EPA/600/8-87/021
April 1987
Direct/Delayed
Quality Ass
Soil Sampling, Pre
Response Project:
jrance Plan for
paration, and Analysis
J.K. Bartz, S.K. Drouse, K.
L.J. Blume, M.A. Stapania
by
A. Cappo, M.L. Papp, G.A. Raab,
n, F.C. Garner, and D.S. Coffey
National Add Puclp
U.J
Be^
23C
A Contribution to tho
tatlon Assessment Program
!. Environmental Pro-bsotioa Agency
ion 5, Library (5PL-16)
S. Dearborn Stvest, Room 1670
Onojcago, IL 60604
U.S. Environmental Protection Agency
Office of Modeling, Monitoring Systems, and Quality Assurance
Office of Ecological Procesaea and Effecta Research
Office of Research and Development
Waahlngton. D.C. 20460
Environmental Monitoring Systems Laboratory, Las Vegas, Nevada 89103
Environmental Research Laboratory, Corvallls, Oregon 97333
-------
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 Management
Services Company, Inc. and contract number 68-03-3246 to Northrop Services, Inc. It has been
subject to the Agency's peer and administrative review, and it has been approved for publication
as an Agency document.
Mention of trade names or commercial products is for illustration purposes and 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
report, quality assurance plan, analytical methods manual, 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:
Bartz, J.K., S.K Drous6, K.A. Cappo, M.L Papp, G.A. Raab, LJ. Blume, M.A. Stapanian, F.C. Garner,
and D.S. Coffey. 1987. Direct/Delayed Response Project: Quality Assurance Plan for Soil Sampling,
Preparation, and Analysis. EPA/600/8-87/021. U.S. Environmental Protection Agency, Environmental
Monitoring Systems Laboratory, Las Vegas, Nevada. 315 pp.
-------
Abstract
The Direct/Delayed Response Project (DDRP) focuses on regions of the United States that have
been identified as potentially sensitive to surface water acidification. The Northeastern Soil Survey
includes the New England states of Maine, New Hampshire, Vermont, Massachusetts, Connecticut,
and Rhode Island, and portions of New York and Pennsylvania. The Southeastern Soil Survey,
conducted in the physiographic region known as the Southern Blue Ridge Province, includes the
bordering portions of Tennessee, North Carolina, South Carolina, and Georgia.
The specific goals of the DDRP soil surveys are (1) to define soil-physical and soil-chemical
characteristics and other watershed characteristics across these regions, (2) to assess the
variability of these characteristics, and (3) to determine which of these characteristics are related
most strongly to surface-water chemistry.
The purpose of the quality assurance (QA) project plan is to specify the policies, organization,
objectives, and QA and quality control (QC) activities needed to achieve the data quality goals of
the DDRP. The QA plan is designed to meet the following objectives:
• standardizing sampling, processing, and analytical methods and procedures
• simplifying field operations
• training all personnel
• using QA/QC samples and procedures to verify data
• using field and laboratory audits to ensure that all activities are properly performed and that
problems are identified and resolved
• evaluating the reported data and verifying data quality.
This report was submitted in partial fulfillment of Contract Number 68-03-3249 by Lockheed
Engineering and Management Services Company, Inc., under the sponsorship of the U.S.
Environmental Protection Agency.
in
-------
Table of Contents
Revision 2
Date: 2/87
Page 1 of 5
Direct/Delayed Response Project:
Quality Assurance Plan for
Soil Sampling, Preparation, and Analysis
Section page Revision
1 Introduction 1 of 2 2
2 Project Description 1 of 1 2
3 Project Organization 1 of 3 2
4 Quality Assurance Objectives 1 of 7 2
4.1 Soil Sampling 1 of 7 2
4.1.1 Precision and Accuracy 1 of 7 2
4.1.2 Representativeness 2 of 7 2
4.1.3 Completeness 2 of 7 2
4.1.4 Comparability 2 of 7 2
4.2 Sample Preparation 2 of 7 2
4.2.1 Precision and Accuracy 2 of 7 2
4.2,2 Representativeness 2 of 7 2
4.2.3 Completeness 2 of 7 2
4.2.4 Comparability 2 of 7 2
4.3 Laboratory Analysis 3 of 7 2
4.3.1 Precision and Accuracy 3 of 7 2
4.3.2 Representativeness 3 of 7 2
4.3.3 Completeness 3 of 7 2
4.3.4 Comparability 7 of 7 2
5 Sampling Strategy 1 of 7 2
5.1 Northeastern Soil Survey 1 of 7 2
5.1.1 Watershed Selection 1 of 7 2
5.1.2 Watershed Mapping 1 of 7 2
5.1.3 Sampling Classes 2 of 7 2
5.1.4 Watershed and Sampling Class Selection 2 of 7 2
5.2 Southeastern Soil Survey 5 of 7 2
5.3 Final Sampling Locations 5 of 7 2
5.3.1 Sampling Site Selection 5 of 7 2
5.3.2 Sampling Site Locations 6 of 7 2
5.4 Special Conditions 7 of 7 2
5.4.1 Inaccessible Watersheds 7 of 7 2
5.4.2 Inclusions 7 of 7 2
5.4.3 Agricultural Sites 7 of 7 2
5.4.4 Unsuitable Sampling Sites 7 of 7 2
5.5 Paired Pedons 7 of 7 2
-------
Table of Contents
Revision 2
Date: 2/87
Page 2 of 5
Contents (continued)
Sect/on Page Revision
6 Operations 1 of 1 2
6.1 Profile Description 1 of 1 2
6.2 Sampling 1 of 1 2
6.3 Sample Custody 1 of 1 2
7 Soil Sampling Internal Quality Control 1 of 1 2
8 Preparation Laboratory Internal
Quality Control 1 of 1 2
8.1 Sample Receipt 1 of 1 2
8.2 Sample Processing 1 of 1 2
8.3 Inorganic Carbon 1 of 1 2
8.4 Bulk Density 1 of 1 2
8.5 Raw Data 1 of 1 2
9 Analytical Laboratory Procedures and
Internal Quality Control 1 of 23 2
9.1 Sample Receipt 1 of 23 2
9.2 Sample Analysis 1 of 23 2
9.3 Analytical Laboratory Documentation for
Quality Control 1 of 23 2
9.4 Internal Quality Control Within
Each Method 4 of 23 2
9.4.1 Initial Calibration 4 of 23 2
9.4.2 Calibration Blank 19 of 23 2
9.4.3 Quality Control Calibration
Samples (QCCS) 19 of 23 2
9.4.4 Detection Limit Quality Control Samples 19 of 23 2
9.4.5 Reagent Blank 20 of 23 2
9.4.6 Preliminary Sample Analysis 20 of 23 2
9.4.7 Matrix Spike Analysis 20 of 23 2
9.4.8 Duplicate Sample Analysis 20 of 23 2
9.4.9 Ion Chromatography Resolution Test 21 of 23 2
9.4.10 Continuing Sample Analysis 21 of 23 2
9.5 Instrumental Detection Limits 21 of 23 2
9.6 Reagent Blank Correction for Spectrometric and Ion
Chromatographic Procedures 21 of 23 2
9.7 Data Reporting 22 of 23 2
9.8 Evaluation of Quality Control Data 22 of 23 2
10 Performance and System Audits 1 of 2 2
10.1 Soil Samples to Estimate Precision 1 of 2 2
10.2 Field Sampling On-Site Evaluation 1 of 2 2
10.3 Preparation Laboratory On-Site Evaluation 1 of 2 2
10.4 Analytical Laboratory On-Site Evaluation 2 of 2 2
-------
Table of Contents
Revision 2
Date: 2/87
Page 3 of 5
Contents (continued)
Section Page Revision
11 Acceptance Criteria 1 of 2 2
11.1 Audit Sample Results 1 of 2 2
11.2 Replicate Analysis Results 2 of 2 2
11.3 Corrective Action 2 of 2 2
12 Data Management System 1 of 3 2
12.1 Raw Data Base 1 of 3 2
12.2 Verified Data Base 1 of 3 2
12.3 Validated Data Base 1 of 3 2
13 Review of Data 1 of 2 2
13.1 Field Data Review 1 of 2 2
13.2 Preparation Laboratory Batch Assignment and
Data Review 1 of 2 2
13.3 Analytical Laboratory Data Review 1 of 2 2
14 Data Verification 1 of 9 2
14.1 Verification of Field Data 1 of 9 2
14.1.1 Verification of Sampling Class and
Vegetation Class 1 of 9 2
14.1.2 Review of the Field Data Forms for
Completeness and Misnomers 1 of 9 2
14.1.3 Verification of Soil
Descriptive Parameters 1 of 9 2
14.1.4 Methods Used to Treat Outliers 4 of 9 2
14.2 Verification of Physical and Chemical Data 5 of 9 2
14.2.1 Exceptions Programs for Internal
Consistency of Data 5 of 9 2
14.2.2 Other Exceptions Programs 6 of 9 2
14.2.3 Methods Used to Treat Outliers 7 of 9 2
14.3 Reporting Scheme 7 of 9 2
15 Quality Assurance Plan for Mineralogy 1 of 10 2
15.1 Introduction 1 of 10 2
15.2 Project Description '.'. 1 of 10 2
15.3 Project Organization 1 of 10 2
15.4 Quality Assurance Objectives 1 of 10 2
15.4.1 Soil Sampling 1 of 10 2
15.4.2 Sample Preparation 1 of 10 2
15.4.3 Laboratory Analysis 2 of 10 2
15.5 Strategy of Sample Selection for
Mineralogical Analysis 3 of 10 2
-------
Table of Contents
Revision 2
Date: 2/87
Page 4 of 5
Contents (continued)
Section Page Revision
15.5.1 Constraints 3 of 10 2
15.5.2 Limitations to Selection Criteria 4 of 10 2
15.5.3 Selection Procedure 4 of 10 2
15.6 Sampling Internal Quality Control 4 of 10 2
15.7 Preparation Laboratory Internal Quality Control 4 of 10 2
15.8 Laboratory Procedures 5 of 10 2
15.9 Mineralogical Laboratory Internal Quality Central 5 of 10 2
15.9.1 Sample Receipt 5 of 10 2
15.9.2 X-ray Diffraction Spectrometry 5 of 10 2
15.9.3 Wavelength-dispersive X-ray Spectrometry 6 of 10 2
15.9.4 Scanning Electron Microscopy/
Energy-Dispersive X-Ray
Spectrometry (SEM/EDXRF) 8 of 10 2
15.10 Acceptance Criteria 9 of 10 2
15.11 Data Management System 9 of 10 2
15.12 Performance and System Audits 9 of 10 2
15.12.1 QA/QC Samples 9 of 10 2
15.12.2 Laboratory On-Site Evaluations 9 of 10 2
15.13 Review of Mineralogical Data 9 of 10 2
15.13.1 Communications 9 of 10 2
15.13.2 Preliminary Data Package Review 9 of 10 2
15.13.3 Quality Assurance Reports to Management 10 of 10 2
15.14 Data Verification 10 of 10 2
16 References 1 of 2 2
Appendices
Appendix A Forms and Legends for Reporting
Field Data 1 of 40 2
Appendix B Forms for Reporting Analytical
Laboratory Data 1 of 64 2
Appendix C Plan for Laboratory Audit Samples 1 of 2 2
Appendix D Field Sampling On-Site Evaluation
Questionnaires 1 of 31 2
Appendix E Preparation Laboratory On-Site
Evaluation Questionnaires 1 of 17 2
Appendix F Facsimile of instructions for Pre-award
Performance Evaluation Samples 1 of 2 2
Appendix Q Pre-award Performance Evaluation
Scoring Sheet 1 of 5 2
