0.0002 0.12 0.7341
0.0000 0.00 0.8842
0.0020
0.0104 10.86 0.0030*
0.0008 0.88 0.3324
0.0041 4.33 0.0482*
0.0010
A Lab
Error
Bs Lab
Error
Bw Lab
Error
C Lab
Error
6
68
7
52
7
40
7
40
Sum of
Mean
Pr> F
squares square F a - .05
0.3435
0.1653
02810
0.1652
0.1825
0.0650
0.0648
0.0312
0.0572 23.80 00001*
0.0024
0.0401 12.63 04001*
0.0032
0.0261 16.05 00001*
0.0016
0.0083 11.68 00001*
0.0006
DORP and Non-Contract Laboratories
Lower
limit
-0.3148
0.1601
•0.3258
0.1482
-0.3625
0.1125
Bw
Upper
Labs limit Difference
3andp 0.3840 0.2888
1 and p 0.3751 0.2764
4 and p 0.3682 0.2631
2andc -0.0435 -0.1419
2 and p 0.3215 0.2231
Lower
limit
0.1836
0.1818
0.1578
-0.2403
0.1247
Upper
Labs limit
Sand
3 and
3 and
land
4 and
2 and
2 and
2 and
c -0.0281
1 0.1468
p 0.1718
C -0.0757
C -0.0825
C -0.0844
C -0.1188
p 0.3552
C
Difference
-0.1010
0.0740
0.0980
-0.1433
•0.1517
•0.1636
-02513
0.2237
Lower
limit
-0.1738
0.0011
0.0261
•0.2108
-0.2208
-02328
•0.3827
0.0823
' .05 level of significance; Tukey's Studentlzed Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summery Statistic* for DDRP and Non-Contract Laboratories
Audit
samples
A
Ba
Bw
C
Table 3b.
Audit
samples
A
Ba
Bw
C
Number
Group of labs Mean Sd
NC 4 0.3013 0.2171
DDRP 3 0.2920 0.0381
NC 4 0.2638 0.1048
DDRP 4 0.2758 0.0322
NC 4 0.2325 0.1544
DDRP 4 02784 0.0289
NC 4 0.1013 0.0893
DDRP 4 0.0901 0.0272
SE
0.1085
0.0220
0.0974
0.0161
0.0772
0.0144
0.0446
0.0136
Min
0.0450
0.2525
0.0100
0.2337
0.0150
0.2381
0.0300
0.0664
Max
0.5750
0.3266
0.4850
0.3046
0.3800
0.3038
0.2300
0.1290
Wlthln-Oroup and Between-Qroup Variabilities for DORP
and Non-Contract Laboratorlee
Pr > F*
F df o - .05 Variances |T|
32.40 (3.2) 0.0602 Equal 0.0709
36.51 (3.3) 0.0147* Unequal 4.1223
28.63 (3.3) 0.0208* Unequal -0.5838
10.75 (3.3) 0.0821 Equal 0.2387
df
5.0
3.2
3.2
6.0
Pr > |T|
a - .05
0.9462
0.9101
0.5983
0.8192
• If Pr > F Is less than 0.05. there Is a significant difference within groups.
* If Pr > |T| is less than 0.05. there is a significant difference between
groups.
-------
D-120
-------
MAGNESIUM EXCHANGEABLE IN 1M NH4CL
AUDIT
SOIL X Y LAB
(A) 0.220 0.240 a
0.240 0.220 b
0.600 0.210 1
0.260 0.240 k
0.090 0.090 p
Bs) 0.060 0.060 a
0.050 0.230 b
0.050 0.040 1
0.060 0.060 k
0.020 0.020 p
(Bw) 0.060 0.080 a
0.050 0.050 b
0.040 0.060 1
0.060 0.070 k
0.020 0.020 p
(C) 0.040 0.040 a
0.020 0.020 b
0.020 0.020 1
0.030 0.040 k
0.020 0.050 p
{B} 0.060 0.080 a
0.080 0.080 b
0.080 0.050 1
0.090 0.090 k
0.020 0.020 p
{0} 1.800 1.750 a
2.040 2.220 b
2.490 2.303 1
2.510 2.540 k
1.380 1.480 p
D-121
-------
D-122
-------
POTASSIUM EXCHANGEABLE IN 1M NH4C1
AUDIT
SOIL X
(A) 0.201
0.306
0.260
0.290
0.130
0.280
0.260
0.250
{Bs} -0.053
0.126
0.050
0.060
0.020
0.030
0.030
0.020
{Bw} 0.035
0.095
0.060
0.090
0.030
0.060
0.060
0.060
0.201
0.306
0.250
0.290
0.130
0.270
0.250
0.230
-0.053
0.126
0.030
0.320
0.160
0.040
0.030
0.040
0.035
0.095
0.070
0.070
0.280
0.060
0.060
0.070
LAB
*
*
a
b
c
1
k
P
*
*
a
b
c
i
k
P
a
b
c
1
k
P
AUDIT
SOIL X
{C} 0.021
{
0.038
0.030
0.010
0.010
0.030
0.030
0.020
J) 0.065
0.095
0.080
0.090
0.130
0.090
0.080
0.070
{0} 0.912
1.168
0.980
0.990
1.250
1.120
0.950
0.950
0.021
0.038
0.030
0.020
0.060
0.030
0.030
0.060
0.065
0.095
0.080
0.100
0.030
0.090
0.080
0.080
0.912
.168
.080
.110
0.890
1.090
0.950
1.020
LAB
*
*
a
b
c
i
k
P
a
b
c
i
k
P
*
*
a
b
c
i
k
P
D-123
-------
Exchangeable Potassium in Ammonium Chloride
A
a
S
0.6
0.5-
0.4
O
o
0.3-
cr
-------
Exchangeable Potassium in Ammonium Chloride
Bs
N>
0.20-
en
O
O
0.04-
cr
0)
E
-0.04-
-0.12-
N 6
Mc*n 0.069
Sd 0.063
Median 0.038
-0.12 -0.04 0.04
meq/100g
0.12
0.20
Lab b not shown
-------
Exchangeable Potassium in Ammonium Chloride
Bw
.20 -i
.15-
en
O
O
.10
CT
Q)
E
.05
.00-
.00
.05 .10
meq/100g
Lab c not shown
N 6
Mean 0.061
Sd 0.037
Median 0.065
15
.20
-------
Exchangeable Potassium in Ammonium Chloride
C
0.08-f
0.06-
0.04-
cr
(D
E 0.02-
0.00-
-0.02-
c p
D
-0.02 0.00 0.02 0.04
meq/1 OOg
Lab c not shown
N 6
Mean 0.030
Sd 0.008
Median 0.030
0.06 0.08
-------
Exchangeable Potassium in Ammonium Chloride
B
K)
oo
0.100-f
0.090-
cn
O
O
0.080-
cr
0)
E
0.070-
0.060-
D
N 6
Mean 0.083
Sd 0.006
Median 0.060
0.060 0.070 0.080
meq/1 OOg
0.090 0.100
Lab c not shown
-------
Exchangeable Potassium in Ammonium Chloride
0
O
»—'
10
\0
1.20.1
1.14-
o»1.08-l
o
CT
-------
Table 1a. Summary Statistic* for Tim*
Effect
Audit Number Standard
samples Lab of labs Mean deviation
A
Bs
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
02725
02508
02550
02900
0.0188
0.0335
0.0400
0.1900
0.0598
0.0596
0.0650
0.0800
0.0326
0.0267
0.0300
0.0150
0.1294
0.0191
0.0071
0.0000
0.0268
0.0164
0.0141
0.1839
0.0120
0.0070
0.0071
0.0141
0.0174
0.0066
0.0000
0.0071
Potassium Exchangeable In 1M NH4CI
meq/100g
Table 1b. Analysis of Variance (or Tim* Effect
Audit
samples
A
Ba
"~
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab*time 1
Error 24
Sum of
squares
0.0002
0.0004
0.0030
0.4284
0.0244
0.0283
0.0163
0.0490
0.0002
0.0006
0.0002
0.0029
0.0004
0.0002
0.0001
0.0044
Mean
square
0.0002
0.0004
0.0030
0.0079
0.0244
0.0283
0.0163
0.0014
0.0002
0.0006
0.0002
0.0001
0.0004
0.0002
0.0001
0.0002
F
0.02
0.06
0.38
17.90
20.84
12.01
1.83
5.48
1.91
2.04
0.95
0.39
FT > F
o - .05
0.8876
0.8141
0.5403
0.0002*
0.0001*
0.0014*
0.1868
0.0265*
0.1774
0.1665
0.3390
0.5385
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 6 0.0427 0.0071 1.13 0.3541
Error 69 0.4346 0.0063
Be Lab 7 0.0094 0.0013 2.68 0)0180*
Error 52 0.0259 0.0005
Bw Lab 7 0.0175 0.0025 2.90 00150*
Error 40 0.0345 0.0009
C Lab 7 0.0006 0.0001 0.46 0.6569
Error 40 0.0071 0.0002
Table 2b. Palrwlee Comparison for Significant Difference Between DORP and Non-Contract Laboratorlea
Be
Bw
Upper Lower
Labs limit Difference limit
2
3
4
1
Labs
and
and
and
and
c
c
c
c
Upper
limit Difference
-0.00445
-0.00013
-0.00650
-0.01816
•O.056S
-0.0576
-0.0610
•0.0714
Lower
limit
•0.1086
•0.1152
•0.1157
•0.1247
Labs
1
4
2
3
and
and
and
c
c
c
andc
Upper
limit
-0.0953
-0.0954
•O.0954
-0.0973
Lower Upper Lower
Difference limit Labs limit Difference limit
-0.0249
•0.0188
-0.0237
•0.0207
-0.1656
-0.1720
•0.1671
-0.1740
' .05 level of significance; Tuke/s Studentlzed Range Test; DDRP labs -1 to 4; NC laba - c to r.
-------
Table 3a. Summary Statistics (or DORP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean Sd
NC 4 0.2250 0.0649
DORP 3 0.2557 0.0150
NC 4 0.0463 0.0283
DORP 4 0.0283 0.0068
NC 4 0.0850 0.0467
DORP 4 0.0592 0.0010
NC 4 0.0338 0.0048
ODRP 4 0.0290 0.0029
SE
0.0325
0.0087
0.0146
0.0034
0.0234
0.0005
0.0024
0.0014
Min
0.1300
0.2439
0.0300
0.0186
0.0600
0.0577
0.0300
0.0266
Max
0.2750
0.2725
0.0900
0.0335
0.1550
0.0598
0.0400
0.0326
Table 36. Wlthln-Group and Batwa«n-Group Variabilities -for DORP
Audit
samples
A
Bs
Bw
C
and Non-Contract Laboratories
Pr > F'
F df a - .05 Variances |T|
18.77 (3.2) 0.1020 Equal -0.7848
18.57 (3.3) 0.0386* Unequal 1.1932
2219.92 (3.3) 0.0000* Unequal 1.1062
2.75 (3.3) 0.4289 Equal 1.7150
df
5.0
3.3
3.0
6.0
Pr>|T|
a- .05
0.4681
0.3122
0.3493
0.1372
' If Pr > F Is less than 0.05. there Is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there is a significant difference between
groups.
-------
D-132
-------
SODIUM EXCHANGEABLE IN 1M NH4CL
AUDIT
SOIL X Y LAB
{A} 0.030 0.030 a
0.050 0.050 b
0.080 0.090 1
0.040 0.040 k
0.020 0.010 p
(Bs) 0.010 0.030 a
0.030 0.060 b
0.040 0.070 1
0.060 0.060 k
0.010 0.010 p
(Bw) 0.020 0.030 a
0.050 0.030 b
0.070 0.060 1
0.030 0.010 k
0.010 0.010 p
(C) 0.010 0.010 b
0.020 0.010 k
| 0.010 0.010 p
(B) 0.060 0.060 a
0.080 0.070 b
0.100 0.110 1
0.070 0.060 k
0.030 0.040 p
{0} 0.410 0.530 a
0.440 0.460 b
0.510 0.440 1
0.390 0.370 k
0.310 0.370 p
D-133
-------
D-134
-------
AUDIT
SOIL X
(A) 0.215
0.350
0.270
0.260
0.580
0.280
0.270
0.230
0.260
0.620
0.210
0.320
0.320
0.380
0.320
0.200
{Bs} 0.087
0.297
0.230
0.180
0.470
0.170
0.140
0.130
0.200
0.180
0.140
0.200
0.180
0.250
0.160
0.120
{Bw} 0.175
0.325
0.280
0.260
0.340
0.240
0.220
0.190
0.250
0.320
0.200
0.260
0.230
0.250
0.240
0.180
CALCIUM EXCHANGEABLE IN 1M NH4OAc
Y LAB
0.215
0.350
0.280
0.320
0.450
0.250
0.240
0.300
0.290
0.370
0.230
0.300
0.300
0.250
0.260
0.210
0.087
0.297
0.260
0.270
0.480
0.160
0.120
0.180
0.220
0.210
0.140
0.200
0.200
.250
,160
,120
.175
0.325
0.280
.240
.500
.220
.280
.250
.280
0.370
0.200
.250
.240
0.380
0.250
0.170
0.
0.
0.
0.
0.
0.
0.
0.
0.
0,
0.
0.
*
*
a
b
c
d
e
g
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
AUDIT
SOIL X
{C} 0.012
0.162
0.090
0.030
0.170
0.070
0.110
0.060
0.100
0.300
0.080
0.130
0.100
0.250
0.030
0.060
(B) 0.195
0.390
0.610
0.290
0.380
0.280
0.240
0.200
0.280
0.510
0.220
0.300
0.260
0.250
0.340
0.190
{0} 3.400
10.000
9.640
6.890
5.950
4.690
5.040
7.200
7.760
6.970
6.230
8.970
6.850
1.750
9.970
6.000
Y
0.012
0.162
0.050
0.040
0.550
0.050
0.070
0.110
0.070
0.190
0.130
0.090
0.120
0.250
0.050
0.060
0.195
0.390
0.350
0.300
0.400
0.280
0.290
0.250
0.280
0.350
0.220
0.310
0.320
0.380
0.320
0.180
3.400
10.000
9.960
6.750
6.000
4.550
5.020
6.150
7.850
7.030
6.700
8.770
6.600
1.750
10.710
5.210
LAB
*
*
a
b
c
d
e
9
h
j
k
1
m
0
P
r
*
*
a
b
c
d
e
9
h
0
k
1
m
0
P
r
*
• *
a
b
c
d
e
9
h
j
k
1
m
0
P
r
D-135
-------
LIQUID EXTRACT RESULTS
CALCIUM EXCHANGEABLE IN 1M NH4OAc
NATURAL EXTRACT SYNTHETIC EXTRACT
X Y LAB X Y LAB
0.064 0.064 * 0.085 0.085 *
0.131 0.131 * 0.115 0.115
0.120 0.070 a 0.100 0.100 a
0.090 0.090 b 0.090 0 090 b
0.130 0.130 c 0.130 0.130 c
0.110 0.110 d 0.100 0.100 d
0.100 0.090 e 0.100 0.100 e
0.120 0.120 g 0.120 0.110 g
0.100 0.100 h 0.100 0.100 h
0.030 0.030 j 0.040 0 050 j
0.110 0.120 k 0.100 0.110 k
0.110 0.110 1 0.100 0.100 1
0.080 0.080 p 0.080 0.080 p
0.090 0.090 r 0.100 0 090 r
D-136
-------
Exchangeable Calcium in Ammonium Acetate
A
0.45,
0.40-
0.35-
go.30
0.20-
0.15-
0.10-
o
N 14
Mean 0.306
Sd 0.090
Median 0.281
0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45
rneq/100g
Lab c not shown
-------
Exchangeable Calcium in Ammonium Acetate
Bs
OJ
oo
0.40-r
0.30-
o
o
0.20-
cr
-------
Exchangeable Calcium in Ammonium Acetate
Bw
0.55-
0.45-
o
cr
-------
Exchangeable Calcium in Ammonium Acetate
C
0.30-f
D
0.20-
en
O
O
cr
0)
E
0.10-
0.00-
0.00
Lab c not shown
0.10 0.20
meq/100g
o
N 14
Mean 0.122
Sd 0.095
Median 0.086
0.30
-------
Exchangeable Calcium in Ammonium Acetate
B
I
I—*
.p.
