United States
Environmental Protection
Agency
Office of Acid Deposition,
Environmental Monitoring and
Quality Assurance
Washington DC 20460
EPA/600/4-87/030b
September 1987
Research and Development
Direct/Delayed Response
Project: Field
Operations and Quality
Assurance Report for Soil
Sampling and
Preparation in the
Northeastern United
States
Volume II. Preparation
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EPA/600/4-87/030b
September 1987
Direct/Delayed Response Project:
Field Operations and Quality Assurance
Report for Soil Sampling and Preparation
in the Northeastern United States
Volume II: Preparation
by
M.L Papp and R.D. Van Remortel
A Contribution to the
National Acid Precipitation Assessment Program
U.S. Environmental Protection Agency
Office of Research and Development
Washington, DC 20460
Environmental Monitoring Systems Laboratory, Las Vegas, Nevada 69193
Environmental Research Laboratory, Corvallis, Oregon 97333
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Notice
The information in this document has been funded wholly or in part by the U.S. Environmental
Protection Agency under Contract Number 68-03-3249 to Lockheed Engineering and Sciences
Company. It has been subject to the Agency's peer and administrative review, and it has been
approved for publication as an EPA document.
Mention of corporation names, trade names, or commercial products does not constitute
endorsement or recommendation for use.
This document is one volume of a set which fully describes the Direct/Delayed Response
Project, Northeast and Southeast soil surveys. The complete document set includes the major data
reports, quality assurance plans, analytical methods manuals, field operations reports, and quality
assurance reports. Similar sets are being produced for each Aquatic Effects Research Program
component project. Colored covers, artwork, and the use of the project name in the document title
serve to identify each companion document. The proper citation of this document remains:
Papp, M. L1., and R. D. Van Remortel1. 1987. Direct/Delayed Response Project: Field Operations
and Quality Assurance Report for Soil Sampling and Preparation in the Northeastern United
States, Volume II: Preparation. EPA/600/4-87/030b. U.S. Environmental Protection Agency,
Environmental Monitoring Systems Laboratory, Las Vegas, Nevada. 96 pp.
Lockheed Engineering and Sciences Company; Las Vegas, Nevada 89119
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Abstract
The Direct/Delayed Response Project Soil Survey includes the mapping, characterization,
sampling, preparation, and analysis of soils in order to characterize watershed response to acidic
deposition within the Northeastern region of the United States. Soil samples collected by sampling
crews were delivered to preparation laboratories where the samples were processed and organized
into batches for shipment to analytical laboratories. This document summarizes the procedures
and assesses the compliance with protocols used at the preparation laboratories. Difficulties at
the laboratories are discussed, and recommendations are made for program improvement.
In general, the preparation laboratories observed protocol. Soil sample integrity appears to
have been maintained at the preparation laboratory.
This report was submitted in fulfillment of Contract Number 68-03-3249 to Lockheed
Engineering and Sciences Company, under the sponsorship of the U.S. Environmental Protection
Agency. This report covers a period from July 1985 to December 1986 and work was completed as
of September 1987.
in
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Contents
Section Page
Notice ii
Abstract iii
Figures vii
Tables viii
Acknowledgments , ix
1. Introduction 1
Summary 1
Objectives 2
2. Sample Preparation Methods and Analysis 3
Sample Processing and Rock Fragment Determination 3
Qualitative Test for Inorganic Carbon 3
Bulk Density Determination 3
3. Preparation Laboratory Operations 5
Sample Storage 5
Equipment 5
Record Keeping 5
Sample Drying 6
Rock Fragment Determination 6
Soil Homogenization 6
Qualitative Test for Inorganic Carbon 6
Moisture Determination 6
Bulk Density Determination 7
Laboratory 1 7
Laboratory 2 8
Laboratory 3 8
Laboratory 4 8
Sample Shipment 8
4. Quality Assurance/Quality Control 9
Design Components 9
Training 9
Communications 9
Data Quality Objectives 9
On-Site Systems Audits 10
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Contents (continued)
Section Page
Data Evaluation 11
Quality Assurance Samples 11
Method of Estimating Analytical Precision 11
Precision Results for Bulk Density Determination 12
Precision Results for Rock Fragment Determination 13
Completeness Results 14
5. Conclusions and Recommendations 15
Data Recording 15
Preparation Laboratory Forms 15
Data Entry Procedures 15
Sample Drying 22
Moisture Determination 22
Bulk Density Determination 22
Quality Assurance/Quality Control 23
Communications 23
Data Quality Objectives 23
On-Site Systems Audits 23
Audit Samples 23
References 24
Appendices
A Sampling and Preparation Laboratory Protocols for the Northeastern
Direct/Delayed Response Project Soil Survey 25
B Laboratory 3 Ammonium Test 94
VI
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Figures
Number Page
1 Sample receipt form 16
2 Bulk density raw data form 17
3 Rock fragment raw data form 18
4 Inorganic carbon raw data form 19
5 Percent moisture raw data form 20
6 Sample processing form 21
VII
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Tables
Number Page
1 Precision Estimates for Bulk Density 12
2 Precision Estimates for Rock Fragments 13
VIII
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Acknowledgments
Critical reviews by the following individuals are gratefully acknowledged: D. E. Corrigan,
Ontario Ministry of the Environment, Toronto, Ontario, Canada; J. C. Foss, University of Tennessee,
Knoxville, Tennessee; J. S. Lohse, Illinois Department of Agriculture, Bureau of Farmland Protection,
Springfield, Illinois; and W. R. Smith, Clemson University, Clemson, South Carolina.
The guidance of the following individuals was important in the development of the statistical
analyses: T. Starks, Environmental Research Center, University of Nevada, Las Vegas, Nevada;
J. E. Teberg, M. J. Miah, M. A. Stapanian, and F. C. Garner, Lockheed Engineering and Sciences
Company, Las Vegas, Nevada.
The following individuals provided internal reviews during the preparation of this document:
C. J. Palmer, Environmental Research Center, University of Nevada, Las Vegas, Nevada; E. Levine,
NASA/Goddard Research Center, Greenbelt, Maryland; S. Bodine, University of Massachusetts,
Amherst, Massachusetts; I. Fernandez and C. Spencer, University of Maine, Orono, Maine;
D. S. Coffey, Northrop Services, Inc., Corvallis, Oregon; and J. K. Bartz, Lockheed Engineering and
Sciences Company, Las Vegas, Nevada.
J. L. Engels, Lockheed Engineering and Sciences Company, Las Vegas, Nevada provided
editorial support. The Computer Sciences Corporation staff at the U.S. Environmental Protection
Agency, Environmental Monitoring Systems Laboratory, Las Vegas, Nevada, and A. M. Tippett,
Lockheed Engineering and Sciences Company, Las Vegas, Nevada provided word processing
support.
Finally, the assistance of the Technical Monitor, L J. Blume, U.S. Environmental Protection
Agency, Environmental Monitoring System Laboratory, Las Vegas, Nevada is gratefully acknowl-
edged.
IX
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Section 1
Introduction
Summary
The U.S. Environmental Protection Agency
(EPA), in conjunction with the National Acid
Precipitation Assessment Program (NAPAP),
has designed and implemented a research
program to predict the long-term response of
watersheds and surface waters in the United
States to acidic deposition. Based on this
research, each watershed system studied will
be classified according to the time scale in
which it will reach an acidic steady state,
assuming current levels of acidic deposition.
The Direct/Delayed Response Project (DDRP)
was designed as the soil study complement to
the aquatic resources program.
As part of the DDRP, four preparation
laboratories were established in the Northeast-
ern region of the United States to process soil
samples and to perform preliminary analyses
on these samples. The preparation laborato-
ries were located within the soil science de-
partments at the following land grant universi-
ties:
University of Massachusetts, Amherst,
Massachusetts.
University of Connecticut, Storrs,
Connecticut.
University of Maine, Orono, Maine.
Cornell University. Ithaca, New York.
Each laboratory was under the direction
of a laboratory manager, who was a soil
scientist and a member of the university facul-
ty. The manager was responsible for ensuring
that the integrity of the soil samples was
maintained after the samples arrived at the
preparation laboratory. Laboratory personnel
were required to comply with protocols speci-
fied for DDRP (Appendix A), which are referred
to as the protocols throughout this report.
Each laboratory manager employed at least
one full-time assistant as well as a number of
college students. Most of the student assis-
tants were majoring in soil science, with the
remainder studying related fields.
The preparation laboratories performed
the following analyses on the bulk samples
collected by the sampling crews:
percent moisture (air-dry).
percent rock fragments (in the 2- to
20-mm fractions).
qualitative test for inorganic carbon.
clod analysis for bulk density.
Laboratory personnel prepared one-
kilogram analytical samples derived from
homogenized air-dry bulk samples. The analyt-
ical samples were labeled and placed into
batches. The samples were then randomized
within each batch. In addition to the routine
samples, each sampling crew collected one
duplicate soil sample per day for quality assur-
ance (QA) purposes. Natural audit samples
and a preparation laboratory duplicate also
were placed into each batch for QA purposes.
The batches were then shipped from the
preparation laboratories to various analytical
laboratories contracted by the EPA.
The results of analyses performed by the
preparation laboratories were recorded on a
Form 101 for each batch of samples. Copies
of the completed Form 101 were required to be
sent to the data base management personnel
at Oak Ridge National Laboratory (ORNL), to
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the QA staff at the EPA Environmental Monitor-
ing Systems Laboratory in Las Vegas (EMSL-
LV), and to the EPA Environmental Research
Laboratory in Corvallis (ERL-C) within 24 hours
of batch shipment to the analytical laborato-
ries.
Because the bulk density analysis was
not completed when batches were sent to the
analytical laboratories, copies of the Form 101
were not always sent within the specified time
limit. Copies specifically were not sent to the
analytical laboratories because the forms
identified the types of soil horizons being
analyzed. Instead, analytical laboratories
received copies of the shipping form (Form
102), on which the sample codes from the
Form 101 had been removed. Each sample on
the Form 102 was identified only by batch and
by sample number in order to disguise the
identity of the soil horizon from which the
sample originated.
Any surplus soil material at the prepara-
tion laboratories was archived and placed in
cold storage. After the sample preparation
and shipping activities were completed, the
archived samples were shipped to Las Vegas
via refrigerated truck and were placed in long-
term cold storage facilities.
Information concerning sample collection,
labeling, and analysis was documented in
sample receipt and sample processing log
books. These log books were later sent to
EMSL-LV for reference during the data verifica-
tion procedure.
Quality assurance/quality control (QA/QC)
measures were applied in order to maintain
consistency in the soi) preparation protocols
and to ensure that soil sample analyses would
yield results of known quality. Personnel at
the preparation laboratories received training
on the analytical methods and soil preparation
procedures. QA staff from EMSL-LV con-
ducted on-site systems audits of the prepara-
tion laboratories. Weekly communication
between QA personnel and laboratory person-
nel was established to identify, discuss, and
resolve issues. Representatives of three of the
preparation laboratories attended an exit
meeting held in Las Vegas on January 6 and
7, 1986. The purposes of the meeting were to
review the mapping, sampling, and preparation
activities, resolve any remaining issues, and to
generate suggestions for future surveys.
Objectives
This document reports the results of the
preparation laboratory operations and QA
program for the Northeastern DDRP Soil Sur-
vey. Difficulties encountered with the data or
methods are identified, and suggestions for
corrective actions are made. The preparation
laboratories are identified by number rather
than by name in order to prevent disclosure of
their identity. Information concerning the
specified protocols for soil preparation can be
found in the protocols (Appendix A).
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Section 2
Sample Preparation Methods
and Analysis
The detailed methods and analytical
procedures used in soil preparation activities
for the Northeastern soil survey are given in
the protocols (Appendix A). Brief explanations
of the methods and procedures for the prepa-
ration laboratory analyses are given below,
including two corrections to the protocols. The
methods are discussed in sequential order as
performed in the preparation laboratories.
Sample Processing and Rock
Fragment Determination
Each bulk sample is spread on a tray to
air-dry until constant weight is achieved. This
is confirmed by comparing the weight of a
subsample on two consecutive days. If the
weight change is less than 2.5 percent, the
sample is considered air-dry.
After recording the weight of the air-dry
bulk sample, the soil is passed through
a No. 10 mesh sieve to collect the less than
2-mm soil fraction. The rock fragments that
are retained on the sieve constitute the 2- to
20-mm pebble fraction. The fragments are
weighed, bagged, and placed in storage. The
fragment weight is divided by the total air-dry
sample weight and is multiplied by 100 to
obtain the percent rock fragments.
A Jones-type 3/8-inch riffle splitter is
used to homogenize the less than 2-mm frac-
tion of the sample. The soil is placed through
the riffle splitter at least seven times in suc-
cession. One-half of the sample is placed into
a plastic bag for archiving, and the other half
is placed through the riffle splitter until
an approximately one-kilogram sample is
obtained.
Qualitative Test for Inorganic
Carbon
One gram of soil is placed in the well of
a porcelain spot plate, saturated with deion-
ized water, and stirred to release any en-
trapped air. Three drops of 4N HCI are added
to the sample while the analyst uses a stereo-
scope to observe the chemical reaction.
Bulk Density Determination
Replicate soil clods are collected by the
sampling crews. Upon arrival at the laborato-
ry, the clods are weighed and dipped in a 1:4
or 1:7 Saran:acetone mixture. The clods are
suspended from a line, allowed to dry, and
reweighed. This procedure is repeated, usually
three of four times, until each clod is impervi-
ous to water.
Approximately 800-mL of deionized water
contained in a one-liter beaker is de-gassed by
boiling, allowed to cool to room temperature,
and tared on a balance. Each clod is sub-
merged in water to determine its weight dis-
placement on the balance. The clods are
placed in a drying oven for 48 hours and, after
cooling, are weighed. A two-hour heat treat-
ment in a 400°C muffle furnace vaporizes the
Saran, then the clods are cooled and re-
weighed. Each clod is crushed and passed
through a No. 10 2-mm mesh sieve. The rock
fragments are weighed, and the data is used
to correct for the rock fragment content.
Bulk density is defined as the mass of a
unit volume of soil particles and pore space
expressed as grams per cubic centimeter
(g/crrr3). Bulk density in mineral soils normally
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ranges from 1.0 to 1.8 g/cm3 (U.S. Department
of Agriculture, Soil Conservation Service
[USDA-SCS], 1983).
Two of the bulk density algorithms were
given incorrectly in the protocols. The first
algorithm originally was written as:
BDcU =
where:
MOD" =
0.85 =
Mv =
rH20T =
2.65 =
1.30 =
MOO- [MCF + MTS (0.85)]
M,
'CF
rH20T
2.65
MTS
1.30
bulk density in g/cm3
oven-dry clod weight
rock fragment weight
Saran coating weight
air-dry to oven-dry Saran weight
conversion
clod weight in water
density of water at laboratory temper-
ature, T
density of rock fragments
density of Saran
Using this algorithm, the Saran volume
would be added to the clod volume rather than
subtracted, thereby underestimating the bulk
density value.
The correct algorithm is as follows:
MOD-[MCF + MTS(0.85)]
BDFM =
Mu
M(
CF
M
'TS
rH20T
,2.65
1.30)
The second algorithm was used to
estimate the air-dry Saran weight and was
incorrectly written as:
M
'TS
where:
X (Ma - MJ
a - 1
MTS = air-dry Saran weight
X = total number of coatings (field and
laboratory)
Ma = clod weight after final coating
M, = initial clod weight after unpacking
a = number of laboratory coatings
The correct algorithm is as follows:
X (Ma - M,)
MTS
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Section 3
Preparation Laboratory
Operations
Detailed discussions of the operations
performed by the preparation laboratories
follow. Deviations from the specified protocols
and difficulties with the methods are noted.
Sample Storage
The specified temperature for storage of
soil samples was 4°C, which was monitored
on a daily basis. All preparation laboratories
had adequate facilities to store the samples at
the required temperature.
An ammonia leak was discovered in the
cold storage facility at Laboratory 3. The
Nessler Reagent Colorimetric test (Greweling
and Peech, 1960), a test for ammonium con-
tent, was used to assess the possible con-
tamination of soil samples that were exposed
(unbagged), single-bagged in plastic, and
double-bagged in plastic (Appendix B). The
conclusions of the experiment were that the
leak had no effect on single- or double-bagged
samples. All samples processed by Labora-
tory 3 were double-bagged in cold storage.
Equipment
EMSL-LV shipped sampling equipment to
the preparation laboratories where laboratory
personnel were responsible for distributing
equipment to the sampling crews. The crews
usually picked up supplies while samples were
being delivered to the cold storage facility. All
supplies taken by the sampling crews were
required to be listed in the equipment log
book.
Laboratory personnel were tasked with
mixing the Saran solution used for coating
clods in the field. Equipment shortages were
reported to EMSL-LV during the weekly confer-
ence calls. After the soil preparation activities
were completed, leftover supplies were inven-
toried and shipped to EMSL-LV for storage. A
list of the equipment provided to the sampling
crews can be found in Appendix A.
Record Keeping
Preparation laboratory data for the
Northeastern Soil Survey were placed in log
books or on forms produced by individual
laboratories. Each preparation laboratory
maintained the following log books:
Label A - Labels that the sampling
crews had placed on the inner soil
sampling bags were removed from the
bags and affixed to pages of the
Label A log book.
Clod Labels - Labels that the sampling
crews had attached either to the clods
or to the clod box were removed and
affixed to pages of the clod label log
book.
Sample Receipt - Information gathered
upon receipt of the soil samples from
the field.
Percent Moisture - Raw data from the
moisture analyses.
Rock Fragment - Raw data from the
rock fragment analyses.
Bulk Density - Raw data from the bulk
density analyses.
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Inorganic Carbon - Raw data from the
inorganic carbon analyses,
Sample Processing - Tracking of the
soil samples through the various
preparation activities.
Because a standard format for record
keeping was not specified, there was great
variation from laboratory to laboratory. As a
result, verification of data was a difficult
process.
Sample Drying
There were no deviations from the speci-
fied sample drying procedure. Because the
procedure was not sufficiently detailed, the
sample drying operations did not proceed as
efficiently as possible. Laboratory 1 identified
wet organic soils of which the outer layer of
the bulk sample had dried to a hard crust,
thereby inhibiting the flow of air to the rest of
the sample. Laboratory 3 used cafeteria trays
on which to dry the samples, and this resulted
in the collection of water on the tray surface
beneath the sample. Both situations created
conditions favoring microbial growth that may
have altered the composition of the affected
soil samples. Specifications for the drying
area did not stipulate any ventilation require-
ments to accelerate the drying process. In
addition, there were no requirements to limit
access to the drying room or to the prevent
soil contamination, e.g., by smoke.
Rock Fragment Determination
There were no deviations from the speci-
fied procedures for rock fragment determina-
tion. Laboratory 4 reported that bulk samples
containing rock fragments greater than 20 mm
in diameter were brought in from the field for
a few pedons. If this were the case, rock
fragment data for these samples may have
identified all rock fragments greater than 2 mm
rather than only the 2- to 20-mm fraction.
Soil Homogenization
There were no deviations from the speci-
fied procedures for soil homogenization. Label
B, identifying each sample for the analytical
laboratories, was placed on the appropriate
sample bag, and each Label A was placed into
the Label A log book according to protocol.
Remaining sample material was stored as
specified in the protocols.
Qualitative Test for Inorganic
Carbon
There were no deviations from the speci-
fied procedures for the inorganic carbon test.
Moisture Determination
The protocols do not specify a procedure
for determining soil moisture content. Conse-
quently, laboratories 1, 2, and 3 used one
method (Method 1), whereas Laboratory 4
used a slightly different approach (Method 2).
Method 1 utilized two subsamples of soil. The
first air-dry sample was oven-dried to deter-
mine its moisture content. On the following
day or at least 24 hours later, a second air-dry
sample went through the same procedure.
Unless the absolute difference between the
moisture contents of the two samples was
less than 2.5 percent, the procedure was
repeated. In contrast, Method 2 utilized only
one soil sample. The air-dry sample was
weighed one day, reweighed the following day,
and oven-dried. The moisture content of
the sample on the different days was then
determined.