-------
Table of Contents
Revision 2
Date: 2/87
Page 5 of 5
Contents (continued)
Appendix H Analytical Laboratory On-Site
Evaluation Questionnaire 1 of 80 2
Appendix I Facsimile of the Data Package
Completeness Checklist 1 of 3 2
Appendix J Forms for Reporting Mineralogical
Laboratory Data 1 of 8 2
Appendix K Mineralogical Laboratory On-Slte
Evaluation Queetionnaire 1 of 29 2
Appendix L Mineralogical Data Package Completeness
Checklist 1 of 2 2
Appendix M Example Verification Report 1 of 28 2
-------
Section Figures
Revision 2
Date: 2/87
Page 1 of 1
Figures
Figure Page Revision
3-1 Operational management structure for the soil surveys
of the Direct/Delayed Response Project, a project of
the Aquatic Effects Research Program 2 of 3 2
12-1 Data management for the DDRP Soil Survey 2 of 3 2
-------
Section Tables
Revision 2
Date 2/87
Page 1 of 1
Tables
Table Page Revision
1-1 Section in this QA Project Plan and in the OORP
Soil Sampling and Analytical Methods Manual
where QA subjects are treated 1 of 2 2
4-1 Data Quality Objectives 4 of 7 2
5-1 Comparison of Coniferous, Deciduous, and Mixed Vegetation
Types to Society of American Foresters Forest
Cover Types 3 of 7 2
9-1 List of Parameters and Corresponding Analytical Techniques 2 of 23 2
9-2 Required Detection Limits, Expected Ranges, and
Intralaboratory Relative Precision Goal 3 of 23 2
9-3 Maximum Control Limits for QC Samples 5 of 23 2
9-4 Laboratory/Field Data Qualifiers 5 of 23 2
9-5 Summary of Internal Quality Control 6 of 23 2
9-6 List of Decimal-Place Reporting Requirements 23 of 23 2
14-1 Flags for the Verification of Field data 5 of 9 2
14-2 Flags for the Verification of Analytical Data 7 of 9 2
15-1 Mineralogical Data Quality Objectives 2 of 10 2
15-2 Mineralogical Parameters and Corresponding
Analytical Techniques 5 of 10 2
-------
Ackno wledgments
Critical reviews by the following individuals were instrumental in the documentation of this
project plan and are gratefully acknowledged: E. Knox, M. Meyer, R. W. Arnold, F. T. Miller, E. H.
Sautter, K. J. LaFlamme, K. A. Wheeler, 0. G. Van Houten, G. H. Lipscomb, T. Gerald, and H. Smith,
U.S. Department of Agriculture, Soil Conservation Service; I. Fernandez, University of Maine-Orono;
E. Levine, National Aeronautics and Space Administration, Goddard Space Flight Center; D. Coffey,
Tetra Tech, Inc., Bellevue, Washington; J. J. Lee and L H. Liegel, U.S. Environmental Protection
Agency; and 0. Lammers, U.S. Forest Service.
The support of S. J. Simon, R. E. Cameron, and S. L Pierett, Lockheed Engineering and
Management Services Company, Inc., is gratefully acknowledged.
The following people were instrumental in the completion of this project plan: K. Thornton,
FTN and Associates, Little Rock, Arkansas; J. L Engels, M. L Faber, and J. M. Nicholson of
Lockheed Engineering and Management Services Company, Inc.; Computer Sciences Corporation
word processing staff at the U.S. Environmental Protection Agency Environmental Monitoring
Systems Laboratory, Las Vegas, Nevada; and Donald Clark Associates graphic arts staff at the U.S.
Environmental Protection Agency Environmental Monitoring Systems Laboratory, Las Vegas, Nevada.
Finally, recognition belongs to E. P. Meier and P. A. Arberg who have served as technical
monitors of this project.
-------
Section 1
Revision 2
Date: 2/87
Page 1 of 2
Section 1
Introduction
The quality assurance policy of the U.S.
Environmental Protection Agency (EPA) re-
quires every monitoring and measurement
project to have a written and approved quality
assurance (QA) project plan (Costle, 1979a and
1979b). This requirement applies to all environ-
mental monitoring and measurement efforts
authorized or supported by EPA through regu-
lations, grants, contracts, or other formal
means. The purpose of this QA project plan is
to specify the policies, organization, objectives,
and quality control (QC) activities needed to
achieve the data quality goals of the Direct/-
Delayed Response Project. All project person-
nel are expected to be familiar with the poli-
cies and objectives outlined in this QA
project plan to assure proper interactions
between field and laboratory operations and
data management.
EPA guidance (U.S. EPA, 1980) states
that the QA project plan must address, in
detail or by reference, all 14 items listed in
Table 1.1. Method-specific discussions pres-
ented in the Soil Sampling Manual for the
Direct/Delayed Response Project Soil Survey
(Blume et al., 1987), Preparation Laboratory
Manual for the Direct/Delayed Response Proj-
ect So/7 Survey (Bartz et al., 1987), or the
Analytical Methods Manual for the
Direct/Delayed Response Project Soil Survey
(Cappo et al., 1987) might not be repeated in
this project plan. In these cases, Table 1-1
serves as an index to the appropriate
references.
Table 1-1. Section* In thl* QA Pro|*ct Plan and In th* DORP Soil Sampling and Analytical Method* manual* where
QA *ub|ect* are treated
Section Number
1.
2.
3.
4.
5.
6.
7.
8.
9.
Subject
Project Description
Project Organization
and Responsibility
QA Objectives for
Measurement Data
Sampling Procedures
Sample Custody
Calibration Procedures
Analytical Procedures
Data Reduction, Validation.
and Reporting
Internal QC Checks
QA Project
Plan
2
3
4
6,7
6.7.8
9
9
6, 9, 11
7,8,9
Soil
Sampling
Manual
1
1,2,
7
—
6
6,7
—
11
5,6,
11
11
Analytical
Methods
Manual
1
2
2
2.
3
2,
2
3- 19
- 19
3-19
(continued)
-------
Table 1-1. Continued
Section 1
Revision 2
Date: 2/87
Page 2 of 2
11. Preventive Maintenance
Section Number
10.
Subject
Performance and System Audits
QA Project
Plan
12
Soil
Sampling
Manual
2
Analytical
Methods
Manual
—
3- 19
12. Procedures for Routine Assessment of
Data Precision, Representativeness,
Comparability, Accuracy, and Completeness
4, 10
13. Corrective Actions
9, 10
14. QA Reports to Management
9,12
-------
Section 2
Project Description
Section 2
Revision 2
Date: 2/87
Page 1 of 1
The Direct/Delayed Response Project
(DDRP) focuses on regions of the United
States that have been identified as potentially
sensitive to surface water acidification. The
Northeastern Soil Survey includes the New
England states of Maine, New Hampshire,
Vermont, Massachusetts, Connecticut, and
Rhode Island, and portions of New York and
Pennyslvania. The Southeastern Soil Survey,
conducted in the physiographic region known
as the Southern Blue Ridge Province, includes
the bordering portions of Tennessee, North
Carolina, South Carolina, and Georgia. Surface
waters in these two regions were studied
during the Eastern Lake Survey (1984) and the
National Stream Survey Phase I - Pilot Study
(1985), respectively.
The specific goals of the DDRP soil
surveys are (1) to define soil-physical and soil-
chemical characteristics and other watershed
characteristics across these regions, (2) to
assess the variability of these characteristics,
and (3) to determine which of these character-
istics are related most strongly to surface-
water chemistry.
-------
Section 3
Revision 2
Date: 2/87
Page 1 of 3
Section 3
Project Organization
Figure 3-1 illustrates the operational
management structure. The director of the
Office of Acid Deposition, Environmental Moni-
toring, and Quality Assurance (OADEMQA) is
the EPA official who has overall responsibility
for programs within EPA which address the
effects of acidic deposition. The responsibili-
ties of the program director and technical
director are as follows:
Program Director
The director of the Aquatic Effects Re-
search Program (program director) is the EPA
Headquarters representative for DDRP and is
the liaison between the headquarters staff, the
laboratory directors, and the National Acid
Precipitation Assessment Program (NAPAP).
Questions regarding general management and
resources should be forwarded to the program
director through the technical director.
Technical Director
The technical director performs responsi-
bilities at the discretion of the program direc-
tor. The technical director's primary role is to
maintain the integrity of program objectives, to
integrate components of the program, and to
see that deadlines are met. The technical
director coordinates and integrates the activi-
ties of the Environmental Research Laboratory
at Corvallis, Oregon (ERL-C), the Environmental
Monitoring Systems Laboratory at Las Vegas,
Nevada (EMSL-LV), and Oak Ridge National
Laboratory (ORNL) at Oak Ridge, Tennessee.
The technical director also coordinates peer
review, resolves issues of responsibility, and
disseminates information to the public. The
technical director represents the program
director as necessary and informs the program
director of EPA laboratory activities, progress,
and performance.
The roles of the laboratories are as
follows:
ERL-C: ERL-C is a focal point for the
soil surveys. Responsibilities of ERL-C staff
for all phases of the program include:
• Developing experimental design for
soil sampling.
• Developing protocol for selection of
sampling sites.
• Preparing sampling protocols (jointly
with EMSL-LV).
• Collecting supplemental historical and
other available data on each sampling
site.
• Analyzing data (jointly with EMSL-LV).
• Interpreting data.
• Preparing reports (final and progress
reports with contributions from the
other laboratories relative to their
responsibilities).
• Assessing and resolving all science-
related issues other than quality
assurance/quality control (QA/QC)
data management (jointly with other
laboratories as necessary).
• Coordinating survey activities with
NAPAP management staff.