0.65-j
0.55-
^0.45-
o
cr
a>
E0.35-
0.25-
0.15-
m
N 14
Mean 0.306
Sd 0081
Median 0.293
I
0.15 0.25 0.35 0.45
meq/100g
0.55
0.65
-------
Exchangeable Calcium in Ammonium Acetate
0
11-T
9-
§ 7*
O
cr
E 5J
3-
1 -
3
5 7
meq/100g
N 14
Mean 6.677
&J 2.189
Median 6.700
1 1
-------
Exchangeable Calcium in Ammonium Acetate
NE
0.15-f
0.10
en
O
O
cr
(D
E
0.05-
0.00-
0.00
0.05
0.10
meq/100g
N 12
Mean 0.097
Sd 0.026
Median 0.098
0.15
-------
Exchangeable Calcium in Ammonium Acetate
SE
0.14-f
0.10-
CT>
O
o
O"
E
0.06-
0.02-
0.02
0.06 0.10
meq/100g
N 12
Mean 0097
Sd 0.020
Median 0.100
I
0.14
-------
Table la. Summary Statlatlca for Tim*
Effect
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
•
b
1
2
•
b
Number
of labs
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
Mean
0.2688
0.2394
0.2750
0.2900
0.2029
0.1848
0.2450
0.2250
0.2723
0.2089
0.2800
0.2500
0.0830
0.0514
0.0700
0.0350
Standard
deviation
0.0307
0.0457
0.0071
0.0424
0.0427
0.0362
0.0212
0.0636
0.0662
0.0360
0.0000
0.0141
0.0318
0.0243
0.0283
0.0071
Ca Exchangeable in 1M NH4OAc
meq/IOOg
Table 1b. Analysis of Variance for Time Effect
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 36
Lab 1
Time 1
Lab'tlme 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
Sum of
squares
0.0002
0.0030
0.0018
0.0817
0.0013
0.0061
0.0000
0.0558
0.0076
0.0021
0.0010
0.0801
0.0038
0.0007
0.0000
0.0193
Mean
square
0.0002
0.0030
0.0018
0.0015
0.0013
0.0061
0.0000
0.0015
0.0076
0.0021
0.0010
0.0029
0.0038
0.0007
0.0000
0.0008
F
0.13
1.98
122
0.84
3.91
0.00
2.66
0.73
0.34
4.71
0.92
0.01
Pr > F
a - .05
0.7200
0.1655
0.2743
0.3651
0.0556
0.9649
0.1140
0.4014
0.5643
0.0401
0.3476
0.9127
Table 2a. Analyala of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 14 0.3156 0.0225 10.23 OXXX>1*
Error 77 0.1696 0.0022
Bs Lab 15 0.2085 0.0138 11.68 OXJ001*
Error 60 0.0714 0.0012
Bw Lab 15 0.1397 0.0093 3.85 00302*
Error 48 0.1161 0.0024
C Lab 15 0.2769 0.0185 7.69 0X1001*
Error 48 0.1153 0.0024
Table 2b. Palrwlse Comparison for Significant Difference Between DORP and Non-Contract Laboratories
Labs
3 andc
1 andc
1andj
2 andc
2andj
Upper
limit
•0.0048
•0.0721
•0.0521
•0.1021
•0.0821
A'
Difference
•0.1840
•0.2461
-0.2261
•0.2756
•0.2556
Lower
limit
-0.3632
•0.4200
-0.4000
•0.4491
-0.4291
Labs
3 and c
4 andc
1 andc
2 and c
Upper
limit
-0.0962
•0.1231
•0.1352
•0.1565
Bs
Difference
-0.2440
-0.2634
-0.2721
•0.2902
Bw
Lower Upper Lower
limit Labs limit Difference limit
•0.3918 2 andc -0.0116 -02111 -0.4105
•0.4037
•0.4090
-0.4240
Labs
3 and c
landc
4 and c
2 and c
Upper
limit
-0.0160
•0.0803
•0.0826
•0.1070
C
Difference
-0.2285
•0.2770
•0.2842
•0.3066
Lower
limit
•0.4410
-0.4737
•0.4858
-0.5102
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summery Statistics for DORP and Non-Contract Laboratories
o
>-»
ON
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean
NC 12 0.3100
DDRP 3 02788
NC 12 0.1992
DORP 4 0.2076
NC 12 02629
DDRP 4 02496
NC 12 0.1333
DDRP 4 0.0854
Sd
0.0973
0.0468
0.0944
0.0192
0.0675
0.0347
0.0979
0.0336
SE
0.0281
0.0270
0.0273
0.0096
0.0195
0.0173
0.0283
0.0168
Min
0.2050
0.2394
0.1200
0.1848
0.1750
0.2089
0.0400
0.0514
Max
0.5150
0.3310
0.4750
0.2310
0.4200
0.2838
0.3600
0.1315
Wlthln-Group and Between-Qraup Variabilities for DDRP and
Non-Contract Laboratories
Pr> F*
F df a - .05 Variances |T|
4.33 (112) 0.4050
24.18 (11.3) 0.0237*
3.79 (11,3) 0.3000
8.51 (11.3) 0.1042
Equal 0.5127
Unequal -02909
Equal 0.3717
Equal 0.9414
df
13.0
132
14.0
14.0
Pr>|T|
a - .05
0.6168
0.7756
0.7157
0.3624
* If Pr > F Is less than 0.05. there is a significant difference within groups.
* If Ft > |T| Is less than 0.05. than is a significant difference between
groups.
-------
AUDIT
SOIL X
{A} 0.166
{1
{
0.301
0.220
0.220
0.340
0.210
0.220
0.250
0.220
0.310
0.220
0.260
0.270
0.150
0.280
0.200
s) 0.020
0.080
0.040
0.040
0.150
0.050
0.010
0.050
0.060
0.030
0.040
0.050
0.060
0.020
0.070
0.030
3w) 0.030
0.075
0.040
0.050
0.130
0.050
0.010
0.060
0.070
0.050
0.050
0.060
0.070
0.020
0.070
0.040
MAGNESIUM EXCHANGEABLE IN 1M NH4OAc
Y LAB
0.166
0.301
0.250
0.220
0.300
0.210
0.200
0.260
0.230
0.260
250
240
280
100
220
0.200
0.020
0.080
0.060
0.230
150
050
0.010
0.060
060
050
050
0.050
0.060
020
020
030
030
075
0.060
0.050
130
050
020
0.070
0.070
0.080
0.050
0.050
0.060
0.020
0.040
0.040
0.
0.
0.
0,
0.
0.
0.
0.
0.
0.
0.
0.
0.
*
*
a
b
c
d
e
g
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
g
h
j
k
1
m
o
P
r
AUDIT
SOIL X
{C} 0.005
0.065
0.020
0.020
0.090
0.030
0.030
0.050
0.150
0.030
0.040
0.040
0.020
0.060
0.020
{B} 0.035
0.125
0.060
0.080
0.180
0.060
0.050
0.080
0.090
0.160
0.080
0.080
0.090
0.020
0.060
0.060
{0} 1.455
3.195
2.280
2.200
2.940
1.840
1.920
1.830
2.260
2.400
2.170
2.560
2.670
0.520
2.500
1.950
0.
0.
0.
0.
0.005
0.065
.020
.020
0.090
0.030
.040
.030
0.050
0.040
0.030
0.050
0.020
0.020
0.020
.035
125
.080
0.080
0.160
0.060
.050
.090
.090
0.110
0.080
.080
.100
0.020
0.070
0.060
1.455
0.
0.
0.
0.
0.
0.
0.
0.
195
510
,520
,980
,800
,970
,230
,320
.430
.280
.490
.630
.520
,730
1.920
LAB
*
*
a
b
c
d
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
g
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
g
h
j
k
1
m
o
P
r
D-147
-------
LIQUID EXTRACT RESULTS
MAGNESIUM EXCHANGEABLE IN 1M NH4OAc
NATURAL EXTRACT SYNTHETIC EXTRACT
X Y LAB X Y LAB
0.011 0.011 * 0.028 0.028 *
0.049 0.049 * 0.118 0.118 *
0.030 0.020 a 0.070 0.070 a
0.030 0.030 b 0.080 0.080 b
0.040 0.080 c 0.060 0.040 c
0.040 0.040 d 0.080 0.080 d
0.010 0.010 e 0.050 0.050 e
0.040 0.040 g 0.100 0.090 g
0.030 0.030 h 0.080 0.080 h
0.030 0.030 j 0.080 0.070 j
0.040 0.040 k 0.090 0.100 k
0.030 0.030 1 0.030 0.080 1
0.010 0.010 p 0.010 0.010 p
0.080 0.080 r 0.030 0.010 r
D-148
-------
Exchangeable Magnesium in Ammonium Acetate
A
0.36-
0.321
0.28-
00.24-j
£0.20^
0.16-
0.12-
0.08-
o
N 14
Mean 0.235
Sd 0.045
Mcduo 0.23S
0.08 0.12 0.16 0.20 0.24 0.28 0.32 0.36
meq/100g
-------
Exchangeable Magnesium in Ammonium Acetate
Bs
0.24
0.20-
0.16-
cn
O
O
0.12-
cr
(U
£
0.08-
0.04-
0.00-
a
N 14
Mean 0.057
Sd 0.039
Median 0.050
0.00 0.04
0.08 0.12 0.16
meq/100g
0.20 0.24
-------
Exchangeable Magnesium in Ammonium Acetate
Bw
0.10-
0.08-
^0.06-
o
cr
-------
Exchangeable Magnesium in Ammonium Acetate
C
Lft
K)
0.16
0.13
0.10-
O
o
0.07-
cr
-------
Exchangeable Magnesium in Ammonium Acetate
B
9
U)
0.20-f
0.16-
0.0.124
O
O"
E 0.08-
0.04-
0.00-
o
I ' I
0.00 0.04
0.08 0.12
meq/1OOg
N 14
Mem 0.061
Sd 0.036
Median 0.080
0.16 0.20
-------
Exchangeable Magnesium in Ammonium Acetate
0
3-
cr>
O
O
2-
cr
E
0-
0
O
N 14
Mean 2.192
Sd 0^76
Median 2.325
meq/1 OOg
-------
Exchangeable Magnesium in Ammonium Acetate
NE
0.104
9
O
O
0.05-
cr
(L>
£
A
0.00-
0.00
0.05
meq/100g
N 12
Mean 0.035
Sd 0.019
Median 0.030
0.10
-------
Exchangeable Magnesium in Ammonium Acetate
SE
o\
0.15
0.10-
O
O
0.05-
cr
-------
Table 1a. Summery Statistics for Tim*
Effect
Mg Exchangeable in 1M NH4OAc
meq/100g
Table 1b. Anslysls of Variance for Time Effect
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
9
>—*
Oi
Audit
samples
A
Bs
Bw
C
Number Standard Audit Sum of Mean Pr > F Audit Sum of Mean Pr > F
Lab of labs Mean deviation samples Source df squares square F a - .05 samples Source df squares square F a - .05
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26 02426 0.0277
28 02230 0.0200
2 02350 0.0212
2 02200 0.0000
14 0.0511 0.0183
22 0.0430 0.0075
2 0.0500 0.0141
2 0.1350 0.1344
16 0.0571 0.0167
12 0.0461 0.0052
2 0.0500 0.0141
2 0.0500 0.0000
14 0.0246 0.0210
10 0.0280 0.0101
2 0.0200 0.0000
2 0.0200 0.0000
A Lab 1 0.0011 0.0011 1.88 0.1647
Time 1 0.0001 0.0001 0.18 0.6688
Labxtlme 1 0.0000 0.0000 0.04 0.6508
Error 54 0.0304 0.0006
Bs Lab 1 0.0053 0.0053 7.85 0.0081*
Time 1 0.0074 0.0074 10.87 0.0021*
Labxtime 1 0.0078 0.0078 11.52 0.0017*
Error 36 0.0243 0.0007 .
Bw Lab 1 0.0001 0.0001 0.64 0.4316
Time 1 0.0000 0.0000 0.05 0.8183
Labxtlme 1 0.0001 0.0001 0.64 0.4316
Error 28 0.0047 0.0002
C Lab 1 0.0000 0.0000 0.04 0.8508
Time 1 0.0001 0.0001 0.48 0.4827
Labxtime 1 0.0000 0.0000 0.04 0.8508
Error 24 0.0067 0.0003
Table 2b. Palrwlse Comparison for Significant Difference Between
Ubs
1 and c
1 and o
2ande
2 and]
2 and o
3andc
3 and o
Upper
limit
-0.1357
0.0593
-0.1552
-0.1202
0.0388
-0.1478
0.1072
A*
Difference
-0.0774
0.1176
-0.0870
•0.0620
0.0880
•0.0878
0.1072
Lower
limit
-0.0181
0.1758
•0.0388
-0.0038
0.1561
-0.0277
0.1673
Labs
1 and c
1ande
1 and o
2 and c
2ande
3 and c
3 and e
3 and o
4andc
4ande
Upper
limit
-0.1032
0.0118
0.0068
-0.1148
0.0002
-0.1070
0.0080
0.0030
-0.1135
0.0015
Bs
Difference
•0.0728
0.0421
0.0371
•0.0838
0.0311
-0.0740
0.0410
0.0360
•0.0805
0.0345
A Lab 14 0.0592 0.0042 8.22 00001*
Error 77 0.0396 0.0005
Bs Lab 15 0.0275 0.0018 13.67 0.0001*
Error 60 0.0080 0.0001
Bw Lab 15 0.0197 0.0013 10.46 0.0001*
Error 48 0.0060 0.0001
C Lab 15 0.0203 0.0014 4.84 0X5001*
Error 48 0.0134 0.0003
DDRP and Non-Contract Laboratories
Lower
limit
-0.0424
0.0723
0.0675
-0.0530
0.0620
-0.0410
0.0740
0.0680
•0.0475
0.0675
Upper
Labs limit
1 and c -0.1301
1 and e 0.0098
2andc -0.1376
2 and e 0.0023
3 and c -0.1348
3ande 0.0052
4 and c -0.1334
Bw
Difference
•0.0989
0.0411
•0.1070
0.0330
•0.1014
0.0390
•0.1014
Lower
limit
-0.0676
0.0724
•0.0763
0.0636
•0.0693
0.0728
•0.0693
Labs
1 and c
1 and j
2 and c
2 and]
3 andc
3 and]
4 and c
4 and]
Upper
limit
-0.1111
-0.1211
-0.1088
•0.1188
-0.1005
•0.1005
•0.1050
•0.1150
C
Difference
•0.0654
•0.0754
•0.0620
-0.0720
-0.0512
•0.0612
-0.0582
•0.0682
Lower
limit
•0.0198
-0.0298
-0.0152
•0.0252
-0.0018
-0.0119
-0.0115
-0.0215
* .05 level of significance; Tukey's Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statlatlca for DDRP and Non-Contract Laboratories
D
>—•
o»
oo
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean
NC
DORP
NC
DDRP
NC
DDRP
NC
DDRP
12
3
12
4
12
4
12
4
0.2367
0.2326
0.0513
0.0479
0.0567
0.0522
0.0408
0.0308
Sd
0.0494
0.0098
0.0347
0.0035
0.0289
0.0053
0.0281
0.0061
SE
0.0143
0.0057
0.0100
0.0017
0.0084
0.0026
0.0081
0.0031
Min
0.1250
0.2230
0.0100
0.0430
0.0150
0.0461
0.0000
0.0246
Max
0.3200
0.2426
0.1500
0.0511
0.1300
0.0571
0.1000
0.0388
Wlthln-Group and Between-Qroup Variabilities for DDRP and
Non-Contract Laboratories
F
25.22
00.66
30.17
21.15
df
(11.2)
(11.3)
(11.3)
(11.3)
Pr > F'
a - .05 Variances |T|
0.0775
0.0029*
0.0171*
0.0287*
Equal 0.1383
Unequal 0.3249
Unequal 0.5119
Unequal 1.1581
df
13.0
11.6
12.8
13.4
Pr>|T|
o- .05
0.8921
0.7511
0.6174
0.2671
' If Pr > F Is lees than 0.05. there Is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there Is a significant difference between
groups.
-------
AUDIT
SOIL X
(A) 0.220
0.310
0.260
0.230
0.370
0.250
0.300
0.220
0.300
0.290
0.250
0.300
0.280
0.200
0.290
0.230
{Bs} 0.001
0.061
0.030
0.020
0.070
0.040
0.030
0.030
0.100
0.050
0.030
0.050
0.020
0.030
0.020
0.030
(Bw) 0.021
0.098
0.060
0.060
0.100
0.070
0.080
0.060
0.100
0.080
0.060
0.090
0.030
0.050
0.030
0.050
POTASSIUM EXCHANGEABLE IN 1H NH4OAc
Y LAB
0.
0.
0.220
0.310
0.270
0.240
0.300
0.250
0.230
0.270
0.300
0.260
0.260
0.290
.260
180
0.250
0.240
0.001
0.061
0.030
0.240
0.070
0.040
0.030
0.040
0.100
0.030
0.030
0.050
0.020
0.030
0.030
0.030
0.021
0.098
0.070
0.060
0.110
0.070
.020
.060
,100
0.070
0.060
.090
.050
0.040
0.030
0.050
0.
0.
0.
0.
0.
a
b
c
d
e
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
AUDIT
SOIL X
(C) 0.006
0.053
0.010
0.030
0.070
0.030
0.040
0.030
0.100
0.040
0.020
0.050
0.030
0.030
0.010
0.020
{B} 0.038
0.128
0.070
0.080
0.130
0.090
0.080
0.080
0.200
0.110
0.080
0.130
0.070
0.050
0.070
0.080
{0} 0.630
1.305
1.100
0.900
1.260
0.930
0.870
0.810
1.100
1.050
1.000
1.240
0.990
0.270
0.960
0.960
0.
0.
0.
0.
0.006
0.053
0.030
0.020
0.060
0.030
0.020
0.040
0.100
0.040
0.030
0.050
0.020
0.030
0.020
.020
.038
126
100
0.080
0.130
0.090
0.100
0.080
0.200
0.100
0.080
0.110
0.070
0.060
0.060
0.070
0.630
1.305
1.300
1.060
1.300
0.920
.980
.000
.200
.110
.020
1.320
0.910
0.260
0.950
0.880
0.