Both methods were supposed to ensure
that samples had reached an equilibrium air-
dry state. If the absolute moisture content of
a sample changed less than 2.5 percent in 24
hours, the soil was considered air-dry. This
could be an erroneous assumption in a humid
laboratory where, for example, a soil contain-
ing 20 percent moisture may dry slowly enough
to remain within 2.5 percent of the initial
measurement for 24 hours. By adhering to the
methodology, the soil would be considered air-
dry and ready for further analyses when, in
fact, it was not. However, when the moisture
data were reviewed, less than 3 percent of the
soils had an air-dry moisture content greater
than 10 percent.
A concern with Method 1 is the amount
of soil used in the procedure. After a sample
had been oven-dried, it could not be placed
back into the bulk sample. If the moisture
values of the initial two samples were
not within 2.5 percent, a third sample was
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measured, and a comparison was made
between samples two and three. This process
continued until an equilibrium was reached,
occasionally consuming a substantial amount
of soil. Because the bulk sample was not ho-
mogenized before this determination and was
discarded after measurement, the quantity of
soil consumed adversely affected the represen-
tativeness of the sample and the determination
of rock fragments in the bulk sample.
Another concern relates to moisture
retention. An individual moisture sample will
dehydrate at a faster rate than the bulk sam-
ple from which it is taken. The difference
between the initial and second measurement,
as used in Method 1, would better assess the
air-dry moisture content of the bulk sample.
Bulk Density Determination
Clod analysis was chosen as the general
method for determining bulk density, despite a
few disadvantages. Obtaining clods from dry,
loose, or extremely wet soils and from hori-
zons containing many rock fragments can be
difficult or impossible. Another concern is that
the bulk density values obtained may be higher
than the average bulk density of the soil
horizon that they represent, because sampling
could be biased toward the collection of firmer,
more compact clods capable of withstanding
disturbance during sampling and transport.
Two very similar methods were used to
determine bulk density. The methods varied
because of the manner in which the volume of
the clod was determined. The first method
(Method 1) determines clod volume by placing
a beaker of water on a balance, taring the
balance, submerging the clod in water, and
using the weight of the submerged clod as a
direct estimate of the volume of the clod. This
method of determining volume is described in
the protocols. The second method (Method 2)
utilizes a stand and a beam that are placed on
a balance and tared. A clod is suspended
from the beam and allowed to submerge in
water. The weight of the clod is recorded, and
this value is subtracted from the air-dry clod
weight in order to determine the volume of the
clod.
The use of either Method 1 or Method 2
was based on each laboratory's familiarity
with the method. Both methods are valid,
although each method has its limitations. If a
clod floats when Method 1 is used, the weight
of the floating clod does not reflect its true
volume because some of the clod is above
water. The advantage of this method is that
the clod can be forcibly submerged, and its
true volume can be recorded. If Method 2 is
employed, the measured weight of the floating
clod is zero. Using this method, bulk density
values for floating clods would have to be
removed from the data base because there is
no alternative method for identifying their true
volume.
Another common source of error associ-
ated with both methods was the failure to
subtract the weight of the clod tag and the
hairnet surrounding the clod. Laboratory 1
attempted to compensate for the error by
subtracting the oven-dry weight of the tag and
hairnet from the oven-dry clod weight. The
error surfaced during QAdata evaluation, when
it was observed that clods from the field
occasionally weighed more than the same
clods with additional laboratory coatings of
Saran. The major effect of this error occurs in
the calculation of Saran weight and density.
Variations in bulk density measurements
also occur when clods are allowed to air-dry
between the initial and second weighing, i.e.,
after the clods have been coated with Saran.
Because water vapor can permeate Saran, any
loss of moisture could affect the recorded
Saran weight and density. If laboratory per-
sonnel initially weighed a moist clod from the
field, dipped the clod a number of times, and
allowed it to dry for several hours, the clod
could lose an amount of moisture greater than
the weight of the laboratory Saran coatings.
The effect on the bulk density value would be
dependent upon the size and original moisture
content of the clod.
Each preparation laboratory used a
slightly different procedure for bulk density
determination. The following paragraphs
describe the actual bulk density procedure for
each laboratory.
Laboratory 1
Method 2 was used to determine clod
volume in water. An extra step was included
in the calculation to subtract the oven-dry
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weight of the hairnet and the tag that were
attached to each clod.
Laboratory 2
Method 2 was used to determine clod
volume in water. The laboratory underesti-
mated bulk density values by failing to sub-
tract the Saran density from the buik density
measurement. For a number of raw data
observations (187), a field clod weight and a
clod weight after one Saran coating were
recorded. The remainder of the raw data
observations (690) did not contain field clod
weights. The bulk density, minus Saran densi-
ty, was calculated using the 137 data observa-
tions. Regression analyses that compared the
187 field clod weights with the corrected bulk
density values produced an algorithm that
could be used to calculate corrected bulk
density values for the remaining data. The
algorithm generated a strong correlation (r2 =
0.9987) and was used to convert the bulk
density values for the remaining 690 data
observations. The average increase in bulk
density due to the subtraction of Saran was
slight, i.e., 0.57 percent.
The relationship identified by the regres-
sion analyses is as follows:
Db = a(uDb) + b
where:
Db = corrected bulk density, minus Saran
a = slope of the line (1.0413)
uDb = unconnected bulk density, including
Saran
b = y-intercept (0.0438)
Laboratory 3
Method 2 was used to determine clod
volume in water. While calculating the bulk
density, the laboratory used an erroneous
algorithm from the protocols. The Saran
volume was added to the clod volume in the
denominator of the equation, rather than being
subtracted from it. This discrepancy skewed
each bulk density value an average of 4.7
percent. All values were later recalculated
using raw data supplied by the laboratory.
Laboratory 4
Method 1 was used to determine clod
volume in water. Because the clod tag and
the hairnet weights were not subtracted from
the clod weight, there were instances of labo-
ratory clod weights that were less than the
field clod weights. The data for the 22
affected clods were later removed from the
data base.
Because this laboratory used Method 1,
an attempt was made to identify any floating
clods. This method involves the use of a
closed system, i.e., a floating clod should
weigh the same amount in water as it does in
air. The bulk density values for clods whose
weight in water was within 10 grams of the
air-dried weight were reviewed, as well as the
values for clods weighing more in water than
in air. It was concluded that the floating clods
were forcibly submerged in order to record the
true volume, and the laboratory manager
confirmed this.
Sample Shipment
There were no deviations from the speci-
fied procedure for sample shipment. Samples
were shipped from the preparation laboratories
to the analytical laboratories via overnight air
courier.
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Section 4
Quality Assurance/Quality
Control
A QA/QC program must be followed
during the course of survey activities to ensure
that the resulting data are of known quality.
The QA/QC program for the Northeastern Soil
Survey consisted of design and evaluation
components that aided survey participants in
obtaining data that meets the needs of the
end users.
The QA/QC design for the preparation
laboratories included the training of personnel
in the protocols to be followed, establishment
of a communications network, assessment of
data quality objectives, and accomplishment of
on-site systems audits. The data were sys-
tematically evaluated to ensure data quality,
and QA samples were included in each batch
of routine samples to facilitate this evaluation.
The following sections explain some of these
aspects of the QA/QC program in relation to
preparation laboratory activities. Other as-
pects of the program will be addressed in the
quality assurance report on the analytical
laboratory data.
Design Components
Training
Preparation laboratory personnel
attended a regional workshop held in Orono,
Maine, on August 7 and 8, 1985. The purpose
of the workshop was to review the laboratory
protocols and to establish a consistent meth-
odology for the laboratories that would ensure
the comparability of data.
Communications
Weekly conference calls assisted in
keeping the preparation laboratories operating
efficiently and consistently by providing a
forum that allowed potential difficulties to be
identified, discussed, and resolved. Prepara-
tion laboratory managers, QA personnel, and
scientists involved in the study of soil mineral-
ogy participated in these calls. Issues dis-
cussed during the conference calls included
supply shortages and clarification of proce-
dures, e.g., sample labeling, record keeping,
and drying of organic samples.
Data Quality Objectives
Data quality objectives for the prepara-
tion laboratories were not established before
the Northeastern Survey was conducted. The
preparation laboratories were assessed ac-
cording to the following data characteristics:
Precision and Accuracy - These are
quantitative measurements that esti-
mate the amount of variability and
bias inherent in a given data set.
Precision refers to the level of agree-
ment among repeated measurements
of the same parameter. Accuracy
refers to the difference between an
estimate based on the analytical
results and the true value of the
parameter being measured.
Representativeness - This refers to the
degree to which the collected data
accurately reflect the population or
medium that is sampled.
-------
Completeness - This refers to the
amount of data that is successfully
collected with respect to the amount
intended in the design. A defined
percentage of the intended amount
must be successfully collected fot
conclusions based on the data to be
valid. Lack of data completeness may
reduce the precision of estimates,
introduce bias, and therefore reduce
the level of confidence in the conclu-
sions.
Comparability - This refers to the
similarity of data from different
sources included in a single data set.
If more than one laboratory is
analyzing samples, uniform procedures
must be used to ensure that the data
from different sources are based on
measurements of the same parame-
ter.
These five data quality characteristics
were identified \r\ the DDRP QA Plan (Bartz et
al., 1987), and their application to preparation
laboratory activities were iterated. A brief
description of the specific characteristics
follows:
Precision and Accu^cy - The prepara-
tion laboratory combines sets of field
samples into one batch containing a
maximum of 39 routine and duplicate
samples. After processing, i.e., air-
drying, crushing, sieving, and homoge-
nization, one bulk sample is split into
two subsamples which are termed
preparation duplicates. Comparison
of physical and chemical data for
these duplicates allows evaluation of
the subsampling procedure.
Representativeness - Each bulk sam-
ple is processed by a preparation
laboratory to obtain a homogeneous
sample. Homogenization is accom-
plished by passing the sample
through a Jones-type riffle splitter at
least seven times. The riffle splitter
also is used for subsampling. All
samples not being processed are
stored at 4°C by the preparation
laboratory.
Completeness - Each batch of sam-
ples sent to a contractor analytical
laboratory includes the preparation
duplicates.
» Comparability - All preparation labora-
tories process bulk samples accord-
ing to the protocols. Strict adherence
to protocols should result in compara-
bility among preparation laboratories.
Precision is identified in this QA report
by evaluating field duplicate data from the rock
fragment and inorganic carbon analyses and
replicate data from the bulk density analyses.
Additional precision estimates are made by
evaluating analytical data from the preparation
laboratory duplicates and will be documented
in the QA report on the analytical laboratory
data.
Accuracy cannot be assessed because:
(1) true values for the parameters in question
are not known, and (2) it was not known how
to provide preparation laboratories with audit
samples and quality control calibration sam-
ples to evaluate the rock fragment and bulk
density analyses.
Representativeness of the subsampling
procedure will be assessed in the QA report
for the analytical data.
Completeness is evaluated in this report
by assessing each laboratory's ability to
accomplish the processing and analyses tasks
ior the number of routine and duplicate sam-
ples assigned.
Comparability will be evaluated by using
the precision data from the preparation dupli-
cates. This evaluation will be documented in
the QA report on the analytical laboratory data.
On-Site Systems Audits
Each preparation laboratory was audited
at least once by QA staff. A round of pre-
saiTipte audits was performed before sample
processing was underway. The purpose of the
pre-sample audit was to evaluate the facilities
and equipment and to ensure the capacity arid
suitability of the laboratory to function as a
preparation laboratory for the Northeastern
10
-------
Soil Survey. The same QA auditor performed
all pre-sample audits, which ensured a consis-
tency of observation and inquiry. Issues not
treated in the protocols, e.g., log books and
deviations from written methods, were dis-
cussed and resolved. An on-site evaluation
form contained specific questions relating to
the type of equipment available, sample proce-
dures, and methodology.
The pre-sample auditor concluded that all
preparation laboratories selected for the North-
eastern Soil Survey either had or could obtain
adequate facilities and equipment to perform
the functions specified in the protocols. The
following comments highlight specific concerns
of the auditor:
The soil drying room of Laboratory 2
was located on the seventh floor of
an office building, whereas the other
laboratories used greenhouses. The
auditor was concerned about inade-
quate drying space as well as proper
ventilation for efficient drying. The
laboratory planned on adding extra
shelving.
The existence of an ammonia leak in
the cold storage area of Laboratory 3
was identified. A test to determine
whether the leakage would contami-
nate the soils was proposed (see
Section 3). All samples were double-
bagged in order to decrease the
likelihood of contamination.
A second round of audits was performed
on laboratories 3 and 4 while the laboratories
were preparing samples. The QA auditor
evaluated their procedures and followed up on
concerns identified in the pre-sample audit.
The auditor found that the laboratories were
operating in adherence to protocol, and the
only area of concern identified was the need
for better record keeping at Laboratory 3. An
ERL-C representative performed systems
audits at laboratories 1 and 2 during the soil
preparation activities; however, written
audit reports documenting these visits are
unavailable.
Data Evaluation
Quality Assurance Samples
Three types of paired QA samples were
included in each batch of samples submitted
to the analytical laboratory: (1) field dupli-
cates, (2) preparation duplicates, and (3) audit
samples.
One horizon per sampling crew per day
was sampled in duplicate as specified in the
protocols. The first of the duplicate pair was
considered the routine sample, and the second
of the pair was referred to as the field dupli-
cate. The field duplicate underwent the same
preparation steps as its associated routine
sample in order to allow an estimate to be
made of sampling and horizon variability.
One sample per batch was chosen by
the preparation laboratory to be homogenized
and split into two subsamples. The prepara-
tion duplicates were designed to allow a
quantitative estimate of physical and chemical
variability in splits of the sample material.
Comparing data from analyses of preparation
duplicates allows a reliable estimate to be
made of how well the soil samples were
homogenized before being subsampled. An
evaluation of preparation duplicate data will be
presented in the QA report on the analytical
laboratory data.
Two natural audit sample pairs supplied
by EMSL-LV were included in each batch sent
to an analytical laboratory via a preparation
laboratory, but the audit samples did not
undergo any processing at the preparation
laboratory. These samples are used to as-
sess analytical performance. More information
on these audit samples can be found in the
QA plan (Bartz et al., 1987). An evaluation of
the audit sample data will be presented in the
QA report on the analytical data.
Method of Estimating Analytical
Precision
Data for the bulk density and rock frag-
ment determinations were grouped into data
11
-------
sets, by laboratory. A scatter plot of horizon
standard deviation versus horizon mean was
generated from each data set to evaluate the
relationship between precision and concentra-
tion. The data for both parameters displayed
a random pattern of standard deviation, indi-
cating that precision was independent o1
concentration. On this basis, a completely
randomized design model was selected for the
statistical estimation of precision (Steel and
Torrie, 1960). The model that represents data
collected at a specific sampling site can be
demonstrated as follows:
y, = u + h, + e,j
where:
y,, = the variable of interest for the jth
number of observations from the
ith number of individual horizons
represented
u = the general mean of the population
hj = the effect of the ith horizon on the
variable of interest
e^ - the random error of analytical mea-
surement for the jth number of
observations from the ith number
of individual horizons represented.
The model was used to perform statisti-
cal analyses of: (1) bulk density data from
theclod replicates, and (2) rock fragment data
from the field duplicates. A root mean square
error statistic was used to estimate the pooled
standard deviation (S ) across all pedons and
horizons for each laboratory data set. The
coefficient of variation (CV) was derived by
dividing the Sp by the general mean (JQ and
multiplying by 100.
Precision Results for Bulk
Density Determination
Data from the bulk density determination
were analyzed by the completely randomized
design model to provide overall S- and CV
values for the sets of replicate clods at each
preparation laboratory. In addition, CV values
were generated for sets having a within-set
mean bulk density that was either greater than
or less than the general mean bulk density.
Summary statistics for the Sp and CV values
are given in Table 1.
The CV values less than and greater than
the mean were evaluated in order to determine
whether or not the statistical relationship of
higher CV values at lower concentrations, in
this case at lower bulk densities, would hold
true for bulk density data. The CV values
presented in Table 1 appear to confirm this
relationship.
The Sp and CV values for the Laboratory
3 replicates suggest a higher imprecision than
values for the other laboratories. The mean
bulk density of samples analyzed by Labora-
tory 3 also is higher than that of the other
laboratories. Because they finished sampling
earlier in the season when the weather was
warm and dry, the sampling crews supplying
Laboratory 3 may have had difficulty collecting
clods from surface horizons. Soil conditions
may have favored the collection of clods from
the lower, moister horizons. The collection of
replicates may not have been as representative
of a horizon as desired.
Table 1. Precision Estimates for Bulk Density
Laboratory 1
Laboratory 2
Laboratory 3
Laboratory 4
Number of
horizons
sampled
235
303
50
251
Mean bulk
density
(g/cm3)
1.24
1.38
1.61
1.35
SP
0.110
0.096
0.178
0.087
CV
6.82
6.97
10.99
6.48
cvX
7.66
5.26
8.49
5.79
12
-------
The overall Sp values suggest a consis-
tency of bulk density values within a horizon.
Audit reports indicated that the sampling
crews were able to choose representative
clods from each horizon and that the laborato-
ries were consistent in their use of measure-
ment techniques. However, the exact percent-
age of error contributed to the Sp by horizon
variability, sampling bias, or laboratory impreci-
sion cannot be determined because: (1) inher-
ent spatial variability made it impossible to
sample identical field clods or to provide an
audit sample for estimation of potential sampl-
ing bias, and (2) the preparation laboratories
were not provided with calibration samples to
allow estimation of laboratory bias.
The following types of sampling errors
could contribute to sampling bias for the bulk
density replicate clods:
Collection of replicates from transi-
tional zones or adjacent horizons.
Mislabeling or careless handling of
clods.
Inconsistent Saran coating procedure.
Bias relating to the structural coher-
ency of clods.
Based on the experience of the Soil
Conservation Service (SCS) sampling crews
and the fact that the various field audit reports
did not indicate any major deviation from the
protocols, sampling bias is not presumed to
have been a significant factor affecting the Sp
values. Some variability in the use of Saran,
e.g., the length of time clods were allowed to
be submerged in Saran, was mentioned in a
few audit reports. The Sp values would not be
affected if the coating procedure was consis-
tent for all replicates from a horizon.
At the preparation laboratory, measure-
ment or method errors can introduce bias,
including:
Transcription errors in recording clod
weight or sample code.
Inconsistent Saran coating proce-
dures.
Improper clod handling, e.g., compac-
tion.
Incomplete drying.
Loss of soil material during sieving.
Inaccurate calculations.
Faulty weights, e.g., clod tags and
hairnets not subtracted.
Because audit samples and calibration
samples were not provided, laboratory bias
could not be measured. Therefore, it is diffi-
cult to quantify the potential effect of prepara-
tion laboratory bias on the Sp and CV values.
Precision Results for Rock Frag-
ment Determination
Field duplicate data for the rock fragment
determination were analyzed by the completely
randomized design model to provide overall Sp
and CV values for each preparation laboratory.
Summary statistics incorporating these values
are provided in Table 2.
Table 2. Precision Estimates for Rock Fragments
Field duplicate
pairs
Mean
% rock
fragments
CV
Laboratory 1
Laboratory 2
Laboratory 3
Laboratory 4
64
76
21
62
25.1
16.2
14.2
12.0
4.002
1.792
3.367
1.135
15.97
11.04
23.70
9.47
13
-------
Because of the simplicity of the method
used for determining the percentage of rock
fragments in the bulk soil samples, a greater
amount of imprecision can be attributed to a
combination of sampling bias and horizon
variability and a lesser amount to preparation
laboratory bias. The imprecision may be an
indication of improper field duplicate sampling
technique or considerable spatial variability in
rock fragments.
Completeness Results
The requested analyses and soil pro-
cessing steps were performed on 100 percent
of the bulk samples and clods received by the
preparation laboratories, which satisfied the
theoretical maximum design level of complete-
ness. Preparation duplicates were created for
each batch of samples sent to the analytical
laboratories, for a 100 percent level-of
completeness.
14
-------
Section 5
Conclusions and
Recommendations
Hie conclusions and recommendations
discussed below are summarized from discus-
sions at the exit meeting, conference call
notes, and the examination of raw data.
Data Recording
Verifying the data from the Northeastern
Soil Survey was difficult because the format of
log books in which the data were recorded
was not consistent from one laboratory to
another. A system has been designed that
would allow -the raw data to be entered into
log books containing pre-printed data forms,
followed by data entry into a computer data
set having the same format. This would
facilitate the verification process and would
relieve preparation laboratory personnel of
calculating final values as well. Possible
components of a data recording system are
discussed below.