EMSL-LV: The Las Vegas laboratory has
expertise in matters relating to QA/QC, logis-
tics, analytical services, and sampling proto-
cols. The responsibilities of personnel at
EMSL-LV include:
• Developing QA/QC procedures for all
components of the survey except data
management (a joint responsibility of
ORNL and ERL-C).
-------
Section 3
Revision 2
Date: 2/87
Page 2 of 3
OFFICE OF ENVIRONMENTAL
PROCESSES AND EFFECTS RESEARCH
DIRECTOR OF ACID DEPOSITION
AND ATMOSPHERIC RESEARCH
DIVISION
DIRECTOR OF AQUATIC EFFECTS
RESEARCH PROGRAM
PEER REVIEW
DIRECTORS OF
ERL-C AND EMSL-LV
ERL-CORVALLIS
SAMPLING DESIGN
SITE SELECTION
DATA VALIDATION
DATA INTERPRETATION
REPORTING
EMSL-LAS VEGAS
OPERATIONS AND
LOGISTICS
ANALYTICAL METHODS
DATA VERIFICATION
ERL-CORVALLIS AND
OAK RIDGE NATIONAL
LABORATORY
DATA ENTRY
DATA MANAGEMENT
QA/QC
Figure 3-t. Operational management atructure for the aoll aurvaya of the Direct/Delayed Reaponae Project, a
project of the Aquatic Effecta Reaaarch Program.
-------
Section 3
Revision 2
Date: 2/87
Page 3 of 3
• Preparing all sampling protocols
(jointly with ERL-C).
• Preparing a soil sampling and prepa-
ration manual.
• Preparing an analytical methods
manual.
• Coordinating logistical support and
equipment needs for all field opera-
tions.
• Training field personnel in DDRP soil
survey protocols.
• Distributing all samples to analytical
laboratories.
• Developing and implementing QA/QC
procedures for verification of field
data and analytical laboratory data.
• Preparing and implementing the QA
project plan.
• Independently assessing field mea-
surements and laboratory data quality,
i.e., bias and variability.
• Assessing and resolving problems
pertaining to QA/QC, logistics, and
analytical services.
ORNL: ORNL has expertise in managing,
manipulating, and restructuring large data
bases to satisfy data analysis needs. ERL-C
oversees the activities of ORNL, which has
responsibilities for:
• Developing and maintaining a data
management system.
• Entering all field, laboratory, and
support data into the data base and
simultaneously assuring entry quality.
• Preparing computer-generated summa-
ry tables, statistics, and graphics for
reports.
-------
Section 4
Revision 2
Date: 2/87
Page 1 of 7
Section 4
Quality Assurance Objectives
Quality assurance (QA) objectives are
required for three phases of data collection:
(1) soil description and sample collection, (2)
sample preparation, and (3) laboratory analy-
sis. The approach selected for data collection
provides a balance between constraints of
time and cost and the quality of data neces-
sary to complete the research objectives of the
project. The QA plan is designed to meet the
following objectives:
• Standardizing sampling, processing,
and analytical methods and proce-
dures.
• Simplifying field operations.
• Training all personnel.
• Using QA/QC samples and procedures
to verify data.
• Using field and laboratory audits to
ensure that all activities are properly
performed and that problems are
identified and resolved.
• Evaluating the reported data and
verifying data quality.
Each phase of data collection is ad-
dressed in the following sections.
4.1 Soil Sampling
4.1.1 Precision and Accuracy
A representative of the Soil Conservation
Service (SCS) state soils staff independently
describes a minimum of one site per field
crew. These independent pedon descriptions
are used to assess the variability in site de-
scriptions among soil scientists. The SCS
representative monitors adherence to protocol
for site selection, labeling, and sampling. The
soil profile is described on the same face of
the pit as described by the field crew. The
representative makes the assessment while
the crew is describing and sampling the
pedons. Written reviews are submitted to the
sampling task leader at ERL-C within two
weeks. Major problems are reported verbally
within two working days.
The Regional Coordinator/Correlator
(RCC) must be a qualified soil scientist with
several years experience in soil profile descrip-
tion and soil mapping. The RCC monitors one
site per field crew for adherence to SCS stan-
dards, procedures, and sampling protocol
modifications as presented in this document,
and performs an independent duplicate profile
description. At least one site in each state is
monitored with the SCS state soils staff
representative while the remaining sites may
be monitored independently. The RCC also
ensures that state soils staff performs dupli-
cate profile descriptions. During this process,
the RCC identifies, discusses, and resolves
any significant problems. Written reports are
submitted to the sampling task leader at ERL-
C within two weeks. The resolution of major
problems is reported verbally within two work-
ing days.
The quality assurance/quality control
(QA/QC) representative audits each field sam-
pling crew at least once to ensure adherence
to sampling protocol. Written reports are
submitted to the QA manager at EMSL-LV
within two weeks. Major problems are re-
ported verbally within two working days. The
QA manager is responsible for conveying any
major problems to the technical monitor or
technical director.
A small percent of the sampling units is
selected randomly by EPA for sampling to de-
termine the within-delineation variability. These
replicate pedons, called paired pedons, are
selected before sampling begins. The paired
pedon and the routine pedon from a represen-
tative site for each selected unit are sampled
on the same day by the same field crew.
-------
Section 4
Revision 2
Date: 2/87
Page 2 of 7
Sample pits are located accurately on the
soil survey maps, and the pit dimensions and
the long azimuth are recorded. The pit face
from which samples are removed is recorded,
and the location of the pit in the field is
flagged or identified so that the site can be
revisited. The soil profile is described accord-
ing to SCS protocols.
r
One horizon per day is sampled in dupli-
cate by each field crew (see Section 7.0). One
field duplicate is included in each set of sam-
ples sent to a preparation laboratory.
4.1.2 Representativeness
The primary concerns in the selection of
sampling sites are (1) to assess soil charac-
teristics, (2) to integrate information on parent
material, internal drainage, soil depth, slope,
and vegetative cover, and (3) to determine
representative sampling classes. Soils which
have been identified in the study regions have
been combined into groups, or sampling
classes, which are either known to have or are
expected to have similar chemical and physical
characteristics. Each of the sampling classes
can be sampled across a number of water-
sheds in which they occur. In this approach,
a given soil sample does not represent the
specific watershed from which it came. In-
stead it contributes to a set of samples which
collectively represent a specific sampling class
on all DORP watersheds within the sampling
region. The lead soil scientist of the sampling
party selects a sampling site representing the
designated sampling class and vegetation
class within the designated watershed accord-
ing to the protocols documented in Blume et
al. (1987).
4.1.3 Completeness
Soil sampling protocols require the
sampling of 100 percent of the designated
pedons and of the prerequisite number of
horizons. If samples are lost, spilled, or
mislabeled, it is possible to return to the field
and resample the same site. If a sampling
site is inaccessible, the reason for excluding
the site must be formally documented by the
field crew (refer to Section 5.4.1).
4.1.4 Comparability
The use of standard SCS methods,
protocols, and forms for the sampling phase
provide field and analytical data that are
comparable to data generated from SCS
investigations and other studies which have
utilized these standardized methods.
4.2 Sample Preparation
4.2.1 Precision and Accuracy
The preparation laboratory combines
sets of field samples into one batch containing
a maximum of 39 routine and duplicate sam-
ples. After processing, i.e., air-drying, crushing,
sieving, and homogenization, one bulk sample
is split into two subsamples which are termed
preparation duplicates. Comparison of physi-
cal and chemical data for these duplicates
allows evaluation of the subsampling proce-
dure.
4.2.2 Representativeness
Each bulk soil sample is processed by a
preparation laboratory tc obtain a homoge-
neous 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.
4.2.3 Completeness
Each batch of samples sent to a con-
tractor analytical laboratory includes the prepa-
ration duplicates.
4.2.4 Comparability
All preparation laboratories process bulk
samples according to protocols documented in
Bartz et al. (1987). Strict adherence to proto-
cols should result in comparability among
preparation laboratories.
-------
Section 4
Revision 2
Date: 2/87
Page 3 of 7
4.3 Laboratory Analysis
4.3.1 Precision and Accuracy
The data quality objectives (OQOs) for
precision and accuracy of the physical and
chemical analyses of routine soil samples are
presented in Table 4-1 (U.S. EPA, 1985). The
structure of Table 4-1 is as follows:
Reporting Units - specifies the units in
which the laboratory data should
be reported.
Reporting Format - specifies the
significant figures to which the data
should be reported.
Expected Range - specifies the range
of values expected to occur naturally
in the soil sampled, independent of
measurement error.
Lower Reporting Limit - this value has
been extrapolated to that of the
reporting unit; if the sample values are
lower than stated, the "limit of repro-
ducibility" is approached.
Precision at the Lower Limit - serves
as a guideline to define the acceptable
absolute percent standard deviation
beyond which the analytical re-
producibility for low concentration
samples is questionable and often not
attainable.
Precision at the Upper Limit - serves
as a guideline to define the acceptable
percent relative standard deviation
beyond which the analytical reproduc-
ibility for high concentration samples
is questionable.
The values given for precision at the
lower limit are absolute; the upper limit values
are relative. This eliminates unrealistic, restric-
tive precision requirements for low concentra-
tion samples.
Initial DQOs were established on the
basis of the requirements of EPA data users
and the selection of appropriate methods to
obtain the data. The initial DQO values were
reviewed by persons familiar with analytical
methods and techniques for soil characteriza-
tion including soil chemists, laboratory direc-
tors, and laboratory personnel. Modifications
were implemented based on reviewers' com-
ments and the limitations of the particular
analytical procedure or instrument. Because
of the greater heterogeneity of the material in
the organic horizons, attaining specific preci-
sion limits for organic horizons may be difficult
for many of the analyses. Precision objectives
for organic horizons should be reevaluated as
data become available and should be changed
if necessary. If the data quality goals cannot
be met during the course of the project, the
actual quality of the data will be used to
reassess the intended use of the data and to
document the implications derived from the
survey. Therefore, the actual data quality
achieved may require different conclusions or
modifications in the level of confidence of
conclusions and decisions.
4.3.2 Representativeness
A representative subsample is shipped
from the preparation laboratory to the contrac-
tor analytical laboratory. For each analysis,
the analytical laboratory must remove an
aliquot from the subsample. Personnel at the
analytical laboratory mix the soil material
thoroughly to ensure the representativeness of
the aliquot. All samples not in use are stored
at 4°C by the contractor analytical laboratory.
4.3.3 Completeness
The objective for the complete analysis
of all samples collected is 90 percent or better
for all parameters. One hundred percent
completeness is possible if sufficient sample
is available to complete all analyses, reanaly-
ses, and duplicate analyses.