1
1,
1,
1
LAB
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
*
*
a
b
c
d
e
9
h
j
k
1
m
o
P
r
D-159
-------
LIQUID EXTRACT RESULTS
POTASSIUM EXCHANGEABLE IN 1M NH4OAc
NATURAL EXTRACT SYNTHETIC EXTRACT
X Y LAB X Y LAB
0.033 0.033 * 0.005 0.005 *
0.048 0.048 * 0.035 0.035 *
0.040 0.040 a 0.020 0.020 a
0.040 0.030 b 0.020 0.020 b
0.040 0.040 c 0.040 0.040 c
0.040 0.040 d 0.020 0.020 d
0.030 0.040 g 0.020 0.030 g
0.050 0.080 h 0.050 0.060 h
0.040 0.040 j 0.020 0.020 j
0.040 0.040 k 0.030 0.030 k
0.030 0.030 1 0.020 0.020 1
0.010 0.020 p 0.010 0.010 p
0.040 0.030 r 0.020 0.020 r
D-160
-------
9
•—>
o\
Exchangeable Potassium in Ammonium Acetate
A
0.40-1
0.36-
0.32-
cn
O
O
0.28-
cr
E
0.24-
0.20-
0.16-
I ' I 'I ' I
N 14
Mean 0.263
Sd 0.034
Median 0.26S
I ' I
0.16 0.20 0.24 0.28 0.32 0.36 0.40
meq/1 OOg
-------
Exchangeable Potassium in Ammonium Acetate
Bs
ov
to
en
O
O
cr
0)
E
0.25-f
0.20-
0.15-
0.10-
0.05-
0.00.-
-0.05-
D
h
1 ' r
n ' r
N 14
Mean 0.047
Sd 0.032
Median 0.031
-0.05 0.00 0.05 0.10 0.15
meq/100g
0.20 0.25
-------
Exchangeable Potassium in Ammonium Acetate
Bw
O
i—*
o\
0.12-
0.10-
0.08,
o
o
0.06-
cr
a)
E
0.04-
0.02-
0.00-
m
0.00 0.02
0.04 0.06 0.08
meq/100g
N 14
Me.n 0.064
Sd 0.022
Median 0.060
0.10 0.12
-------
Exchangeable Potassium in Ammonium Acetate
C
0.08
0.06
en
O
O
0.04-
cr
-------
Exchangeable Potassium in Ammonium Acetate
B
O
i—«
85
0.21-
0.16-
cn
O
O
cr
0)
E
0.06-
0.01 -
0.01
N 14
Mean 0.095
Sd 0.037
Mcdiio 0.083
0.06 0.11
meq/100g
0.16
0.21
-------
Exchangeable Potassium in Ammonium Acetate
0
1.40-
1.20-
1.00-
O
o
0.80,
cr
0)
E
0.60-
0.40-
0.20-
a
m
N 14
Mean 0.968
Sd 0.247
Median 0.968
I
0.20 0.40
0.60 0.80 1.00
meq/100g
V.20 1.40
-------
Exchangeable Potassium in Ammonium Acetate
NE
0.08-f
0.06-
CT>
O
o
0.04-
cr
(U
E
0.02-
0.00-
N 11
Mean 0.025
Sd 0.012
Median 0.020
0.00
0.02 0.04
meq/100g
0.06 0.08
-------
Exchangeable Potassium in Ammonium Acetate
SE
0.104
O
o
0.05-
cr
(U
E
0.00-
0.00
N 11
Mean 0.038
Sd 0.012
Median 0.020
0.05
meq/100g
0.10
-------
Table la. Summary Statistics for Time
Effect
Audit Number Standard
samples Lab of labs Mean deviation
D
H-»
ON
A
Bs
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
02654
0.2510
0.2650
0.2350
0.0311
0.0247
0.0300
0.1300
0.0672
0.0501
0.0650
0.0600
0.0229
0.0199
0.0200
0.0250
0.0537
0.0179
0.0070
0.0071
0.0147
0.0051
0.0000
0.1556
0.0298
0.0108
0.0071
0.0000
0.0138
0.0070
0.0141
0.0071
K Exchangeable In 1M NH4OAc
meq/100g
Table 1b. Analysis ol Variance for Tim* Effect
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*tlme 1
Error 54
Lab 1
Time 1
Lab'time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
Sum of
squares
0.0018
0.0002
0.0002
0.0807
0.0078
0.0097
0.0101
0.0275
0.0004
0.0001
0.0001
0.0146
0.0000
0.0000
0.0001
0.0032
Mean
square
0.0018
0.0002
0.0002
0.0015
0.0078
0.0097
0.0101
0.0008
0.0004
0.0001
0.0001
0.0005
0.0000
0.0000
0.0001
0.0001
F
1.22
0.17
0.15
10.25
12.69
13.25
0.82
0.10
0.24
0.03
0.03
0.41
FT > F
a - .05
0.2734
0.6850
0.6976
0.0029*
0.0011*
0.0008*
0.3739
0.7543
0.6246
0.8711
0.8587
0.5291
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
Lab 14 0.0342
Error 77 0.0906
0.0024 2.07 04)225*
0.0011
Be Lab 15 0.0150 0.0010 15.70 OflOOl*
Error 60 0.0038 0.0001
Bw Lab 15 0.0150 0.0010 2.75 OXXMO*
Error 48 0.0174 0.0004
C Lab 15 0.0159 0.0011 11.84 04001*
Error 48 0.0043 0.0001
Table 26. Palrwlse Comparison for Significant Difference Between DORP and Non-Contract Laboratorlee
Be
Bw
Upper Lower
Labs limit Difference limit
3
3
1
1
4
4
4
2
2
2
Labs
and
and
and
and
and
and
and
and
and
and
h
c
h
c
h
c
I
h
c
1
Upper
limit
-0.0406
-0.0106
•0.0473
-0.0173
-0.0507
-0.0207
-0.0007
•0.0542
-0.0242
-0.0042
Difference
•0.0638
-0.0338
•O.06B9
-0.0389
•0.0728
-0.0428
-0.0228
•0.0753
•0.0453
-0.0253
Lower Upper Lower
limit Labs limit Difference limit
-0.0871 2andc -0.0024 -O.0549 -0.1074
•0.0571
•0.0904
•0.0604
•0.0949
-0.0649
-0.0449
-0.0963
-0.0663
•0.0463
Labs
3
3
4
4
1
1
1
2
2
2
and
and
and
and
and
and
and
and
and
and
h
c
h
c
h
c
1
h
c
1
Upper
limit
•0.0432
•0.0082
-0.0474
•0.0124
•0.0513
•0.0163
-0.0013
-0.0536
•0.0186
-0.0036
Lower
Difference limit
-0.0712
•0.0362
•0.0738
•0.0388
•0.0771
•0.0421
-0.0271
-0.0801
-0.0451
•0.0301
-0.0991
-0.0641
•0.1003
-0.0653
•0.1030
-0.0680
-0.0530
•0.1066
•0.0716
-0.0566
' .05 level of significance; Tuke/s Studentized Range Test; ODRP labs -1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistic* for DORP and Non-Contract Laboratories
9
»—*
o
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean
NC
DORP
NC
DORP
NC
DORP
NC
ODRP
12
3
12
4
12
4
12
4
0.2654
02550
0.0417
0.0288
0.0646
0.0602
0.0368
0.0244
Sd
0.0362
0.0091
0.0226
0.0050
0.0240
0.0073
0.0236
0.0039
SE
0.0105
0.0052
0.0065
0.0025
0.0069
0.0036
0.0068
0.0019
Min
0.1900
0.2486
0.0200
0.0247
0.0300
0.0501
0.0150
0.0199
Max
0.3350
0.2653
0.1000
0.0362
0.1050
0.0672
0.1000
0.0268
Wlthln-Group and Between-Group Variabilities for DORP and
Non-Contract Laboratories
F
15.95
20.47
10.88
36.70
df
(11.2)
(11.3)
(11.3)
(11.3)
Pr > F*
a - .05 Variances |T|
0.1208
0.0301*
0.0741
0.0129*
Equal 0.4630
Unequal 1.6976
Equal 0.3508
Unequal 2.0232
df
13.0
13.4
14.0
12.6
Pr>|T|
a- .05
0.6371
0.1127
0.7310
0.0649
' If Pr > F Is toss than 0.05. there Is a significant difference within groups.
* If Pr > |T| is toss than 0.05. there Is a significant difference between
groups.
-------
AUDIT
SOIL X
(A) -0.049
0.154
0.020
0.040
0.100
0.090
0.070
0.020
0.110
0.040
0.090
0.270
0.010
0.030
{Bs} -0.002
0.073
0.020
0.030
0.020
0.060
0.040
0.070
0.020
0.040
0.160
0.010
0.020
{Bw> -0.014
0.084
0.020
0.030
0.050
0.040
0.050
0.030
0.080
0.030
0.060
0.210
0.010
0.020
SODIUM EXCHANGEABLE IN 1M NH4OAc
AUDIT
Y LAB SOIL X
-0.049
0.154
0.020
0.040
0.120
0.060
0.060
0.010
0.090
0.040
0.080
0.230
0.030
0.030
-0.002
0.073
0.040
0.040
0.040
0.030
0.040
0.050
0.010
0.050
.210
.030
0.020
-0.014
0.084
0.010
0.030
0.070
0.040
0.020
0.040
0.080
0.020
0.050
0.220
0.040
0.020
0,
0,
*
*
a
b
d
e
9
h
j
k
m
o
P
r
*
*
a
b
d
9
h
j
k
m
o
P
r
*
*
a
b
d
e
9
h
j
k
m
o
P
r
{C}
(B>
(0)
0.
0.
0.
-0.019
0.079
.010
.010
.050
0.050
0.020
0.030
0.180
0.010
-0.041
,181
.060
0.070
0.090
.030
.190
.040
150
0.060
0.100
0.230
0.060
0.293
0.578
0.390
.430
.660
.360
0.430
0.480
.480
.390
0.450
0.320
0.050
0.330
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
Y
-0.019
0.079
-0.020
0.050
0.040
0.050
0.010
0.030
0.170
0.020
-0.041
0.181
0.050
0.060
0.110
0.040
0.070
0.040
0.110
0.050
0.110
0.230
0.080
0.293
0.578
0.420
0.450
0.750
0.560
0.300
0.440
0.500
0.390
0.420
0.290
0.480
0.330
LAB
*
*
a
d
g
j
k
m
0
p
*
*
a
b
d
e
g
h
j
k
m
0
P
*
*
a
b
d
e
g
h
j
k
ID
0
P
r
D-171
-------
LIQUID EXTRACT RESULTS
SODIUM EXCHANGEABLE IN 1M NH4OAc
NATURAL EXTRACT SYNTHETIC EXTRACT
X Y LAB X Y LAB
0.003 0.003 * 0.018 0.018 *
0.077 0.077 * 0.063 0.063 *
0.050 0.040 a 0.040 0.040 a
0.040 0.040 b 0.040 0.040 b
0.040 0.040 d 0.040 0.040 d
0.020 0.020 e 0.100 0.090 g
0.900 0.090 g 0.020 0.020 h
0.020 0.020 h 0.050 0.050 k
0.050 0.050 k 0.010 0.010 p
0.010 0.010 p 0.040 0.040 r
0.040 0.040 r
D-172
-------
Exchangeable Sodium in Ammonium Acetate
A
0.24-
0.16H
en
O
O
0.08J
O"
-------
Exchangeable Sodium in Ammonium Acetate
Bs
0.14-
0.10-
cn
O
O
0.06^
cr
d)
E
0.02-
-0.02-
-0.02 0.02
0.06
meq/1 OOg
N 11
Mean 0.045
Sd 0.047
Median 0.035
0.10
0.14
Lab o not shown
-------
Exchangeable Sodium in Ammonium Acetate
Bw
d
>—•
Lf»
en
O
O
cr
0)
£
0.16-
0.08.
0.00-
-0.08-
-0.08
0.00 0.08
meq/100g
Lab o not shown
N 12
Mean 0.053
Sd O.QS4
Median 0035
0.16
-------
Exchangeable Sodium in Ammonium Acetate
C
o
t—»
ON
0.12
0.08-
CJ>
O
o
0.04-
cr
0)
E
0.00-
-0.04-
-0.04
0.00 0.04
meq/1 OOg
N 8
Mean 0.044
Sd 0056
Median 0.030
0.08 0.12
Lab o not shown
-------
Exchangeable Sodium in Ammonium Acetate
B
0.24-
0.16-
cn
O
O
O.OSn
CT
(U
E
0.00-
-0.08-
-0.08 0.00
0.08
meq/1 OOg
o
N II
Mean 0.092
Sd 0057
Median 0.070
0.16
0.24
Lab o not shown
-------
Exchangeable Sodium in Ammonium Acetate
O
00
cn
O
O
cr
0)
E
0.8-
0.7-
0.6-
0.5-
0.4-
0.3-
0.2-
0.1 -
0.0-
i i
0.0 0.1
m
o
N 12
Mean 0.421
Sd 0.113
Median 0.420
I
I
0.2 0.3 0.4 0.5
meq/100g
0.6 0.7 0.8
-------
Exchangeable Sodium in Ammonium Acetate
NE
0.10-
0.05-
cn
O
O
cr
0)
£
0.00-
-0.05-
N 9
Mean 0.084
Sd 0.1S5
Median 0.040
-0.05
0.00
0.05
0.10
meq/100g
-------
Exchangeable Sodium in Ammonium Acetate
SE
9
•—••.
00
O
0.15-f
0.10-
cn
O
O
cr
-------
oo
Table la. Summary Statistics for Time
Effect
Na Exchangeable in 1M NH4OAc
meq/IOOg
Table 1b. Analysis of Variance for Time Effect
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Number Standard Audit Sum of
samples Lab of labs Mean deviation samples Source df squares
A
Bs
Bw
C
Table
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26 0.0404 0.0272
28 0.0384 0.0061
2 0.0200 0.0000
2 0.0400 0.0000
14 0.0230 0.0403
22 0.0170 0.0058
2 0.0300 0.0141
2 0.0350 0.0071
16 0.0333 0.0521
12 0.0230 0.0081
2 0.0150 0.0071
2 0.0300 0.0000
14 0.0067 0.0084
10 0.0015 0.0037
2 -0.0050 0.0212
2 0.0050 0.0071
2b. Palrwlse Comparison for Significant
Upper
Labs limit
1 and
1 and
1 and
1 and
2 and
2 and
2 and
2 and
3 and
3 and
3 and
3 and
o -0.1653
d -0.0253
j -0.0153
m -0.0003
o -0.1674
d -0.0274
j -0.0174
m -0.0024
0 -0.1687
d -0.0287
j -0.0187
m -0.0047
A'
Lower
Difference limit Labs
-0.2096 -0.2538 1 and o
•0.0686 -0.1138 4 and o
•0.0586 -0.1038 3 and o
•0.0446 -0.0888 2 and o
-0.2118 -0.2558
-0.0716 -0.1158
-0.0616 -0.1058
-0.0466 -0.0808
-0.2154 -0.2610
•0.0754 -0.1210
-0.0654 -0.1110
•0.0504 -0.0860
A Lab 1
Time 1
Lab*time 1
Error 54
Bs Lab
Time
Lab'time
Error 36
C Lab
Time
Lab*tlme 1
Error 28
C Lab 1
Time 1
Lab*time 1
Error 24
Difference Between
Bs
Upper
limit Difference
-0.1056 -0.1620
4.1081 -0.1658
-0.1068 -0.1678
-0.1128 -0.1680
0.0003
0.0003
0.0005
0.0203
0.0000
0.0006
0.0001
0.0220
0.0000
0.0001
0.0006
0.0415
0.0000
0.0001
0.0002
0.0018
Mean Pr > F Audit
square F a - .05 samples Source
0.0003 0.80 0.3738
0.0003 0.87 0.3540
0.0005 1.20 0.2784
0.0004
0.0000 0.00 0.8687
0.0006 0.81 0.3453
0.0001 0.18 0.6764
0.0006
0.0000 0.01 0.8081
0.0001 0.07 0.7868
0.0006 0.36 0.5451
0.0015
0.0000 0.26 0.6123
0.0001 0.78 0.3868
0.0002 2.67 0.1156
0.0001
A Lab
Error
Bs Lab
Error
Bw Lab
Error
C Lab
Error
df
12
75
13
58
13
46
13
46
Sum of
squares
0.1106
0.0233
0.0578
0.0264
0.0733
0.0543
0.0607
0.0041
Mean
square
FT > F
F a -.05
0.0082 28.60 OXM01*
0.0003
0.0045
0.0005
0.0056
0.0012
8.78 0.0001*
4.77 OXW01*
0.0047 52.77 0X1001*
0.0001
DDRP and Non-Contract Laboratories
Lower
limit
-0.2184
•0.2237
-0.2288
-0.2231
Bw
Upper
Labs limit Difference
3ando -0.0777 -0.1770
Undo -0.0805 -0.1817
4 and o -0.0820 -0.1812
2ando -0.0881 -O.1820
Lower
limit
-0.2763
-0.2730
-0.2905
•0.2848
Labs limit
3
3
3
1
1
4
2
2
2
2
2
and
and
and
and
and
and
and
and
and
and
and
and
and
and
and
and
0 -0.1347
| -0.0087
g -0.0047
o -0.1431
| -0.0181
g -0.0131
0 -0.1452
} -0.0202
g -0.0152
d -0.0002
m 4.0002
o -0.1477
j -0.0227
g -0.0177
d -0.0027
m -0.0027
C
Lower
Difference limit
-0.1618
-0.0368
•0.0318
-0.1683
•0.0433
-0.0363
-0.1710
-0.0460
-0.0410
-0.0260
-0.0260
-0.1735
•0.0485
4.0435
-0.0285
-0.0285
-0.1890
-0.0640
-0.0580
-0.1835
•0.0685
-0.0635
•0.1868
-0.0718
-0.0668
•0.0518
-0.0518
•0.1883
4.0743
4.0683
4.0543
4.0543
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistic* for DORP and Non-Contract Laboratories
D
»—>
oo
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Group
NC
DORP
NC
DORP
NC
DORP
NC
DDRP
Number
of labs Mean
10 0.0790
3 0.0378
10 0.0480
4 04)191
10 0.0590
4 0.0295
10 0.0395
4 0.0063
Sd
0.0686
0.0029
0.0498
0.0028
0.0579
0.0073
0.0500
0.0050
SE
0.0217
0.0017
0.0157
0.0014
0.0183
0.0037
0.0158
0.0025
Min
0.0150
0.0346
0.0150
0.0170
0.0200
0.0230
0.0050
0.0015
Max
0.2500
0.0404
0.1850
0.0230
0.2150
0.0380
0.1750
0.0132
Wlthln-Group and Between-Group Variabilities for DDRP and
Non-Contract Laboratories
F
554.15 |
318.13
62.16
98.97
df
9.2
9.3
9.3
9.3
Pr > F*
a - .05
0.0036*
0.0005*
0.0060*
0.0030*
Variances |T|
Unequal 1.8924
Unequal 1.8943
Unequal 1.5606
Unequal 2.0723
df
9.1
9.1
9.7
9.4
Pr>IT|
a - .05
0.0906
0.0903
0.1461
0.0667
• If FT > F Is less than 0.05. there Is a significant difference within groups.
* If Pr > |T| Is less than 0.05, there Is a significant difference between
groups.
-------
AUDIT
SOIL X
{A} 3.425
11.255
7.190
7.390
5.300
5.270
26.750
(Bs) 5.093
9.846
7.700
7.530
5.880
4.970
29.600
(Bw) 0.806
7.753
4.830
4.020
2.850
3.200
22.900
CATION EXCHANGE CAPACITY 1M NH4CL
Y LAB
3.425
11.255
8.330
7,
4.