Preparation Laboratory Forms
Standardized forms should be developed
on which to record data from all preparation
laboratory procedures. Recommended formats
are presented for the following forms:
Figure 1 - Sample receipt.
Figure 2 - Bulk density.
Figure 3 - Rock fragment.
Figure 4 - Inorganic carbon.
Figure 5 - Percent moisture.
Figure 6 - Sample processing.
Note that most of the forms use data-
file variable names as the column headings.
Data Entry Procedures
Preparation laboratory personnel will not
be required to calculate final values, so there
will be no entry field for final values on the
raw data forms. However, the preparation
laboratory supervisor should calculate bulk
density from random samples in order to
ensure placement of the variables into the
correct fields. Soil samples do not have to be
analyzed in the order they appear in the batch
because the sample code information linking
the data to a master form will be placed on
each raw data form.
On a weekly basis, the preparation
laboratory personnel will enter all raw data
into a data base file by using dBase III soft-
ware. The program format will have data
entry screens that display facsimiles of the
raw data forms. If a preparation laboratory
does not have access to a computer system,
QA personnel will enter the data. After data
are entered, either of two options exist:
Option 1 - The software can be pro-
grammed to calculate final data. The
calculated final data can be generated
on the Form 101 under the correct
sample code, and the preparation
laboratory can access and print these
data. Algorithms to calculate percent
relative standard deviations for field
duplicates, routine samples, and the
15
-------
9t
uuo|
«|dui*8
MIM*K <*>) »(
*!»!
Kit
Ift/tl
IB/Ml 'JO/I »R
>»!*»
0
01
01
-------
11 wlfhlt lit .0.01 gr..t
jw coot w ritio or mio m
MILS OtNIITT KAK DATA
IAI_MT CtOO_Mjfl tOV CLOO_00
tiiu rioAr OAFC
CWtdKIJ
MM.1ST
mriAtt
Figure 2. Bulk density raw data form.
17
-------
All weight
SAM_CODE
s to the
TOT WT
F
nearest 0.
4.75-20iran
WT_2
ercent Rock
1 9
2. 0-4. 75mm
WT_2
Fragments Page
Prep Lab:
Comments
/
/
Analyst
Initials
/'
Figure 3. Rock fragment raw data form.
18
-------
SAM_CODE
REP
Test
YES
for
NO
Inorganic carbon Page /
Prep Lab: /
Comments
Analyst
Initials
Figure 4. Inorganic carbon raw data form.
19
-------
CONT WT=CO
AD_SOIL =
OD_SOIL =
% Moist (R
SAM_CODE
ntaine
Air dr
oven d
J2P1) -
REP
r Weight
y soil w
ry soil
% Moist
CONT WT
Pe
eight plus
weight plu
(REP2) =
AD_SOIL
rcent Mo
contain
s contai
s2.5 (Ab
OD_SOIL
isture Page
Prep Lab:
er weight
ner weight
solute Value)
Comments
/
/
Analyst
Initials
Figure 5. Percent moisture raw data form.
20
-------
S«1_COOE
ANPIEO
RECEIVED
AIR DftlCD
STAR!
1HISH
!
SIEVED
AWLE PROCt!
MORGAN 1C
CARBOH
SIMG DATES
UBSAHPLE.O
BULK
CHSITT
RCHIYt
SAMPLE
TORtO
PWl /
nit LAI -- -
COHMCNTS
Figure 6. Sample processing form.
21
-------
bulk density replicates can be incorpo-
rated into the software. Outliers,
erroneous values, and invalid sample
code entries can be identified at this
stage.
Option 2 - Preparation laboratory
personnel can enter the raw data. No
statistical calculations or conversions
of raw data to final data would occur
at the preparation laboratories.
Instead, the raw data would be sent
electronically to the QA staff. QA
personnel can convert the dBase II
data into a SAS data set and can
calculate final values. Next the data
can be analyzed statistically, and the
findings reported to the laboratories.
Either option should work equally well.
Data entry errors can be identified before
batches are sent to the analytical laboratories.
In fact, data verification may be completed
shortly after the final batch of soil samples is
assembled at the preparation laboratory.
The sample processing form will provide
a record of the sample codes from the master
form and the date of specific laboratory analy-
ses from the raw data forms. The sample
processing form can verify that all required
analyses were performed on the samples.
Sample Drying
Certain procedural details concerning
sample drying were inadequately addressed in
the protocols. The procedure should be ex-
panded as follows:
Drying efficiency would improve if the
samples were stirred every 24 hours
to facilitate uniform drying. Steel
mesh trays covered with kraft paper
could be used for sample drying. This
would eliminate the water condensa-
tion that occurred with the cafeteria-
type trays.
Specifications for drying facilities, e.g.,
temperature and humidity controls,
space allocation, access, and air
circulation, should be stipulated.
Special procedures for handling cer-
tain soil types, e.g., organic or clayey
soils, should be provided.
Soils that are known to harden upon
drying, e.g., mucky or clayey soils,
should be crushed and mixed before
they reach constant moisture content.
When handling the samples, Jhe
analyst should wear rubber or plastic
gloves to lessen the possibility of
contamination.
Elimination of all sources of contami-
nation, e.g., smoking and food, should
be stipulated.
Moisture Determination
Analysis of the initial raw data values for
percent moisture suggests that the preparation
laboratory personnel were capable of assess-
ing the air-dry condition of samples. The
following protocol modifications should be
made for the moisture determination:
The bulk sample should be allowed to
dry until the preparation laboratory
personnel judge the sample to be air-
dry.
A 10-gram air-dry subsample can be
removed for determination of percent
moisture.
A determination of field moisture
should be made on all samples upon
their arrival at the preparation labora-
tories. A consistent method for mea-
suring field moisture must be added
to the protocols.
Bulk Density Determination
The following recommendations are
made to alleviate difficulties with the bulk
density procedure:
An audit sample should be included to
provide data for estimating within-
and among-laboratory precision and
interlaboratory bias. (See page 23.)
A mineral of known density, e.g.,
quartz, should be used as a quality
22
-------
control calibration sample. Because
the data have demonstrated that
measurement precision is not depen-
dent upon the level of bulk density, it
is not necessary for the quality con-
trol calibration sample to have a bulk
density within the range of soil bulk
density values.
Clods should air-dry before pro-
cessing for the bulk density determi-
nation. Clod weight should be re-
corded immediately before and soon
after laboratory Saran coating.
Method 1, which was outlined in the
protocols, is the preferred method for
determining bulk density. The method
should be rewritten to correct errone-
ous algorithms (see Section 2) and to
add specific instructions for sub-
merging clods.
Floating clods should be identified on
the bulk density raw data form.
Clod tags should be removed or
should be dried before the clods are
weighed.
Because Saran and acetone are carci-
nogenic, laboratory managers should
take extra care to ensure that Saran
mixing, clod coating, and clod ignition
are performed in an operating exhaust
hood. Operators should wear respira-
tors.
Quality Assurance/Quality
Control
Communications
Although the conference calls met the
objective of establishing a forum where ques-
tions could be answered or issues could be
identified and resolved quickly, documentation
of the discussions and dissemination of the
information were not done consistently. The
following suggestions are made:
The QA auditor should lead all confer-
ence calls. This person or another
member of the QA staff will be
present for all conference calls.
The frequency of conferences should
be weekly, unless the QA auditor
decides that biweekly calls would be
equally effective.
All pertinent information should be
documented by the conference leader
in a log book established specifically
for the soil survey region. This book
can identify the participants involved
in the discussions as well as key
personnel not in attendance.
Log book notes should be compiled
and sent to the appropriate partici-
pants weekly.
Data Quality Objectives
Data quality objectives should be estab-
lished for the determinations of bulk density
and percent rock fragments.
Qn-Site Systems Audits
The pre-sample audit achieved the objec-
tive of assessing the ability of each laboratory
to function as a ODRP preparation laboratory.
The second audit was instrumental in evalu-
ating adherence to protocol during soil pro-
cessing. Each laboratory should be evaluated
before or during sample processing. It is
recommended that one QA auditor should
evaluate all the laboratories for both the pre-
sample and the second audits, and another,
the second evaluations. This would facilitate
a consistent assessment of all laboratories.
Audit Samples
Audit samples are needed to evaluate
preparation laboratory accuracy for the bulk
density determination. The following has been
suggested, but has not been tested at EMSL-
LV. QA personnel could provide the prepara-
tion laboratories with synthetic samples, e.g.,
plastic eggs filled with materials of known
densities. The eggs would be coded, and the
bulk density of each egg would be determined
at the QA laboratory. A set of 24 eggs could
be sent to each preparation laboratory, which
would be required to calculate the bulk density
of one egg for each day the laboratory was
analyzing clods.
23
-------
References
Bartz, J. K., S. K. Drous6, K. A. Cappo, M. L Steel, R. G. D., and J. H. Torrie. 1960. Princi-
Papp, G. A. Raab, L. J. Blume, M. A. pies and Procedures of Statistics.
Stapanian, F. C. Garner and D. S. Coffey. McGraw-Hill Book Company, New York.
1987. Direct/Delayed Response Project: 481 pp.
Quality Assurance Plan for Soil Sampling,
Preparation, and Analysis. EPA/600/8- USDA-SCS. 1983. National Soils Handbook,
87/020. U.S. Environmental Protection Parts 600-606. U.S. Government Printing
Agency, Las Vegas, Nevada. 315 pp. Office, Washington, D;C. 609 pp.
Greweling, T., and M. Peech. 1960. Chemical
Soil Tests. Cornell Univ. Agric. Exp. Stn.
Bulletin 960. 60 pp.
24
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Appendix A
Sampling and Preparation Laboratory Protocols
for the Direct/Delayed Response Project Soil Survey
The following protocols were used by the sampling crews and the preparation laboratory
personnel participating in the Northeastern DORP Soil Survey. The draft manual was revised using
the information obtained from the sampling and preparation laboratory training workshop held on
August 7 and 8, 1985. The draft did not undergo external review and was not formally released by
EPA. It is presented here without editorial correction. Note that various Soil Conservation Service
documents were used in the preparation of this draft; however, because no editorial corrections
have been made, those documents are not cited.
25
-------
Field Sampling Manual for the
National Acid Deposition Soil Survey
by
L J. Blume1, D. S. Coffey2 and K. Thornton3
'Lockheed Engineering and Management Services Company, Inc.
Las Vegas, Nevada 89109
2Northrop Services, Inc.
Corvallis, Oregon 97333
3FTN and Associates
Little Rock, Arkansas 72211
Contract No. 68-03-3249
Project Officer
Phillip A. Arberg
Exposure Assessment Research Division
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89114
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89114
26
-------
Notice
This document is a preliminary draft. It has not been formally released by the U.S.
Environmental Protection Agency and should not at this stage be construed to represent Agency
policy. It is being circulated for comments on its technical merit and policy implications, and is for
internal Agency use/distribution only.
The mention of trade names or commercial products in this manual is for illustration
purposes, and does not constitute endorsement or recommendation for use.
27
-------
Contents
Revision 2
Date: 9/85
Page 1 of 2
Contents
Section Page Revision
Notice 1 of 1 2
Figures 1 of 1 2
Tables 1 of 1 2
Acknowledgments 1 of 1 2
1.0 Introduction 1 of 2 2
1.1 Scope 1 of 2 2
1.2 Personnel 1 of 2 2
2.0 Site Selection 1 of 8 2
2.1 Watershed Selection 1 of 8 2
2.2 Watershed Mapping 1 of 8 2
2.3 Sampling Classes 2 of 8 2
2.4 Watershed and Sampling Class Selection 3 of 8 2
2.5 Final Selection of Sampling Locations 5 of 8 2
2.6 Special Conditions 8 of 8 2
2.7 Paired Pedons 8 of 8 2
3.0 Site and Profile Description 1 of 5 2
3.1 Scope 1 of 5 2
3.2 Field Properties 2 of 5 2
3.3 Profile Excavation 2 of 5 2
3.4 Photographs of Profile and Site 3 of 5 2
3.5 Important Points Concerning Horizon Descriptions 3 of 5 2
3.6 Field Data Form-SCS-232 4 of 5 2
4.0 Sampling Procedures 1 of 5 2
4.1 Scope 1 of 5 2
4.2 Sampling the Pedon 1 of 5 2
4.3 Delivery 5 of 5 2
5.0 Soil Preparation Laboratory 1 of 8 2
5.1 Scope 1 of 8 2
5.2 Sample Storage 1 of 8 2
5.3 Sample Preparation 1 of 8 2
5.4 Shipment of Subsample to Analytical Laboratories 5 of 8 2
5.5 Sample Receipt by the Analytical Laboratory from the
Preparation Laboratory 6 of 8 2
5.6 Shipment of Mineraiogical Samples 6 of 8 2
6.0 Summary of Physical and Chemical Parameters and Methods 1 of 3 2
6.1 Physical Parameters 1 of 3 2
6.2 Chemical Parameters 1 of 3 2
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Contents
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Contents (continued}
Sect/on Page Revision
7.0 Bulk-Density Determination 1 of 5 2
7.1 Scope 1 of 5 2
7.2 Apparatus and Materials 1 of 5 2
7.3 Procedure 1 of 5 2
8.0 Crews, Supplies, and Equipment 1 of 3 2
8.1 Scope 1 of 3 2
8.2 Equipment Notes 2 of 3 2
9.0 References 1 of 1 2
Appendices
A. Field Data Forms and Legends 1 of 22 2
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Figures
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Figures
Figure Page Revision
4-1 NADSS Label A 4 of 5 2
5-1 National Acid Deposition Soil Survey (NADSS) Form, 101 2 of 8 2
5-2 NADSS Label B 4 of 8 2
5-3 National Acid Deposition Soil Survey (NADSS) Form 102 7 of 8 2
5-4 National Acid Deposition Soil Survey (NADSS) Form 115 9 of 8 2
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Tables
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Tables
Table Page Revision
2-1 Comparison of Coniferous, Deciduous, and Mixed Vegetation
Types to Society of American Foresters (SAF)
Forest Cover Types 7 of 8 2
4-1 Visual Estimate of Percent Volume of Rock Fragments Greater
than 75 mm Correlated to Percent Weight 4 of 5 2
7-1 Specific Gravity of Water 5 of 5 2
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Acknowledgments
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Ackno wledgments
Contributions provided by the following individuals were greatly appreciated: D. Lammers,
B. Jordan, M. Mausbach, R. Nettleton, W. Lynn, F. Kaisacki, B. Waltman, W. Hanna, B. Rohrke,
G. Raab, J. Bartz, B. Blasdell, and R. Harding.
The following people were instrumental in the timely completion and documentation of this
manual: Computer Sciences Corporation word processing staff at the Environmental Monitoring
Systems Laboratory-Las Vegas, C. Roberts at the Environmental Research Laboratory-Corvallis, and
M. Faber at Lockheed Engineering and Sciences Company.
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1.0 Introduction
1.1 Scope
This field sampling manual is written to guide personnel involved in the collection of soil
samples for the U.S. Environmental Protection Agency's (EPA) Direct/Delayed Response Project
(DDRP) Soil Survey. All field and laboratory personnel must be trained by a field manager or
another person knowledgeable in the procedures and protocols detailed in this manual. The scope
of the field sampling manual covers field operations, shipping of samples from the preparation
laboratory to the analytical laboratory, and sample receipt by the analytical laboratory.
This manual is a companion to the [laboratory] methods manual for the National Acid
Deposition Soil Survey (NADSS) and the quality assurance plan for the National Acid Deposition
Soil Survey (NADSS). There is some repetition among the manuals which is necessary to maintain
continuity and to document concisely the methodology of the soil survey.
The basic goals of the NADSS procedures are to collect representative samples without
contamination, to preserve sample integrity for analysis, and to analyze samples correctly.
Analytical methods have been chosen that offer the best balance between precision, accuracy,
sensitivity, and the needs of the data user.
The overall objective of NADSS is to predict the long-term response of watersheds and
surface waters to acidic deposition. Based on this research, each watershed system will be
classified according to the time scale in which it will reach an acidic steady state, given current
levels of deposition. Three classes of watershed systems are defined:
Direct response systems: Watersheds with surface waters that either are presently acidic
(alkalinity <0), or will become acidic within a few (3 to 4) mean water residence times (<10
years). NOTE: Most lakes in the northeast have relatively short residence times, i.e., less
than 2 to 4 years.
Delayed response systems: Watersheds in which surface waters will become acidic in the
time frame of a few mean residence times to several decades (10 to 100 years).
Capacity protected systems: Watersheds in which surface waters will not become acidic for
centuries to millennia.
The objective of this manual is to define the means by which to characterize and sample soil
mapping units using U.S. Department of Agriculture-Soil Conservation Service (USDA-SCS)
descriptive techniques.
1.2 Personnel
1.2.1 Field Sampling Crews
The field sampling crews will consist of soil scientists experienced in the National Cooperative
Soil Survey. Crews will be numbered consecutively beginning with 01. For example, if Maine has
three crews, they will be ME01, ME02, and ME03. These crews will be responsible for selecting the
pedon location, sampling the soil, and describing the profile. The field crew leader will have
ultimate responsibility for each crew's daily activities, such as placement of the pedon within each
sample class, correct labeling of sample bags and forms, and prompt shipment of samples.
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1.2.2 Regional Coordinator/Correlator
The Regional Coordinator/Correlator (RCC) will monitor six to ten percent of the sampling
units to ensure adherence to SCS standards and field sampling protocol. Three to five percent of
the sites will be monitored in conjunction with the monitoring responsibilities of the SCS staff of
each state. The remaining sites will be monitored independently of the state SCS staff. Monitoring
will include a review of profile descriptions and selection of sites for sampling. The RCC will be
a qualified soil correlator with many years of experience with soil profile description and soil
mapping. He will also ensure that the SCS State Office Staff perform duplicate profile descriptions.
In this process, he will review these descriptions and point out potential problems.
1.2.3 Quality Assurance/Quality Control Representative
The quality assurance/quality control (QA/QC) representative will review five percent of the
sampling units to ensure adherence to sampling protocol as specified in this manual.
1.2.4 SCS State Office Staff
Members of the SCS State Office Staff will independently describe five to ten percent of the
sample pedons and site descriptions and will monitor field sampling protocol. At least one site per
state will be audited by the RCC representative. The use of duplicate profiles, determined prior to
sampling, will assess variability in site description and sampling techniques between soil scientists
and will check adequacy of site selection and labeling. This process requires that the staff perform
their assessment while the crew is describing and sampling the pedons. NOTE: Reviews by the
RCC, QA/QC representative, and the SCS State Office Staff should be documented and all reports
should be submitted to the EPA-Las Vegas QA Manager.
1.2.5 Soil Preparation Laboratory
Four soil preparation laboratories will participate in NADSS. These laboratories include the
Cornell University Characterization Laboratory at Ithaca, New York, the University of Maine Soils
Laboratory at Orono, Maine, the University of Connecticut Soil Testing Laboratory at Storrs,
Connecticut, and the University of Massachusetts Soil Testing Laboratory at Amherst,
Massachusetts.
Small bags, data forms, labels, audit samples, shipping containers, and other equipment will
be shipped to these soil preparation laboratories by EPA-Las Vegas. The field soil scientists will
use these laboratories as sample drop-off points and supply pick-up points.
1.2.6 Analytical Laboratories
Routine and QA samples will be shipped in batches to each analytical laboratory from the
preparation laboratory. Each batch will consist of a maximum of 39 routine samples and field
duplicates, 2 audit samples, and a preparation laboratory duplicate.
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2.0 Site Selection
2.1 Watershed Selection
Because the objectives of DORP are focused on making regional inferences, it was critical that
the 150 watersheds selected for mapping of soils and watershed characteristics constitute a
representative sample of the region. The 773 watersheds included in Region I of the National
Surface Water Survey (NSWS) provided an excellent starting point from which to draw a subsample
of 150 for the northeastern portion of DDRP, because: (1) the NSWS lakes were selected according
to a rigorous probability sampling method (stratified by five subregions and three alkalinity classes
within each subregion), and (2) water-chemistry information was available from NSWS for these
lakes.
The 150 watersheds to be studied in DDRP also are part of the Phase II lake-monitoring
program of NSWS that will provide a data set that contains both water-chemistry and watershed
information. Therefore, the procedure used to select these watershed incorporated criteria relevant
to both DDRP and NSWS. The procedure consisted of five steps, which are summarized as
follows:
Step 1: Lakes of low interest (too shallow, highly enriched, capacity protected, polluted by
local activities, or physically disturbed) were excluded.