-------
Tabla 4-1. Data Quality Objectives (U.S. EPA, 1966)
Reporting
Parameter Unit
1. SantT drywt
2. Silt'
3. Clay"
4. Rock
Fragments
(2-20mm)»
5. Buk Density g/cm*
6. pH in Water pH units
7. pH in 0.01 M
CaCI,
8. pH in 0.002 M
Cad,
9. Organic C % dry wt
10. Inorganic C
11. Total N
12. Total S
13. CEC(NA.OAc) meq/IOOg
14. CEC(NH.CI)
15. Exchangeable Ca •
(in NH.OAc)
Reporting
Format
±0.1%
•
•
Expected
Range
0-98% (of <2-mm
10-80%
0-70%
±5% of total 0-100%
sample weight
±0.01%
±0.01 units
•
•
±0.01%
•
0.01%
±0.001%
±0.01
meo/IOOg
•
•
02-2.0
2.5-7.0
2.0-7.0
^0-7.0
0-50%
0-20%
0-2.0%
00250%
1.0-200
02-100
0-10.0 (
-------
Table 4-1. (Continued)
ffeirhnrtSnn
itapomng
Parameter IMt
17. "Na
18. "K
19. Exchangeable Ca *
OnNHLCQ
20. "Mg
21. 'Na
22. -K
23. Ca Exchange- mg/L
able in
24. Mg 0.002 M
25. NaCaCI, meq/tOOg
26. K
27. Fe
28. Al
29. Fe (Pyrophosphate % dry wt
30. Al Extractabte)
31. Fe (Atid-Oxalate *
32. Al Extractabte)
33. Fe (Citrate-
Dithionite
34. Al Extractabte)
35. SO. -Water mg S/kg
Extractabte dry wt
Reporting Expected Lower
Format Range Reporting
Limit
O05 (20 T
0-1XJ (5JO T
0-10.0 (100.0 T
0-25 (WJO T
0-0.25 (1.0 T
0-1.0 (5.0 T
±0.1% 0-WO 10 mg/L
to support specific data quality objectives.
±0.01% 0-75 0.05%
0-6.0
0-75
0-6.0
0-75
0-6.0
±0.1 0-100 1.0 mg/kg
Precision at Precision at
Lower Limit* Upper Limn*
•
-
• "
•
•
-
±5.0% of ±5.0% of reported
reported value value
+0.05% wt % +15% of reported
value
• •
.
+1.0 mg/kg +10% or reported
value
* Because of the greater Inherent heterogeneity of the material hi organic horbona, attaining theae preclakm Unite for organic horbona auiy
ba difficult for may of the analyses. Precision obfeetlves for organic horizons will be Devaluated as data become available and will ba
changed If necessary.
b Parameter determined on mineral horbona only.
c The Initial range Hated la for mineral aoll horbona; the second range hi parantheaea la for organic horbona.
(continued}
i?.?-?.?
ro
-------
Table 4-1. (Continued)
Reporting
Parameter Unit
36. SO. - PO.
Extractable
37. Six points on mg S/L (in
thru suit ate adsorption equilibrated
42. isotherm solution)
Reporting
Format
0.01
Expected
Range
0-200
0-35
Lower Precision at
Reporting Lower Limit*
Limit
±1.0 mg/kg ±0.05 mg/L
±0.05 mg/L +0.05 mg/L
Precision at
Upper Limit"
+5% of reported
value
+5% of reported
value
43. BaCI,-TEA
Exchangeable
Acidity
meq/100 g +.0.01
44. KCI Exchangeable *
Acidity
45. KCI Exchangeable "
0-100 C<250 in
0 horizon)'
0-20
0.5meq/100g +_0.5meq/100g +.20% of reported
value
* Because of the greater Inherent heterogeneity of the material In organic horizons, attaining these prec
difficult for many of the analyses. Precision objective* for organic horlzona will be reevaluated as data become available and will be
changed If necessary.
c The Initial range listed Is for mineral soil horizons; the second range In parentheses I* for organic horlzona
TJD3JW
Q> (k) CD (D
(Q •* £ O
® R w ~
°> 5' 3
-------
Section 4
Revision 2
Date: 2/87
Page 7 of 7
434 Comparability
Comparability is assured by the uniform
use of procedures documented in Cappo et al.
(1987) and by the use of uniform units for
reporting data as specified on the data sum-
mary sheets. The QA procedures required for
contractor analytical laboratories (see sections
9 and 10) allow for determination of interlabo-
ratory and intralaboratory bias so that results
can be compared. In addition, the analytical
techniques and methods used to determine the
soil parameters allow the data to be compared
to other data bases compiled from results that
were obtained by using the same or compara-
ble techniques and methods.
-------
Section 5
Revision 2
Date: 2/87
Page 1 of 7
Section 5
Sampling Strategy
5.1 Northeastern Soil Survey
5.1.1 Watershed Selection
The objectives of the DDRP focus on
making regional inferences. For this reason,
the 150 watersheds selected for mapping of
soils and watershed characteristics must
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 soil survey of the DDRP for
two reasons: (1) the Region I NSWS lakes
were selected according to a rigorous probabil-
ity sampling method, i.e., 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 studied in the DDRP
also are part of the Phase II Lake Monitoring
Program of the NSWS. This provides a data
set that contains both water-chemistry and
watershed information; therefore, the proce-
dure used to select these watersheds incorpo-
rated criteria relevant to both the DDRP and
the NSWS. The preliminary selection proce-
dure for the NSWS consisted of five steps
which are summarized as follows:
1. Lakes of low interest, e.g., too shallow,
highly enriched, capacity-protected, pol-
luted by local activities, or physically dis-
turbed, were excluded.
2. Lakes too large to be sampled, i.e.,
greater than 2,000 ha, were excluded.
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 characteris-
tics.
4. A subsample of 60 lakes was selected
from each cluster, then the three sub-
samples were weighted to represent the
overall population of lakes in the North-
east.
5. Lakes with watersheds too large to be
mapped at the required level of detail,
i.e., watersheds greater than 3,000 ha,
were excluded from the subsamples.
This procedure identified 148 lakes and
watersheds spread across the three clusters.
The three groups differ primarily in their alka-
linities, pH levels, and calcium concentrations.
To maintain the ability to regionalize conclu-
sions drawn from the sample of 148 water-
sheds, the precision of information characteriz-
ing each of these watersheds should be
comparable, and each cluster should be de-
scribed at the same level of detail as the
others.
5.1.2 Watershed Mapping
During the spring and summer of 1985,
145 of the 148 watersheds were mapped.
Approximately 440 mapping units were identi-
fied in the 148 watersheds. Sampling each of
the 440 mapping units is not necessarily the
best way to describe the chemistry of the soils
in a region. A better procedure is to combine
the mapping units into groups, or sampling
classes, which are either known or expected to
have similar chemical characteristics. Each of
these sampling classes can be sampled from
a number of watersheds, and the mean char-
acteristics of each sampling class can be
computed. The mean values and the variance
about the mean can be used to construct
area- or volume-weighted estimates of the
characteristics for each watershed. For this
procedure to work, at least five samples must
be taken to characterize the variability of each
sampling class. The goal of this sampling
plan is to develop a method of grouping the
-------
Section 5
Revision 2
Date: 2/87
Page 2 of 7
large number of soils into a reasonable num-
ber of sampling classes.
5.1.3 Sampling Classes
5.1.3.1 Soil Mapping Data Base-
The data base contains about 2,200
observations initially recorded on field forms
during the soil mapping of 145 watersheds
selected as part of the ODRP and the Phase II
lakes survey. This information, which was
considered in aggregating similar soils into
sampling classes, includes:
soil taxonomic class (series, sub-
group, great group)
family texture
parent material
- origin
- mode of deposition
drainage class
slope class
slope configuration
geomorphic position
dominant landform
surface stoniness
percent inclusions
percent of soils occurring in com-
plexes
estimated depth to bedrock
estimated depth to permeable mate-
rial.
The data base also includes the area of
each mapping unit, the number of occurrences,
and the percent of the watershed area. Sepa-
rate data files exist for vegetation type, vege-
tation class, and geology. A comparison of
vegetation types to Society of American For-
esters (SAP) cover types is given in Table 5-1.
5.1.3.2 Evaluation of Sampling
Classes-
Initially, a taxonomic approach was used
to identify 38 sampling classes as a founda-
tion for aggregating similar soils. Taxonomic
classification is based on similarities among
soil properties. This taxonomic scheme was
modified to reflect the major factors which are
thought to influence soil chemistry, e.g., drain-
age class and parent material.
5.1.4 Watershed and Sampling
Class Selection
5.1.4.1 Sampling Class Objectives-
The goal of this part of the sample
selection procedure is to determine which
sampling classes are sampled in which water-
sheds. The sites are selected to meet the
following objectives:
1. To characterize all the sampling classes
with similar levels of precision.
2. To describe the variation in watershed
characteristics.
3. To describe the variation in the acid-neu-
tralizing capacity (ANC) clusters devel-
oped from the lake survey.
5.1.4.2 Sampling Class Constraints-
To meet these three objectives, a series
of constraints based on the allocation of
samples to sampling classes and watersheds
must be met. These constraints are:
1. Approximately equal numbers of samples
must be taken from each sampling class.
2. Approximately two samples must be
taken from each watershed.
3. Not more than one sample may be taken
from each sampling class in each water-
shed.
4. Samples must be selected over the range
of ANC clusters within each sampling
class.
The method uses a simple selection
algorithm to randomly select watersheds and
sampling classes within these constraints.
-------
Section 5
Revision 2
Date: 2/87
Page 3 of 7
Table 5-1. Comparison of Coniferous, Deciduous, and Mixed Vegetation Types to Society of American Foresters
(SAP) Forest Covsr 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 Vegitation 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
-------
Section 5
Revision 2
Date: 2/87
Page 4 of 7
5.1.4.3 Selection Algorithm-
The selection method proceeds through
a series of stages. Whenever possible, the
rationale for the particular approach taken is
described and cross-referenced with the objec-
tives 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 deter-
mined (Constraint 1).
5.1.4.3,1 The first step in the selection process
involves constructing a matrix of the occur-
rences of each sampling class in each water-
shed. This matrix is used to: (1) prepare a list
of the watersheds that contain each sampling
class, and (2) determine the number of differ-
ent sampling classes in each watershed.
After the number of watersheds repre-
sented in each sampling class is determined,
it is possible to allocate the samples to be
taken from each watershed into sampling
classes (given Constraint 3).
Using eight samples per sampling class
as a goal for selection, the following sample
allocation occurs: eight samples are allocated
to each sampling class when there are more
than eight watersheds; when there are eight or
fewer watersheds, one sample is allocated to
each watershed.
5.1.4.3.2 Next, watersheds are selected within
each sampling class. Constraints 2 and 4 are
important in this process.