5.
290
740
030
24.450
5.093
9.846
7,
7,
670
410
6.320
5.290
27.450
0.806
.753
.890
.540
.440
.890
7.
5.
4.
2.
2,
22.800
*
*
a
b
i
k
P
*
a
b
i
k
P
*
a
b
i
k
P
AUDIT
SOIL X
{C} -0.555
1.575
0.690
0.300
0.300
0.250
2.300
{8} 4.330
11.170
8.540
6.910
5.130
5.810
38.550
{0} 19.073
33.906
29.980
24.990
25.640
26.180
99.990
Y
-0.555
1.575
1.300
0.720
0.230
0.320
1.300
4.330
11.170
8.140
8.590
4.940
6.310
40.050
19.073
33.906
32.400
27.500
24.270
26.800
99.990
LAI
*
*
a
b
i
k
p
r
*
*
a
b
i
k
p
*
*
a
b
i
k
P
D-183
-------
Cation Exchange Capacity by Ammonium Chloride
A
15-
10-
en
O
O
cr
0)
E
5-
0-
N 5
Meaa 10.962
Sd 9.862
Median 7.470
I
0
Lab p not shown
10
15
meq/1 OOg
-------
Cation Exchange Capacity by Ammonium Chloride
Bs
O
i—»
oo
in
20-
CJi
O
O
10
CT
-------
Cation Exchange Capacity by Ammonium Chloride
Bw
oo
o\
en
O
O
cr
0)
E
15
5-
0-
0
Lab p not shown
5 10
meq/1 OOg
N 5
Mean 7.636
Sd 8.572
Median 4.280
15
-------
Cation Exchange Capacity by Ammonium Chloride
C
2.5-
2.0-
1.5-
cn
8
0.5-
0.0-
-.5-
-1 -.5
N 5
Mean 0.771
Sd 0.646
McdUn OJ10
I
0.0 0.5 1.0
meq/1 OOg
1.5 2.0
-------
Cation Exchange Capacity by Ammonium Chloride
B
O
»—»
oo
00
50-
40-
^30
o
cr
Q)
E 20
10-
0-
0
10
20 30
meq/100g
N 5
Mean 41.774
Sd 32.630
Median 26.490
1
40
50
-------
Cation Exchange Capacity by Ammonium Chloride
0
d
40
30-
en
O
O
cr
-------
D
§
Table 1a. Summary Statistic* for Tim*
Effect
Audit Number Standard
samples Lab of labs Mean deviation
Cation Exchange Capacity In 1M NH4CI
meq/100g
Table 1b. Analysis of Variance for Time Effect
A
Bs
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
8.0288
7.1711
7.7600
7.3400
8.0426
7.3503
7.6850
7.4700
5.5474
3.8275
5.3600
42800
0.5762
0.6450
0.9950
0.5100
0.9036
0.5002
0.8061
0.0707
0.7993
0.7321
0.0212
0.0849
0.9119
0.4372
0.7495
0.3677
0.2676
0.3890
0.4313
0.2970
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab'time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
Sum of
squares
1.5198
0.0093
0.1784
27.8201
0.7372
0.0507
0.2040
19.5871
6.8419
0.0613
0.3574
152736
0.1479
0.0687
02618
2.5670
Mean
square
1.5198
0.0093
0.1784
0.5152
0.7372
0.0507
0.2040
0.5435
6.8419
0.0613
0.3574
0.5455
O.J479
0.0687
0.2618
0.1070
F
2.95
0.02
0.35
1.36
0.09
. 0.38
12.54
0.11
0.66
1.38
0.64
2.45
Pr>F
a- .05
0.0916
0.8937
0.5587
0.2518
0.7619
0.5439
0.0014*
0.7399
0.4251
0.2512
0.4306
0.1308
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 5 769.6892 153.9376 166.61 00001*
Error 68 62.8270 0.9239
Bs Lab 6 077.1944 162.6657 216.64 00001*
Error 51 38.3046 0.7511
Bw Lab 6 747.5238 124.5873 276.95 00001*
Error 39 17.5441 0.4498
C Lab 6 6.9071 1.1512 9.47 00001*
Error 39 4.7411 0.1216
Table 2b. Palrwlee Comparison for Significant Difference Between ODRP and Non-Contract Laboratories
Bs
Bw
Upper
Labs limit
3 and p -12.5290
3 and k 7.9210
3 and I 8.0510
1 and p -15.5030
1 and k 4.9470
1 and I 5.0770
2 and p -16.3660
2 and I 42140
Difference
-14.6600
5.7900
5.9200
-17.5710
2.8790
3.0090
-18.4290
2.1510
Lower
limit
-16.7910
3.6590
3.7890
-19.6400
0.8100
0.9400
-20.4920
0.0880
Upper
Labs limit Difference
3 and p -13.4270 -15.5990
3 and I 8.9980 6.8260
3 and k 9.9680 7.7960
4 and p -18.0570 -20.1170
4 and i 4.3680 2.3080
4 and k 5.3380 32780
1 and p -18.4720 -20.4820
landk 4.9230 2.9130
Lower
limit
-17.7700
4.6550
5.6250
-22.1770
02480
12180
-22.4930
0.9020
Upper
Labs limit
3 and p -11.9350
3andk 7.8700
3 and i 8.2700
1 and p -15.7400
1 and k 4.0650
1 and 1 4.4650
4 and p -16.8830
2 and p -17.4310
2 and p -19.2100
2 and k 4.1850
Difference
-13.6360
6.1690
6.5690
-17.3030
2.5020
2.9020
-18.5850
-19.0220
-21.1750
2.2200
Lower
limit
-15.3380
4.4670
4.8670
-18.8660
0.9390
1.3390
-20.2870
-20.6140
-23.1390
0.2560
Labs
3andk
3 and!
2 and p
4 and p
1 and p
Upper
limit
1.1860
1.2060
-1.1550
-1.1700
-1.2240
Difference
2.0710
2.0910
-0.3160
•0.3310
•0.4050
Lower
limit
0.3020
0.3220
-1.9940
-2.0090
-2.0430
' .05 level of significance; Tuke/s Studentized Range Test; DDRP labs -1 to 4; NC labs - c to r.
-------
Table 3*. Summary Statistic* lor ODRP and Non-Contract Laboratories
o
>—•
vO
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Group
NC
DORP
NC
ODRP
NC
DORP
NC
DORP
Number
of labs Mean
3 11.9233
3 8.7133
3 13.2517
4 9.1818
3 9.5133
4 5.7134
3 0.7833
4 0.8306
Sd
11.6445
1.9755
13.2360
2.5346
11.5516
2.4451
0.8805
0.4282
SE
6.6384
1.1406
7.6418
1.2673
6.6693
12225
0.5064
02141
Min
5.0200
7.1711
5.1300
7.3503
2.6450
3.8275
0.2650
0.5762
Max
25.6000
10.9401
28.5250
12.9263
22.6500
9.2138
1.8000
1.4713
Wlthln-Group and Between-Qroup Variabilities for DORP
and Non-Contract Laboratories
F
35.85
27.27
22.32
4.23
df
(22)
(2.3)
(2.3)
(2.3)
Pr > F*
o- .05
0.0541
0.0238*
0.0316*
0.2680
Variances |T|
Equal 0.4630
Unequal 0.5254
Unequal 0.5604
Equal -0.0954
df
4.0
2.1
21
5.0
Pr>|T|
a- .05
0.6674
0.6500
0.6293
0.9277
• If Pr > F Is less than 0.05, there Is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there Is a significant difference between
groups.
-------
D-192
-------
AUDIT
SOIL X
(A) 12.160
21.940
18.330
14.770
16.500
13.040
16.800
17.200
22.130
15.060
17.420
17.800
27.200
{Bs> 7.200
{1
34.800
20.930
18.410
16.800
18.850
16.800
25.300
33.260
20.540
21.260
25.700
29.350
Jw) 3.787
16.733
11.430
9.510
8.700
9.660
9.960
12.900
17.130
9.590
10.130
13.700
20.200
CATION EXCHANGE CAPACITY 1M NH4OAc
Y LAB
12.160
21.940
18.840
15.880
16.800
11.500
18.100
16.800
17.020
14.440
16.680
18.800
23.200
7.200
34.800
23.860
15.170
16.800
19.570
19.900
29.800
28.550
20.250
20.740
26.900
27.700
3.787
16.733
13.830
9.460
8.700
9.630
10.200
13.600
13.790
9.020
10.390
13.900
19.200
*
*
a
b
c
e
g
h
j
k
l
0
P
*
*
a
b
c
e
9
h
j
k
1
0
P
*
*
a
b
c
e
9
h
j
k
1
0
P
AUDIT
SOIL X
{C} -0.002
1.602
1.110
0.940
0.800
0.540
1.210
0.500
5.170
0.590
0.930
0.480
0.900
{B} 9.770
30.650
21.730
19.490
15.000
19.340
18.000
25.500
29.930
19.570
22.500
19.800
34.600
{0} 43.443
126.558
82.290
81.260
74.400
62.460
91.500
85.000
61.620
84.460
99.990
34.100
99.990
LAB
-0.002
1.602
1.270
0.680
0.800
0.770
1.300
0.600
2.420
0.770
0.800
0.470
0.700
9.770
30.650
24.160
20.930
15.000
18.040
18.200
25.800
29.080
19.630
21.380
19.900
35.400
43.443
126.558
89.890
89.600
79.200
68.130
94.500
85.000
53.700
84.980
99.510
31.600
99.990
*
*
a
b
c
e
g
h
j
k
1
0
P
*
• *
a
b
c
e
g
h
j
k
1
0
P
*
*
a
b
c
e
g
h
j
k
1
0
P
D-193
-------
Cation Exchange Capacity by Ammonium Acetate
A
30-
25-
en
O
O
20-
CT
-------
Cation Exchange Capacity by Ammonium Acetate
Bs
VO
Ol
40-
30-,
en
O
O
20,
cr
0)
E
10-
0-
0
N
11
22.565
&J 4.967
Medua 21.000
Mean
\
10 20
meq/100g
30
40
-------
Cation Exchange Capacity by Ammonium Acetate
Bw
o
20-
en
o
o
10H
cr
0)
E
5-
0-
0
N 11
Mean 12.029
Sd 1364
Median 10.260
10
meq/100g
15
20
-------
Cation Exchange Capacity by Ammonium Acetate
C
3.04
2.0-
O
O
1.0-
or
0>
E
0.0-
-1.0-
-1.0
0.0 1.0
meq/1 OOg
Lab j not shown
N II
Mean 1.060
Sd 0.932
MedUo 0^00
2.0
3.0
-------
Cation Exchange Capacity by Ammonium Acetate
B
O
oo
40
30,
en
o
O
20-
cr
-------
Cation Exchange Capacity by Ammonium Acetate
0
D
§
CT>
O
O
cr
a>
E
140-
120-
100-
80-
60-
40-
20-
20 40 60 80 100
meq/1 OOg
N 11
Mean 78.780
Sd 20.012
Median 85.000
I
120 140
-------
Cation Exchange Capacity In 1M NH4OAc
meq/100g
Table 1§. Summery Statistics for Tim*
Effect
TabU 1b. Analysis of Varlancs for Tims Effsct
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
O
to
8
Audit
samples
A
Bs
Bw
C
Table 2b.
Labs
3 and p
3 ando
3 and I
3andh
3 and c
3andk
3 and e
1 and p
1 andk
Number
Lab of labs Mean
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26 18.7644
28 15.4466
2 18.5850
2 15.3250
14 24.4112
22 21.6660
2 22.3850
2 16.7800
16 13.8384
12 10.1450
2 12.6300
2 8.4850
14 1.2691
10 0.8320
2 1.1900
2 0.8100
Standard Audit
deviation samples Source df
0.6615
1.0692
0.3606
0.7849
Z1985
1.7558
2.0718
2.2910
1.7122
1.2280
1.6970
0.0354
0.1256
0.2830
0.1131
0.1839
A Lab 1
Time 1
Lab*time 1
Error 54
Bs Lab 1
Time 1
Lab*time 1
Sum of
squares
40.2803
0.0843
0.0031
42.5506
62.4285
42.5320
7.3227
Error 36 137.1110
Palrwlse Comparison for Significant
Upper
limit
•1.366
6.384
6.784
6.834
7.184
9.084
11.564
-3.562
6.888
A'
Difference
Lower
limit
-7.287 -4.326
0.463
0.863
0.913
1.263
3.163
5.643
3.424
3.824
3.874
4.224
6.124
8.604
-0.309 -6.436
1.141
4.014
Labs
3 andk
Sande
3 and g
3 and c
4 and]
4ande
4 and g
4 and c
land)
Bw Lab 1
Time 1
Lab*time 1
Error 28
C Lab 1
Time 1
Lab*time 1
Error 24
40.8117
3.0465
0.2624
63.4439
0.5699
0.0087
0.0028
0.9724
Mean Pr > F Audit
Sum of
square F a - .05 samples Source df squares
40.2803 51.12 0.0001
0.0843 0.11 0.7448
0.0031 0.00 0.9501
0.7880
62.4285 16.39 0.0003*
42.5320 11.17 0.0020*
7.3227 1.92 0.1741
3.8088
40.8117 18.01 0.0002*
3.0465 1.34 0.2560
0.2624 0.12 0.7361
2.2659
0.5699 14.07 0.0010*
0.0087 0.22 0.6469
0.0028 0.07 0.7956
0.0405
A Lab
Error
Bs Lab
Error
Bw Lab
Error
C Lab
Error
11 512.8820
74 99.6584
12 587.5250
57 218.3954
12 378.1499
45 78.9234
12 21.7974
45 5.5203
Mean
square
46.6256
1.3467
48.9604
3.8315
31.5125
1.7539
1.8164
0.1227
Pr > F
F a -.05
34.62 OJ0001*
12.78 04001*
17.97 OJ0001*
14.81 04001*
Difference Between DORP and Non-Contract Laboratories
Bs
Upper
Lower
limit Difference limit
11.597 0.547
12.782 1.732
13.642 2.592
15.192 4.142
-0.458 -10.940
11.237 0.755
12.097 1.615
13.647 3.165
-1.379 -11.609
6.072
7.257
8.117
9.667
-5.699
5.996
6.856
8.406
-6.494
Bw
Upper
Labs limit Difference
3 and p -0.051 -7.611
3 and 1 9.389 1.829
3andg 9.569 2.009
3ande 10.004 2.444
3 and k 10.344 2.784
3andc 10.949 3.369
landp -2.389 -9.334
1 and 1 7.051 0.106
1 and g 7.231 0.266
Lower
limit
-3.831
5.609
5.789
6.224
6.564
7.169
-5.662
3.578
3.758
Upper
Labs limit
3 and ] -1.001
3 and k 2.114
3 and e 2.139
3 and h 2.244
3 and o 2.319
1 and j -1.600
4 and j -1.998
2 and j -2.015
C
Lower
Difference limit
-3.000
0.115
0.140
0.245
0.320
-3.451
-3.895
•3.911
-2.000
1.115
1.140
1.245
1.320
-2.526
-2.947
-2.963
(Continued)
-------
Table 2b. Continued
Bs
Bw
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
lande 9.368 3.621
2andp -6.687 -12.620
2 and j -1.262 -6.905
2 and • 6.043 0.310
• .05 level
Table 3a.
Audit
samples
A
Bs
Bw
C
6.494
-9.753
-4.128
3.177
1 and e 10.316 0.086
1 and o 11.176 0.946
1andc 12.726 2.496
2 and j -4.242 -14236
2andp -1.862 -11.856
2andh -0.887 -10.881
5201
6.061
7.611
-9.239
•6.859
-5.884
lande 7.666 0.721 4.193
1 and k 8.006 1.061 4.533
1 and c 8.611 1.666 5.138
4 and p -4.029 -11.589 -7.809
2 and p -6.019 -13.091 -9.555
2 and) -1.779 -8.851 -5.315
2ando -0.119 -7.191 -3.655
2andh 0.431 -6.641 -3.105
of significance; Tuke/s Studenttzed Range Test; DORP labs - 1 to 4; NC labs - c to r.
Summary Statistic* for DDRP and Non-Contract Laboratories
Group
NC
DDRP
NC
DDRP
NC
DDRP
NC
DDRP
Number
of labs
9
3
8
4
9
4
9
4
Mean
17.5828
18.3616
232261
24.4375
12.2444
12.9356
1.0972
1.1861
Sd
3.5402
2.7359
5.1157
£0323
3.6390
2.4698
1.0362
0.4534
SE
1.1801
1.5796
1.7052
1.0162
12130
12349
0.3454
02267
Min
122700
15.4466
16.8000
21.6660
8.7000
10.1450
0.4750
0.8320
Max
252000
20.8737
30.9050
26.4670
19.7000
15.8692
3.7950
1.7947
Table 3b. Wlthln-Group and Between-Graup Variabilities for DDRP
and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
F
1.67
6.34
2.17
522
Pr> FJ
df o - .05
(82]
(8.3
(8.3
(8.3
0.8537
0.1566
0.5652
02014
Variances
Equal
Equal
Equal
Equal
|T|
•0.3441
4.4490
-0.3424
-0.1616
df
10.0
11.0
11.0
11.0
Pr>|T|
0- .05
0.7379
0.6622
0.7385
0.8746
• If Pr > F Is less than 0.05. there is a significant difference within groups.
6 If Pr > |T| Is less than 0.05. there is a significant difference between
groups.
-------
D-202
-------
EXCHANGEABLE ACIDITY IN 1M KC1
AUDIT
SOIL X Y LAB
{A} 3.040 2.910 a
2.530 3.170 b
4.180 4.210 i
{Bs} 3.710 3.980 a
4.270 4.050 b
5.910 5.930 1
(Bw> 1.320 1.310 a
1.130 1.650 b
1.970 2.360 i
(C) 0.020 0.080 a
0.060 0.140 b
0.210 0.200 1
(B) 2.380 2.400 a
2.610 2.440 b
4.000 3.530 i
{0} 7.050 7.360 a
I 6.390 6.210 b
7.680 6.690 1
D-203
-------
D-204
-------
EXCHANGEABLE ACIDITY IN BaCl
AUDIT
SOIL
(A)
(Bs)
(Bw)
(C)
10.911
28.559
18.450
20.550
20.800
27.900
25.541
48.769
33.960
33.900
32.930
41.520
12.401
25.984
17.980
21.400
16.600
21.090
-0.615
.440
.000
,900
.630
4.