Step 2: Lakes too large to be sampled (>200 ha) were excluded.
Step 3: A cluster analysis was performed on a set of chemical and physical variables to
group the remaining 510 lakes into three clusters of lakes with similar characteristics.
Step 4: A subsample of 60 lakes was selected from each cluster, then the three subsamples
were weighted to represent the overall population of lakes in the northeast.
Step 5: Lakes with watersheds too large to be mapped at the required level of detail
(watersheds >300 ha) were excluded from the subsamples.
This procedure identified 148 lakes and watersheds, spread across the three clusters. Note
that the three groups differ primarily in their alkalinities, pH levels, and calcium concentrations. To
maintain the ability to regionalize conclusions drawn on the sample of 148 watersheds, the
precision of information characterizing each of these watersheds should be comparable, and each
cluster should be described at the same level of detail as the others.
2.2 Watershed Mapping
During the spring and summer of 1985. 145 of the 148 watersheds were mapped. The
logistics and protocols of the watershed mapping are described in chapters 6 and 7, Volume 5,
Appendix B.2 Soil Survey - Action Plan/Implementation Protocol.
A total of about 440 mapping units were identified in the 150 watersheds. Sampling each of
the 440 mapping units would not necessarily be the best way to describe adequately the chemistry
of the region's soils. A better procedure is to combine the identified soils into groups, or sampling
classes, which are either known or expected to have similar soil-chemical characteristics. Each of
these sampling classes can then be sampled across a number of watersheds in which they occur,
and the mean characteristics of the sampling class can be computed. These mean values and the
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variance about the mean can then be used to build "back-up" area- or volume-weighted estimates
of each watershed's characteristics.
For this procedure to work, it is critical that a sufficient number of samples are taken (five
or more) to characterize the variability of each sampling class. This necessitates aggregating the
number of mapping units into a reasonable number of sampling classes, given budgetary
constraints. Thus, the central goal is to develop a method of grouping the large number of soils
into a reasonable number of sampling classes.
2.3 Sampling Classes
2.3.1 Data Base
The data base contains about 2200 observations that were recorded on the field forms during
the soil mapping of 145 watersheds selected as part of the DDRP and the Phase II lakes survey.
This information includes:
Taxonomic class (series, subgroup, great group).
Parent material.
Origin.
Mode of deposition.
Drainage class.
Slope class.
Slope configuration.
Family texture.
Geomorphic position.
Dominant landform.
Surface stoniness.
Percent inclusions.
Percent complexes.
Estimated depth to bedrock.
Estimated depth to permeable material.
This information was considered in aggregating similar mapping units into sampling classes.
The data base also includes the area of each mapping unit, number of occurrences, and percent
of the watershed area.
Separate data files also exist for vegetation type, vegetation class, and geology. The data
management system, dBase III, runs on an IBM PC-XT microcomputer at the EPA Environmental
Research Laboratory in Corvallis, Oregon (ERL-C).
2.3.2 Evaluation of Sampling Classes
A taxonomic approach was used to identify 38 sampling classes as a foundation for
aggregating similar mapping units. Taxonomic classification is based on similarities among soil
properties. This taxonomic scheme was modified to reflect the major factors influencing soil
chemistry.
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2.4 Watershed and Sampling Class Selection
2.4.1 Sampling Class Objectives
The primary goal of this part of the sample selection procedure is to determine which
sampling classes will be sampled in which watersheds. The sample sites should be selected to
meet the following objectives:
Objective 1: To characterize all the sampling classes with similar levels of precision.
Objective 2: To describe the variation in watershed characteristics.
Objective 3: To describe the variation in the acid neutralizing capacity (ANC) clusters
developed from the lake survey.
2.4.2 Sampling Class Constraints
To meet these three objectives, a series of constraints was developed based on the allocation
of samples to sampling classes and watersheds. The constraints that must be met follow:
Constraint 1: Approximately equal numbers of samples will be taken from each sampling
class.
Constraint 2: Approximately two samples will be taken from each watershed.
Constraint 3: Not more than one sample will be taken from each sampling class in each
watershed.
Constraint 4: Samples will be selected over the range of ANC clusters within each sampling
class.
The method outlined here was developed to randomly select watersheds and sampling
classes, within these constraints, using a simple selection algorithm.
2.4.3 Selection Algorithm
The method selection proceeds through a series of stages. Wherever possible, the rationale
for the particular approach taken is described and cross-referenced with the objectives and
constraints.
The selection method is based on the use of a systematic, weighted, random sample of the
watersheds that contain any given sampling class. First, the number of samples to be taken in
each sampling class is determined (Constraint 1).
2.4.3.1-
The first task is to construct a matrix of the occurrences of each sampling class in each
watershed. This matrix is used to: (1) prepare a list of the watersheds that contain each sampling
class, and (2) determine the number of different sampling classes in each watershed.
When the number of watersheds represented in each sampling class has been determined,
it is possible to allocate the samples to sampling classes (given Constraint 3).
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Using eight samples per sampling class as a base, the following sample allocation occurs.
Eight samples will be allocated to each sampling class where there are more than eight
watersheds; where there are eight watersheds or less, one sample will be allocated to each
watershed.
2.4.3.2-
The next task is to determine which watersheds will be selected within each sampling class.
In this process, constraints 2 and 4 are centrally important.
If watersheds are selected randomly within each sampling class, the watersheds that contain
a large number of sampling classes will have more samples allocated to them than will the
watersheds that have fewer sampling classes. To counteract this effect, and to help approach an
approximately equal number of samples per watershed, the watersheds will be weighted (during
the random selection procedure) by the inverse of the number of sampling classes that they
contain.
For example, if one watershed contains four different sampling classes, it will be exposed to
the sample selection procedure four times. Thus, it will be given one quarter of the weight of a
watershed that contains only one sampling class. Using this technique, both watersheds have an
approximately equal probability of being selected. This scheme will work accurately if there are
equal numbers of watersheds considered in each sampling class; the presence of unequal numbers
will cause some deviation from the most desirable distribution of samples.
To avoid overemphasizing the very common soils, only one sample will be taken from each
watershed that contains only one sampling class. All named soils in a complex soil series are
counted as occurrences in their respective sampling classes. For example, a Tunbridge-Lyman soil
complex in a watershed mapping unit would be considered as one occurrence of sampling class
S12, which contains the Tunbridge series, and one occurrence of sampling class S13, which
contains the Lyman series.
The method used to select watersheds within sampling classes will be to sort the watersheds
by ANC cluster and then take a systematic, weighted, random sample using the weights described
above. This procedure selects a random starting point in the list of watersheds and then selects
watersheds at regular intervals from the (weighted) list. This method ensures a selection across
the range of ANC clusters.
To ensure that a watershed is not sampled more than once for a given sampling class, the
weight assigned should not be larger than the interval used in the systematic sampling. Weights
should be scaled down if they exceed the systematic sampling interval.
2.4.3.3-
Once this procedure has been followed for each sampling class, the initial selection of
watersheds and sampling classes can be summarized. Three options are possible at this point:
The weighing factors can be adjusted iteratively until the allocation is acceptable.
Samples can be arbitrarily moved among watersheds to reach the desired allocation.
The selection can be accepted as adequate.
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If the selection is not considered adequate, the most acceptable solution is to repeat the
procedure using adjusted weights. This process could be automated, if necessary, with the weight
of a watershed being increased until it receives sufficient samples.
The method of sampling class and watershed selection outlined here is designed to satisfy
the objectives and constraints listed in sections 2.4.1 and 2.4.2. Given the nature of the constraints,
it is likely that there is no single, perfect solution; however, this method allows the production of
an acceptable selection that is a compromise between the demands of the different objectives.
2.5 Final Selection of Sampling Locations
2.5.1 Rationale and Objectives
Soil surveys generally have a holotypic purpose of describing the typical soil series or soil
phases found in a watershed. The DDRP is interested in obtaining samples that are integrative or
that represent the sampling class in the watershed. This sampling class may contain six or seven
similar soils. The sampling purpose is not to describe the characteristics of a specific soil phase,
but rather to describe the characteristics of the sampling class. Because all soils within a
sampling class are considered similar in soil chemistry, the specific sampling location within a
sampling class can be selected at random with respect to the soil series. The procedures
described in this section are intended to: (1) characterize the range of variability that occurs within
a sampling class, and (2) characterize the soils within a sampling class using similar levels of
precision.
Determining the sampling location within the watershed sampling class is a two-step process.
2.5.2 Sampling Site Selection
There are five steps in selecting representative sampling sites within a sampling class:
NOTE: Steps 1 through 5 will be completed by ERL-C. Maps that show the five random
points, as discussed in Step 3, will be given to each SCS sampling crew.
Step 1: Prepare a list of all mapping units and the sampling class or classes in which they
occur. Most mapping units will occur only in one sampling class; complexes may
occur in two or more sampling classes. For each complex, record the proportion
of area occupied by each soil series in the complex (from the mapping unit
description). This proportion should be average proportion, excluding the area
occupied by inclusions.
Step 2: For each watershed, obtain the watershed map and identify the sampling classes
selected for that watershed. Mapping-unit delineations for each soil series must
be aggregated and identified for each sampling class.
Step 3: Transfer a grid that has a cell size of about 2 acres to a Mylar sheet. Overlay the
grid on the watershed map. Select a set of random coordinates (using a
computer program) and determine if the point they represent intersects one of the
sampling classes selected on that watershed. If the point does not fall within the
selected sampling classes, draw another pair of random coordinates. Continue
this process until five random points have been identified in each sampling class.
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Record their order of selection from 1 through 5. Some sampling locations may
not be accessible, so alternate locations must be provided.
Step 4: If the point falls on a sampling unit that is a complex, draw a random number,
Y, between zero and the total percentage of the soils in the complex (e.g., a 50-
30 percent complex of Tunbridge-Lyman would sum to 80, so the maximum random
number is 80). Determine the percentage of the area in the desired sampling class
(e.g., Tunbridge is 50 percent). Call this number X If X is less than Y, draw
another set of coordinates. This procedure minimizes the probability that
complexes will be overselected for sampling.
Step 5: For each location selected, overlay appropriate maps and note the vegetation class
associate with each point as: (1) coniferous, (2) deciduous, (3) mixed, (4) open
dryland, or (5) open wetland.
NOTE: For comparison of coniferous, deciduous, and mixed vegetation types to
Society of American Foresters (SAF) forest cover types, see Table 2.1.
Within the sampling class, sample the pedons that have one or more of the soils in the
sampling class and that have one or more of the vegetation classes noted above.
2.5.3 Sampling Site Locations
The procedure described above is to locate the general vicinity of the site on the watershed
soil maps. This procedure is completed, and the soil maps marked with the random points are
distributed, before the sampling crew leaves for the field. The point marked on the map may
represent an area of 100 m2 in the field. Within this general vicinity there may be inclusions, rock
outcrops, a complex soil, or other factors that make finding a soil of the specific sampling class
difficult. The following procedures will be used to select the specific sampling site in the
watershed.
2.5.3.1--
Obtain a list of the sampling classes to be determined on that watershed. Also obtain a map
that clearly shows the five predetermined random points for selection.
2.5.3.2-
As best as can be determined, the sampling crew will go to the location of the first potential
sampling site indicated on the map. If that location is inaccessible, go to the second potential
sampling site but note the reasons in the field logbook and, if possible, on the SCS-232 field form.
2.5.3.3-
If the location is accessible and the soil series at the site is in the selected sampling class
and the vegetation class is appropriate, sample the pedon.
2.5.3.4-
If the randomly selected site contains a soil series that is not a member of the sampling
class, or if the vegetation class is not appropriate from a random-number table, select a random
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number between 1 and 8, where 1 represents the direction north, 2 represents northeast, 3
represents east,... 8 represents northwest. Walk along a straight line in the direction chosen until
the first occurrence of the proper combination of soil series and vegetation class is found. The
maximum distance walked corresponds to a radius of 155 m around the randomly selected site.
If a proper combination of soil series and vegetation class is not obtained after five tries, go to
the next potential site on the list. The number of traits at each site and the number of alternative
sites attempted should be recorded on Form SCS-232.
These procedures provide a method for selecting a specific site and locating that site in the
field.
Table 2-1. Comparison of Coniferous, Deciduous, and Mixed Vegetation Types to Society of American Foresters
(SAP) Forest Cover Types
SAP Cover Type Name Cover Type Number
Coniferous Vegetation Types
Jack Pine 1
Balsam Fir 5
Black Spruce 12
Black Spruce - Tamarack 13
White Spruce 107
Tamarack 38
Red Spruce 32
Red Spruce - Balsam Fir 33
Red Spruce - Frasier Fir 34
Northern White Cedar 37
Red Pine 15
Eastern White Pine 21
White Pine - Hemlock 22
Eastern Hemlock 23
Deciduous Vegetation Types
Aspen 16
Pin Cherry 17
Paper Birch 18
Sugar Maple 27
Sugar Maple - Beech - Yellow Birch 25
Sugar Maple - Basswood 26
Black Cherry - Maple 28
Hawthorn 109
Gray Birch - Red Maple 19
Beech - Sugar Maple 60
Red Maple 108
Northern Pin Oak 14
Black Ash - American Elm - Red Maple 39
Mixed Vegetation Types
Hemlock - Yellow Birch 24
Red Spruce - Yellow Birch 30
Paper Birch - Red Spruce - Balsam Fir 35
White Pine - Chestnut Oak 51
White Pine - Northern Red Oak - Red Maple 20
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2.6 Special Conditions
2.6.1 Inaccessible Watersheds
An attempt should be made to sample every watershed. However, some watersheds may
have inaccessible areas or areas where sampling access is denied. Alternative sampling classes
are selected during the random selection process as back-up sampling locations to ensure an
equitable distribution of samples among sampling classes. Initial estimates of watersheds that
may be remote and difficult to sample or that may be inaccessible include one in New Hampshire,
one in Massachusetts, two in Connecticut/Rhode Island, three in Maine, and five in New York. Each
state will formally document the reasons for excluding each watershed.
2.6.2 Inclusions
Inclusions are not representative of the soils in the sampling class and should not be
sampled if the randomly selected site is located on an inclusion. The procedures described earlier
accommodate this contingency. Generally, inclusions are soils associated with a sampling class
other than the one being sampled. The chemical properties of the inclusion, therefore, are
described when the other sampling class is sampled.
2.6.3 Agricultural Sites
The open-dryland class contains some cultivated fields. If these sites are randomly selected
and access permission is obtained, the sites will be sampled. Agricultural practices, however,
generally alter the chemical characteristics of the soil through fertilization, liming, and other
activities.
Note samples taken from agricultural sites on the field forms. During subsequent modeling
and statistical analyses, these samples may or may not be incorporated in representing watershed
soil chemistry.
2.7 Paired Pedons
Paired pedon sites for sampling are selected and assigned in advance by ERL-C. These sites
will be sampled in conjunction with the corresponding routine pedon. The sample code identifying
the paired pedon should be treated as a routine pedon.
The location of the paired pedon is determined by the crew leader using the following criteria:
Establish sufficient distance between the two sampling locations to avoid disturbance of
the paired pedon from sampling of the routine pedon.
Use the same sampling unit and vegetation class as the routine pedon.
Use the same slope position as the routine pedon.
Use the same profile description and sampling protocol as the routine pedon.
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3.0 Site and Profile Description
3.1 Scope
Complete descriptions of the soils are essential to the soil survey and serve as a basis for
soil identification, classification, correlation, mapping, and interpretation. Standards and guidelines
are necessary for describing soil properties. Precisely defined standard terms are needed if
different people are to record their observations so that others can understand those observations.
However, the field scientist must always evaluate the adequacy of standard terms and add needed
information.
The description of a body of soil in the field, whether an entire pedon or a sample within it,
records the kinds of layers, their depth and thickness, and the properties of each layer. These
properties include color, texture, structure, characteristics of failure and disruption, roots and
animals (and their traces), reaction, salts, and boundaries between layers. Some properties that
apply to the entire sampling unit are also measured- and recorded. Generally, external features are
observed from study of a pedon that is judged to be representative of the polypedon.
For a soil description to be of greatest value, the part of the landscape that the pedon
represents should be known and recorded. Descriptions of pedons that represent an extensive,
mappable area are generally more useful than are descriptions of pedons that represent the border
of an area or a small inclusion. Consideration is given to external and internal features of the soil,
related features such as vegetation and climate, and the setting - the position of the particular soil
in relation to other soils and to the landscape as a whole.
Pedons used for detailed study of a soil are selected tentatively at first. Areas that previous
studies have shown to contain the kind of soil to be described and sampled are most commonly
chosen. The pedon is usually selected on the basis of external evidence. Depending on the
purpose of the study, the selected pedon may be one that has properties either near the middle
of the range of the taxon or near the limits of the range. After a sampling site is tentatively
located, it is probed with an auger, spade, or sampling tube to verify that the soil at the site does
have the diagnostic features of the soil and that its properties at the site represent the desired
segment of the soil's range.
A pit that exposes at least one clean, vertical face (approximately 1 m across) to an
appropriate depth is convenient for studying most soils in detail. Horizontal variations in the pedon,
as well as features too large or too widely spaced to be seen otherwise, can be observed. The
sides of the pit are cleaned of all loose material disturbed by digging. The exposed vertical faces
are then examined starting at the top and working downward, to identify significant differences in
any property that would distinguish between adjacent layers. Boundaries between layers are
marked on the face of the pit, and the layers are identified and described.
Photographs can be taken after the layers have been identified but before the vertical section
has been disturbed for description. If point counts are to be made for estimation of volume of
stones or other features, the counts are made before the layers are disturbed. If samples are to
be taken to the laboratory for analyses or other studies, they are collected after the soil has been
described.
Horizontal relationships between soil features can be observed in a cross section of each
exposed layer by removing the soil above it. Each horizontal section must be large enough to
expose any structural units. A great deal more about a layer is apparent when it is viewed from
above, in horizontal section, as well as in vertical section. Structural units that are otherwise not
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obvious, as well as in vertical section. Structural units that are otherwise not obvious, as well as
the third dimension of many other features, can be seen and recorded. Patterns or color within
structural units, variations of particle size from the outside to the inside of structural units, the
pattern in which roots penetrate structural units, and similar features are often seen in horizontal
section more clearly than in a vertical exposure.
3.2 Field Properties
The following parameters will be determined in the field by established SCS methods and
protocols tiZ".
Horizon type.
Horizon depth.
Color.
Texture.
Structure.
Consistence.
Boundary type.
USDA/SCS soil taxonomic designation.
Surface vegetation type and abundance.
Parent material.
Physiography.
Relief.
Slope.
Aspect.
Permeability.
Erosion class.
Root distribution.
Drainage class.
Depth to bedrock.
Bedrock exposure.
Volume percent coarse fragments by visual estimation.
20 to 75 mm.
75 to 250 mm.
>250 mm.
Diagnostic features.
Mottle type and abundance.
The field crew will use Form SCS-SOI-232 for field description which is coded for easy input
onto a computerized data file. The protocol for horizon description is discussed in detail in the SCS
Soil Survey Manual2, the SCS National Soils Handbook ', and Principles and Procedures for Using
Soil Survey Laboratory Data 3.
3.3 Profile Excavation
The exposed face of the pedon must be wide enough to permit pedon description, the
collection of bulk-density clods, and the collection of 5.5 kg or more of sample from each of the
significant horizons. The pedon face should be photographed (Section 3.4) before destructive
sampling begins.
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3.4 Photographs of Profile and Site
Photographic documentation of the sampling phase will be useful for later reference and
future discussions concerning specific site considerations, and will complement field descriptions.
Field crews will provide their own single-lens reflex, 35-mm cameras or equivalent and will obtain
film locally. Ektachrome, ASA 400 slide film is recommended, but field crews should determine film
speed suitability based on their knowledge of the site. If flash attachments and tripods are
available, they should be included in the sampling equipment. For film-quality consistency, all slides
should be developed using prepaid Kodak mailers.
Photographic documentation requires that a precise logbook be kept to identify corresponding
slides. The indexing system can be developed by the field crew, but must be based on the sample
code from NADSS Label A to identify the site. The system must be fully explained in the logbook.
Once the slides have been developed, they should be labeled on the slide mounts with the sample
code and any other information the field crew deems necessary. Slides will be stored in 3-ring
binders in slide files and will be submitted with the logbook to ERL-C at the conclusion of the
sampling phase of the survey. Histosols should be photographed by sequential placement of the
augered horizons on the surface.