If watersheds are selected randomly
within each sampling class, the watersheds
that contain a large number of sampling
classes have more samples allocated to them
than the watersheds that have few sampling
classes. To counteract this effect and to
approach an approximately equal number of
samples per watershed, the watersheds are
weighted (during the random selection proce-
dure) by the inverse of the number of sampling
classes that they contain.
For example, if one watershed contains
four different sampling classes, it is exposed
to the sample selection procedure four times.
In other words, it Is given one quarter of the
weight of a watershed that contains only one
sampling class. When this technique is used,
both watersheds have an approximately equal
probability of being selected. This scheme
works properly if there are equal numbers of
watersheds considered in each sampling
class; the presence of unequal numbers
causes some deviation from the most desir-
able distribution of samples.
To avoid overemphasizing the very com-
mon soils, only one sample is taken from each
watershed that contains only one sampling
class. All named soils in a soil complex are
counted as occurrences in their respective
sampling classes. For example, a Tunbridge-
Lyman soil complex in a watershed mapping
unit is considered one occurrence of sampling
class S12, which contains the Tunbridge series,
and one occurrence of sampling class S13,
which contains the Lyman series.
Watersheds within sampling classes are
sorted by ANC cluster. When the weights
described above are used, a systematic,
weighted, random sample is taken. A random
starting point is selected from the list of
watersheds; then watersheds are selected 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 sam-
pled 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.
5.1.4.3.3 After this procedure has been fol-
lowed for each sampling class, the initial
selection of watersheds and sampling classes
can be summarized. Three options are possi-
ble at this point:
1. The weighting factors can be adjusted
iteratively until the allocation is accept-
able.
-------
Section 5
Revision 2
Date: 2/87
Page 5 of 7
3.
Samples can be moved arbitrarily among
watersheds to reach the desired alloca-
tion.
The selection can be accepted as ade-
quate.
If the selection is not considered ade-
quate, the most acceptable solution is to
repeat the procedure with adjusted weights.
This process could be automated, if necessary,
with the weight of a watershed being
increased until the watershed receives suffi-
cient samples.
The method of sampling class and
watershed selection outlined here is designed
to satisfy the objectives and constraints listed
in sections 5.1.4.1 and 5.1.4.2. 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 selec-
tion that is a compromise between the de-
mands of the different objectives.
5.2 Southeastern Soil Survey
The sampling strategy for the South-
eastern soil survey is similar to that for the
Northeastern soil survey.
5.3 Final Sampling Locations
Generally, soil surveys identify and de-
scribe soils at the level of series and phases.
The DORP is interested in obtaining soil sam-
ples that are integrative or representative of
the sampling classes in the region. A sam-
pling class may contain six or seven similar
soils. The sampling purpose Is to describe the
characteristics of the sampling class rather
than to describe the characteristics of a spe-
cific soil phase. All soils within a sampling
class are considered similar in soil chemistry;
therefore, the specific sampling location within
a sampling class can be selected at random.
The procedures described in this section are
Intended (1) to describe the range of variability
of soil characteristics within each sampling
class, and (2) to ensure that each sampling
class is characterized at the same level of
precision.
Determining the potential sampling
locations within the watershed is a two-step
process.
5.3.1 Sampling Site Selection
There are five steps in selecting repre-
sentative sampling sites within a sampling
class:
NOTE: Steps 1 through 5 are completed
by ERL-C. Maps that show the
five random points, as discussed
in Step 3, are given to each SCS
sampling crew.
1. Prepare a list of all mapping units and
the sampling class or classes in which
they occur. Most mapping units 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 the average proportion, excluding the
area occupied by inclusions.
2. For each watershed, obtain the water-
shed maps, 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.
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 water-
shed. If the point does not fall within
the selected sampling class, draw anoth-
er pair of random coordinates. Continue
this process until five random points
have been identified in each sampling
class. Record their order of selection
from 1 through 5. Some sampling loca-
tions may not be accessible; therefore,
alternate locations must be provided.
-------
Section 5
Revision 2
Date: 2/87
Page 6 of 7
4. If the point falls on a mapping 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 to
30 percent complex of Tunbridge-Lyman
would sum to 80, so the maximum ran-
dom number is 80. Determine the per-
centage of the area in the desired sam-
pling 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 are overselected for sampling.
5. For each location selected, overlay ap-
propriate maps and note the vegetation
class associated with each point as (1)
coniferous, (2) deciduous, (3) mixed, (4)
open dryland, or (5) open wetland.
Within the sampling class, sample the
pedon that has one or more of the soils in the
sampling class and that has one or more of
the vegetation classes noted above.
5.3.2 Sampling Site Locations
The general vicinity of the site is located
on the watershed soil map. Soil maps marked
with the random points are distributed before
the sampling crew leaves for the field. Each
point, i.e., starting point, marked on the map
represents the origin of a circle with a 150-m
radius, i.e., a sampling site. Within the area
of the sampling site, there may be inclusions,
rock outcrops, a soil complex, or other factors
that make finding a soil of the specific sam-
pling class difficult. The following procedure
is used by the sampling crew to select the
specific sampling site in the watershed:
1. Refer to the assigned sampling class
and vegetation class for a specific water-
shed. For each sampling class to be
sampled on the watershed, refer to a list
of the soil series that are part of the
sampling class. Also refer to a map that
clearly shows the five predetermined
random points prioritized from first to
fifth for selection.
2. Go to the location of the starting point
of the first potential sampling site indi-
cated on the map. If that location is
inaccessible but some part of the sampl-
ing site is accessible, go to Step 4. If
the entire sampling site is inaccessible,
note the reasons in the field logbook and
on the SCS-232 field data form (refer to
Appendix A), and go to the next potential
sampling site.
3. If the location is accessible and the soil
at the site is in the selected sampling
class and the vegetation class is appro-
priate, sample the pedon.
4. If the starting point is inaccessible as
described in Step 2 or if the starting
point is accessible but does not contain
the specified sampling class or vegeta-
tion class, then the following procedures
are required:
• From a random-number table, select
a random number between 1 and 8
where 1 represents the direction
northeast, 2 represents east, 3 repre-
sents southeast, 8 represents north.
• Transect potential sampling points in
10-m intervals along a 150-m straight
line in the chosen direction until the
first occurrence of the proper combi-
nation of sampling class and vegeta-
tion class is found. If a proper com-
bination of sampling class and vege-
tation class is not obtained after five
transects, go to the next potential
sampling site on the list.
• Record the direction of each transect,
e.g., southwest (SW) or north (N), and
the number of the sampling point, i.e.,
1 through 15, on the SCS-232 field
data form.
• If none of the five potential sampling
sites yields an accessible pedon with
the specified sampling class and
vegetation class, call the sampling
task leader as soon as possible.
-------
Section 5
Revision 2
Date: 2/87
Page 7 of 7
5.4 Special Conditions
5.4.1 Inaccessible Watersheds
An attempt should be made to sample
every watershed. Some watersheds may be
inaccessible or may have inaccessible areas.
In addition, access to a sampling site may be
denied by the landowner. Alternative sampling
classes are selected during the random selec-
tion process for backup sampling locations to
ensure an equitable distribution of samples
among watersheds. Each field crew must
formally document the reasons for excluding a
watershed or sampling site.
5.4.2 Inclusions
For this study, an inclusion is a soil
associated with a sampling class other than
the one being sampled; therefore, its chemical
properties are described when the other sam-
pling class is sampled. Because it is not rep-
resentative of the soils in the sampling class,
an inclusion located on a randomly selected
site should not be sampled. The procedure
described earlier accommodates this contin-
gency.
5.4.3 Agricultural Sites
The open-dryland class contains some
cultivated land. If a cultivated site has been
selected randomly as a sampling location and
if access permission has been obtained, the
site is sampled. Agricultural practices may
alter the chemical characteristics of the soils;
therefore, if a cultivated site is sampled, that
land use must be noted on the field form.
During statistical analyses and subsequent
modeling, these samples may or may not be
incorporated as representative of watershed
soil chemistry.
5.4.4 Unsuitable Sampling Sites
Some land use classes generally are
unsuitable for sampling, e.g., urban land,
barren land, and waste disposal land. The
crew leader decides if a sampling site is
unsuitable. Documentation of the land use
and reasons for the decision whether sampled
or not sampled are entered into the log book.
5.5 Paired Pedons
Paired pedon sites for sampling are
selected and assigned in advance by ERL-C.
These sites are sampled in conjunction with
the corresponding routine pedon. The paired
pedon should be treated as a routine pedon
when assigning the sample code.
The crew leader determines the location
of the paired pedon by:
• Establishing sufficient distance be-
tween the two sampling locations to
avoid disturbance of the paired pedon
from sampling of the routine pedon.
• Using the same sampling unit and
vegetation class as the routine pedon.
• Using the same slope position as the
routine pedon.
• Using the same profile description and
sampling protocol as the routine
pedon.
-------
Section 6
Revision 2
Date: 2/87
Page 1 of 1
Section 6
Operations
6.1 Profile Description
After the sampling site is located as
described in Section 5.0, a pit large enough for
sampling all major horizons is excavated to a
depth of 1.5 m in the Northeast, 2.0 m in the
Southeast, or to bedrock. The soil profile is
described according to SCS protocols, and the
data is recorded on the SCS-232 field data
form (see Appendix A). Other descriptive infor-
mation such as pesticide and herbicide con-
tamination also is recorded on the field data
form.
The sampling site is identified by a
unique descriptor composed of the following
numbers separated by hyphens: (1) the six-
digit site identification code (ID) which incor-
porates the region, subregion, alkalinity class,
and ID numbers, (2) the random site ID, i.e., a
number from one to five, (3) the three-digit
sampling class ID, and (4) the three-digit
azimuth, measured in degrees and perpendicu-
lar to the described pit face.
6.2 Sampling
Precautions should be taken to avoid
contamination when sampling the pedon. A
wet pedon of mineral soil should be sampled
from the base of the profile toward the top in
order to avoid the sloughing of upper horizons
onto the lower horizons. Other precautions
include the draining of saturated soils before
sampling; however, soil water should not be
drained from sampled material. Also, handling
the sample should be minimized.
Samples of approximately 5.5 kg of less
than 20-mm material are taken so that at least
2 kg of less than 2-mm material are available
after processing. Sample bags are labeled with
Label A which identifies the date the sample
was taken, the crew that took the sample, the
site, the sample code, the horizon depth, and
the assigned set ID. The twelve-digit sample
code is an alpha-numeric coding of the sample
type, i.e., routine or field duplicate; number of
bags filled per sample; the two-digit SCS state
code; the three-digit SCS county code; the
three-digit county pedon number; and the two-
digit horizon number. The identification and
sample numbering scheme yields unique alpha-
numeric labels for each pedon and for each
sample taken within the pedon.