2.
0.
4.
2.420
10.911
28.559
17.370
21.550
16.040
26.190
25.541
48.769
36.310
44.450
28.210
42.510
12.401
25.984
17.290
20.100
13.190
20.580
-0.615
4.440
0.620
1.500
2.100
2.610
LAB
a
b
j
m
*
*
a
b
j
m
*
*
a
b
j
m
*
*
a
b
j
m
BaCl 2 TRIETHANOLAMINE
AUDIT
SOIL X Y
(B) 23.070
42.255
30.880
34.050
29.000
35.200
40.090
19.200
(0) -3.520
156.425
108.860
71.400
50.720
99.990
81.220
31.200
23.070
42.255
31.620
34.100
28.410
35.000
36.540
19.200
-3.520
156.425
109.690
68.750
42.630
99.990
84.440
28.800
LAB
*
*
a
b
j
1
m
o
*
*
a
b
j
1
m
0
D-205
-------
D-206
-------
CALCIUM EXTRACTABLE IN 0.002M
CaCl,
AUDIT
SOIL
(A)
(Bs)
{Bw}
(C)
(B)
{0}
0.270
0.440
0.470
0.450
0.530
0.620
0.053
0.670
0.690
0.740
0.780
0.820
0.450
0.540
0.570
.350
.030
1,
2.
1.520
0.
0.
0.
0.
.320
,460
0.050
0.048
.590
.065
0.710
0.650
0.700
0.570
0.810
0.830
0.420
.560
.580
.410
.020
0.
0.
1,
2.
1.360
LAB
a
b
e
a
b
e .
a
b
e
a
b
e
a
b
e
a
b
e
MAGNESIUM EXTRACTABLE IN 0.002M
CaCl,
LAB
AUDIT
SOIL X
(A) 0.170
0.150
0.140
0.210
{Bs} 0.040
0.040
0.030
0.050
{Bw} 0.030
0.040
0.030
0.040
{C} 0.020
0.010
0.020
0.020
{8} 0.060
0.050
0.060
0.080
{0} 0.490
0.600
0.530
1.220
0.180
0.140
0.120
0.210
0.040
0.030
0.030
0.060
0.030
0.050
0.030
0.060
0.010
0.010
0.010
0.020
0.050
0.060
0.050.
0.080
0.660
0.560
0.520
1.100
a
b
e
k
a
b
e
k
a
b
e
k
a
b
e
k
a
b
e
k
a
b
e
k
D-207
-------
D-208
-------
SODIUM EXTRACTABLE IN 0.002M
CaCl,
POTASSIUM EXTRACTABLE IN 0.002M
CaCl,
AUDIT
SOIL
(A)
{Bs}
(Bw)
(C)
(B)
{0}
0.060
0.040
0.100
0.030
0.010
0.010
0.060
0.010
0.020
0.020
0.080
0.020
0.050
0.050
0.040
0.120
0.060
0.320
,170
.480
0.
0.
0.360
0.040
0.030
0.050
0.040
0.020
0.010
0.050
0.020
0.020
0.020
0.070
030
040
050
0.040
0.110
0.060
270
160
560
0.
0.
0.
0.
0.
0.
0.370
LAB
a
b
e
k
a
b
e
k
a
b
e
k
e
a
b
e
k
a
b
e
k
AUDIT
SOIL X
{A} 0.090
0.070
0.070
0.120
{Bs} 0.020
0.010
0.010
0.020
{Bw} 0.010
0.010
0.010
0.020
{C} 0.010
0.010
0.010
0.020
{B} 0.020
0.020
0.020
0.040
{0} 0.590
0.290
0.410
0.800
Y
0.080
0.060
0.060
0.120
0.010
0.010
0.010
0.020
0.010
0.010
0.010
0.020
0.010
0.010
0.010
0.020
0.020
0.020
0.020
0.040
0.540
0.350
0.510
0.780
LAB
a
b
e
k
a
b
e
k
a
b
e
k
a
b
e
k
a
b
e
k
a
b
e
k
D-209
-------
D-210
-------
IRON EXTRACTABLE IN 0.002M
CaCl,
ALUMINUM EXTRACTABLE IN 0.002M CaCl,
AUDIT
SOIL
{A}
{Bs}
{Bw}
{C}
{B}
{0}
0.020
0.020
1.470
0.050
0.050
0.010
1.750
0.030
0.130
0.540
0.030
0.010
1.020
0.020
0.020
1.430
0.050
0.040
0.010
720
030
100
540
0.030
0.010
0.940
1.
0.
0.
0.
LAB
a
b
9
a
b
e
g
g
g
g
a
b
g
AUDIT
SOIL
{A}
{Bs}
{Bw}
{C}
{B}
{0}
0.120
0.120
0.020
5.770
0.200
0.250
0.040
11.120
1.440
0.410
0.020
0.040
3.090
0.270
0.160
0.040
10.280
0.120
0.100
0.020
5.560
0.220
0.190
0.040
11.340
1.110
0.890
0.030
0.020
3.340
0.280
0.140
0.050
11.120
LAB
a
b
e
g
a
b
e
g
g
g
a
b
g
a
b
e
g
D-211
-------
D-212
-------
ALUMINUM EXTRACTABLE IN 1M KCL
AUDIT
SOIL X
{A} 2.055
3.765
2.640
2.980
0.930
3.590
2.590
3.110
{Bs} 3.140
4.670
3.750
4.100
1.240
4.980
3.720
4.110
{Bw} 1.010
1.730
1.470
1.150
0.450
1.910
1.190
1.370
055
765
370
840
0.920
,770
,490
,110
.140
,670
,310
,710
0.870
4,
3.
3,
1.
1,
670
350
980
010
730
1.000
1.590
0.450
.710
.090
1.390
LAB
*
*
a
b
e
j
k
m
*
*
a
b
e
j
k
m
*
*
a
.b
e
j
k
m
AUDIT
SOIL
LAB
{C} 0.018
0.152
0.050
0.060
0.070
0.120
0.120
{B} 1.435
3.100
2.170
2.640
0.830
3.360
2.100
2.590
{0} 2.373
4.847
3.790
4.040
1.260
4.830
3.220
3.390
0.018
0.152
0.120
0.060
0.070
0.110
0.130
1.435
3.100
1.990
2.270
0.820
3.160
1.950
2.570
2.373
4.847
3.750
3.710
1.140
3.760
2.880
3.510
*
*
b
e
j
k
m
*
*
a
b
e
j
k
m
*
*
a
b
e
j
k
m
D-213
-------
Exchangeable Aluminum in Potassium Chloride
A
4.5-
3.5-
CT>
O
o
2.5-
cr
0)
E
1.5-
0.5-
0.5 1.5
N 6
Mean 2.612
Sd 0.932
Median 2.725
I
2.5
meq/100g
3.5 4.5
-------
Exchangeable Aluminum in Potassium Chloride
Bs
O
6.04
5.0-
4.0-
cn
O
O
3.0-
cr
Q)
E
2.0-
1.0-
0.0-
0.0 1.0
2.0 3.0 4.0
meq/100g
N 6
Mean 3.481
Sd 1.280
Median 3.720
I ' I
5.0 6.0
-------
Exchangeable Aluminum in Potassium Chloride
Bw
O
N>
ON
2.25
1.75
C7>
O
O
1.25
cr
E
0.75-
0.25-
0.25
0.75 1.25
meq/100g
N 6
Mean 1.231
Sd 0.446
Median 1J03
1.75
2.25
-------
Exchangeable Aluminum in Potassium Chloride
C
O
K)
0.304
0.20-
CJ>
O
O
0.10-
cr
0)
E
0.00-
-0.10-
-0.10
0.00 0.10
meq/100g
\
N J
Mean 0.091
Sd 0.028
Median 0.085
\
0.20
0.30
-------
Exchangeable Aluminum in Potassium Chloride
B
9
to
»—'
oo
en
O
O
cr
-------
Exchangeable Aluminum in Potassium Chloride
0
O
K>
ND
5.5-
4.5-
O
O
5-
H
cr
0)
E2.5
1.5-
0.5-
0
.5 1.5
a
2.5 3.5
meq/100g
N 6
Mean 3.273
Sd 1.098
Median 3.610
4.5 5.5
-------
o
to
K>
O
Table la. Summary Statistics for Tlma
Effect
Aluminum Extractable in 1M KCL
meq/IOOg
Table 1b. Analysis of Variance for Time Effect
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit
samples
A
Bs
Bw
C
Number Standard Audit Sum of
Lab of labs Mean deviation samples Source df squares
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26 2.6385 02238
28 3.1429 0.3051
2 2.9750 0.0919
2 2.8500 0.4526
14 3.7206 0.5248
22 3.9265 0.5725
2 3.6450 0.1909
2 4.1600 0.1556
16 1.4416 0.1672
12 1.3133 02165
2 1.3150 0.0071
2 1.3900 0.3677
14 0.0546 0.0407
10 0.1176 0.0393
2 0.0500 0.0424
2 0.1000 0.0566
A Lab 1
Time 1
Lab'time 1
Error 54
Bs Lab 1
Time 1
Lab*tlme 1
0.1340
0.0018
0.3688
3.9786
0.2430
0.1147
0.0107
Error 36 10.5229
Bw Lab 1
Time 1
Lab*time 1
Error 28
C Lab 1
Time 1
Lab*time 1
Error 24
Table 2b. Palrwlae Comparison for Significant Oil ferance Between
Labs
2 and I
2 and o
2 and)
2 and)
2 and m
3 and 1
3 and o
3 and]
Sandl
3 and m
landi
Upper
limit
•0.4842
3.7008
3.7008
3.7008
3.7008
•0.5503
3.6447
3.6447
3.6447
3.6447
-0.9971
A"
Lower
Difference limit
-1.0521 -1.6101
3.1429 2.5649
3.1429 2.5649
3.1429 2.5649
3.1429 2.5649
-1.1266 -1.7028
3.0684 2.4922
3.0684 2.4922
3.0664 2.4922
3.0664 2.4922
-1.5565 -2.1159
Labs
4andj
4andl
4 and m
4 ando
2 and I
2 and |
2 and I
2 and m
2 and o
land!
land)
Bs
Upper
limit Difference
6.700 4.781
6.700 4.781
6.700 4.781
6.700 4.781
-0.164 -1.994
5.756 3.926
5.756 3.926
5.756 3.928
5.756 3.926
•0.327 -2.199
5.593 3.721
0.0025
0.0022
0.0360
1.1859
0.0109
0.0004
0.0001
0.0405
Mean Pr > F Audit Sum of
square F o - .05 samples Source df squares
0.1340 1.82 0.1831
0.0018 0.02 0.8772
0.3688 5.01 0.0294*
0.0737
0.2430 0.83 0:3680
0.1147 0.39 0.5350
0.0107 0.04 0.6497
02923
0.0025 0.06 0.8108
0.0022 0.05 0.8225
0.0360 0.85 0.3641
0.0424
0.0109 6.46 0.0179*
0.0004 0.25 0.6213
0.0001 0.00 0.7731
0.0017
A Lab
Error
Bs Lab
Error
Bw Lab
Error
C Lab
Error
Mean
square F
Pr >F
a -.05
7 70.1901 10.0272168.44 00001*
70 4.1672 0.0595
8130.7737 16.3467 27.85 00001*
53 31.1137 0.5671
8 17.6609
41 1.2612
8 0.1949
41 0.0565
2.2326 72.58 00001*
0.0308
0.0244 17.09
0.0014
04001*
>
ODRP and Non-Contract Laboratories
Lower
limit
2.862
2.662
2.662
2.862
-3.623
2.097
2.097
2.097
2.097
-4.072
1.648
Bw
Upper
Labs limit Difference
4 and j 2.3478 1.8792
4 and I 2.3478 1.8792
4 and m 2.3478 1.8792
4 and o 2.3478 1.6792
3 and I -0.0995 -0.5682
3 and j 2.0655 1.5968
3 and 1 2.0655 1.5968
3 and m 2.0655 1.5966
3 ando 2.0655 1.5968
1 and I -0.2930 -0.7234
1 and j 1.8720 1.4416
Lower
limit
1.4105
1.4105
1.4105
1.4105
-1.0368
1.1282
1.1262
1.1282
1.1282
-1.1539
1.0111
Labs
Sandj
3 and!
3 and m
3 and o
4 and!
4 and I
4 and m
4 and o
2 and]
2 and!
2 and m
Upper
limit
0.2857
0.2857
0.2857
0.2857
0.2362
0.2382
0.2382
0.2382
0.2133
0.2133
02133
C
Difference
0.1848
0.1648
01848
0.1848
0.1425
0.1425
0.1425
0.1425
0.1176
0.1176
0.1176
Lower
limit
0.0839
0.0839
0.0839
0.0839
0.0468
0.0468
0.0468
0.0468
0.0219
0.0219
0.0219
(Continued)
-------
Table 2b. Continued
d
to
Bs
Bw
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
1 and o
land |
1 andl
1 and m
3.1979
3.1979
3.1979
3.1979
2.6385
2.6385
2.6385
26385
20791
20791
20791
20791
1 and I 5.593
1 and m 5.593
1 and o 5.593
3 and I -0.262
3 and j 5.658
,3 and I 5.658
3 and m 5.658
3 and o 5.658
3.721
3.721
3.721
-2.265
3.635
3.635
3.635
3.635
1.848
1.848
1.848
-4.308
1.612
1.612
1.612
1.612
1andl
1 and m
1 ando
2andi
2 and j
2 andl
2 and m
2 and o
1.8720
1.8720
1.8720
-0.4133
1.7517
1.7517
1.7517
1.7517
1.4416
1.4416
1.4416
•0.8517
1.3133
1.3133
1.3133
1.3133
1.0111
1.0111
1.0111
-1.2901
0.8749
0.8749
0.8749
0.8749
2 ando 0.2133 0.1176 0.0219
1 and 1 -0.0569 -0.1504 -0.2438
' .05 level of significance; Tuke/s Studentlzed Range Test; DDRP labs -1 to 4; NC labs - c to r.
Table 3a. Summary Statistics for DORP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Group
NC
DDRP
NC
DDRP
NC
DDRP
NC
DDRP
Number
of labs
5
3
5
4
5
4
5
4
Mean
0.8390
29499
1.1840
4.0157
0.4330
1.5577
0.0410
0.1249
Sd
1.8761
0.2723
26475
0.5246
0.9682
0.2436
0.0917
0.0544
SE
0.6390
0.1572
1.1840
0.2623
0.4330
0.1218
0.0410
0.0272
Min
0.0000
2.6385
0.0000
3.6350
0.0000
1.3133
0.0000
0.0546
Max
4.1950
3.1429
5.9200
4.7809
21650
1.8792
0.2050
0.1848
Table 3b. Wlthln-Croup and Between-Group Variabilities for DDRP
and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
F
47.47
25.47
15.79
284
df
(4.2)
4.3
(4.3)
(4.3)
Pr > f
o - .05
0.0415*
0.0238*
0.0470*
0.4182
Variances
Unequal
Unequal
Unequal
Equal
m
-2.4730
-23351
-25004
-1.6048
df
4.3
4.4
4.6
7.0
Pr>|T|
a - .05
0.0653
0.0748
0.0591
0.1526
* If Pr > F Is less than 0.05, there is a significant difference within groups.
* If Pr > |T| is less than 0.05. there Is a significant difference between
groups.
-------
D-222
-------
IRON EXTRACTABLE IN SODIUM PYROPHOSPHATE
AUDIT
SOIL X
(A) 0.206
0.641
0.500
0.480
0.320
0.440
0.360
0.370
0.510
(Bs) 0.306
0.893
0.540
0.590
0.440
0.590
0.630
0.320
0.620
(Bw> 0.325
1.015
0.660
0.620
0.470
0.720
0.580
0.490
0.750
Y
0.206
0.641
0.570
0.550
0.330
0.410
0.390
0.370
0.490
0.306
0.893
0.540
0.610
0.470
0.670
0.880
0.290
0.680
0.325
1.015
0.720
0.720
0.490
0.730
0.600
0.500
0.740
LAB
*
*
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
AUDIT
SOIL X
(C) 0.005
0.065
0.040
0.040
0.030
0.010
0.040
0.020
0.020
(B) 0.250
0.940
0.540
0.610
0.430
0.600
0.720
0.410
0.680
{0} 0.052
0.126
0.090
0.110
0.080
0.140
0.090
0.060
0.110
0.
0.
0.005
0.065
0.030
0.060
0.040
0.030
0.040
0.020
0.030
.250
.940
0.610
0.680
0.430
0.590
0.710
0.410
0.640
.052
127
0.090
0.110
0.090
0.180
0.080
0.060
0.110
0.
0.