The pedon face, tree canopy, understory vegetation, and representative landscape or landform
will be photographed for each site sampled. Scale should be provided by including a meter stick,
rule, or other suitable item in the photograph. Pedon face identification can be positively made by
including NADSS Label A or an index card displaying Label A information in the photograph. SCS
protocols for field photography are outlined in the SCS National Soil Survey Manual2, Chapter 9.
3.5 Important Points Concerning Horizon Descriptions
The sample site should be free of road dust and chemical contamination. State all known
spraying of pesticides and herbicides.
Soils will be sampled only from freshly dug pits large enough (1 m x 1 m) to allow sampling
of all major horizons to a depth of 1.5 m or to bedrock.
Samples will be taken from continuous horizons >3 cm thick, including the C horizon if
present. Discontinuous horizons will be sampled when considered significant by the crew leader.
Clods will be collected for all horizons sampled, except the O, horizon. The bulk density
procedure is detailed in Section 7.0.
All obvious horizons in a pedon are to be sampled, although a maximum of six horizons had
been previously specified as a limit for cost estimates and planning purposes. It is the decision
of the field soil scientist whether or not a horizon is significant enough, for DDRP purposes, to be
sampled and described. Therefore, if the field soil scientist believes there are eight significant
horizons, he should sample all eight. Pedons can not be dug in wetlands. The recommended
procedure for obtaining a 5.5-kg sample is to use a peat-sampling corer.
Sample pits will be accurately located on the soil survey maps, and the pit dimensions and
the azimuth perpendicular to the pit face will be recorded. The location of the pit in the field should
be flagged or identified so that it can be revisited, except in areas where this is not possible due
to landowner restrictions. One horizons per day will be sampled twice by each field crew. This will
be the field duplicate (FD). The choice of which horizon to duplicate is at the discretion of the field
crew. The procedure for obtaining this duplicate sample is to alternate when placing trowel or
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shovelfuls of sample into each sample bag. The horizon that is chosen for a field duplicate should
be alternated each day so that a complete range of field duplicates by horizon is achieved.
3.6 Field Data Form - SCS-232
All field data should be recorded on Form SCS-SOI-232, which is reproduced along with a
modified legend in Appendix A. The SCS is responsible for making sure that completed copies of
these forms are sent weekly to the following groups:
One copy to the preassigned soil preparation laboratory for each crew.
One copy to the EPA Environmental Monitoring Systems Laboratory-Las Vegas (EMSL-LV) to:
Lockheed Engineering and
Sciences Company
1050 E. Flamingo, Suite 120
Las Vegas, Nevada 89109
One copy to Oak Ridge National Laboratory (ORNL) to:
Oak Ridge National Laboratory
P.O. Box X
Building 1505, Room 343
Oak Ridge, Tennessee 37831
and one copy to the EPA ERL-C to:
Environmental Research Laboratory-Corvallis
200 S.W. 35th Street
Corvallis, Oregon 97333
NOTE: The following changes and additions from the normal procedure should be made to
complete Form SCS-232.
Page 1 of 4
Under "Sample Number," "unit" is synonymous with "pedon."
Under "Date" add the day as: / /
Month Year Day
Under "Describers Name" add the Crew ID in the upper right hand corner.
Under "Location Description and Free Form Site Notes" the first six digits of line 1 should be
the site ID (Lake ID), the seventh digit is a dash, the eight digit is the random number point (1 to
5), the ninth digit is a dash and digits 10 through 12 are the sampling class, digit 13 is a dash,
digits 14 through 16 are the azimuth perpendicular to the described pit face, the digit 17 is a degree
symbol"°".
Under "Vegetation" describe the three major species by decreasing basal area. Clearcut
should be noted as "CC." Describe dominant vegetation types prior to clearcut in the free form site
notes.
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The following soil description parameters need not be completed by field crews, but may be
if information is accessible: Precep, Temperatures °C, Weather Station Number, ER.
Page 2 of 4
Dry color should be determined when needed for classification.
"VOL (LAT/TOT)" need not be completed but may be if information is accessible.
Page 3 of 4
Mottles should be described as indicated in Chapter 4 of the National Soils Survey Handbook1.
"Effervescence" will be determined at the preparation laboratory and need not be completed
here.
Page 4 of 4
The three divisions under "Rock Fragments" correspond to the three volume particle size
estimates:
line 1 = 2 to 75mm
line 2 = 75 to 250 mm
line 3 = >250 mm
Legend
Under "Site Description Codes" for page 1 add "AA" for a local site description.
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4.0 Sampling Procedures
4.1 Scope
The objective of the field sampling phase of the DDRP is to characterize the soil and
watershed characteristics across the regions of concern, the northeastern United States, and the
southwestern portion of the Blue Ridge Province.
Field sampling includes the collection of a 5.5-kg field sample that will yield a minimum of
2 kg of air-dried material of particle sizes <2 mm. This requires 5.5 kg of mineral soil, or as much
soil possible to fill the presupplied 46 cm x 53 cm sample bags, and twice this volume for organic
soils. In addition, bulk-density clods will be sampled for laboratory determination of field bulk
density.
4.2 Sampling the Pedon
4.2.1 Field Sampling Protocols
Field sampling protocols are based on the standard methods routinely used by SCS. The
following procedural steps were developed by the National Soil Survey Laboratory, Lincoln,
Nebraska, and are detailed in a publication titled Principles and Procedures for Using Soil Survey
Laboratory Data 3. An edited version of these procedures is reproduced here. The protocol for
collecting bulk-density samples is specified in Chapter 7.0 of this manual.
4.2.2 Sampling Party Responsibilities
The sampling party has responsibility to obtain samples representative of the pedons selected
for characterization. Although some sampling protocol has been specified, field-crew decisions are
necessary on how deep to sample, horizon delineation, thickness of horizon (or interval) sampled,
what material should be excluded from the sample, and the usefulness of compositing samples.
The sampling party ensures that site and pedon descriptions are adequate.
4.2.3 Pedons for Characterization
Pedons for characterization studies should be sampled to a depth of 1.5 m where possible.
In cases where the lower depths of the profile appear homogenous and the C horizon material is
particularly difficult to penetrate in (e.g., dense basal till), it may be feasible to dig the pit to 1.5 m.
However, it is still possible that a dense basal till will show a variable pH from the upper to the
lower sections of the C horizon. If this were true, a sample would be desirable even if the material
is hard to dig. These types of decisions are judments to be made to the best of the ability of the
sampling-crew leader and should be documented in the field sampling notebook. The sampling
party needs to be alert to taxonomic questions that may arise and sample appropriately to resolve
the questions (i.e., base saturation for Alfisol versus Ultisol may require subsamping at a specific
depth). Appropriate sampling increments depend on the kind of material and the proximity of the
horizon to the soil surface. Horizons in the upper 1 m would usually be split for sampling if they
are more than 30 cm thick, excluding organic horizons. Uniform horizons below 1 m are usually split
for sampling if they are more than 75 cm thick. The sampling party must exercise good judgment
in this decision process. The ideal sample contains each soil material within the horizon in
proportion to its occurrence in the pedon. The sampler attempts to approximate the ideal sample
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by carefully sampling a selected section of the horizon. The sample is usually taken along a pit
face from horizon boundary to horizon boundary and between arbitrary lateral limits.
4.2.4 Lateral Limits
Lateral limits encompass short-range variability observed at the site. If a recurring pattern
(i.e., mottles, durinodes, nodules, plinthite) is discerned, extend the lateral limits to four or five
cycles of the pattern. If this produces too much material, the sample is mixed, quartered, and
subsampled. At some point, the repeat cycles become too large or soil properties change
sufficiently that lateral extension is impractical or undersirable. An example is the gilgai pattern in
Vertisols. Proper characterization may warrant the sampling of two sets of horizons or pedons.
4.2.5 Stratified Horizons
If a horizon is stratified or otherwise contains contrasting materials, each material should be
carefully described. Some contrasting materials can be sampled independently, but in many cases
the materials are intertwined to the point that practicality dictates they be sampled together. Each
material should be described and the proportions should be noted, however. A decision on what,
if any, materials should be excluded from the sample is an integral part of collecting a
representative sample. The sampling party may decide to include soil material in cicada casts and
nodules as part of the sample, but to exclude material from a badger tunnel.
Coarse fragments (>20 mm) will be excluded from all samples sent to the laboratory except
for bulk-density clods.
4.2.6 Composite Samples
One sampling technique designed and used here to average lateral variability is to sample
three or four relatively small segments (20 to 30 cm wide) of the same pedon at several points
around the pit. The samples are composited, mixed, and a representative sample is sent to the
laboratory for analysis.
4.2.7 Filling Sample Bag
Approximately 5.5 kg or more of soil less than 20 mm in diameter should be placed in each
plastic sample bag. However, the amount of soil obtained for chemical analysis is highly dependent
on the amount of coarse fragments contained in each horizon.
For example, if the horizon is determined to contain 50 percent coarse fragments by a visual
estimate, the corresponding weight estimate for coarse fragments is 65 percent (Table 4.1). This
estimate indicates that a 5.5-kg sample will contain 35 percent of material <2 mm or only 1.8 kg
of sample. Field sampling protocols specify that a minimum of 2 kg of soil of particle size <2 mm
is necessary for the chemical and physical analyses specified. Care must be taken to ensure that
field samples will yield the minimum 2 kg of soil in the <2 mm particle-size class. Table 4.1
illustrates that a 5-kg sample from horizons containing coarse fragments greater than 60 percert
by weight or 45 percent by volume will not be sufficient to obtain a minimum 2-kg sample.
Minimum sample weights for horizons with coarse fragments and weights in this category are
provided in Table 4.1.
NOTE: This table is included as a guide and probably will not be most useful in the field, but
the concept explained is important.
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The general rule to follow is that the minimum amount of Held sample is 5.5 kg of the
^20-mm particle-size fraction. If the estimated 2- to 20-mm size class exceeds 45 percent by the
volume estimate, then two 5.5 kg samples or two full sample bags of mineral soil is necessary.
Two full bags of organic horizon material are requested in every case possible. Plastic sample
bags should be pre-labeled with NADSS Label A. Attach the label to the center of the bag, not near
the top of the bag. Double check that all designations are correct, complete, and legible. Large,
easily removed nonmineral material should not be included in the sample. Limit handling of the soil
sample to avoid contamination.
Table 4-1. visual Estimate of Percent Volume of Rock Fragments Greater than 75 mm Correlated to Percent
Weight
% Volume
0
3
7
10
13
16
20
23
27
31
35
40
45
50
56
62
68
74
80
% Weight
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
Weight of <20 mm
particles in a
5-kg sample
5.00
4.75
4.50
4.25
4.00
3.75
3.50
3.25
3.00
2.75
2.50
2.25
2.00
1.75
1.50
1.25
1.00
0.75
0.50
Sample weight
required to ob-
tain a minimum
2-kg sample
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.7
6.6
8.0
10.0
13.0
20.0
bag.
In wet soils, such as Histosols, excess water should be drained before sealing the sample
The top of the plastic sample bags should be folded down in 2.5-cm sections. The folded
sections should then be stapled or tied with twist-ties to seal.
The plastic bags should then be placed within pre-labeled canvas bags. Label the canvas bag
below the center with indelible ink or use presupplied label stamps. Record exactly the same
information contained on NADSS Label A. Seal the canvas bag by tying or stapling. Place the
samples in coolers with Blue Ice as soon as possible after field sampling. Transport samples to
the preparation laboratory as soon as possible.
4.2.8 NADSS Label A (Figure 4-1)
The date sampled is entered in the format DD MMM YY. For example, March 14, 1985, will be
1 4 M A R 8 5. The crew ID will consist of four digits: the first two are alphabetic, representing
the state; the second two are the number assigned to each crew for the state, for example, NY 01.
The site ID consists of six digits and appears on the assigned watershed map as:
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1
Region
2
Subregion
Alkalinity Class
456
Watershed 10
The sample code represents the SCS (PIPS) soil ID code and the sample type. The first three
digits of the sample code represent the type of sample (R11 = routine sample, one bag, one
sample; R23 = routine sample, 2nd of 3 bags; R33 = routine sample, 3rd of 3 bags; Field Duplicate
= FDO, [FD1, FD2 are used for compound bags of field duplicates] etc.), digits 4 to 5 are the SCS
state code, 6 to 8 are the SCS county code, digit 9 is a dash, digits 10 to 11 are the county pedon
number and digits 12 to 13 are the horizon number. Upper and lower split horizons will be identified
by the depth designations (written after the horizon designation). A "U" or an T" can also be
written after the horizon depth to help to differentiate these samples for the preparation
laboratories. The Set ID is a four-digit number beginning with 0. The field sampling crews are
assigned the following ideal set of 100 Set ID numbers for sampling in the Northeast:
100-199 ME02
200-299 ME03
300-399 NH01
400-499 NY01
500-599 NY02
700-799 MA01
800-899 MA02
900-999 CT01
1000-1099 PA01
1100-1199 VT01
The field sample will be passed through a 75-mm sieve. All coarse fragments remaining on
the sieve can be subdivided manually into two size classes; 75 to 250 mm and 2250 mm.
Figure 4-1. NADSS Ubel A.
^ NADSS Ubel
v'
Date Sampled:
0 MMMY Y
Crew 10:
Site 10:
Depth:
cm
An estimate will be made of the volume percent of material in these classes. A volume estimate
of the percent coarse fragments for the 20- to 75-mm fraction will be made as well. This
information will be entered on SCS Form 232 under the Rock Fragments category, Size (SZ, 1 » 20
to 75 mm, 2 = 75 to 250 mm, and 3 = £250 mm). The preparation laboratory will determine the
percent coarse fragments in the 2- to 20-mm fraction. The sieved soil <20 mm should be used as
the soil sample and should be placed in the sample bag according to procedures in Section 4.2.7.
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4.3 Delivery
The soil samples should be delivered to the pre-assigned soil preparation laboratory. The
following preparation laboratory assignments are for the Northeast sampling crews. Preparation
laboratories for the southeastern sampling crews will be assigned at a later date.
Field Crew Preparation Laboratory
Maine University of Maine
New Hampshire, Vermont, Massachusetts University of Massachusetts
Connecticut, Rhode Island University of Connecticut
New York, Pennsylvania Cornell University
Samples will be kept as cold as possible in the field by storage in coolers with Blue Ice gel
packs until delivery to the preparation laboratory. Temperature checks in the cooler should be made
routinely to keep a 4 °C ambient air temperature. These readings should be recorded in the field
logbook. Due to the location of some watersheds, some samples may not be delivered to the
preparation laboratory until three to four days after they are sampled. Each field sampling crew
will deliver field samples as soon as possible after collection. If major problems occur, notice must
be given as soon as possible to the QA Officer. Every effort should be made to get the field
samples to the preparation laboratory as soon as possible.
Great care should be taken not to drop or puncture sample bags in transport to the
preparation laboratory.
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5.0 Soil Preparation Laboratory
5.1 Scope
The samples will be received by the preparation laboratory supervisor. The supervisor will
check the samples for spillage or other problems and to be certain that each sample has an
accompanying NADSS Label A (Figure 4-1). Field samples and all QC samples will be logged in on
NADSS Form 101 (Figure 5-1). The QC samples will be randomly assigned in the batch by the
preparation laboratory. One set of samples will be defined as the total number of samples taken
in one day by one crew. Each set will include one field duplicate, because one horizon per day is
to be sampled twice as a field duplicate. Two pre-assigned audit samples will be randomly
inserted into each batch. In addition, one sample per batch will be randomly selected, divided into
two samples, and tracked as the preparation laboratory duplicate (PLO). One batch including
routine field samples, field duplicates, a preparation laboratory duplicate, and two audit samples
will contain a maximum of 42 samples. Therefore, the number of sets combined to make one
analytical batch depends on the number of samples in each set. The total number of samples in
the combined sets should not exceed 39.
5.2 Sample Storage
The samples will be sealed and stored at 4 °C at all times when not involved in processing.
This procedure will greatly reduce microbia! decomposition of organic matter without alteration of
the crystalline structures. If the samples cannot be dried immediately at the preparation laboratory,
they should be placed in storage until processing.
5.3 Sample Preparation
After the samples are received, sample numbers are assigned on NADSS Form 101. The
samples should be air-dried and sieved (<2 mm) (see Section 5.3.1). Care must be taken to be
certain that the soils are not separated from their labels during the air-drying process. The
percentage of coarse fragments (>2 mm) must be weighed as specified in Section 5.3.2 and the
percent coarse fragments reported on NADSS Form 101. The coarse-fragment fraction should be
labeled and set aside. If the qualitative test for inorganic carbon is positive, the analysis for total
inorganic carbon must be performed on this sample, and the 2- to 20-mm fraction must be crushed
and shipped to the analytical laboratory. The results of the determination of effervescence are
recorded on NADSS Form 101.
5.3.1 Sample Drying and Mixing
5.3.1.1--
The soil is laid out on a tray and allowed to air-dry at room temperature until constant weight
is achieved (30 to 35 °C is ideal). Constant weight is defined as that time when a subsample does
not change by more than 2.5 percent moisture content on two consecutive days. Constant weight
must be determined before the sieving process is started. The drying period could range from two
days to seven or more days, depending on organic matter content and particle size of the sample.
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Date Received D D M H H Y Y
By Data Mgt.
National Acid Depoaition Soil Survey (NADSS) Form 101
Batch ID
Crew ID
Prep Lab ID
Lab Set Sent
Date Shipped
Set ID
to
Date Sampled
Date Received
Date Prep Completed
No. of Samples
Sample
No.
'01
02
03
04
05
06
07
~08 '
"09
10
11
_
H I
14
15
16
nr?
18
19
f- ,
20
21
22
23
24
25
26
27
_>8
29
30
31
32
33
34
35
36
37
38
39
40
41
42
Site
ID
Sample
Code
Set
ID
Coarse
Fragments
i
CF
Air-dried
Moisture
%
W
RSD
Signature of Preparation Laboratory Supervisor:
t'oiiunent :
Inorg.
Carbon
(1C)
Y=yes
N=no
Bulk
Density
g/cc
Figure 5-1. National Acid Deposition Soil Survey (NADSS) Form 101.
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5.3.1.2--
After the soil is air-dried, place the complete sample in the orginal sample bags and store
them at 4 °C until further preparation laboratory analysis is performed.
5.3.1.3-
After the soil is air-dried, place the complete sample minus the calibration sample in the
original sample bags and store them at 4 °C until preparation laboratory analysis.
5.3.2 Coarse Fragment Determination
5.3.2.1-
The fragment size class that will be separated during this procedure is the class that is small
enough to pass through a 20-mm sieve. Coarse fragments larger than 20 mm will be determined
in the field.
5.3.2.2-
The total sample should be weighed and quantitatively passed through a clean, dry, square-
holed, 2-mm sieve to segregate coarse fragments (2 mm to 20 'mm) from the soil. The material
larger than 2 mm should be saved until the test for inorganic carbon is complete. The soil that
passed through the sieve (0 to 2 mm) should be placed in a sealed container if further processing
will not occur at this time.
5.3.2.3-
The amount of soil that did not pass through the sieve should be weighed and divided by the
inital amount and multiplied by 100. This percentage is then recorded as percent coarse fragments
(%CF). The coarse fragments (2 to 20 mm) must be saved until the qualitative test for inorganic
carbon has been completed.
5.3.3 Soil Mixing
After the soil has passed through a 2-mm sieve and %CF is determined, quantitatively load
the soil into the Jones type 3/8-inch riffle splitter. The soil should be passed through the riffle
splitter at least seven times. Before reloading the splitter each time, level the soil on the tray to
ensure random particle addition. It is best to remove the 1-kg subsample for the analytical
laboratory at this time. If the 1-kg subsample is to be removed later, the entire sample must again
be passed through the riffle splitter before a well-mixed subsample can be removed. After
completion of the soil preparation procedures, the soils should be placed into a new inner plastic
liner supplied by EPA-LV. Complete NADSS Label B (Figure 5-2) and place it on the exterior of the
inner bag that is to be sent to the analytical lab.
Remove NADSS Label A from the original field bag and tape it into a preparation laboratory
notebook, grouped in order by set number and batch number. Record the date either on the label
or below it. Initial the label by writing partially on the label and partially on the page. This
procedure will help to replace labels that may become unattached. The air-dried soil in the inner
bag should be sealed with a plastic-coated wire twist.