Samples are kept as cool as possible in
the field and in transport to the preparation
laboratory. To maintain an ambient air tem-
perature of 4°C, samples are stored in coolers
with frozen gel packs. When sampling sites
are remote, samples are stored in rented cold
lockers prior to delivery to the preparation
laboratory.
For the determination of bulk density,
natural soil clods are sampled in triplicate
from each mineral soil horizon. The clods are
placed in hairnets, are moistened with a water
mist, and are dipped in a saran solution to
preserve their structural integrity for transport
to the preparation laboratory.
For further information regarding sam-
pling protocols, refer to Blume et al. (1987).
6.3 Sample Custody
Legal chain-of-custody procedures are
unnecessary for this study; however, sample
handling and storage procedures must be
documented. Prior to delivery of the samples
to the preparation laboratory by SCS person-
nel, the amount of time that samples are
unrefrigerated must be minimized. An over-
night air courier is used for shipment of all
samples from the preparation laboratory to the
analytical laboratory.
-------
Section 7
Revision 2
Date: 2/87
Page 1 of 1
Section 7
Soil Sampling Internal Quality Control
Each field crew samples one horizon in
duplicate on each day of sampling activity.
The horizon for replicate sampling is chosen at
the discretion of the field crew; however, the
type of horizon is alternated so that field
duplicates for each field crew are sampled
across the complete range of possible hori-
zons.
The sampling procedure specifies that
the field duplicate and paired routine sample
are sampled simultaneously. Trowelsful of soil
are removed from the pit face and are placed
alternately into sample bag 1 and then into
sample bag 2, until two samples of fine earth
material equal to approximately 5.5 kg each
are collected. If sieving is necessary to re-
move rock fragments greater than 20 mm, two
options exist: (1) each sample may be collect-
ed on a plastic sheet then sieved into a sam-
ple bag, or (2) if two 20-mm sieves are avail-
able, each sample may be sieved directly into
a sample bag.
The field duplicates are processed by a
preparation laboratory and are analyzed by a
contractor analytical laboratory. The analytical
results are used to assess the variability
attributed to sampling, preparation, and analy-
sis.
For the determination of bulk density,
natural soil clods are sampled in triplicate
from each mineral horizon; however, a dupli-
cate set of three clods is not taken.
-------
Section 8
Revision 2
Date: 2/87
Page 1 of 1
Section 8
Preparation Laboratory Internal Quality Control
8.1 Sample Receipt
All field samples received by the prepara-
tion laboratory are checked in by preparation
laboratory personnel. The following informa-
tion is recorded in a logbook: (1) date re-
ceived, (2) time received, (3) who delivered
samples, (4) who received samples, (5) condi-
tion of samples, including notation by sample
code of any problems, (6) set ID numbers, and
(7) total number of samples. This logbook
must be submitted to EMSL-LV at the end of
the project.
8.2 Sample Processing
Each preparation laboratory splits one
routine sample per batch into two samples.
The preparation duplicates are analyzed by a
contractor analytical laboratory. The results
provide a measure of the variability attributed
to subsampling and analysis.
8.3 Inorganic Carbon
detection limit sample is used to test the
ability of the analyst to see effervescence.
The QC detection limit sample is prepared by
spiking noncalcareous, less than 2-mm soil
material with 1 percent (wt/wt) reagent-grade
CaCO, powder or natural dolomite,
CaMgfCOJ* ground to pass a 60-mesh sieve.
A QC calibration sample, prepared by spiking
noncalcareous, less than 2-mm soil material
with 5 percent (wt/wt) reagent grade CaCO, or
natural dolomite, also is used by the analyst.
8.4 Bulk Density
Two or three soil clods are collected for
each horizon sampled; therefore, duplicate or
triplicate analyses are possible.
8.5 Raw Data
All raw data recorded in logbooks or on
data sheets must be submitted to EMSL-LV at
the end of the project (see Section 13.2).
For the visual determination of inorganic
or carbonate carbon, a quality control (QC)
-------
Section 9
Revision 2
Date: 2/87
Page 1 of 23
Section 9
Analytical Laboratory Procedures and
Internal Quality Control
9.1 Sample Receipt
All samples received by the contractor
analytical laboratory are checked in by a
receiving clerk who (1) records on the shipping
form the date samples are received, (2) checks
the samples to identify discrepancies with the
shipping form, and (3) mails copies of the
completed shipping forms to the Sample
Management Office (SMO) and the project
officer or designee. If there are any discrep-
ancies or problems such as leakage in ship-
ping or insufficient sample, the QA manager
designee must be notified immediately. The
receiving clerk retains a copy of the completed
shipping form for the laboratory records. The
samples are refrigerated at 4°C as soon as
possible and must be refrigerated when not in
use.
The samples received by the contract or
analytical laboratory have been prepared, i.e.,
air-dried and crushed to pass a 2-mm sieve.
During shipping, the sample material within
each container segregates both by particle size
and by density; therefore, each sample must
be homogenized by thorough mixing prior to
the removal of aliquots for analysis. One
method of mixing is to place sample material
on a large square of heavy paper. Each corner
of the paper is lifted alternately and the soil is
rolled toward the opposite corner. This pro-
cess is continued until the soil is mixed thor-
oughly, at least 20 passes from each corner is
recommended. Alternative methods of homog-
enizing the sample may be used. Prior to the
removal of an aliquot for analysis, the sample
is mixed thoroughly by rolling the sample
container. After an aliquot is removed for
analysis the sample should be returned to the
refrigerator as soon as possible. After all
analyses have been completed and the results
have been checked, samples should remain in
refrigerated storage at 4°C in case reanalyses
are necessary.
9.2 Sample Analysis
Procedures specified in the analytical
methods manual (Cappo et al., 1987) are to be
followed exactly for each parameter. Table 9-
1 summarizes the parameters to be measured
and the corresponding analytical techniques.
Table 4-1 lists the required precision and
expected range for parameters specified by
ERL-C. Required detection limits for each
parameter are given in Table 9-2.
9.3 Analytical Laboratory Docu-
mentation for Quality
Control
The following documents must be up-
dated constantly at the analytical laboratory
and must be available to the analysts and the
supervisor involved in the project:
-------
Table 9-1. Uat of Parameters and Corresponding Analytical Techniques
Section 9
Revision 2
Date: 2/87
Page 2 of 23
Parameter
Moisture
Sand
Silt
Clay
pH in deionized water
pH in 0.01 M CaCI,
pH in 0.002 M CaCI,
Total C
Total N
Total S
Inorganic C
CEC (NH.OAc saturating solution)
CEC (NH.CI saturating solution)
Ca
Mg Exchangeable in NH.OAc, NH.CI, and CaCI,
Na
K Exchangeable in NH.OAc, NH.CI, and CaCI,
Fe Exchangeable in CaCI,: extractable in
pyrophosphate, acid-oxalate, and citrate-dithionite
Al Extractable in pyrophosphate, acidoxalate, and
citrate-dithionite
Al Exchangeable in CaCI, and KCI
Nitrate (NO,') water extractable
Sulfate (SO,'"} water extractable, phosphate
extractable, and sulfate adsorption 6-point isotherm
Exchangeable acidity in BaCI.-Triethanolamine and
KCI saturating solutions
Method
Gravimetric
Sieve/gravimetric
Pipet/gravimetric
Pipet/gravimetric
Combination electrode/millivoltmeter
Elemental analyzer
Elemental analyzer
Elemental analyzer
Coulometric
Autotitration/flow injection analyzer
Flame atomic absorption spectroscopy,
inductively coupled plasma atomic
emission spectroscopy (or flame atomic
emission spectroscopy for Na only)
Flame atomic absorption spectroscopy
orf lame atomic emission spectroscopy
Flame atomic absorption spectroscopy
or inductively coupled plasma atomic
emission spectroscopy
Inductively coupled plasma atomic
emission spectroscopy
Ion chromatography
Ion chromatography
Titrimetric
Specific surface
Gravimetric
-------
Table 9-2. Required
Section 9
Revision 2
Date: 2/87
Page 3 of 23
Detection Limits, Expected Ranges, and Intralaboratory Relative Precision Goal
Contract-
Required
Parameter Matrix Calculated Calculated
Reporting Units Detection Limit
Particle size
PH
Total C
Inorganic C
Total N
Total S
CEC (FIA)
CEC (titration)
Na+
K+
Mg"
Ca"
Ca1*
AT*
AT
AT
Fe"
Fe"
so-.
NO,-
SO1'. adsorption
Exchangeable
acidity
Exchangeable
acidity
Specific surface
- wt % + —
PH —
— wt % 0.010%
— wt % 0.010%
— wt % 0.010%
— wt % 0.010%
— meq/100g —
— meq/100g O.OImeq
all meq/100g —
all meq/100g —
all meq/100g —
CaCI, meq/100g —
other meq/100g —
CaCI, meq/100g —
KCI meq/100g —
other wt % —
CaCI, meq/100g —
other wt % —
all mg S/kg soil 0.32 mg/kg
water mgN/kg soil —
mg S/L 0.32 mg/L
KCI meq/100g 0.40 meq
BaCI,-TEA meq/100g 0.25 meq
m'/g —
Contract-
Required
Instrumental Expected
Detection Limit Range
— 0-100%a
— 2.5-7.0
— 0-50%
— 0
— 0-20%
— 0-0.25%
0.010 meq 0.2-200
— 0.2-200
0.50 mg/L 0.00-0.50
0.050 mg/L 0.00-1.00
0.050 mg/L 0.00-1.50
2.00 mg/L —
0.050 mg/L 0.00-8.00
0.050 mg/L —
0.10 mg/L —
0.50 mg/L —
0.050 mg/L —
0.50 mg/L —
0.10 mg S/L 0-200
0.10 mg N/L —
0.10 mg S/L 0.35
— 0-100
—
— 1.0-800
Intralaboratory
Relative
Precision Goal (%)*
5%
0.05
10%
15%
10%
10%
10%
10%
10%
10%
10%
10%
10%
10%
10%
10%
10%
10%
5%
5%
5%
10%
10%
* Unless otherwise noted, this Is the relative precision at concentrations above 10 times Instrumental detection
limits.
All values are determined on an oven-dry weight basis.
-------
Section 9
Revision 2
Date: 2/87
Page 4 of 23
• Laboratory standard operating proce-
dures (SOPs) - detailed instructions
about the laboratory and instrument
operations.
• Laboratory quality assurance plan -
clearly defined laboratory protocol,
including personnel responsibilities
and use of QC samples.
• List of in-house samples - includes
dates for completion of analyses,
allowing the analysts to schedule
further analyses.
• Instrument performance study infor-
mation - information about baseline
noise, calibration standard response,
precision as a function of concentra-
tion, and detection limits; used by
analysts and supervisor to evaluate
daily instrument performance.