LAB
*
*
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
D-223
-------
Extractable iron in Sodium Pyrophosphate
A
a
0.75-T
0.65-
0.55-
,0.45-
0.35-
0.25-
0.15-
N 7
Mean 0.435
Sd 0.082
Median 0.42S
i • r • i ' i
0.15 0.25 0.35 0.45
T
0.55 0:65 0.75
weight
-------
Extractable Iron in Sodium Pyrophosphate
Bs
K>
IO
1.0-
0.8-
^0.6-
'(U
0.4-
0.2-
0
.2
m
0.4 0.6
weight %
N 7
Mean 0.562
Sd 0.147
Median 0.600
I
0.8 1.0
-------
Extroctoble Iron in Sodium Pyrophosphate
Bw
O
fe
o\
1.2
1.0-
0.8
0.6-
0.4-
0.2-
0
.2 0.4
0.6 0.8
weight %
N 7
Mean 0.628
Sd 0.108
Median 0.670
1.0 1.2
-------
Extractable Iron in Sodium Pyrophosphate
C
o
0.08-
0.06^
CJ»
0.04-
0.02-
0.00-
0.00 0.02
0.04
weight %
N 7
Mean 0.032
Sd 0.011
Median 0.015
0.06 0.08
-------
10
00
0.9-
0.7-
0.5-
0.3-
Extractable Iron in Sodium Pyrophosphate
B
1.1
0.1 -
0.1 0.3
0.5 0.7
weight %
N 7
Mean 0376
Sd 0.116
Median 0.595
0.9 1.1
-------
Extroctoble Iron in Sodium Pyrophosphate
0
D
N)
0.184
0.15-
0.12-
0.09-
0.06-
0.03-
i ' i
0.03 0.06
N 7
Mean 0.100
Sd 0.031
Median 0.090
0.09 0.12
weight %
0.15 0.18
-------
Iron Extractable in Sodium Pyrophosphate
wt%
Table 1a. Summary Statistics for Tim*
Effect
Tabl* 1b. Analysis of Variance for Tim* Effect
Tabl* 2a. Analysis of Variance for Homogeneity of
Laboratories
d
to
o
Audit
samples
A
Bs
Bw
C
Table 2b.
3
3
3
3
3
2
2
2
Labs
and p
and d
andk
and m
and c
andd
andk
and m
Number
Lab of labs Mean
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26 0.6232
28 0.6410
2 0.5350
2 0.5150
14 0.5936
22 0.5930
2 0.5400
2 0.6000
16 0.8115
12 0.8215
2 0.6900
2 0.6700
14 0.0389
10 0.0329
2 0.0350
2 0.0500
Standard Audit
Sum of
deviation samples Source df squares
0.0689
0.0589
0.0495
0.0495
0.0478
0.0875
0.0000
0.0141
0.0716
0.1265
0.0424
0.0707
0.0102
0.0065
0.0071
0.0141
A
Bs
Bw
C
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab'time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
Palrwlse Comparison for Significant Difference Between
Upper
limit
0.3160
0.3910
0.4410
0.4460
0.4910
0.3656
0.4156
0.4206
A'
Lower
Difference
0.1616
0.2366
0.2866
0.2916
0.3366
0.2160
0.2660
0.2710
limit Labs
0.0071 4 and c
0.0821 4 and m
0.
0.
0.
1321 3 and c
1371 3 and m
1821 1 and m
0.0664 2 and m
0.
0
.1164
1214
Bs
Upper
limit Difference
0.3996 0.2113
0.5496 0.3613
0.3971 0.1987
0.5471 0.3487
0.4724 0.2886
0.4675 0.2880
0.0000
0.0427
0.0013
0.2173
0.0032
0.0020
0.0033
0.1907
0.0001
0.0650
0.0008
0.2595
0.0001
0.0001
0.0004
0.0020
Mean
square
0.0000
Pt > F Audit Sum of Mean Pr > f
F o = .05 samples Source df squares square F a - .05
0.00 0.9735
0.0427 10.61 0.0010*
0.0013
0.0040
0.0032
0.0020
0.0033
0.0053
0.0001
0.0650
0.33 0.5677
0.60 0.4450
0.37 0.5477
0.62 0.4360
0.01 0.9232
7.02 0.0131*
A Lab 7 0.5490 0.0784 18.34 00301*
Error 70 0.2994 0.0043
Bs Lab 8 0.3321 0.0415 7.35 00001*
Error 53 0.2995 0.0057
Bw Lab 8 0.6295 0.0787 10.25 0.0001*
Error 41 0.3146 0.0077
0.0008 0.08 0.7733
0.0093
0.0001
0.0001
0.0004
0.0001
0.83 0.3705
1.79 0.1934
4.57 0.0430*
C Lab 8 0.0018 0.0002 2.81 0.0141*
Error 41 0.0033 0.0001
ODRP and Non-Contract Laboratories
Lower
limit
0.0231
0.1731
0.0002
0.1502
0.1049
0.1086
Bw
Upper
Labs limit Difference
3 and
3 and
3 and
2 and
2 and
2 and
land
1 and
k 0.5848 0.3507
m 0.6798 0.4457
C 0.6948 0.4607
k 0.4504 0.2315
m 0.5454 0.3265
C 0.5604 0.3415
k 0.4365 0.2215
m 0.5315 0.3165
C
Lower Upper Lower
limit Labs limit Difference limit
0.1166
0.2116
0.2266
0.0125
0.1075
0.1225
0.0065
0.1015
(Continued)
-------
Table 2b. Continued
Bs
Bw
Upper Lower
Labs limit Difference limit
2andc 0.4656 0.3160 0.1664
1 and d 0.3481 0.1982 0.0483
1 and k 0.3981 0.2482 0.0983
1 and m 0.4031 0.2532 0.1033
1 and c 0.4481 0.2982 0.1483
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
Upper Lower
Labs limit Difference limit
1 and c 0.5465
4 and m 0.4691
4 and c 0.4841
0.3315 0.1165
0.2350 0.0009
0.2500 0.0159
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC labs - c to r.
Table 3a. Summary Statistics for DORP end Non-Contract Laboratories
Audit Number
samples Group of labs Mean
Sd
SE
Win
Max
A
Bs
Bw
NC
DDRP
NC
DDRP
NC
DDRP
5
3
5
4
5
4
0.3990
0.6419
0.5590
0.6267
0.6070
0.8259
0.0667
0.0192
0.1782
0.0388
0.1244
0.0868
0.0298
0.0111
0.0797
0.0194
0.0556
0.0434
0.3250
0.6232
0.3050
0.5930
0.4800
0.7300
0.5000
0.6616
0.7550
0.6663
0.7450
0.9407
C
NC
DDRP
5
4
0.0280
0.0381
0.0091
0.0036
0.0041
0.0018
0.0200
0.0329
0.0400
0.0415
Table 3b. Wlthln-Group and B«twe«n-Group Variabilities for DDRP
and Non-Contract Laboratories
Audit
samples
df
Pr > F*
a - .05
Variances
m
df
Pr > |T|
a - .05
A
Bs
Bw
C
12.04
21.07
2.06
6.20
(4.2)
(4.3)
(4.3)
(4.3)
0.1563
0.0312*
0.5801
0.1656
Equal
Unequal
Equal
Equal
-5.9891
-0.8248
-2.9699
-2.0646
6.0
4.5
7.0
7.0
0.0010*
0.4517
0.0208*
0.0778
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| is less than 0.05, there is a significant difference between
groups.
-------
D-232
-------
ALUMINUM EXTRACTABLE IN SODIUM PYROPHOSPHATE
AUDIT
SOIL X
(A) 0.308
0.532
0.590
0.460
0.460
0.420
0.370
0.400
0.420
(Bs) 0.657
0.972
0.850
0.750
0.770
0.830
0.830
0.520
0.800
(Bw) 0.415
0.625
0.540
0.490
0.630
0.550
0.520
0.360
0.510
0.
0.
0.
0.308
0.532
0.750
,500
.430
.420
0.370
0.410
0.420
0.657
0.972
.780
.790
0.770
0.920
.220
.480
0.870
0.415
0.625
0.600
0.530
0.750
0.560
0.520
0.340
0.490
0.
0.
1
0,
LAB
*
*
a
b
c
d
k
m
P
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
AUDIT
SOIL
LAB
{C} 0.005
0.095
0.070
0.060
0.040
0.040
0.060
0.020
0.040
{B> 0.667
0.982
0.800
0.800
0.780
0.810
0.960
0.630
0.910
{0} 0.148
0.282
0.220
0.240
0.280
0.200
0.210
0.160
0.250
0.005
0.095
0.050
0.070
0.030
0.060
0.070
0.020
0.050
0.667
0.982
0.860
0.840
0.770
0.840
1.000
0.610
0.850
0.148
0.282
0.210
0.230
0.280
0.210
0.220
0.160
0.250
*
*
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
*
*
a
b
c
d
k
m
P
.D-233
-------
Extroctoble Aluminum in Sodium Pyrophosphcite
A
1.0-r
9
to
0.8
0.6-
0.4-
0.2-
0.0-
0
.0 0.2
0.4 0.6
weight %
N 7
Mean 0.459
Sd 0.099
Median 0.420
0.8 1.0
-------
Extractoble Aluminum in Sodium Pyrophosphate
Bs
1.4
a
N>
Ul
1.2-
1.0
(D
0.8-
0.6-
0.4-
m
0.4 0.6
I T I
0.8 1.0
N 7
Mean 0.799
Sd 0.158
Median 0.815
I
1.2 1.4
weight %
-------
Extractable Aluminum in Sodium Pyrophosphate
0.8-T
o
to
o\
0.6-
CT»
0.4-
0.2-
0.2
m
0.4 0.6
weight %
N 7
Mean 0.528
Sd 0.101
Median 0.520
0.8
-------
Extroctoble Aluminum in Sodium Pyrophosphate
C
0.12-
o
to
O.OSi
K 0.06J
1 0.04J
0.02-
0.00-
-.02-
N 7
Mean 0.049
Sd 0.017
Median 0.050
I ' I T I ' I ' I ' I ' I ' I
-.02 0.00 0.02 0.04 0.06 0.08 0.10 0.12
weight %
-------
Extroctoble Aluminum in Sodium Pyrophosphote
B
o
oo
1.104
1.00-
0.90-
.0.80-1
0.70-
0.60-
0.50-
m /
T^ ' I^ I ' I ' I
0.50 0.60 0.70 0.80 0.90
N 7
Mean 0.819
Sd 0.109
Median 0.825
I r I
r.oo 1.10
weight
-------
Extendable Aluminum in Sodium Pyrophosphate
O
N>
UJ
VO
0.30-1
0.27-
0.24-
,0.21
0.18-
0.15-
0.12-
N 7
Mean 0.223
Sd 0.038
Median 0.215
I
0.12 0.15 0.18 0.21 0.24
weight %
0.27 0.30
-------
Aluminum Extractable in Sodium Pyrophosphate
wt %
Table 1a. Summary Statistics for Tim*
Effect
Audit Number Standard
samples Lab of labs Mean deviation
Table 1b. Analysis of Variance for Tim* Effect
A
Bs
Bw
C
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
0.6493
0.6379
0.6700
0.4800
0.7678
0.7951
0.8150
0.7700
0.6115
0.5444
0.5700
0.5100
0.0566
0.0464
0.0600
0.0650
0.1339
0.1068
0.1131
0.0283
0.0569
0.1079
0.0495
0.0283
0.0796
0.0595
0.0424
0.0283
0.0091
0.0115
0.0141
0.0071
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab* time 1
Error 24
Sum of
squares
0.0378
0.0175
0.0297
0.7697
0.0013
0.0000
0.0024
0.2898
0.0141
0.0050
0.0000
0.1365
0.0000
0.0004
0.0002
0.0025
Mean
square
0.0378
0.0175
0.0297
0.0143
0.0013
0.0000
0.0024
0.0080
0.0141
0.0050
0.0000
0.0049
0.0000
0.0004
0.0002
0.0001
F
2.65
1.23
2.08
0.16
0.00
0.30
2.89
1.03
0.01
0.22
3.92
1.89
Pr > F
a = .05
0.1094
0.2724
0.1547
0.6932
0.9822
0.5847
0.1000
0.3187
0.9248
0.6407
0.0593
0.1820
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F a - .05
A Lab 7 0.51B9 0.07413 6.44 0X1001*
Error 70 0.6054 0.0115
Bs Lab 8 0.3553 0.0444 4.36 0X1004*
Error 53 0.5399 0.0102
Bw Lab 8 0.1844 0.0231 4.93 00000*
Error 41 0.1915 0.0047
C Lab 8 0.0049 0.0006 5.26 00001*
Error 41 0.0047 0.0001
Table 2b. Palrwlse Comparison for Significant Difference Between ODRP and Non-Contract Laboratories
Bs
Bw
Labs
1 and k
2andk
Upper
limit Difference
0.5252 0.2793
0.5132 0.2679
Lower
limit
0.0334
0.0226
Labs
4 and m
3 and m
2 and m
1 and m
Upper
limit
0.6281
0.5998
0.5361
0.5345
Difference
0.3753
0.3333
0.2951
0.2878
Lower
limit
0.1226
0.0669
0.0541
0.0411
Upper
Labs limit
1 and m 0.4293
3 and m 0.4220
2 and m 0.3652
4 and m 0.3693
Difference
0.2615
0.2393
0.1944
0.1866
Lower
limit
0.0937
0.0567
0.0235
0.0040
Upper
Labs limit Difference
3 and c 0.02933 0.05807
3 and m 0.07307 0.04433
4 and m 0.06488 0.03762
1 and m 0.06324 0.03664
Lower
limit
0.00060
0.01560
0.01036
0.01004
" .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to14; NC labs - c to r.
-------
Table 3a. Summary Statistic* (or DORP and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Number
Group of labs Mean
NC
DORP
NC
DORP
NC
DDRP
NC
DORP
Wlthln-Group
Non-Contract
F df
5.20 (2.4)
22.87 (4.3)
11.52 (4.3)
5.16 (4.3)
5
3
5
4
5
4
5
4
0.4120
0.6075
0.8010
0.8229
0.5230
0.5705
0.0430
0.0562
Sd
0.0275
0.0628
0.1926
0.0403
0.1218
0.0359
0.0168
0.0074
SE
0.0123
0.0362
0.0861
0.0201
0.0545
0.0179
0.0075
0.0037
Min
0.3700
0.5354
0.5000
0.7878
0.3500
0.5366
0.0200
0.0464
Max
0.4450
0.6493
1.0250
0.8753
0.6900
0.6115
0.0650
0.0643
and B«tws«n-Group Variabilities tor DORP and
Laboratories
Pr > F'
o - .05 Variances |T|
0.1544
0.0278*
0.0728
0.2090
Equal -6.2796
Unequal -0.2474
Equal -0.7443
Equal -1.4524
df
6.0
4.4
7.0
7.0
Pr> |T|
a - .05
0.0008*
0.8157
0.4810
0.1897
If Pr > F is less than 0.05. there is a significant difference within groups.
If Pr > |T| is less than 0.05. there is a significant difference between
groups.
-------
D-242
-------
IRON EXTRACTABLE IN CITRATE-OITHIONATE
AUDIT
SOIL X
.{A} 1.053
2.041
1.250
1.600
1.600
1.720
1.460
0.550
(Bs) 0.738
1.006
0.640
0.890
1.180
0.900
0.910
0.780
(Bw) 1.190
1.940
1.240
1.670
1.600
1.610
1.550
0.970
1.053
2.041
1.310
1.620
1.600
1.600
1.530
0.520
0.738
1.006
0.720
0.780
1.220
0.920
0.910
0.860
190
1.940
1.440
510
1.520
1.720
1.590
1.040
1
1
LAB
*
*
a
b
d
j
m
P
*
*
a
b
d
j
m
P
*
a
b
d
j
m
P
AUDIT
SOIL
LAB
(C) 0.046
0.241
0.140
0.150
0.650
0.180
0.200
0.050
{B} 0.805
1.795
1.020
1.420
1.480
1.290
1.310
0.960
{0} 0.106
0.273
0.170
0.230
0.700
0.250
0.190
0.060
0.046
0.241
0.120
0.150
0.640
0.100
0.190
0.060
0.805
1.795
1.190
1.460
1.390
1.320
1.280
0.960
0.106
0.273
0.200
0.240
0.630
0.110
0.200
0.070
*
*
a
b
d
j
m
p
r
*
*
a
b
d
j
m
p
r
*
*
a
b
d
j
m
P
D-243
-------
Extractable Iron in Citrate Dithionite
A
2.60-
2.20-
1.80-
-gj.40,
1.00-
0.60-
0.20-
0.20 0.60
1.00 1.40
weight
N 6
Mean 1.363
Sd 0.428
Median 1-548
I
I
1.80 2.20 2.60
-------
Extractoble Iron in Citrate Dithionite
Bs
o
to
1.4-j
1.2-
1.0-
SI
cr>
0.8-
0.6-
0.4-
' i • i • i
0.4 0.6 0.8 1.0
N 6
Me*n 0.891
Sd 0.173
Median OJ71
I
1.2 1.4
weight
-------
Extractable Iron in Citrate Dithionite
Bw .