55
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NAOSS Ubtl B.:.:.
.......',. ; .' '.,. ;'.
Batch 10: J^,/'.
Samola No:-, .;'''
Section 5.0
Revision 2
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Page 4 of 8
Figure 5-2. NADSS Latwi B.
At this point, the exterior canvas bag will have the field coding written on it and the inner bag
will show the batch number and sample number.
The field coding on the outer plastic bag should be crossed out so it is not legible, and the
batch number and the sample number should be written on the exterior with indelible ink. The soil
should be packed tightly in the boxes supplied by EPA-LV. After all subsamples have been removed
for shipment to the analytical laboratories, the remaining sample should be placed in a clean plastic
bag and stored at 4 °C. The samples should be clearly and permanently labeled with NADSS Label
B and stored in such a manner that they are easily retrievable if necessary.
5.3.4 Qualitative Test for Inorganic Carbon
5.3.4.1-
Carbonates are used frequently as criteria to differentiate soil series. A qualitative test for
carbonates will be performed on the «s2-mm size class. If the test for effervescence is positive,
the coarse-fragment size class (2 to 20 mm) will be crushed and sent to the analytical laboratory
for quantitative total inorganic carbon analysis. For the following procedures, the word "soil" is
defined as that material which has been air-dried and passed through a 2-mm sieve.
5.3.4.2-
Place 1 g of soil in a porcelain spot plate. Saturate the soil with deionized (DI) water and
stir with a glass rod to remove entrapped air. Place plate under a binocular microscope.
5.3.4.3-
Add 4 N HCt by dropwise addition and observe through microscope for effervescence.
5.3.4.4-
Repeat this procedure with another 1 g of soil from the sample.
5.3.4.5-
noted.
Record in laboratory notebook for each subsample whether effervescence was or was not
56
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5.3.4.6-
If effervescence was noted either time, inorganic carbon must be determined for this sample.
5.3.4.7-
If effervescence was observed, the coarse-fragment fraction from this soil sample should be
crushed to pass an 80-mesh sieve. A 100-gram subsample should be prepared using a riffle
splitter, and should be shipped separately (without the soil sample) for inorganic carbon
determination. The subsample should be packaged in a plastic bag and labeled with NADSS Label
B. Coarse-fragment subsamples do not require storage at 4 °C until shipment to the analytical
laboratory.
5.4 Shipment of Subsample to Analytical Laboratories
5.4.1 Shipping Method
Subsample will be shipped to the analytical laboratories by batch. Each box shipped must
contain copies of NADSS Shipping Form 102 (Figure 5-3). The results of the bulk density
determination and percent coarse fragment determinations must also appear on Form 102. If Form
102 indicates a positive inorganic carbon test, the coarse fragment sample must be shipped to the
analytical laboratory for total inorganic carbon analysis. As indicated on the bottom of NADSS
Form 101, the canary, pink, and gold copies should be enclosed with each sample box. The white
copy should be sent to the Sample Management Office (SMO) after a photocopy is made to keep
at the preparation laboratory. The address for shipment to SMO is:
National Acid Deposition Soil Survey
Sample Management Office
P.O. Box 818
Alexandria, Virginia 22313
The shipping carrier to be used and specific shipping protocols required to ship samples to
the analytical laboratory will be supplied to the preparation laboratory by the QA Manager.
5.4.2 NADSS Form 101
NADSS Form 101 is used to combine field sets into an analytical set. A maximum of six sets
should be combined to achieve a maximum of 39 routine and field duplicate samples. In addition,
there will always be one preparation laboratory duplicate (PLD) and two audit samples per batch
for a combined maximum number of 42 samples. If four to six sets are used for one batch, the
second section of Form 101 should be modified to fit, ignoring the predrawn lines and utilizing
space as necessary. Air-dried moisture (or column "w") should be the final moisture content used
to verify air-dryness, reported to two decimal places. NADSS Form 101 should be completed in
black ink and should not contain any mistakes, crosscuts, or white out. The form should be mailed
within 24 hours after the batch has been shipped to the analytical laboratory. The white copy
should be sent to ORNL at the following address:
Oak Ridge National Laboratory (ORNL)
P.O. Box X
Building 1505, Room 343
Oak Ridge, Tennessee 37831
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Page 6 of 8
The gold copy should be sent to the EPA ERL-C, in care of:
Environmental Research Laboratory, Corvallis
200 S.W. 35th Street
Corvallis, Oregon 97333
The pink copy should be sent to EPA EMSL-LV, in care of:
Lockheed Engineering and Sciences
Company, Inc.
1050 E. Flamingo Road, Suite 120
Las Vegas, Nevada 89109
5.5 Sample Receipt by the Analytical Laboratory from the
Preparation Laboratory
The analytical laboratory should immediately compare the samples and the data on Form 102.
Record should be made as to when the samples were received, and their condition upon receipt.
All missing samples should be noted. This information should be recorded on Form 102 and
initialed by the recipient.
If NADSS Form 102 is incomplete, immediately notify SMO at (703) 557-2490. The gold NADSS
Form 102 should be kept as the analytical laboratory. The canary NADSS Form 102 should be sent
to SMO at the address indicated in Section 5-4 and the pink copy should be mailed to EMSL-LV at
the following address:
Lockheed Engineering and Sciences
Company, Inc.
1050 E. Flamingo Road, Suite 120
Las Vegas, Nevada 89109
The recipient should check to be sure that all samples for inorganic carbon analysis have
been included.
5.6 Shipment of Mineralogical Samples
Horizons to be subsampled for mineralogical analysis will be designated by the QA Manager.
Approximately 10 percent of the pedons sampled will require this analysis. Subsamples (100 g
EMSL-LV. NADSS Label B (Figure 5-2) will be placed on those bottles and shipping Form 115
(Figure 5-4) will be included in each box shipped. Sample receipt protocol by the mineralogical
laboratory is the same as that specified in Section 5-4 for analytical examples.
58
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Section 5.0
Revision 2
Date: 9/85
7 of 8
Data Received D D M M M Y Y
By Data Mgt.
National Acid Deposition Soil Survey (NAOSS) Form 102
Prep Lab
Batch ID
Analytica
Sample
No.
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
JO
31
32
33
34
35
36
37
33
39
40
41
D D M M M Y Y
ID Date Recieved
Date Shipped
1 Lab ID
Air-dried
Moisture t
W RSD
-j
Inorganic
Carbon
(1C)
Y-y«e N»no
Signature of Preparation Laboratory M.anaqer:
Comments :
Coarse Fragments
Shipped?
(Check Y if yes)
bHL = White Canary = ANA. Lab w/copy to SMC Pink * ANA. Lab w/copy to EMSL-LV Gold « ANA. Lab
Flgurt 5-3. National Acid Dapoaltlon Soil Survey (NAOSS) Form 102.
59
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Section 5.0
Revision 2
Date: 9/85
Page 8 of 8
Date Received D D M M M Y ₯
By Data Mgt.
National Acid Deposition Soil Survey (NADSS) Form 115
D D M M M Y V
Prep Lab ID Date Reoieved
Analytical Lab ID _ Date Shipped
Sample No.
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
iO
31
32
33
34
35
36
37
38
39
40
41
12
Batch ID
Sample Ho.
Signature of Preparation Laboratory Manager:
Comments:
SML = White Canary = ANA. Lab w/copy to SMC Pink = ANA. Lab w/copy to EMSL-LV Gold « ANA. Lab
Figure 5-4. National Acid Deposition Soil Survey (NADSS) Form 115.
60
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Section 6.0
Revision 2
Date: 9/85
Page 1 of 3
6.0 Summary of Physical and Chemical Parameters
and Methods
6.1 Physical Parameters
6.1.1 Particle Size
Soil-texture analysis is routinely determined for soil characterization and classification
purposes. The standard pipet method is used. Particles greater than 20 mm will be determined
by field sieving and weighing; coarse fragments (2 to 20 mm) will be determined at the soil
preparation laboratory and soil less than 2 mm will be determined at the analytical laboratory. This
analysis will be performed on all mineral horizon samples, including the additional samples from
each impervious layer less than 3 cm thick.
6.1.2 Mineralogy
Clay minerals are identified by X-ray diffraction, whereas light and heavy minerals of the fine-
sand fraction are identified by optical mineralogy. Mineralogical identification is necessary to:
(1) help characterize the soil, (2) provide an indication of weathering rates, and (3) yield information
about minerals weathered from the parent material. This analysis will be performed only on
samples selected by ERL-C.
6.1.3 Specific Surface Area
Specific surface is measured because this is highly correlated with anion adsorption/
desorption, cation exchange capacity, and the type of clay mineral. The method specified is
saturation with ethylene glycol monomethyl ether. This analysis will be performed on all mineral
horizon samples.
6.2 Chemical Parameters
6.2.1 pH
pH is a measurement of free hydrogen ion activity. pH measurements are determined in three
different soil extracts. The extracts are DI water 0.01 M CaCI2, and 0.002 M CaCI2 in a 1:2 ratio
in a mineral soil and a 1:5 ratio for organic horizon samples. These analyses will be performed on
all samples.
6.2.2 Total Carbon and Total Nitrogen
Total carbon and total nitrogen are critical parameters due to their close relationship with
microbial decomposition of soil organic matter. The method specified is oxidation followed by
thermal conductivity detection using an automated CHN analyzer. These analyses will be performed
on all samples.
61
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Section 6.0
Revision 2
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6.2.3 Inorganic Carbon
Quantification of inorganic carbon is necessary due to the inherent ability of carbonates to
buffer acid inputs. If carbonates exist, they will be determined by manometric detection of evolved
CO2 after extraction with a strong acid, or by an automated CHN analyzer. Carbonates are not
expected because the soils being sampled are generally thought to be acid sensitive. Inorganic
carbon analyses will be performed only on soil samples reacting positively to a test for
effervescence upon the addition of drops of 4 N HCI.
6.2.4 Ext/-actable Sulfate
The amount of extractable sulfate will indicate the sulfate saturation of the anion exchange
sites. Extractable sulfate is determined in two different extracts (01 water and 500 mg/L P).
Extractable sulfate is then determined by ion chromatography. These analyses will be performed
on all samples.
6.2.5 Sulfate Adsorption Isotherms
The ability of soil to adsorb suffate is perhaps the most important parameter in determining
if a soil unit will show direct or delayed response to added sulfate deposition. Isotherms will be
developed by placing soil samples in six separate sulfate solutions for 1 hour and determining the
amount adsorbed by analysis of the solution for sulfate after contact with the solution. These
isotherms will represent the maximum sulfate adsorption capacity of the soil at the given
conditions. Sulfate adsorption isotherms will not be required for organic horizons, but will be
performed on all mineral horizons.
6.2.6 Total Sulfur
Total sulfur is measured because of its close relationship with extractable sulfate, and to
inventory existing sulfur levels to monitor future inputs of anthropogenic sulfur. An automated
method involving sample combustion followed by titration of evolved sulfur will be used.
6.2.7 Cation Exchange Capacity
Cation Exchange Capacity (CEC) is a standard soil characterization parameter and indicates
the ability of the soil to adsorb exchangeable bases. Therefore, it is well correlated with soil
buffering capacity. Ammonium chloride (NH4CI, pH 7.0), and ammonium acetate (NH4OAc, pH 7.0),
and 0.002 M calcium chloride (CaCI2) will be used as the replacement solutions. The extractable
bases (Na+, K+, Ca2+, Mg2+) will then be determined on the extracts by flame atomic absorption
spectroscopy (AA) or inductively-coupled plasma-atomic emission spectroscopy (ICP). These
analyses will be performed on all samples.
6.2.8 Exchangeable Acidity
Exchangeable acidity is a measure of the remaining exchangeable soil cations that are not
part of the base saturation. Two methods are specified. One employs a BaCI2--triethanolamine
extraction and the other employs a KCI extraction. The former extraction quantifies total
exchangeable acidity and the latter quantifies effective exchangeability acidity. Aluminum acidity
is also determined in the KCI extract by analyzing the extract for Al by AA or ICP. These analyses
will be performed on all samples.
62
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Section 6.0
Revision 2
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Page 3 of 3
6.2.9 Extract able Iron and Aluminum
Iron oxides and aluminum oxides are highly correlated to sulf ate adsorption and are important
in standard soil characterization. Extractable Fe and Al are determined by AA or ICP in three
different extracts. Each extract yields an estimate of a specific Al or Fe fraction. The three
extracts (and fractions) are sodium pyrophosphate (organic Fe and Al), acid-oxalate (organic plus
sesquioxides), and citrate-dithionite (nonsilicate Fe and Al). These analyses will be performed on
all samples.
6.2.10 Lime and Aluminum Potential
Lime potential is used as an input for certain models instead of base saturation; it is defined
as pH-1/2 pCa. Another characteristic shown to be important to watershed models is the
relationship of pH to solution AI3+ levels, defined as the aluminum potential (KJ, which is 3pH-pAL.
The method involves extracting the soil with 0.002 m CaCI2 and determining pH, Ca, and Al in the
extract. The remaining base cations, Na+, K+, and Mg2+, as well as exchangeable Fe, will also be
determined on this extract because of expediency and comparability to other extracts. These
analyses will be performed on all samples.
63
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Section 7.0
Revision 2
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7.0 Bulk-Density Determination
7.1 Scope
Bulk density is defined as the weight per unit volume of a soil. Bulk density generally ranges
between 1.0 and 2.0 g/cm3. For organic soils, bulk density commonly ranges from 0.050 to 0.355
g/cm . Bulk density will be determined by the field collection and Saran coating of clods from each
horizon, followed by weighing the clods by the preparation laboratories.
This method was chosen because of routine use in the field, relative ease of performance,
and elimination of compaction problems inherent in core methods. It will be impossible to collect
clods from certain horizons. Relationships between the particle-size distribution and surface area
data and pre-existing data may be used to derive values for missing data. The laboratory method
was provided by the Soil Morphology Laboratory, University of Massachusetts, Amherst,
Massachusetts.
7.2 Apparatus and Materials
7.2.1 Dow Saran S310 Resin
The Saran resin dissolves readily in acetone or methylethyl ketone. Acetone is preferred and
will be used because it is readily available and less toxic.
7.2.2 Coating Solution
The coating solution will be prepared by the preparation laboratories and will be supplied to
the field crews. To prepare the solution, calculate the amount of acetone required to make a 1:4
solution of resin to acetone. If a 1:7 solution is desired, the stock solution can be diluted with a
precalculated volume of acetone. The resin is not readily soluble in acetone and will require mixing.
Because the solvent is flammable, care should be taken during mixing. The solution should be
made in an exhaust hood. A nonsparking electric stirrer should be used. If a high-speed stirrer
is used, the resin dissolves in about 1 hour. If the solution must be made in the field, mix well and
often with a wooden stick. Metal paint cans will be supplied as mixing containers, although other
containers may be used as well. Some plastic containers are unsuitable because the acetone
dissolves the plastic. Containers that can be tightly closed are most desirable because the solution
is highly volatile and rapid evaporation will result in excesses of acetone being used. If the solution
becomes thick, add more acetone until the desired consistency is reached.
7.3 Procedure
Collect natural clods (three per horizon) of about 100 cm3 to 200 cm3 in volume (approximately
fist-size). Remove a piece of soil larger than the clod from the face of a sampling pit with a spade.
From this piece, prepare a clod by gently cutting or breaking off protruding peaks and material
sheared by the spade. If roots are present, they can be cut conventiently with scissors or side
cutters. In some soils, clods can be removed directly from the face of the pit with a knife or
spatula. No procedure for taking samples will fit all soils; the procedure must be adjusted to meet
the conditions in the field at the time of sampling.
64
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Section 7.0
Revision 2
Date: 9/85
Page 2 of 5
The clods are tied with fine copper wire or placed in hairnets and suspended from a rope or
string, then hung like a clothesline. The clods themselves should be labeled with some type of tag
that can be attached to the hairnet or string. The label should record the sample code, horizon,
and replicate number. Moisten clods with a fine mist spray. The suspended clods are dipped by
raising a container of the dipping mixture upward to submerse each clod momentarily. The number
of times a clod is dipped should be recorded on the label. The Saran-coated clods should be
allowed to dry for 30 minutes or longer.
7.3.1 Transport of Clods
Clods should be sealed in the presupplied 6" x 8" plastic bags, then placed in the
compartmentalized clod boxes. The top (inner face) of the clod box should be labeled with the
same information on the clod tag (i.e., sample code, horizon, replicate number, and how many times
the clod was dipped in the Saran). Great care must be taken to ensure that the clods are not
broken or damaged during handling and shipping. Space not occupied by the clods in each
compartment should be filled with packing material; for example, leaves, newspaper, or extra plastic
bags. Clod boxes may be reused by removing the old labels.
7.3.2 Preparation Laboratory Handling of Clods
Upon receipt of clods, labels should be removed and placed in the Bulk Density Preparation
Laboratory Notebook. However, the clods must be relabeled with the appropriate sample number
to retain identity. Notes should be made in the notebook regarding the condition of the clod upon
arrival, how many times the clod was dipped in Saran in the field, label clarity, and the time of
receipt. At the end of the project, this notebook should be submitted to Lockheed-EMSCO (EPA
EMSL-LV) Data Audit Supervisor.
7.3.3 Bulk-density Procedure
7.3.3.1-
Weigh the clod and record this weight in the laboratory notebook as m,.
7.3.3.2-
Dip the clod briefly in a Saran:acetone (1:6 w/w) solution and allow the coating to dry.
7.3.3.3-
Reweigh the clod and record this weight as m2.
7.3.3.4-
Repeat steps 7.3.3.2 and 7.3.3.3 as needed to obtain an impervious coating. Record weights
after each coating as m3, m4l etc.
7.3.3.5-
Place a 1-L beaker that contains 600 to 700 mL of de-aired and distilled water of known
temperature (recorded as T) on balance pan and record the tare weight as MA.
65
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Section 7.0
Revision 2
Date: 9/85
Page 3 of 5
7.3.3.6-
Suspend the clod over the beaker, lower it gently into the water until totally submerged, then
record the weight displayed on the balance as MB.
7.3,3.7-
Suspend the clod in a convection oven at 105°C for 48 hours.
7.3.3.8-
Remove the clod from the oven, weigh it, and record this weight as MOD.
7.3.3.9-
Place the clod in an appropriate container and put the container into an electric muffle furnace
for 2 hours at 400 °C.
7.3.3.10-
After the sample has cooled, weigh the contents of the container and record this as m,.
7.3.3.11-
Pass the sample through a 2-mm sieve and obtain the weights of coarse fragments and the
fine-earth fraction. Record these as MCF and m,c, respectively.
7.3.3.12 Calculations-
Moo ~ (MCF + MTS (0.85)]
BDfU =
MCF MTS
r H2OT 2.65 1.30
where BDFM is the field moist bulk density.
MQO is the oven-dry weight of the clod (Step 7.3.3.8).
MCF is the weight of the coarse fragments in the clod (Step 7.3.3.11).
MTS is the weight of the air-dry Saran coating which may be estimated as follows:
X (m. - m,)
MTS = T^T
where X is the total number of coatings (field + lab).
a is the number of laboratory coatings.
m, is the clod weight after the final coating.
m, is the initial clod weight after unpacking.
Mv is equal to MB. MA (from steps 7.3.3.5 and 7.3.3.6).
66
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Section 7.0
Revision 2
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Page 4 of 5
r H20T is the density of water obtained from Table 7.1 for the temperatures measured in
Step 7.3.3.5.
The final value to be reported on Form 101 is the coarse-fragment, and Saran-weight corrected
value.
7.3.3.13 Assumptions-
Four assumptions are made concerning the bulk-density procedure:
The weight of the individual, field-applied Saran coatings is equivalent to that applied in
the laboratory, and the Saran has not infiltrated the clod.
The specific gravity of the coarse fragments is 2.65.
The specific gravity of air-dried Saran is 1.30.
The Saran loses 15 percent of its weight upon oven drying at 105°C for 48 hours.