• QC charts - with 99 percent and 95
percent control limits for all quality
control calibration samples (QCCS)
and detection limit QC samples;
generated and updated for each
batch. The same QCCS must be used
throughout each control chart in order
to ensure the continuity of the control
chart. (Note: The purpose of prepar-
ing QCCS control charts is to ensure
that the actual control limits do not
exceed the limits given in Table 9-3.)
• Data QC report - report by laboratory
manager reviewing QC results for
each parameter; specifies flags (see
Table 9-4) that are used (1) to document all
results that are outside statistically estab-
lished QC limits and (2) to identify samples
that will require reanalysis before data are
submitted.
9.4 Internal Quality Control
Within Each Method
Internal quality control is an integral part
of any measurement procedure and ensures
that results are reliable. A summary of inter-
nal QC procedures for each method is given in
Table 9-5. QC procedures are detailed in the
appropriate method description in the analyti-
cal methods manual (Cappo et al., 1987).
Details on internal QC procedures are de-
scribed below.
9.4.1 Initial Calibration
All calibration standards are prepared in
concentration units of mg/L or as specified in
the procedure. A calibration curve for each
analytical method is established by using a
minimum of three points within the linear
range. The use of at least a three-point cali-
bration curve is required in place of the manu-
facturer's recommendations for the instru-
mentation, unless the manufacturer's recom-
mendations for the instrumentation require
more than three points within the linear range.
The concentration of standards must bracket
the expected sample concentration without
exceeding the linear range of the instrument.
Occasionally the standards suggested by a
method must be adjusted to meet this require-
ment. The lowest standard should not be
greater than 10 times the detection limit.
-------
Tab)* 8-3. Maximum Control Limits for QC Samples
Maximum
Control Limit for QC Sample
Parameter (% Deviation from Theoretical
Section 9
Revision 2
Date: 2/87
Page 5 of 23
Table 9-4. Laboratory/Field Data Qualifiers
Data Qualifier
Indicates
Concentration of QC Sample)
Particle
PH
Total C
Inorganic C
Total N
Total S
CEC
Na+
K+
Mg"
Ca"
AT
Fe"
NO,-
so*-.
SO1-. Adsorption
Specific Surface
*Refer to Section 4.12,
in Cappo et a I., 1987.
*
± 0.1 unit
±10%
±15%
±10%
±10%
±10%
±10%
±10%
±10%
±10%
±10%
±10%
± 5%
± 5%
± 5%
±10%
Particle-Size Analysis
B
F
G
J
L
M
N
P
R
S
T
U
X
Y
Instrument unstable.
Redone, first reading not
acceptable.
Result outside criteria with
consent of QA Manager.
Result obtained from method
of standard additions.
Result not available; insuffi-
cient sample volume shipped
to laboratory.
Result not available because
of interference.
Result not available; sample
lost or destroyed by laborato-
ry.
Result outside QA criteria.
Result outside criteria, but
insufficient volume for
reanalysis.
Result from reanalysis.
Contamination suspected.
Container broken.
Result not required by
procedure; unnecessary.
No sample.
Available for miscellaneous
comments.
Result from approved alterna-
tive method.
-------
Section 9
Revision 2
Date: 2/87
Page 6 of 23
I
t
i
8^
!S
<8 gf
:«fi
8|§*S
•lit
11!
:;
ill
iflie
1
!l
i
!
3
I
g-SjgES^
liilll
8
to 5o
! S Al
ill
1
•I
I
£
^
.
i « Al
ill
it!
.si
i
^
is
.Si
2|
« §L-
1>52 =
°ll" -a
^O*-(? &'
X
~ in ">
WOT^W
-------
Table 9-5. ConthWMd
Parameter
Procedure
Control Limits
Corrective Action
Specific Surface
(continued)
Laboratory Triplicate Analysis
Analyze two additional portions
of one sample in every batch.
Reagent Blank Analysis
Analyze three reagent blanks
per batch contammy an amount
of EGME equal to the greatest
quantity required to saturate
the soil samples.
Prasision should be within
10% BSD.
Blanks show no EGME residu-
al at end of equalibrium
period.
Blanks show residual
EGME at end of
equilibrium period.
Calibration and Standardization
Sample Analysis
Calibrate pH meter for the range The value of the QCCS
of pH expected in the soil (usu- must be 4.00 i 0.05.
ally pH - 4 and pH - 7 standards).
Analyze a QCCS immediately after
caKbration and after analyzing
every 10 or fewer samples.
Analyze a second sample
in triplicate. Check for
vacuum In desiccator. Re-
calibrate balance. Reana-
lyze the batch.
No correction.
Determine if EGME reagent
is old or otherwise con-
taminated. Purchase new
reagent and reanalyze
the batch.
Recalibrate pH meter and
reanalyze fresh QCCS.
Check wiring, static elec-
tricity, and solution level
in electrode, then reana-
lyze fresh QCCS.
Replace electrode of pH
meter, then reanalyze
fresh QCCS.
(continued)
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
pH (continued)
Cation Exchange
Capacity
(titration)
Reagent Blank Analysis
Analyze one blank of each
suspension solution.
Laboratory Triplicate Analysis
Analyze two additional portions
of one sample in every batch.
Calibration and Standardization
For Distillationmtration
Method
Acid for titration must be re-
standardized weekly.
Calibrate pH meter (titrator)
for range of pH expected in the
titration (end point pH - 4.60).
Analyze QCCS Immediately after
calibration and after every 10
or fewer samples.
Calculate instrumental detection
limit based upon a minum titra-
tion, I.e., smallest possible
volume, and normality of acid.
The value should be between
pH - 4.5 and 7.5.
Precision should be ±0.10
units.
Normality of acid changes
more than 5 percent.
The value of the pH QCCS
must be 4.00 ± 0.05.
Instrumental detection limit
must not exceed the contract-
required detection limit
(CRDL).
Determine source of con-
tamination. Prepare new
solutions for reanalysis
for batch.
Analyze a second sample in
triplicate. Check for con-
tamination in the suspension
solution. Prepare new solu-
tions for reanalysis of
batch.
Prepare new solution.
Recalibrate pH meter and
reanalyze fresh QCCS.
Check wiring, static elec-
tricity, and solution level
in electrode, then reana-
lyze fresh QCCS.
Replace electrode or pH
meter, then reanalyze
fresh QCCS.
Use a more dilute titrant.
(continued)
tJO 3JC0
u o> o> CD
*S*i
o> o g
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Cation Exchange
Capacity (FIA)
Cation Exchange
Capacity (both)
Calibration and Standardization
for Flow Injection Analysis
Determine instrumental
detection limit.
Analyze a detection limit QC
sample.
One calibration blank ("0" mg/L
standard) and three reagent
blanks (reagents carried through
the analytical procedure) per
analytical batch.
QCCS must be run every 10 or
fewer samples if flow injection
analysis is used.
Laboratory Duplicate Analysis
Analyze a second portion of one
sample in each batch for each
saturating solution.
Instrumental detection
limit must not exceed
the CROL
Value must be within 20%
of the theoretical con-
centration.
Blank is less than the
CRDL
Blank exceeds the CRDL.
Measure each cation exchange
capacity (CEC) and plot the
results on a control chart.
Develop 99% and 95% confi-
dence limits. Required pre-
cision is within 10%
Precision should be within
10% RSD.
Check for possible con-
tamination. Optimize
instrumentation, e.g.,
wavelength.
Identify and correct
problem. Acceptable result
must be obtained prior to
sample analysis.
No correction.
Investigate the element
source of contamination,
then reanalyze all samples
associated with the high
blanks.
Recalibrate. Analyze a
second QCCS and all samples
bracketed by the affected
QCCS.
Analyze a second sample in
duplicate. Check for con-
tamination, e.g., atmos-
pheric NH/ or CO,. Re-
calibrate the balance,
sample diluter how injection
analyzer (FIA), or titrator.
Reanalyze the batch.
(continued)
TJO
n> u
83 s? £ °
» R o> ~
°§ro<°
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Cation Exchange
Capacity (both)
(continued)
Metals - Na, K,
Ca, Mg, Fe, and
Al by AAS and
ICPES
Matrix Spike Sample Analysis
One spike is required for each
analytical batch. Add standard
solution of NH.CI or (NHJ.SO.
at a level approximately equal
to the endogenous level or
10 times the Instrumental detec-
tion limit, whichever is greater.
Samples for flow injection
analysis may be split, and the
spike is added to one split. The
distillation/titration method
requires that a duplicate
sample be extracted, then spiked
for analysis.
§ a libra t ion and Standardization
ample analysis
Calculate the percent
recovery. Acceptable
range is 100 ± 15%.
Calibrate the spectrometer as
required in the analytical
method. Analyze a QCCS immedi-
ately after calibration and
after analysis of every 10 or
fewer samples.
Repeat on two additional
samples. If either or
both are outside the
control limits, analyze
the batch by the method
of standard additions.
Calculate the QCCS value
from the calibration curve,
and plot the result on a con-
trol chart. Develop the
99% and 95% confidence limits
(warning and control).
Acceptable range is ±10%.
Recalibrate instrument,
prepare new stock and
calibration standards if
necessary. Analyze a
second QCCS and all
samples bracketed by the
affected QCCS.
(continued)
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Metals - Ca. Mg,
K, Na, Fe, and
Al by AAS and
ICPES (continued)
Verify calibration linearity.
Determine linear dynamic range.
Linearity as determined
by a least squares fit
should not be toss than
0.89.
Determine the instrumental
detection limits.
Instrumental detection
limits must not exceed
the CRDL for each element.
Analyze a detection limit
QC sample.
One calibration blank ("0" mg/L
standard) and one reagent
blank (any necessary reagents
carried through the analytical
procedure) per analytical batch.
Value must be within 20%
of the theoretical
concentration.
Blank is less than the
CRDL
Blank exceeds the CRDL
Check calibration stan-
dards to see if properly
prepared. Prepare new
stock and calibration
standards, if necessary,
and recalibrate. Follow
instrumental manufac-
turer's troubleshooting
procedures.
Check for possible con-
tamination. Optimize
instrumentation, e.g.,
wavelength, burner or
torch position, oxidant
and fuel pressures, nebu-
lizer flow rate, integ-
rity of impact bead or
spoiler, optical align-
ment.
Identify and correct
problem. Acceptable
result must be obtained
prior to sample analysis.
No correction.
Investigate and eliminate
source of contamination,
then reanalyze all samples
associated with the high
blank.
(continued)
D> 0) (D 0>
2.S*>
CD
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Metals - Ca, Mg.
K. Na, Fe, and
Al by AAS and
ICPES.
(continued)
Exchangeable
Acidity -
BaCI,-TEA, KCI
Matrix Spike Sample Analysis
To one solution in each batch
add standard solution of analyte
at a level approximately equal to
the endogenous level or 10
times the instrumental detection
limits, whichever is greater.