3.0-r
9
to
2.5-
2.0-
JZ
C7>
1.5-
1.0-
0.5-
0.5 1.0
1.5 2.0
weight %
N 6
Mean 1.455
Sd 0.246
Median 1365
2.5 3.0
-------
Extractable Iron in Citrate Dithionite
C
0.3-
0.2-
0.2-
(U
0.1 -
0.1 -
0.0-
I ' I
0.0 0.1
Lab d not shown
I ' I ' I
0.1 0.2 0.2
weight
N 6
Mean 0.219
Sd 0.213
Median 0.145
I
0.2 0.3
-------
o
oo
1.5-
1.0-
Extractable Iron in Citrate Dithionite
B
2.0-r
0.5-
0.5
1.0
1.5
weight %
N 6
Mem 1.257
Sd 0.190
Median 1.300
2.0
-------
Extractoble Iron in Citrate Dithionite
0
0.8-
0.6-
•*-'
c n 4
cnU.^-
Q)
0.2-
0.0-
0
d
/
j
N 6
P Mean 0.2S4
Sd 0.209
Median 0.190
1 ' 1 ' 1 ' 1 ' 1
.0 0.2 0.4 0.6 O.e
weight %
-------
Iron Extractable in Citrate Dithionite
wt %
Table 1a. Summary Statistic* for Tim*
Effect
Table 1b. Analysis of Variance for Tim* Effect
9
N>
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
Mean
1.6984
1.5698
1.2800
1.6100
0.9584
1.0169
0.6800
0.8350
1.6034
1.5624
1.3400
1.5900
0.1789
0.1495
0.1300
0.1500
Standard
deviation
0.2179
0.4634
0.0424
0.0141
0.0685
0.1518
0.0566
0.0778
0.3644
0.2824
0.1414
0.1131
0.0332
0.0453
0.0141
0.0000
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab*time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 36
Lab 1
Time 1
Lab*time 1
Error 28
Lab 1
Time 1
Lab*time 1
Error 24
Sum of
squares
0.0378
0.1331
0.1958
6.9870
0.0408
0.1897
0.0083
0.5542
0.0381
0.0485
0.0739
2.9013
0.0001
0.0020
0.0021
0.0330
Mean
square
0.0378
0.1331
0.1958
0.1294
0.0408
0.1897
0.0083
0.0154
0.0381
0.0485
0.0739
0.1036
0.0001
0.0020
0.0021
0.0014
F
0.29
1.03
1.51
2.65
12.32
0.54
0.37
0.47
0.71
0.05
1.45
1.51
Pr > F
a *> .05
0.5913
0.3150
0.2240
0.1123
0.0012*
0.4662
0.5489
0.4994
0.4056
0.8173
0.2401
0.2305
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F o - .05
A Lab 6 7.2363 1.2061 11.48 00001*
Error 69 7.2503 0.1051
Bs Lab 7 0.6046 0.0864 5.11 00002*
Error 52 0.8787 0.0169
Bw Lab 7 2.3077 0.3297 4.43 00010*
Error 40 2.9742 0.0744
C Lab 7 0.5025 0.0718 61.38 00001*
Error 40 0.0468 0.0012
Table 2b. Palrwlee Comparison for Significant Difference Between DDRP and Non-Contract Laboratories
Bs
Bw
Labs
3
1
2
and
and
and
p
p
p
Upper
limit Difference
2.5929 1.6959
2.0340 1.1633
1.9032 1.0348
Lower Upper Lower Upper Lower
limit Labs limit Difference limit Labs limit Difference limit
0.7990 3andp 0.8599 0.4442 0.0284 3 and p 1.9981 1.1147 0.2313
0.2926
0.1663
Labs
3
3
1
1
2
4
and
and
and
and
and
and
d
P
d
P
d
d
Upper
limit
-0.2999
0.2901
-0.3636
0.2264
-0.3904
-0.3918
Lower
Difference limit
-0.4107
0.1793
•0.4661
0.1239
-0.4955
-0.4969
-0.5215
0.0685
•0.5687
0.0213
-0.6006
-0.6020
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC labs - c to r.
-------
Table 3a. Summary Statistic* for DORP and Non-Contract Laboratories
Audit
samples
A
8s
Bw
C
Group
NC
DORP
NC
DORP
NC
DORP
NC
DORP
Number
of labs
4
3
4
4
4
4
4
4
Mean
1.3225
1.8330
0.9600
1.0633
1.4500
1.7236
0.2588
0.1777
Sd
0.5294
0.3506
0.1655
0.1366
0.3004
0.2648
0.2638
0.0403
SE
0.2647
0.2024
0.0828
0.0683
0.1502
0.1324
0.1319
0.0202
Min
0.5350
1.5698
0.8200
0.9584
1.0050
1.5624
0.0550
0.1481
Max
1.6600
2.2309
1.2000
1.2642
1.6650
2.1197
0.6450
0.2343
s
Ul
Table 3b. Wlthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
Audit
samples
A
Bs
Bw
C
F
2.28
1.47
1.29
42.79
df
(3.2)
(3.3)
(3.3)
(3.3)
Pr > F"
a - .05
0.6386
0.7598
0.8408
0.0116*
Variances
Equal
Equal
Equal
Unequal
|T|
-1.4338
-0.9623
-1.3664
0.6073
df
5.0
6.0
6.0
3.1
Pr> |T|
a - .05
0.2111
0.3731
0.2208
0.5851
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| is toss than 0.05. there is a significant difference between
groups.
-------
D-252
-------
ALUMINUM EXTRACTABLE IN CITRATE-OITHIONATE
AUDIT
SOIL X
{A} 0.285
0.555
0.400
0.490
0.530
0.330
0.440
{8s} 0.295
1.225
0.590
0.820
0.920
0.620
0.970
{Bw> 0.331
0.796
0.480
0.590
0.660
0.480
0.740
0,
0.
0.285
0.555
440
520
0.510
0.380
0.390
0.295
225
660
0.700
0.950
0.610
1.060
0.333
0.798
0.540
0.540
0.670
0.500
0.750
1.
0.
LAB
*
*
a
b
d
m
P
*
*
a
b
d
m
P
*
*
a
b
d
m
P
AUDIT
SOIL
LAB
(C) 0.041
0.058
0.050
0.060
0.070
0.040
0.050
(B) 0.680
1.550
0.800
1.080
1.100
0.670
1.250
{0} 0.190
0.250
0.200
0.260
0.240
0.170
0.230
0.041
0.058
0.050
0.070
0.030
0.040
0.060
0.680
1.550
0.880
1.180
1.130
0.650
1.160
0.190
0.250
0.230
0.270
0.200
0.180
0.240
*
*
a
b
d
m
P
*
*
a
b
d
m
P
*
*
a
b
d
m
P
D-253
-------
Extractoble Aluminum in Citrate Dithionite
A
0.90
0.60
cr>
0.30
0.00-
0.00
0.30 0.60
weight %
N 5
Mean 0.443
Sd 0.069
Medua 0.420
I
0.90
-------
Extroctable Aluminum in Citrate Dithionite
Bs
9
K)
1.20-
0.90-
0.60-
0.30-
0.00-
• i "^ i ' i
0.00 0.30 0.60 0.90
N S
Mem 0.790
Sd 0.181
Median 0.760
! ' I
1.20 1.50
weight
-------
Extroctoble Aluminum in Citrate Dithionite
Bw
9
o\
1.0-
0.8 H
.0.6J
0.4-
0.2-
0
.2
0.4
0.6
weight %
N S
Mean 0.595
sa o.ioe
Median 0.565
I
0.8 1.0
-------
Extractable Aluminum in Citrate Dithionite
C
d
to
-J
0.10-
0.08^
0.06
en
0.04-
0.02-
0.00-
0.00 0.02
45 •
a
m
N 5
Mean 0052
Sd 0.009
Median 0.050
I ' I
0.04 0.06
0.08 0.10
weight %
-------
Extroctoble Aluminum in'Citrate Dithionite
B
oo
1.7
1.4-
cr»
1.1 -
0.8-
0.5-
m
I ' I
0.5 0.8
N S
MCM 0.990
Sd 0.231
Median 1.115
I
1.1
weight %
1.4 1.7
-------
Extractoble Aluminum in Citrate Dithionite
0
0.30T
0.25-
o
to
o«
NO
0.20-
a
m
0.15-
0.15
0.20 0.25
weight %
N S
Meu OJ22
Sd 0.013
MedUa 0.220
0.30
-------
Aluminum Extractable in Citrate Dithionite
Table 1«. Summary Statistics for Tim*
Effect
o
K)
Audit
samples
A
Bs
Bw
C
Lab
1
2
a
b
1
2
a
b
1
2
a
b
1
2
a
b
Number
of labs
26
28
2
2
14
22
2
2
16
12
2
2
14
10
2
2
Mean
0.4524
0.4920
0.4200
0.5050
0.7590
0.8395
0.6250
0.7600
0.5491
0.6805
0.5100
0.5650
0.0542
0.0577
0.0500
0.0650
Standard
deviation
0.0351
0.0904
0.0283
0.0212
0.0664
0.1167
0.0495
0.0849
0.1297
0.0859
0.0424
0.0354
0.0064
0.0218
0.0000
0.0071
Wt %
Table 1b. Analysis of Variance for Time Effect
Audit
samples
A
Bs
Bw
C
Source df
Lab 1
Time 1
Lab'time 1
Error 54
Lab 1
Time 1
Lab*time 1
Error 36
Lab 1
Time 1
Lab'time 1
Error 28
Lab 1
Time 1
Lab'time 1
Error 24
Sum of
squares
0.0145
0.0003
0.0019
0.2528
0.0416
0.0408
0.0027
0.3529
0.0303
0.0209
0.0051
0.3363
0.0003
0.0000
0.0001
0.0049
Mean
square
0.0145
0.0003
0.0019
0.0047
0.0416
0.0408
0.0027
0.0098
0.0303
0.0209
0.0051
0.0120
0.0003
0.0000
0.0001
0.0002
F
3.09
0.07
0.41
4.24
4.16
0.27
2.52
1.74
0.42
1.44
0.04
0.56
Pr > F
a - .05
0.0843
0.7856
0.5255
0.0468*
0.0487
0.6054
0.1234
0.1982
0.5204
0.2420
0.8417
0.4608
Table 2a. Analysis of Variance for Homogeneity of
Laboratories
Audit Sum of Mean Pr > F
samples Source df squares square F o - .05
A Lab 6 0.6092 0.1015 25.30 00001*
Error 69 0.2770 0.0040
Bs Lab 7 1.9297 0.2757 24.64 00001*
Error 52 0.5818 0.0112
Bw Lab 7 1.1639 0.1663 17.78 00001*
Error 40 0.3741 0.0094
C Lab 7 0.0081 0.0012 6.68 00001*
Error 40 0.0070 0.0002
Table 2b. Palrwlse Comparison for Significant Difference Between DORP and Non-Contract Laboratories
Labs
3 and m
3 and j
2 and)
1 andj
Upper
limit
0.3784
0.7334
0.6618
0.6225
A*
Difference
0.2031
0.5581
0.4920
0.4523
Lower
limit
0.0278
0.3828
0.3223
0.2822
Labs
4 and m
4 andj
3 and)
2 andj
1 andj
Upper
limit
0.6948"
1.3098
1.2544
1.1454
1.0722
Bs
Difference
0.3739
0.9889
0.9162
0.8395
0.7590
Lower
limit
0.0530
0.6680
0.5779
0.5335
0.4458
Labs
3 and m
3 and j
2 and j
4 and j
1 andj
Upper
limit
0.6285
1.1185
0.9736
0.9361
0.8369
Bw
Difference
0.3152
0.8052
0.6805
0.6228
0.5491
Lower
limit
0.0019
0.4919
0.3874
0.3095
0.2613
Labs
3 andj
4 andj
2 and j
1 and j
Upper
limit
0.1082
0.1048
0.0982
0.0938
C
Difference
0.0655
0.0642
0.0577
0.0542
Lower
limit
0.0228
0.0237
0.0171
0.0146
* .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC labs • c to r.
-------
Table 3a. Summary Statistics for DDRP and Non-Contract Laboratories
9
K>
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Group
NC
DORP
NC
DORP
NC
DORP
NC
DORP
Number
of labs Mean
4 0.3225
3 0.5008
4 0.6413
4 0.8759
4 0.4750
4 0.6644
4 0.0363
4 0.0604
Sd
0.2256
0.0534
0.4611
0.0990
0.3341
0.1081
0.0250
0.0054
SE
0.1128
0.0309
0.2306
0.0495
0.1670
0.0541
0.0125
0.0027
Min
0.0000
0.4523
0.0000
0.7590
0.0000
0.5491
0.0000
0.0542
Max
0.5200
0.5581
1.0150
0.9889
0.7450
0.8052
0.0550
0.0655
Wlthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
F
17.81
21.71
9.54
21.62
df
(3.2)
(3.3)
(3.3)
(3.3)
Pr > F'
a - .05
0.1073
0.0310*
0.0963
0.0311*
Variances |T|
Equal -1.3122
Unequal -0.9950
Equal -1.0788
Unequal -1.8926
df
5.0
3.3
6.0
3.3
Pr > |T|
a •=• .05
0.2465
0.3884
0.3221
0.1483
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| Is less than 0.05. there is a significant difference between
groups.
-------
D-262
-------
SULFATE EXTRACTABLE IN DEIONIZED WATER
AUDIT
SOIL X
{A} 24.064
30.589
29.945
28.380
24.730
41.600
31.780
25.000
(Bs) 5.267
14.583
9.765
11.650
11.360
22.400
9.140
8.480
(Bw) 17.282
21.568
20.894
18.520
16.260
23.190
19.540
LAB
24.064
30.589
24.708
27.440
26.740
32.000
31.090
26.190
5.267
14.583
6.471
11.710
11.810
19.200
10.710
8.480
17.282
21.568
20.424
19.940
16.260
20.740
19.310
*
*
a
b
e
g
k
q
*
*
a
b
e
g
k
q
*
*
a
b
e
k
q
UDIT
OIL
C)
1}
0}
X
2.045
5.466
4.588
3.200
4.900
1.830
3.900
10.580
16.610
14.322
13.140
13.150
11.820
11.800
29.289
46.320
31.138
43.460
31.200
59.520
38.470
2,
5,
2,
045
466
923
12.220
4,
2.
3
.680
.250
.400
10.580
16.610
30.813
14.380
14.040
11.300
11.700
29.289
46.320
43.158
42.190
37.660
58.250
37.140
LAB
*
*
a
b
e
k
q
a
b
e
k
q
* •
a
b
e
k
q
D-263
-------
Extroctable Sulfate in Water
A
O
K>
50-
40 H
en
E
20-
10-
10
20
30
mg S/kg
N 6
Mean 29.134
Sd 4311
McdUn 27.618
I
40
50
-------
Extractable Sulfate in Water
Bs
16-f
12-
cn
cn
E
8-
I
4
8 12
mg S/kg
N 6
Mean U.76S
Sd 4.672
Median 10.755
\
16
-------
Extractable Sulfote in Water
Bw
9
N)
30-
25-
Qi
2Q]
en
E
15-
10-
10
N 5
Mean 19.508
Sd 2.121
Median 19.425
I
15
20
mg S/kg
25
-------
Extractable Sulfate in Water
C
14-f
12-
10-
CO
01 c
E 6-
4-
2-
0-
0
a
i
2
6 8
mg S/kg
N 5
Mean 4.389
Sd 2.101
Median 3.756
I
10 12 14
-------
o
to
cn
cn
E
60-
50-
40-
30-1
Extractable Sulfate in Water
0
70-f
20-
10-
N 6
Mean 43.982
Sd 9.770
Median 40.315
I ' I
10 20
30 40 50
mg S/kg
60 70
-------
Table 3a. Summary Statistics for DORP and Non-Contract Laboratories
Audit
samples
A
C
Table 3b.
Audit
samples
A
C
Number
Group of labs Mean
NC 4 29.8913
DORP 3 29.7079
NC 3 3.4933
DDRP 4 2.7629
Sd
5.3493
2.4405
1.3817
0.6826
SE
2.6747
1.4090
0.7977
0.3413
Min
25.5950
26.9200
2.0400
1.9992
Max
36.8000
31.4578
4.7900
3.6500
Wlthln-Group and Between-Group Variabilities for DDRP
and Non-Contract Laboratories
Pr > F'
F df a - .05
4.80 (3.2) 0.3542
4.10 (2.3) 0.2775
Variances |T|
Equal 0.0543
Equal 0.9364
df
5.0
5.0
Pr > |T|
a = .05
0.9588
0.3921
M * If Pr > F is less than 0.05. there is a significant difference within groups.
£: * If Pr > |T| is less than 0.05. there is a significant difference between
£4 groups.
-------
NITRATE EXTRACTABLE IN DEIONIZED WATER
AUDIT
SOIL
.{A} 0.029
3.249
1.410
1.430
3.030
1.600
{Bs} 0.849
5.428
2.960
4.780
2.120
3.400
{Bw} 0.346
2.886
1.618
1.650
1.020
2.600
0,
3,
0.
5
3
4,
1.
2.
029
249
897
0.820
220
000
0.849
428
595
720
830
600
0.346
886
555
640
110
2.800
LAB
*
*
a
b
e
k
*
*
a
b
e
k
*
*
a
b
e
k
AUDIT
SOIL
(B)
-0.214
2.041
0.982
0.600
1.220
1.800
-0.549
4.559
1.950
1.910
2.010
3.600
{0} -2.020
5.673
1.572
1.750
1.220
7.000
-0.214
2.041
0.641
0.800
0.810
.200
.549
.559
.039
.120
.220
.400
.020
.673
.675
2.
-0.
4.
2.
2.
1
6.
-2.
5.
2.
1.310
1.510
4.800
LAB
*
*
a
b
e
k
*
*
a
b
e
k
*
*
a
b
e
k
D-273
-------
SULFATE ADSORPTION 6-POINT ISOTHERM
0-point isotherm
AUDIT
SOIL X
{A} 3.870
4.500
4.800
5.900
{Bs} 1.120
1.100
1.520
1.830
(Bw) 2.220
2.100
2.380
2.700
{C} 0.730
0.520
0.540
0.500
{B} 1.240
1.360
1.450
1.570
{0} 9.610
9.160
2.960
2.730
Y
3.450
4.360
4.660
5.130
1.010
1.020
1.510
1.500
2.080
2.010
2.300
2.430
0.310
0.680
0.640
0.570
1.190
1.230
1.290
1.900
8.250
9.350
2.820
3.630
LAB
a
b
k
p
a
b
k
p
a
b
k
p
a
b
k
p
a
b
k
p
r
a
b
k
P
2-point isotherm
AUDIT
SOIL X
{A} 5.180
5.760
6.470
6.570
{Bs} 2.650
2.900
3.300
3.030
{Bw} 2.610
3.020
3.380
3.300
{C} 2.940
2.400
2.310
2.370
{B} 2.020
2.350
2.400
2.800
{0} 12.600
11.340
5.230
5.770
LAB
4.860
5.650
5.820
6.300
2.780
2.580
3.280
3.130
3.140
2.940
3.200
3.730
2.400
2.280
2.820
2.700
2.000
2.140
2.500
2.470
10.160
11.460
5.250
4.900
a
b
k
P
a
b
k
P
a
b
k
P
a
b
k
P
a
b
k
P
a
b
k
P
D-275
-------
16-point isotherm
32-point isotherm
AUDIT
SOIL X
(A) 16.000
17.490
16.860
18.130
{Bs} 14.740
15.630
15.550
15.870
{Bw} 11.120
13.090
12.070
13.100
{C} 16.600
17.350
17.500
{B} 10.470
12.090
12.100
{0} 27.580
25.760
19.720
23.170
Y
15.100
17.040
17.350
16.870
14.800
15.480
15.530
14.370
11.060
12.920
12.340
12.030
15.960
16.900
11.630
10.870
11.370
12.730
25.780
25.540
19.810
26.500
LAB
a
b
k
P
a
b
k
P
a
b
k
P
a
b
P
a
b
P
a
b
k
P
AUDIT
SOIL
{A}
{Bs}
{Bw}
{C}
{B}
{0}
X
29.020
30.940
32.220
27.000
28.580
28.960
29.040
28.170
21.440
24.530
24.190
22.170
31.560
31.750
33.540
32.170
22.150
24.880
24.030
19.30
42.740
39.340
32.830
Y
27.520
28.880
31.640
33.330
28.840
29.120
30.010
32.170
23.170
24.320
24.020
26.500
31.340
30.770
32.680
23.50
21.970
24.010
23.990
22.830
39.580
37.510
37.830
LAB
a
b
k
P
a
b
k
P
a
b
k
P
a
b
k
P
a
b
. k
P
a
b
P
D-277
-------
TOTAL CARBON
AUDIT
SOIL X
{A} 4.074
5.191
4.540
4.870
4.530
4.990
4.140
4.970
4.880
4.670
4.990
4.460
5.170
4.420
(Bs) 2.776
4.719
4.300
3.720
4.090
3.620
3.430
4.220
3.080
3.720
4.220
3.540
3.680
3.750
(Bw) 1.277
1.743
1.600
1.500
1.450
1.530
1.320
1.450
1.620
1.520
1.440
1.330
1.600
1.550
4
5
4
4
4
4
4
4,
4,
4,
5.