67
-------
Table 7-1. Specific Gravity* of Water
c
0
10
20
30
40
50
60
70
80
90
0
0.9999
09997
0.9982
09957
09922
09881
09832
09778
0.9718
09653
1
0.9999
0.9996
0.9980
0.9954
0.9919
0.9876
0.9827
0.9772
0.9712
0.9647
2
1.0000
09995
0.9978
09951
09915
0.9872
0.9822
0.9767
0.9706
09640
3
1.0000
0.9994
09976
0.9947
0.9911
09867
0.9817
09761
09699
0.9633
4
1.0000
0.9993
0.99973
0.9944
0.9907
0.9862
0.9811
0.9755
0.9693
0.9626
5
1.0000
0.9991
0.9971
0.9941
0.9902
0.9857
0.9806
0.9749
0.9686
0.9619
6
1.0000
0.9990
0.9968
0.9937
0.9898
0.9852
0.9800
09743
0.9680
0.9612
7
0.9999
09988
09965
09934
0.9894
0.9848
0.9795
0.9737
0.9673
09605
8
0.9999
0.9986
0.9963
0.9930
0.9890
0.9842
0.9789
0.9731
0.9667
0.9598
9
0.9999
0.9984
0.9960
0.9926
0.9885
0.9838
0.9784
0.9724
0.9660
0.9591
*Also the density or unit weight of water in grams per milliliter.
o>
TJO3JOJ
oj o» CD a>
-------
Section 8.0
Revision 2
Date: 9/85
Page 1 of 3
8.0 Crews, Supplies, and Equipment
8.1 Scope
Field crews will consist of four SCS employees. The lead soil scientist in each crew will
supervise all field operations. This person will be responsible for selecting each sampling site in
the field and for documenting all field data. The following is a list of supplies needed for each
field crew.
35-mm camera (macro lens or wide-angle lens).
ASA-400 film and Kodak premailer envelopes.
2 clinometers.
Munsell color charts.
Magnetic compass.
Hand lens.
2 brass sieves (3/4", 10 mesh, 19 mm)*.
2 thermometers* (centigrade).
5 coolers*.
40 Blue Ice gel packs*.
Stereoscope.
0.1 N HCI or 10% 4 N HCI and drop bottle.
vlsqueen 6-mil sheets, (41 x 4')*-
Spring scale (optional; use an exterior canvas bag for weighing).
Plastic inner sample bags (20/day)*.
Canvas exterior sample bags (20/day)*.
NADSS Label A (30/day)*.
Orange flagging (1 roll/day)*.
Yellow marker flags (20/day)*.
5 indelible-ink markers*.
SCS Form SOI 232 and clipboard.
69
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Section 8.0
Revision 2
Date: 9/85
Page 2 of 3
Field logbook*.
1-gallon paint can with lid*.
Saran* and acetone (Note: acetone must be purchased locally).
Hairnets (1 per clod)*.
6" x 8" plastic bags, 1 mil (enough for one per clod)*.
24-cell, 17.50" x 11.94" x 3.75" boxes (1 box per day - reusable)*.
2' x 2" blank vinyl labels (attach to box for individualized clod compartments)*.
Hand auger (for sampling Histosols; optional, may use spades).
Staplers*.
Saran Dow-310 resin*.
An asterisk indicates that the item will be shipped by EPA EMSL-LV. The amount of
equipment sent to each preparation laboratory is based on the number of crews assigned to that
laboratory.
The crews from New York and Pennsylvania (4) will receive supplies from the Cornell
University soil preparation laboratory. Maine crews (2) will receive supplies from the University of
Maine at Orono Soil Preparation Laboratory. Rhode Island-Connecticut (1), New Hampshire (1), and
Massachusetts crews will receive supplies from the University of Massachusetts at Amherst,
Massachusetts.
8.2 Equipment Notes
8.2.1 Coolers and Gel Packs
For each day of sampling, five coolers and eight gel packs per cooler should be stored in the
field sampling vehicle. The gel packs should be frozen in advance. Enough frozen gel packs should
be stored in a storage cooler to replace softened gel packs if ambient temperature in the cooler
falls below 4 °C. Coolers containing gel packs and soil samples should be taped shut before
transit. Two thermometers per crew will be provided for routine temperature checks on coolers
containing gel packs and soil samples. Temperature readings to the nearest tenth of a degree
should be recorded in the field notebook. Time and date should also be recorded in the notebook.
8.2.2 Marker Flags and Flagging
Upon arrival at the sample site, orange flagging should be tied to surrounding shrubbery at
eye level. This flagging is necessary in case of return visit to the pedon. The 21-inch stake yellow
flags should be placed at least 6 inches into the ground at the four corners of the pedon before
leaving the sample site.
70
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Section 8.0
Revision 2
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Page 3 of 3
8.2.3 Visqueen Plastic Sheets
Visqueen plastic sheets (4* x 4', 6 mil) will be provided for each crew. All soil materials less
than 20 mm should be sieved into these sheets. The sample is then poured into the inner plastic,
prelabeled sample bag. If by visual estimate the 2 to 20 mm particle-size class exceeds 50 percent
by volume, two 5.5-kg samples should be bagged and sieved for that sample. A canvas sheet may
be substituted for the 4* x 4* plastic sheet, but the use of this should be noted in the field notebook
and should be immediately reported to the EPA EMSL-LV QA officer.
8.2.4 Field Notebook
Daily activities of the field crew should be logged in a field notebook. Each day's activities
should be recorded; specific problems, solutions, and other miscellaneous notes should be
recorded, along with location and identification of each sample pedon. These field notebooks will
be submitted to Lockheed-ESC (EPA-EMSL-LV) in care of:
Lockheed Engineering and Sciences
Company
1050 E. Flamingo Road, Suite 120
Las Vegas, Nevada 89109
71
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Section 9.0
Revision 2
Date: 9/85
Page 1 of 1
9.0 References
USDA/SCS. 1983. National Soils Handbook. Part 600-606. U.S. Government Printing Office,
Washington D.C. 609 pp.
USDA/SCS. 1984. SCS National Soil Survey Manual. U.S. Government Printing Office. Washington
D.C.
Mausbach, M., R. Yeck, D. Nettleton, and W. Lynn. 1983. Principles and Procedures for Using Soil
Survey Laboratory Data. National Soil Survey Laboratory. Lincoln, Nebraska. 130 pp.
USDA/SCS. 1972. Soil Survey Laboratory Methods and Procedures for Collecting Soil Samples.
Soil Survey Investigations Report No. 1. U.S. Government Printing Office, Washington D.C.
68 pp.
72
-------
Appendix A
Revision 1
Date: 9/85
Page 1 of 22
Appendix A
Field Data Forms and Legends
73
-------
Appendix A
Revision 1
Date: 9/85
Page 2 of 22
u S Ot««tMlN» Of ar,nieuvtUM
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ici.ioi-
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74
-------
Appendix A
Revision 1
Date: 9/85
Page 3 of 22
'II
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Flgurt A-1. Continued (page 2 of 4).
75
-------
Appendix A
Revision 1
Date: 9/85
Page 4 of 22
Figure A-1. Continued (page 3 of 4).
76
-------
Appendix A
Revision 1
Date: 9/85
Page 5 of 22
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WEATHER
SET 1.0.
UNOERSTORY VEQ.
SUOES It PEO FACE
UNOERSTORY
OVERSTORY
LANDSCAPE
Figure A-1. Continued (page A of 4).
77
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Appendix A
Revision 1
Date: 9/85
Page 6 of 22
2.0 Soil Description Codes for Form SCS-SOI-232
2.1 Great Group Codes
Alfisols
AAQAL
AAQFR
AAQNA
MQPN
MQUM
ABOEU
ABOGL
ABOPA
AUDAG
AUDFR
AUDGL
AUDNA
AUDTR
AUSHA
AUSPN
AXEDU
AXEHA
AXEPA
AXERH
Albaqualf
Fragiaqualf
Natraqualf
Plinthaqualf
Umbraqualf
Eutroboralf
Glossoboralf
Paleboralf
Agrudalf
Fragiudalf
Glossudalf
Natrudalf
Tropudalf
Haplustalf
Plinthustalf
Durixeralf
Haploxeralf
Palexeralf
Rhodoxeralf
Aridisols
DARDU
DARND
DARPA
DORCM
DORGY
DORSA
Durargid
Nadurargid
Paleargid
Camborthid
Gypsiorthid
Salorthid
Entisols
EAQCR
EAQHA
EAQPS
EAQTR
EFLCR
EFLTR
EFLUS
EORCR
EORTR
EORUS
EPSCR
EPSTO
EPSUD
EPSXE
Cryaquent
Haplaquent
Psammaquent
Tropaquent
Cryofluvent
Tropofluvent
Ustifluent
Cryorthent
Troporthent
Ustorthent
Cryopsamment
Torripsamment
Udipsamment
Xeropsamment
AAQDU
AAQGL
AAQOC
AAQTR
ABOCR
ABOFR
ABONA
ASUPA
AUDFE
AUDFS
AUDHA
AUDPA
AUSDU
AUSNA
AUSRH
AXEFR
AXENA
AXEPN
Ouraqualf
Glossaqualf
Ochraqualf
Tropaqualf
Cryoboralf
Fragiboralf
Natriboralf
Paleustalf
Ferrudalf
Fraglossudalf
Hapludalf
Paleudalf
Ourustatf
Natrustalf
Rhodustalf
Fragixeral
Natrixeralf
Plinthoxeralf
DARHA Haplargid
DARNT Natrargid
DORCL Calciorthid
DORDU Durorthid
DORPA Paleorthid
EAQFL Fluvaquent
EAQHY Hydraquent
EAQSU Sulfaquent
EARAR Arent
EFLTO Torrifluvent
EFLUD Udifluvent
EFLXE Xerofluvent
EORTO Torriorthent
EORUD Udorthent
EORXE Xerorthent
EPSQU Quartzipsamment
EPSTR Tropopsamment
EPSUS Ustipsamment
78
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Appendix A
Revision 1
Date: 9/85
Page 7 of 22
Histosols
HFIBO
HFILU
HFISP
HFOBO
HFOTR
HHECR
HHEME
HHESO
HSABO
HSAME
Borofibrist
Luvifibrist
Sphagnofibrist
Borofolist
Tropofolist
Cryohemist
Medihemist
Sulfohemist
Borosaprist
Medisaprist
Inceptisols
IANCR
IANDY
IANHY
IAN VI
IAQCR
IAQHL
IAQHU
IAQPN
IAQTR
IOCDU
IOCEU
IOCUS
IPLPL
ITREU
ITRSO
IUMCR
IUMHA
Cryandept
Dystrandept
Hydrandept
Vitrandepth
Cryaquept
Halaquept
Humaquept
Plinthaquept
Tropaquept
Durochrept
Eutrochrept
Ustochrept
Plaggept
Eutropept
Sombritropept
Cryumbrept
Haplumbrept
Mollisols
MALAR
MAQAR
MAQCR
MAQHA
MBOAR
MBOCR
MBONA
MBOVE
MUDAR
MUDPA
MUSAR
MUSDU
MUSNA
MUSVE
MXECA
MXEHA
MXEPA
Argialboll
Argiaquoll
Cryaquoll
Haplaquoll
Argiboroll
Cryoboroll
Natriboroll
Vermiboroll
Argiudoll
Paleudoil
Argiustoll
Ourustoll
Natrustoll
Vermustoll
Calcixeroll
Haploxeroll
Palexeroll
HFICR
HFIME
HFITR
HFOCR
HHEBO
HHELU
HHESI
HHETR
HSACR
HSATR
IANDU
IANEU
IANPK
IAQAN
IAQFR
IAQHP
IAQPK
IAQSU
IOCCR
IOCDY
IOCFR
IOCXE
ITRDY
ITRHU
ITRUS
IUMFR
IUMXE
Cryofibrist
Medifibrist
Tropofibrist
Cryofolist
Borohemist
Luvihemist
Sulfihemist
Tropohemist
Cryosaprist
Troposaprist
Durandept
Eutrandept
Placandept
Andaquept
Fragiaquept
Haplaquept
Palacaquept
Sulfaquept
Cryochrept
Dystrochrept
Fragiochrept
Xerochrept
Dystropept
Humitropept
Ustropept
Fragiumbrept
Xerumbrept
MALNA
MAQCA
MAQDU
MAQNA
MBOCA
MBOHA
MBOPA
MRERE
MUDHA
MUDVE
MUSCA
MUSHA
MUSPA
MXEAR
MXEDU
MXENA
Natralboll
Calciaquoll
Duraquoll
Natraquoll
Calciboroll
Haploboroll
Paleboroll
Rendoll
Hapludoll
Vermudoll
Caiciustoll
Haplustol!
Paleustoll
Argixeroll
Durixeroll
Natrixeroll
79
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Appendix A
Revision 1
Date: 9/85
Page 8 of 22
Oxisols
OAQGI
OAQPN
OHUAC
OHUHA
OORAC
OORGI
OORSO
OTOTO
OUSEU
OUSSO
Giwsiaquox
Plinthaquox
Acrohumox
Hapiohumox
Acrorthox
Gibbsiorthox
Sombriorthox
Torrox
Eutrustox
Sombriustox
Spodosols
SAQCR
SAQFR
SAQPK
SAQTR
SHUCR
SHUHA
SHUTR
SORFR
SORPK
Cryaquod
Fragiaquod
Placaquod
Tropaquod
Cryohumod
Haplohumod
Tropohumod
Fragiorthod
Placorthod
Ultisols
UAQAL
UAQOC
UAQPN
UAQUM
UHUPA
UHUSO
UUDFR
UUDPA
UUDRH
UUSHA
UUSPN
UXEHA
Albaquult
Ochraquult
Plinthaquult
Umbraquult
Palehumult
Sombrihumult
Fragiudult
Paleudult
Rhodudult
Haplustult
Plinthustult
Haploxerult
Vertisols
VTOTO Torrert
VUDPE Pelludert
VUSPE Pellustert
VXEPE Pelloxerert
OAQOC
OAQUM
OHUGI
OHUSO
OOREU
OORHA
OORUM
OUSAC
OUSHA
SAQDU
SAQHA
SAQSI
SFEFE
SHUFR
SHUPK
SORCR
SORHA
SORTR
Ochraquox
Umbraquox
Gibbsihumox
Sombrihumox
Eutrorthox
Haplorthox
Umbriorthox
Acrustox
Haplustox
Duraquod
Haplaquod
Sideraquod
Ferrod
Fragihumod
Placohumod
Cryorthod
Haplorthod
Troporthod
UAQFR
UAQPA
UAQTR
UHUHA
UHUPN
UHUTR
UUDHA
UUDPN
UUDTR
UUSPA
UUSRH
UXEPA
Fragiaquult
Paleaquult
Tropaquult
Haplohumult
Plinthohumult
Tropohumult
Hapludult
Plinthudult
Tropudult
Paleustult
Rhodustult
Palexerult
VUDCH Chromudert
VUSCH Chromustert
VXECH Chromxerert
80
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Appendix A
Revision 1
Date: 9/85
Page 9 of 22
2.2 Subgroup Codes
AA Typic
AB04 Abruptic aridic
AS 10 Abruptic haplic
AB16 Abruptic xerollic
AE03 Aerie arenic
AE06 Aerie humic
AE09 Aerie tropic
AE12 Aerie xeric
AL02 Albaquultic
AL08 Albic glossic
AL12 Alfic arenic
AL16 Alfic lithic
AN01 Andeptic
AN06 Andic Dystric
AN22 Andic ustic
AN30 Anthropic
AQ02 Aquentic
AQ06 Aquic
AQ14 Aquic duric
AQ18 Aquicdystric
AQ26 Aquiclithic
AQ34 Aquollic
AR Arenic
AR03 Arenicorthoxic
AR06 Arenicplinthic
AR10 Arenicultic
AR16 Arenicustalfic
AR22 Argiaquic
AR26 Argic
AR30 Argicpachic
AR34 Aridic
AR42 Aridicduric
AR52 Aridicpetrocalcic
BO Boraific
' BO04 Boroalficudic
B008 Borollic glossic
BO12 Borollic vertic
CA Calcic
CA06 Calciorthidic
CA20 Cambic
CH06 Chromudic
CR10 Cryic lithic
CD Cumulic
CU04 Cumulic ultic
DU Durargidic
DUOS Durixerollic
DU11 Durochreptic
AB Abruptic
AB08 Abruptic cryic
AB14 Abruptic ultic
AE Aerie
AE05 Aerie grossarenic
AE08 Aerie mollic
AE10 Aerie umbric
AL Albaquic
AL04 Albic
AL10 Alfic
AL13 Alfic andeptic
AN Andic
AN03 Andaquic
AN11 Andeptic glossoboric
AN24 Andaqueptic
AQ Aqualfic
AQ04 Aqueptic
AQ08 Aquic arenic
AQ16 Aquic duriorthidic
AQ24 Aquichaplic
AQ31 Aquicpsammentic
AQ36 Aquultic
AR02 Arenicaridic
AR04 Arenicplinthaquic
AR08 Arenicrhodic
AR14 Arenicumbric
AR18 Arenicustollic
AR24 Argiaquicxeric
AR28 Argiclithic
AR32 Argicvertic
AR36 Aridiccalcic
AR50 Aridicpachic
BO02 Borolficlithic
BO06 Borollic
BO10 Borollic lithic
CA04
CA10
CH
CR
CR14
CU02
Calcic pachic
Calcixerollic
Chromic
Cryic
Cyric pachic
Cumulic udic
DU02 Duric
DU10 Durixerollic lithic
DU12 Durorthidic
81
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Appendix A
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Date: 9/85
Page 10 of 22
DU14 Durorthidic xeric
DY03 Dystric entic
DY06 Dystric tithic
EN Entic
EN06 Enticultic
EP10 Epiaquicorthoxic
EU02 Eutrochreptic
FE Ferrudalfic
FI02 Fibricterric
FL06 Fluventic
FR10 Fragiaquic
GL02 Glossaquic
GL10 Glossicudic
GL14 Glossoboralfic
GR Grossarenic
GR04 Grossarenicplinthic
HA Haplaquodic
HA02 Haplic
HA07 Haploxerollic
HA12 Hapludollic
HE Hemic
HI Histic
HI06 Histicpergelic
HU02 Humiciithic
HU06 Humoxic
HY Hydric
LE Leptic
LI01 Lithic
LI06 Lithicrupticaliic
LI08 Lithicrupticenticerollic
LI10 Lithicudic
LI12 Lithicultic
LI14 Lithicumbric
LI16 Lithicustic
LI20 Lithicvertic
LI24 Lithicxerollic
MO Mollic
OC Ochreptic
OR01 Orthic
OX Oxic
PA Pachic
PA04 Pachicultic
PA08 Paleustollic
PA20 Paralithicverlic
PE01 Pergelicruptichistic
DY02 Dystric
DY04 Dystric Fluventic
DY08 Dystropeptic
EN02 Enticlithic
EP Epiaquic
EU Eutric
EU04 Eutropeptic
FI Fibric
FL02 Fluvaquentic
FL12 Fluventic umbric
FR18 Fragic
GL04 Glossic
GL12 Glossicustollic
GL16 Glossoboric
GR01 Grossarenicentic
HA01 Haplaquic
HA05 Haplohumic
HA09 Hapiudic
HA16 Haplustollic
HE02 Hemicterric
HI02 Histiclithic
HU Humic
HU05 Humicpergelic
HU10 Humaqueptic
HY02 Hydriclithic
LI Limnic
LI04 Lithicmollic
LI07 Lithicruptic-argic
LI09 Lithicruptic-entic
LI11 Lithicrupticxerorthentic
L113 Lithicruptic-ultic
L115 Lithicrupticxerochreptic
L118 Lithicustollic
LI22 Lithicxeric
NA06 Natric
OR Orthidic
OR02 Orthoxic
PA02 Pachicudic
PA06 Paleorthidic
PA10 Palexerollic
PE Pergelic
PE02 Pergelicsideric
82
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Appendix A
Revision 1
Date: 9/85
Page 11 of 22
PE04 Petrocalcic
PE08 Petrocalcicustollic
PE16 Petroferric
PK Placic
PK12 Plaggic
PL04 Plinthic
PS Psammaquentic
QU Quartzipsammentic
RE Rendollic
RU02 Rupticalfic
RU11 Rupticlithic-entic
RU17 Rupticultic
SA Salorthidic
SA04 Sapricterric
SO04 Sombrihumic
SP02 Sphagnicterric
SU Suflic
TE Terric
TH06 Thaptohistictropic
T002 Torrifluventic
T006 Torripsammentic
TR Tropaquodic
TR04 Tropic
UD Udertic
UD02 Udic
UD05 Udorthentic
UL Ultic
UM02 Umbric
US02 Ustertic
US06 Ustochreptic
US12 Ustoxic
VE
Vermic
XE Xeralfic
XE04 Xeric
2.3 Slope Shape Codes
1 convex 2 plane 3 concave
2.4 Geomorphic Position Codes
01 summit crested hills
02 shoulder crested hills
22 shoulder headslope
03 backslope crested hills
PE06 Petrocalcicustalfic
PE14 Petrocalcicxerollic
PE20 Petrogypsic
PK10 Plaggeptic
PL Plinthaquic
PL06 Plinthudic
PS02 Psammentic
RH Rhodic
RU09 Rupticlithic
RU15 Rupticlithicxerochreptic
RU19 Rupticvertic
SA02 Sapric
SI Sideric
SP Sphagnic
SP04 Spodic
TH04 Thaptohistic
TO Torrertic
TO04 Torriorthentic
TO10 Torroxic
TR02 Tropeptic
AA Typic
UD01 Udalfic
UD03 Udollic
UD10 Udoxic
DM Umbreptic
US Ustalfic
US04 Ustic
US08 Ustollic
VE02 Vertic
XE02 Xerertic
XE08 Xerollic
4 undulating 5 complex
11 summit interfluve
12 shoulder interfluve
42 shoulder noseslope
23 backslope headslope
83
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Appendix A
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Date: 9/85
Page 12 Of 22
33 backslope sideslope
24 footslope headslope
44 footslope noseslope
25 toeslope headslope
2.5 Slope Aspect Codes
1 northeast
5 southwest
2 east
6 west
43 backslope noseslope
34 footslope sideslope
05 toeslope crested hills
35 toeslope sideslope
3 southeast 4 south
7 northwest 8 north
2.6 Pedon Position Codes
1 on the crest 2
4 on middle third 5
7 on a slope and depression 8
on slope and crest
on lower third
in a depression
2.7 Regional Landform Codes
A coastal plains
E lake plains
G glaciated uplands
I bolson
L level or undulating uplands
N high hills
R hills
2.8 Local Landform Codes
AA depression
A fan
C cuesta or hogback
E escarpment
G crater
I hillside or mountainside
K kamefield
M mesa or butte
P flood plain
R upland slope
T terrace-stream or lake
V pediment
X salt marsh
Z back barrier flat
2.9 Particle Size Codes
3 on upper third
6 on a slope
9 in a drainageway
B intermountain basin
F river valley
H glaciofluvial landform
M mountains or deeply disected plateaus
P piedmonts
U plateaus or tablelands
V mountain valleys or canyons
B bog
D dome or volcanic cone
F broad plain
H abandoned channel
J moraine
L drumlin
N low sand ridge-nondunal
Q playa or alluvial flat
S sand dune or hill
U terrace-outwash or marine
W swamp or marsh
Y barrier bar
002 not used
005 ashy
008 ashy over loamy
019 ashy over medial
007 ashy over cindery
013 ashy over loamy-skeletal
009 ashy-skeletal
84
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Appendix A
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Page 13 of 22
003 cindery
015 cindery over medial-skeletal
114 clayey
116 clayey over fragmental
120 clayey over loamy-skeletal
056 clayey-skeletal
080 coarse-loamy
084 coarse-loamy over sandy or sandy-skeletal
088 coarse-silty
092 coarse-silty over sandy or sandy-skeletal
126 fine
102 fine-loamy over clayey
100 fine-loamy over sandy or sandy-skeletal
112 fine-silty over clayey
110 fine-silty over sandy or sandy-skeletal
036 fragmental
068 loamy
050 loamy-skeletal
051 loamy-skeletal over fragmental
010 medial
014 medial over clayey
018 medial over loamy
022 medial over sandy or sandy-skeletal
062 sandy
066 sandy over clayey
044 sandy-skeletal
047 sandy-skeletal over clayey
026 thixotropic
034 thixotropic over loamy
030 thixotropic over sandy or sandy-skeletal
134 very fine
006 cindery over loamy
004 cindery over sandy or sandy-skeletal
122 clayey over fine-silty
124 clayey over loamy
118 clayey over sandy or sandy-skeletal
058 clayey-skeletal over sandy
082 coarse-loamy over fragmental
086 coarse-loamy overy clayey
090 coarse-silty over fragmental
094 coarse-silty over clayey
096 fine-loamy
098 fine-loamy over fragmental
106 fine-silty
108 fine-silty over fragmental
072 loamy over sandy or sandy-skeletal
054 loamy-skeletal over clayey .