4.
4.
4.
2.
,074
,191
580
370
400
680
250
320
620
630
260
290
970
070
776
4.719
4
3
3
4
2
4
3,
3,
4,
3.
4.
3.
1.
1.
1.
.050
,270
,430
180
690
700
500
640
880
310
400
720
277
743
630
1.780
510
410
220
480
570
1.560
1.420
1.330
1.540
1.670
LAB
*
*
a
b
c
d
e
f
g
j
k
o
P
q
a
b
c
d
e
f
g
j
k
o
P
q
a
b
c
d
e
f
g
j
k
o
P
q
AUDIT
SOIL X
{C} 0.050
{
0.170
0.110
0.120
0.130
0.080
0.120
0.110
0.070
0.120
0.060
0.100
0.160
} 3.753
5.103
5.010
4.690
4.540
4.140
4.100
4.200
4.400
4.360
4.820
3.250
4.600
4.260
{0} 34.291
43.089
40.650
42.180
40.610
37.780
25.750
37.840
37.750
38.100
44.540
30.040
38.900
38.170
0.050
0.170
.100
.080
.110
0.040
0.100
.120
.140
.190
0.230
0.110
.150
.753
.103
.920
.450
.030
.330
.180
.500
.510
.440
.210
.120
.800
.490
34.291
43.089
39.460
44.480
36.300
40.780
28.010
38.820
36.260
38.970
48.120
32.310
43.390
39.520
0,
0.
0,
0.
0.
0.
0.
3,
5.
4.
4,
5,
4.
4,
4.
4,
4,
5.
4,
4.
4,
LAB
*
*
a
b
c
e
f
g
j
k
0
P
q
*
*
a
b
c
d
e
f
g
j
k
o
P
q
a
b
c
d
e
f
g
j
k
o
P
q
D-279
-------
Total Carbon
Bs
a
K>
OO
(U
7-f
6-
5-
4-
3-
OD
2-
1 -
N 12
Mean 3.798
Sd 0.454
Median 3.746
IT
3
4
weight
6
7
-------
Total Carbon
C
0.25-
D
N>
00
0.20-
0.15i
0.10i
0.05-
0.00-
0.00 0.05
0.10 0.15
weight 7,
N 11
Mean 0.116
Sd 0.028
Median 0.110
0.20 0.25
-------
Total Carbon
0
45-
40-
35-
30-
25-
20-
o
a
N 12
Mean 38.280
Sd 5.091
Median 38.690
i • i 'i n i ^ i
20 25 30 35 40
I
45 50
weight %
-------
Table 3a. Summary Statistics tor DORP and Non-Contract Laboratories
KJ
23
Audit
samples
A
Bs
Bw
C
Tabls 3b.
Audit
samples
A
Bs
Bw
C
Group
NC
DDRP
NC
DDRP
NC
DDRP
NC
DDRP
Number
of labs Mean Sd
12 3.8629 1.8275
3 4.6925 0.0797
12 3.1583 1.5366
4 3.8714 0.5747
12 1.2300 0.5833
4 1.5383 0.0399
12 0.0938 0.0539
4 0.1429 0.0126
SE
0.5276
0.0460
0.4436
0.2874
0.1684
0.0200
0.0156
0.0063
Min
0.0000
4.6010
0.0000
3.5128
0.0000
1.4919
0.0000
0.1305
Max
5.1250
4.7476
4.5500
4.7284
1.6100
1.5725
0.1550
0.1589
Wlthln-Group and BetwMn-Group Variabilities for DDRP
and Non-Contract Laboratories
F
525.24
7.15
213.59
18.25
df
11.2]
11.3
11.3
11.3
Pr > F'
a - .05 Variances |T|
0.0038* Unequal -1.5665
0.1320 Equal -0.8899
0.0009* Unequal -1.8181
0.0355* Unequal -2.9225
df
11.2
14.0
11.3
13.6
Pr > JT|
a - .05
0.1452
0.3885
0.0957
0.0115*
* If Pr > F Is less than 0.05. there is a significant difference within groups.
* V Pr > |T| is less than 0.05, there is a significant difference between
groups.
-------
TOTAL NITROGEN
AUDIT
SOIL X
(A) 0.126
0.194
0.208
0.170
0.140
0.190
0.134
0.170
0.160
0.170
0.160
0.150
0.160
0.100
0.154
(Bs) 0.083
0.157
0.194
0.120
0.119
0.110
0.105
0.140
0.090
0.120
0.120
0.110
0.100
0.130
0.119
(Bw) 0.112
0.128
0.132
0.120
0.130
0.150
0.095
0.120
0.120
0.130
0.130
0.110
0.110
0.120
0.
0,
0.
0.112
0.126
0.194
0.168
0.150
0.151
0.170
0.170
160
160
180
0.190
0.150
0.150
0.190
0.150
0.083
0.157
0.158
0.110
0.118
0.130
1.539
0.160
0.110
0.120
,130
,170
,110
0.120
0.112
0.112
,128
109
.120
,110
.130
.106
,120
.120
.130
140
0.120
0.110
0.100
0.121
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
LAB
*
*
a
b
c
d
e
f
g
h
j
k
1
P
q
a
b
c
d
e
f
g
h
j
k
1
P
q
a
b
c
d
e
f
g
h
j
k
1
P
q
AUDIT
SOIL
LAB
{C} 0.000
0.030
0.021
0.070
0.005
0.010
0.010
0.010
0.020
0.030
0.003
(B) 0.169
0.258
0.206
0.240
0.470
0.190
0.210
0.200
0.200
0.150
0.200
0.220
0.190
0.280
0.202
{0} 1.389
1.751
1.611
1.680
1.800
1.539
1.630
1.510
1.560
1.470
1.420
1.420
1.600
1.580
1.570
0.000
0.030
0.030
0.080
0.005
0.010
0.010
0.030
0.010
0.010
0.003
0.169
0.258
0.277
0.210
0.380
0.240
0.217
0.220
0.200
0.240
0.190
0.240
0.190
0.260
0.211
1.389
1.751
1.591
1.750
1.870
1.490
1.820
1.539
1.590
1.460
1.400
1.510
1.670
1.560
1.570
*
*
a
c
e
f
h
j
k
1
q
*
*
a
b
c
d
e
f
g
h
j
k
1
P
q
*
*
a
b
c
q
d
e
f
g
h
j
k
1
P
D-289
-------
Total Nitrogen
Bs
0.25-T
0.20-
0.15-
.c
CT>
0.10-
0.05-
0.00-
1 i ' r ' F
0.00 0.05 0.10 0.15
N 13
Mean 0.179
Sd Dcv 0.194
Median 0.120
0.20 0.25
weight %
-------
Total Nitrogen
C
OJ
0.064
0.03-
>
0.00-
-0.03-
k I
-0.03
Lab c not shown
0.00 0.03
weight %
N 9
Mean 0.020
Sd 0.022
Median 0.01S
0.06
-------
Total Nitrogen
0
d
1.9-I
1.8-
1.7-
,1.6-]
'(D
1.5
1.4-
1.3-
1.3 1.4 1.5 1.6 1.7
weight %
N 13
Mean 1.58$
Sd 0.119
Median U70
T
1.8 1.9
-------
Table 3a. Summary Statistics lor DORP and Non-Contract Laboratories
D
l
to
Audit
samples
A
Bs
Bw
C
Table 3b.
Audit
samples
A
Bs
Bw
C
Group
NC
DORP
NC
DORP
NC
ODRP
NC
DORP
Number
of labs Mean
12 0.1462
3 0.1598
12 0.1701
4 0.1240
12 0.1097
4 0.1186
12 0.0148
4 0.0036
Sd
0.0476
0.0076
0.2087
0.0158
0.0363
0.0077
0.0205
0.0035
SE
0.0137
0.0044
0.0602
0.0079
0.0105
0.0039
0.0059
0.0018
Min
0.0000
0.1528
0.0000
0.1135
0.0000
0.1087
0.0000
-0.0014
Max
0.1800
0.1678
0.8220
0.1475
0.1400
0.1273
0.0750
0.0062
Wtthln-Group and Between-Group Variabilities for DORP
and Non-Contract Laboratories
F
39.62 i
174.67 i
22.11 i
33.63 i
df
11.2
11.3
11.3
11.3
Pt >F*
a - .05
0.0497
0.0013*
0.0269*
0.0146*
Variances |T|
Unequal -0.9458
Unequal 0.7583
Unequal -0.7910
Unequal 1.8141
df
12.6
11.4
13.3
12.7
f*>m
a - .05
0.3620
0.4637
0.4428
0.0934
* If Pr > F is less than 0.05, there is a significant difference within groups.
* If Pr > |T| is less than 0.05, there is a significant difference between
groups.
-------
TOTAL SULFUR
AUDIT
SOIL X
{A} 0.007
0.053
0.010
0.030
0.050
0.020
0.040
0.020
0.038
{Bs} 0.012
0.028
0.010
0.020
0.020
0.010
0.020
0.020
0.018
{Bw} 0.005
0.035
0.020
0.020
0.020
0.010
0.030
0.020
0.022
0.007
0.053
.010
.030
.040
.020
0.030
0.030
0.031
.012
.028
0.020
0.020
0.020
.020
.030
0.020
0.024
0.005
0.035
0.020
0.020
0.030
0.010
0.030
0.010
0.025
0.
0.
0.
0.
0.
0.
0.
0.
LAB
a
b
d
9
j
k
q
*
a
b
d
9
j
k
q
*
a
b
d
g
j
k
q
AUDIT
SOIL X
{C} -0.006
0.018
0.010
0.002
{B} 0.007
0.053
0.030
0.030
0.040
0.020
0.030
0.030
0.034
{0} 0.083
0.247
0.180
0.210
0.230
0.140
'0.140
0.160
0.166
Y
-0.006
0.018
0.010
0.002
0.007
0.053
0.010
0.030
0.040
0.010
0.040
0.030
0.032
0.083
0.247
0.170
0.210
0.230
0.080
0.170
0.160
0.161
LAB
*
*
j
q
T
*
*
a
b
d
g
j
k
q
T
*
* -
a
b
d
g
j
k
q
D-299
-------
Total Sulfur
Bs
o
o
0.040-f
0.030-
0.020-
0.010-
0.000-
0.000 0.010
0.020
weight %
N 7
Mem 0.019
Sd 0.003
Median 0.020
0.030 0.040
-------
Total Sulfur
C
o
o
0.03-
0.02-1
0.01-
(U
-0.01-
-0.02-
-0.03-
\ ' i
r ' i
-0.03 -0.02 -0.01 0.00 0.01 0.02 0.03
weight %
-------
Total Sulfur
0
0.30-f
0.25-
0.20-
0.15-
0.10-
0.05- .
\ ' i
0.05 0.10
I •i
0.15 0.20
N 7
Mean 0.172
Sd 0.039
Median 0.16S
I
0.25 0.30
weight %
-------
Table 2b. Continued
A* Bs
Upper Lower Upper Lower
Labs limit Difference limit Labs limit Difference limit
1 and p 0.03483 0.02346 0.01209 3 and o 0.03320 0.01667 0.00013
3 and d -0.01043 -0.02214 -0.03386 3 and 1 0.03320 0.01667 0.00013
3 and j -0.00043 -0.01214 -0.02386 3 and h 0.03320 0.01667 0.00013
3 and c 0.03457 0.02266 0.01114 3 and p 0.03320 0.01667 0.00013
3 and o 0.03457 0.02286 0.01114 3 and f 0.03320 0.01667 0.00013
3 and e 0.03457 0.02286 0.01114
3 and f 0.03457 0.02286 0.01114
3 and 1 0.03457 0.02286 0.01114
3 and h 0.03457 0.02286 0.01114
3 and p 0.03457 0.02286 0.01114
' .05 level of significance; Tukey's Studentized Range Test; DDRP labs - 1 to 4; NC
Table 3a. Summary Statistics for DORP and Non-Contract Laboratories
Audit Number
samples Group of labs Mean Sd SE Min
A NC 12 0.0133 0.0174 0.0050 0.0000
DDRP 3 0.0248 0.0028 0.0016 0.0229
Bs NC 12 0.0084 0.0106 0.0031 0.0000
DDRP 4 0.0166 0.0033 0.0017 0.0119
Bw NC . 12 0.0086 0.0117 0.0034 0.0000
DDRP 4 0.0192 0.0013 0.0007 0.0178
C NC 12 0.0014 0.0031 0.0009 0.0000
DDRP 4 0.0024 0.0033 0.0017 -0.0020
Table 3b. Wlthln-Group and Between-Group Variabilities for DDRP
and Non-Contract Laboratories
Audit Pr > F' Pr > IT|
samples F df o = .05 Variances |T| df a - .05
A 38.98 (11.2) 0.0505 Equal -1.1073 13.0 0.2882
Bs 10.18 (11.3) 0.0813 Equal -1.4907 14.0 0.1582
Bw 77.82 (11.3) 0.0042* Unequal -3.0705 11.8 0.0099*
C 1.17 (3.11) 0.7307 Equal -0.5264 14.0 0.6068
* If Pr > F is less than 0.05. there is a significant difference within groups.
If Pr > |T| is less than 0.05, there is a significant difference between
Labs
3 and o
3 and 1
3 and h
3 and p
3 and f
2 and c
2 and e
2 and o
2 and 1
2andh
2 and p
2 and f
labs - c
Max
0.0450
0.0280
0.0250
0.0193
0.0300
0.0206
0.0100
0.0050
Upper
limit
0.03371
0.03371
0.03371
0.03371
0.03371
0.03222
0.03222
0.03222
0.03222
0.03222
0.03222
0.03222
to r.
Bw
Difference
0.01633
0.01833
0.01833
0.01833
0.01833
0.01783
0.01783
0.01783
0.01783
0.01783
0.01783
0.01783
C
Lower Upper Lower
limit Labs limit Difference limit
0.00295
0.00295
0.00295
0.00295
0.00295
0.00345
0.00345
0.00345
0.00345
0.00345
0.00345
0.00345
-
groups.
-------
INORGANIC CARBON
AUDIT
SOIL X Y LAB
{A} 0.020 0.010 p
{Bs} 0.010 0.010 p
{Bw} 0.010 0.010 p
(C) 0.030 0.010 p
{B} 0.010 0.010 p
{0} 0.220 0.240 p
D-309
-------
APPENDIX E
AUDIT SAMPLE
STANDARD DEVIATIONS
E-l
-------
Audit sample standard deviations used to establish the Youden-pair plot precision windows.
Audit samples
Parameter A
MOISTURE 0.41
SAND 1.00
VC SAND 1.92
C SAND 3.18
M SAND 1.08
F SAND 2.54
VF SAND 2.42
SILT 2.29
CLAY 2.75
pH, H20 0.120
pH, .002M 0.076
pH, .01M 0.206
Ca, NH4C1 0.066
K, NH4C1 0.016
Ca, NH4OAc 0.064
Mg,NH4OAc 0.038
K, NH4OAc 0.074
Na, NH4OAc 0.032
CEC, NH4CI 1.62
CEC, NH4OA 2.12
TOT ACID 4.20
Al, KC1 0.774
Fe, Pyrophos 0.100
Al, Pyrophos 0.100
Fe, Dithionite 0.168
Al, Dithionite 0.106
SO* H2O 2.92
TOTAL C 0.65
TOTAL N 0.042
TOTAL S 0.011
Bs
0.41
1.22
1.92
3.82
1.08
2.54
2.42
2.24
0.99
0.120
0.076
0.206
0.072
0.018
0.064
0.020
0.014
0.032
1.62
2.12
3.52
0.774
0.100
0.104
0.168
0.122
1.76
0.65
0.042
0.011
Bw
0.41
2.48
1.92
3.82
1.08
2.54
2.42
3.31
1.27
0.120
0.076
0.206
0.076
0.018
0.064
0.026
0.014
0.032
0.89
2.76
4.20
0.264
0.084
0.100
0.168
0.106
2.37
0.65
0.042
0.011
C
0.41
1.22
1.92
3.82
1.08
2.54
2.42
2.04
0.99
0.120
0.076
0.206
0.088
0.022
0.048
0.020
0.014
0.032
0.57
0.21
1.23
0.184
0.014
0.104
0.046
0.012
1.47
0.042
0.006
0.011
B
0.64
3.80
2.00
1.92
1.16
1.38
2.58
3.48
1.82
0.050
0.076
0.064
0.062
0.010
0.034
0.024
0.008
0.008
0.61
4.92
- 3.24
0.77
0.051
0.054
0.210
0.232
1.61
0.53
0.016
' 0.004
O
0.58
..
..
..
..
..
..
..
..
0.069
0.012
0.064
1.28
0.17
0.66
0.27
0.092
0.013
1.87
1.90
1.40
0.34
0.002
0.003
0.002
0.005
5.20
—
—
—
E-3
------- |