052 loamy-skeletal over sand
012 medial over cindery
016 medial over fragmental
020 medial over loamy-skeletal
024 medial over thixotropic
063 sandy or sandy-skeletal
064 sandy over loamy
046 sandy-skeletal over loamy
028 thixotropic over fragmental
032 thixotropic over loamy-skeletal
027 thixotropic-skeletal
2.10 Mineralogy Codes
02 not used
09 chloritic
10 diatomaceous
18 gibbsitic
24 halloysitic
28 kaolinitic
34 mixed
38 montmorillonitic (calcareous)
04 calcareous
07 clastic
12 ferrihumic
20 glauconitic
26 illitic
30 marly
35 mixed (calcareous)
05 carbonatic
08 coprogenous
14 ferritic
22 gypsic
27 illitic (calcareous)
32 micaceous
37 montmorillonitic
85
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Appendix A
Revision 1
Date: 9/85
Page 14 of 22
40 oxidic
46 siliceous
2.11 Reaction Codes
02 not used
10 euic
42 sepiolitic
50 vermiculitic
04 acid
12 nonacid
2.12 Temperature Regime Codes
02 not used
08 isofrigid
14 isothermic
04 frigid
10 isohyperthermic
16 mesic
2.13 Other Family Codes
02 not used
06 level
14 shallow
16 sloping
04 coated
08 micro
15 shallow and coated
20 uncoated
44 serpentinitic
08 dysic
14 noncalcareous
06 hyperthermic
12 isomesic
18 thermic
05 cracked
12 ortstein
17 shallow and uncoated
2.14 Kind of Water Table Codes
1 flooded
4 ground
2.15 Landuse Codes
2 perched
3 apparent
C cropland
E forest land grazed
G pasture land and native pasture
L waste disposal land
P rangeland grazed
R wetlands
T tundra
2.16 Permeability Codes
1 very slow 2 slow
5 moderately rapid 6 rapid
2.17 Drainage Codes
1 very poorly drained
3 somewhat poorly drained
5 well drained
7 excessively drained
I cropland irrigated
F forest land not grazed
H horticultural land
N barren land
S rangeland not grazed
Q wetlands drained
U urban and built-up land
3 moderately slow
7 very rapid
4 moderate
2 poorly drained
4 moderately well drained
6 somewhat excessively drained
86
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Appendix A
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Date: 9/85
Page 15 of 22
2.18 Parent Material Weathering Codes
1 slight 2 moderate
3 high
2.19 Parent Material Mode of Deposition Codes
A alluvium
0 glacial drift
L lacustrine
M marine
R solid rock
H volcanic ash
E eolian
G glacial outwash
V local colluvium
0 organic
Y solifluctate
S
T
W
X
eolian-sand
glacial till
loess
residuum
U unconsolidated sediments
2.20 Parent Material Origin Codes
Mixed Lithology
YO mixed
Y2 mixed-calcareous
Y4 mixed-igneous-metamorphic and sedimentary
Y6 mixed-igneous and sedimentary
Conglomerate
CO conglomerate
C2 conglomerate-calcareous
Igneous
10 igneous
12 igneous-basic
14 igneous-granite
16 igneous-basalt
18 igneous-acid
Metamorphic
MO metamorphic
M2 metamorphic-acidic
M4 serpentine
M6 metamorphic-acidic
M8 slate
Y1 mixed-noncalcareous
Y3 mixed
Y5 mixed-igneous and metamorphic
Y7 mixed-metamorphic and sedimentary
C1 conglomerate-noncalcareous
11 igneous-coarse
13 igneous-intermediate
15 igneous-fine
17 igneous-andesite
19 igneous-ultrabasic
M1 gneiss
M3 metamorphic-basic
M5 schist and thyllite
M7 metamorphic-basic
M9 quartzite
Sedimentary
SO sedimentary
S2 glauconite
S1 marl
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Interbedded Sedimentary
BO interbedded sedimentary
82 limestone-sandstone
84 limestone-siltstone
B6 sandstone-siltstone
Sandstone
AO sandstone
A2 arkosic-sandstone
A4 sandstone-calcareous
Shale
HO shale
H2 shale-calcareous
Siltstone
TO siltstone
12 siltstone-calcareous
Limestone
LO limestone
l_2 marble
L4 limestone-phosphatic
L6 limestone-argillaceous
Pyroclastic
PO pyroclastic
P2 tuff-acidic
P4 volcanic breccia
P6 breccia-basic
P8 aa
Ejecta Material
EO ejecta-ash
E2 basic-ash
E4 andesitic-ash
E6 pumice
E8 volcanic bombs
Organic Materials
KO organic
K2 herbaceous material
b1 limestone-sandstone-shale
B3 limestone-shale
B5 sandstone-shale
B7 shale-siltstone
A1 sandstone-noncalcareous
A3 other sandstone
H1 shale-noncalcareous
T1 siltstone-noncalcareous
L1 chalk
L3 dolomite
L5 limestone-arenaceous
L7 limestone-cherty
P1 tuff
P3 tuff-basic
P5 breccia-acidic
P7 tuff-breccia
P9 pahoehoe
E1 acidic-ash
E3 basaltic-ash
E5 cinders
E7 scoria
K1 mossy material
K3 woody material
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Date: 9/85
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K4 wood fragments
K6 charcoal
K9 other organics
2.21 Moisture Regime Codes
AQ aquic moisture regime
PU perudic moisture regime
UD udic moisture regime
XE xeric moisture regime
2.22 Erosion Codes
0 none 1 slight
2.23 Runoff Codes
K5 logs and stumps
K7 coal
AR aridic moisture regime
TO torric moisture regime
US ustic moisture regime
0 none
4 moderate
1 ponded
5 rapid
2 moderate
2 very slow
6 very rapid
3 severe
3 slow
2.24 Diagnostic Feature Codes
A anthropic
O ochric
D durinodes
W paralithic contact
T argillic
G gypsic
E
Y
V
petrocalcic
salic
sulfuric
H histic
P plaggen
Z duripan
Q albic
C calcic
N natric
J petrogypsic
I sombric
F fragipan
M mollic
U umbric
L lithic contact
R argic
B cambic
X oxic
K placic
S spodic
2.25 Horizon Codes
Color Location Codes
0 unspecified 1 ped interior
Texture Classes
C clay
CL clay loam
COSL coarse sandy loam
CE coprogenous earth
FB fibric material
FSL fine sandy loam
G gravel
ICE ice or frozen soil
LCOS loamy coarse sand
LS loamy sand
2 ped exterior
3 rubbed or crushed
CIND cinders
COS coarse sand
CSCL coarse sandy clay loam
DE diatomaceous earth
FS fine sand
FM fragmental material
GYP gypsiferous earth
L loam
LFS loamy fine sand
LVFS loamy very fine sand
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MARL marl
MPT mucky peat
PDOM partially decomposed
PEAT peat
SG sand and gravel
SCL sandy clay loam
SP sapric material
SIL silt loam
SICL silty clay loam
U unknown texture
VAR variable
VFSL very fine sandy loam
Texture Modifiers
AY ashy
BYX extremely bouldery
CSV very cobbly
CNV very channery
CRC coarse cherty
CY cindery
FLX extremely flaggy
GRF fine gravelly
GY gritty
MK mucky
SH shaly
SR stratified
STX extremely stony
Grade of Structure
1 weak
4 very strong
MUCK
OPWD
organics
BY
CB
CBX
CNX
CRV
FL
GR
GRV
GYV
PT
SHV
ST
SY
S
SC
SL
SI
SIC
UDOM
UWB
VFS
WB
bouldery
cobbly
extremely cobbly
extremely channery
very cherty
flaggy
gravelly
very gravelly
very gritty
peaty
very shaly
stony
slaty
2 moderate
5 -weak and moderate
Appendix A
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Date: 9/85
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muck
oxide protected weathered
bedrock
sand
sandy clay
sandy loam
silt
silty clay
undecomposed organics
unweathered bedrock
very fine sand
weathered bedrock
BYV very bouldery
CBA angular cobbly
CN channery
CR cherty
CRX extremely cherty
FLV very flaggy
GRC coarse gravelly
GRX extremely gravelly
GYX extremely gritty
SHX extremely shaly
STV very stony
SYV very slaty
SYX extremely slaty
3 strong
6 moderate and strong
Size of Structure
EF extremely fine
F fine
MC medium and coarse
Structure Shape
ABK angular blocky
CDY cloddy
GR granular
PL platy
WEG wedge
Dry Consistence
L loose
VF very fine
FM fine and medium
CO coarse
BK blocky
COL columnar
LP lenticular
PR prismatic
soft
FF very fine and fine
M medium
CV coarse and very coarse
SBK subangular blocky
CR crumb
MA massive
SGR single grain
SH slightly hard
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H hard
SWH somewhat hard
Moist Consistence
L loose
FI firm
Other Consistence
WSM weakly smeary
B brittle
CO uncemented
SC strongly cemented
D deformable
VH very hard
VFR very friable
VFI very firm
SM
R
smeary
rigid
EH extremely hard
FR friable
EFI extremely firm
MS moderately smeary
VR very rigid
VWC very weakly cemented WC weakly cemented
SO semideformable
I
indurated
Stickiness
SO nonsticky
Plasticity
PO nonplastic
SS slightly sticky S sticky
SP slightly plastic P plastic
Cementation Agent
H humus I iron
X lime and silica
Mottle Abundance Codes
F few C common
Mottle Size Codes
1 fine 2 medium
Mottle Contrast Code
L lime
VS very sticky
VP very plastic
S silica
F faint
Surface Features
0 distinct
A skeletans over cutans
C chalcedony on opal
G gibbsite coats
K intersecting slickensides
M manganese or iron-manganese stains
P pressure faces
M many
3 coarse
P prominent
B black stains
D clay bridging
I iron stains
L lime or carbonate coats
O organic coats
Q nonintersecting slickensides
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S skeletans (sand or silt)
U coats
T clay films
X oxide coats
Surface Feature Amount Codes
V very few F few C common M many
Surface Feature Continuity Codes
P patchy 0 discontinuous C continuous
Surface Feature Distinctness Codes
F faint
0 distinct
Location of Surface Features
P on faces of peds
V on vertical faces of peds
U on upper surfaces of peds or stones
L on lower surfaces of peds or stones
M on bottoms of plates
B between sand grains
I in root channels and/or pores
T throughout
P prominent
H on horizontal faces of peds
Z on vertical and horizontal faces of
peds
C on tops of columns
S on sand and gravel
R on rock fragments
F on faces of peds and in pores
N on nodules
Boundary
A abrupt
S smooth
Effervescence
C clear
W wavy
G gradual
I irregular
D diffuse
B broken
0 very slightly effervescent
2 stongly effervescent
1 slightly effervescent
3 violently effervescent
Effervescence Agent Codes
H HCI (10%)
P H2O2 (unspecified)
I HCI (unspecified)
Q H2O2 (3 to 4%)
Field Measured Property Kind Codes
For organic materials
Column 1
F fiber
H hemic
Column 2
B unrubbed
W woody
R rubbed
H herbacious
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L limnic
S sapric
S sphagnum
D diatomaceous earth
F ferrihumic
0 other
C coprogenous earth
M marly
U humilluvic
L sulfidic
For mineral materials
ON
PH
PB
PL
PP
PY
sand
Bromthymol blue
Lamotte-Morgan
Phenol red
Ydrion
OI silt
pC Ore sol red
pM pH meter (1:1 H2O)
pS soiltex
OA clay
pH Hellige-Truog
pN pH (0.1 M CaCl2)
pT Thymol blue
50/7 Moisture Codes
D dry M moist V very moist
Quantity (Roots, Pores, Concretions)
VF very few
CM common to many
FF very few to few
C common
F few
M many
W wet
FC few to common
Size (Roots, Pores, Concretions)
M micro
11 very fine and fine
2 medium
4 very coarse
Location of Roots
C in cracks
P between peds
T throughout
Shape of Pores
IR interstitial
IT interstitial and tubular
TU tubular
TO discontinuous tubular
TS constricted tubular
VT vesicular and tubular
M1 micro and fine
1 fine
23 medium and coarse
5 extremely coarse
V1 very fine
12 fine and medium
3 coarse
13 fine to coarse
M in mat at top of horizon
S matted around stones
IE filled with coarse material
IF void between rock fragment
TC continuous tubular
TE dendritic tubular
VS vesicular
TP total porosity
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Kind of Concentrations
A2 clay bodies
B2 soft masses of barite
02 soft masses of lime
C4 lime nodules
02 soft dark masses
04 dark nodules
E4 gibbsite nodules
F2 soft masses of iron
F4 ironstone nodules
G2 masses of gypsum
H2 salt masses
K3 carbonate concretions
M1 nonmagnetic shot
M3 iron-manganese concretions
31 opal crystals
S3 silica concretions
T2 worm casts
T4 worm nodules
Shape of Concentrations
C cylindrical
P plate like
0 dendritic
T threads
Rock Fragment Kind Codes
B1 barite crystals
C1 calcite crystals
C3 lime concretions
01 mica flakes
03 dark concretions
E3 gibbsite concretions
F1 plinthite segregations
F3 iron concretions
G1 gypsum crystals
H1 halite crystals
K2 soft masses of carbonate
K4 carbonate nodules
M2 soft masses of iron-manganese
M4 magnetic shot
32 soft masses of silica
S4 durinodes
T3 insects casts
O rounded
Z irregular
A sandstone B
F ironstone H
K organic fragments I
O oxide-protected rock P
S sedimentary rocks T
mixed sedimentary rocks
shale
limestone
pyroclastic rocks
siltstone
E ejecta
I igneous rocks
M metamorphic rocks
R saprolite
Y mixed lithogoy
Rock Fragment Size Codes
1 pebbles
2 cobbles
3 stones
4 boulders
5 channers
6 flagstones
C 20- to 75-mm fragments
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Appendix B
Laboratory 3 Ammonium Test
This appendix is an excerpt of a letter from the preparation laboratory manager of Laboratory
3. A test was made on soil samples to determine whether or not an ammonia leak in the cold
storage facility contaminated any of the samples from the Northeastern soil survey.
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Appendix B
Revision 2
Date: 9/85
Page 2 of 2
December 18, 1985
QA Manager
Lockheed-EMSCO
1050 E. Flamingo Road
Suite 120
Las Vegas, Nevada 89109
This letter is to confirm for your records the results of the ammonium test performed on soil
samples, as discussed in our telephone conversation.
At our initial observation visit I pointed out a leak of ammonia gas coming from a room
adjacent to the cooler in which we would be storing NADSS samples. In order to determine the
extent of possible contamination of the NADSS samples by ammonia, the following procedure was
followed.
On September 11, 1985, 3 sets of the same soil samples were placed in the storage cooler.
Each set was repeated in triplicate and represented the following:
1. one set of uncovered soils
2. one set of soils enclosed in plastic liners only
3. one set of soils enclosed in plastic liners and canvas bags
Subsamples of these soils had been previously tested for ammonium content by the Nessler
Reagent Colorimetric test (2M KCI extraction), the standard ammonium test used by the laboratory
(Greweling and Peech, 1960, Chemical soil tests, Cornell Exp. Sta. Bull. 960). These-preliminary
results showed that control samples were below the ammonium detection limit at the beginning
of the experiment.
On October 9, 1985, each set of soils placed in the cooler was removed and analyzed for
ammonium by Nessler Reagent test. Results showed the following:
1. uncovered soils had 10 ppm ammonium
2. soils in plastic liners only were below the ammonium detection limit
3. soils in plastic liners and canvas bags were below the ammonium detection limit
According to these results, it appears that no change occurred in the soils covered with
plastic, and canvas and plastic from the original amount of ammonium. When left uncovered in
the cooler, 10 ppm ammonium was adsorbed by the soil, assumably due to the ammonia leak in
the adjacent room.
Soil samples prepared by the department of the NADSS project were placed in 2 plastic liners,
1 canvas bag, an additional plastic liner, and a cardboard box before being placed in the cooler for
storage. Thus it can be stated that ammonium contamination of these soils would be nil or
negligible.
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