Check recovery in each matrix.
Laboratory Duplicate Analysis
Analyze a second portion of one
sample in each batch for each
analyte.
Standardization
The solutions used for tit-
ration must be restandardized
weekly.
Calculate instrumental detec-
tion limit, based upon a mini-
mum titration, i.e., smallest
possible volume, and normality
of titrants.
Laboratory Duplicate Analysis
Analyze a second portion of
one sample in each batch for
each method.
Calculate the percent
recovery. Acceptable
recovery is 100 t 15%.
Precision should be
within 10% RSD.
Normality of solution
changes more than 5%.
Contract-required instru-
mental detection limits
must not be exceeded.
Precision should be with-
in 10% RSD.
Repeat on two additional
samples. If either or both
are outside the control
limits, analyze batch by
the method of standard
additions.
Analyze a second sample
in duplicate. Recali-
brate balance, repipet,
and sample dilutee. Check
for source of contamina-
tion. Reanalyze the batch.
Prepare new solution.
Use more dilute titrants.
Analyze another sample
in duplicate. Determine
source of difficulty,
e.g., reduce normality
of titrant, replace
electrode, or recalibrate
titrator. Reanlyze the
batch.
(continued)
TJD3J
Q) Q) CD
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Exchangeable
Acidity
(continued)
Suifate and
Nitrate
Reagent Blank Analysis
Three reagent blanks per batch
are required for each exchange-
able acidity method.
Calibration and QA Calibration
Sample Analysis
Calibrate as required in the
analytical methods. Analyze a
QCCS immediately after calibra-
tion and after analysis of every
10 or fewer samples.
Verify calibration linearity.
Determine linear dynamic
range.
Blanks for KCI method are
equal to or less than
twice the CRDL.
Blanks for BAcL,-TEA method
should have a %RSD s5%.
Calculate the QCCS value
from the calibration curve,
and plot the result on a
control chart. Develop the
99% and 95% confidence
limits (warning and control).
Acceptable range is 15%.
Linearity as determined
by a least squares fit
should not be less than
0.99.
Determine source of con-
tamination. Eliminate the
problem, then reanalyze
samples associated with
the high blank(s).
Determine and eliminate
source of variation, then
reanalyze the batch.
Recalibrate instrument.
Prepare new stock and
calibration standards, if
necessary. Analyze a
second QCCS and all samples
bracketed by the affected
QCCS.
Check calibration standards
to see if properly prepared.
Prepare new stock and
calibration standards, if
necessary, and recalibrate.
Follow instrumental manufac-
turers trouble-shooting
procedures.
(continued)
0) CO CD CD
?. w ~
-------
Table »-5. Continued
Parameter
Piumdure
Control Limits
Corrective Action
Sulfateand
Nitrate
(continued)
Determine instrumental
detection Imnts.
Resolution Check
Once per analytical run (day).
check resolution of the anion
separator column by analyzing
a standard containg SO.*-.
NO.-, and NO/ in equal
1-mg/L concentrations. Set
instrument for a nearly full-
scale response on the most
sensitive range used.
Calibration and Reagent Blank
Analysis
One caUbration blank fXT mg/L
standard) and one reagent
blank (necessary reagents
carried through the analytical
procedure) per analytical
batch.
Instnjmental detection
limits must not exceed
theCRDL.
Resolution must exceed
60%.
Blank is equal to or
toss than the CROL.
Blank exceeds the CRDL.
Check for possible con-
tamination. Optimize
instrumentation.
Clean or replace anion
separator column, then
repeat calibration and
resolution check.
No correct ion.
Investigate and eliminate
source of contamination.
than reanalyze aH samples
associated with tha high
blank.
(continued)
-------
Section 9
Revision 2
Date: 2/87
Page 15 of 23
i
I
a
•I
1
«i
|P
•^
!!>'!"
tl"l
M:*J!
'affl*
.still
!!
sif
ll
ii
«.s
si !tg
I Is!
8
1
1
i'
fiSjjfgC .
fill!
111*'
!|il?j
«s>
Mlifif
i^.-g^l
S
9
o'
of
1
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Total S, C. N
(continued)
Verify calibration linearity
Determine linear dynamic range.
Determine instrumental
detection limits.
Calibration Blank Analysis
Analyze one calibration blank
per batch.
Matrix Spike Sample Analysis
To one sample per batch add
a standard amount of analyte
at the endogenous level or 10
times instrumental limit,
whichever is greater.
Linearity as determined by
a least squares fit should
not be less than 0.99.
Instrumental detection
limits must not exceed
the CRDL
Blank is less than the CRDL.
Blank exceeds the CRDL
Calculate the percent
recovery. Acceptable
range is 100 ± 15%.
Check calibration standards
to see if properly prepared.
Prepare new stock and calibra-
tion standards; if necessary,
recalibrate. Follow instru-
mental manufacturer's trouble-
shooting procedures.
Check for possible contamina-
tion, e.g., purity of gas.
Optimize instrumentation.
No correction.
Eliminate source of contami-
nation then reanlyze all
samples associated with high
blank.
Repeat on two additional
samples. If possible, deter-
mine and eliminate the source
of the interference, then
repeat analyses. If either or
both are outside the control
limits, analyze the batch by
the method of standard
additions.
(continued)
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Total S, C, N
(continued)
Inorganic
Carbon
Laboratory Duplicate Analysis
Analyze a second portion of one
sample in every batch for each
procedure.
Calibration and QA Calibration
Sample Analysis
Calibrate as required in
analytical methods. Analyze a
QCCS immediately after calibra-
tion and after analysis of ever
10 or fewer samples.
Verify calibration linearity.
Determine linear dynamic range.
Determine instrumental
detection limit.
Precision should be within
10% RSD.
Calculate the QCCS value
from the calibration curve,
and plot the result on a con-
trol chart. Develop the 99%
and 95% confidence limits
(control and warning).
Acceptable range is 15% RSD.
Linearity as determined
by a least squares fit
should not be less than
0.99.
Instrumental detection
limit must not exceed
CRDL
Analyze a second sample in
duplicate. Increase sample
size, e.g., use two combustion
boats. Decrease particle size
to pass a finer mesh. Sample
may be inhomogenous. Check
for source of contamination.
Recalibrate the instrument,
then reanalyze the batch.
Recalibrate instrument. Pre-
pare new stock and calibration
standards, if necessary.
Analyze a second QCCS.
Check working standards
to see if properly pre-
pared. Prepare new stock and
calibration standards, If
necessary, and recalibrate.
Check for possible contamina-
tion. Optimize instrumenta-
tion.
(continued)
0> cu (D (D
-------
Table 9-5. Continued
Parameter
Procedure
Control Limits
Corrective Action
Inorganic
Carbon
(continued)
Calibration Blank Analysis
Analyze one calibration blank
per batch.
Laboratory Duplicate Analysis
Analyze a second portion of
one sample per batch.
Matrix Spike Sample Analysis
To one sample in each batch,
add analyte at a level approxi-
mately equal to the endogenous
level or 10 times the instru-
mental detection limit, which-
ever is greater.
Blank is equal to or
less than the CRDL
Blank exceeds the
CRDL.
Precision should be within
15% RSD.
Calculate the percent
recovery. Acceptable
range is 100 ± 15%.
No correction.
Investigate and eliminate
source of contamination,
then reanalyze all samples
associated with the high
blank.
Analyze a second sample in
duplicate. Recalibrate
balance. Sample may be
inhomogenous. Check for
source of contamination.
Reanalyze the batch.
Repeat on two additional
samples. If possible,
determine and eliminate the
source of the interference.
then repeat analyses. If
either or both are outside the
control limits, analyze the
batch by the method of stand-
dard additions.
-------
Section 9
Revision 2
Date: 2/87
Page 19 of 23
Next, the linear dynamic range (LDR) for the
initial calibration is determined. If during the
analysis the concentration of a sample falls
above the LDR, two options are available. The
first option is to dilute and reanalyze the
sample. In this case, the diluent should have
the same matrix as the sample matrix The
second option is to calibrate two concentration
ranges. Samples are first analyzed on the
lower concentration range. Any samples
whose concentrations exceed the upper end of
the LDR are then reanalyzed on the higher
concentration range. If this option is per-
formed, separate QC calibration samples
(QCCSs) must be analyzed and reported for
each range.
Spectroscopic-grade or high purity chemi-
cals are required for primary standards when
analysis is done by atomic absorption or
emission methods. Also, calibration standards
must have the same matrix as the solutions
being analyzed. In order to meet the detection
limits, some procedures require that the matrix,
i.e., extracting or saturating solutions, be
prepared from high purity chemicals.
9.4.2 Calibration Blank
One calibration blank per batch is ana-
lyzed immediately after the initial calibration to
check for baseline drift. The calibration blank
is defined as a '0* mg/L standard and contains
only the matrix of the calibration standards.
The observed concentration of the calibration
blank must be less than or equal to the detec-
tion limit. If it is not, rezero the instrument
and recheck the calibration.
9.4.3 Quality Control Calibration
Samples (QCCS)
Immediately after standardization of an
instrument, a QCCS containing the analyte of
interest at a concentration in the midcali-
bration range is analyzed. The QCCS may be
obtained commercially or may be prepared by
the analyst from a source which is indepen-
dent of the calibration standards. The QCCS
is analyzed to verify the calibration curve prior
to any sample analysis, after every 10 sam-
ples, and after the last sample in each batch.
The observed value for the QCCS should
be corrected for the calibration blank. The
observed concentration for the QCCS is
plotted on a control chart, and the 99 percent
and 95 percent confidence intervals are devel-
oped. The 99 percent confidence interval must
not differ from the theoretical value by more
than the limits given in Table 9-3. A value
outside the 99 percent confidence interval is
unacceptable. When an unacceptable value
for the QCCS is obtained, the instrument is
recalibrated, and all samples up to the last
acceptable QCCS are reanalyzed.
After each day of analysis, the control
charts are updated. Cumulative means and
new warning and control limits, i.e., 95 percent
and 99 percent confidence intervals, are calcu-
lated. Bias for a given analysis is indicated by
at least seven successive points on one side
of the cumulative mean. If bias is indicated,
analysis must be stopped until an explanation
is found.
The same QCCS must be used to estab-
lish all values on a given control chart to
ensure continuity.
9.4.4 Detection Limit Quality
Control Samples
One detection limit QC sample is ana-
lyzed per batch. This is a low-level QC sample
that contains the analyte of interest at a
concentration two to three times above the
required detection limit. The purpose of the
detection limit QC sample is to eliminate the
necessity of formally determining the detection
limit on a daily basis. The measured value
must be within 20 percent of the theoretical
concentration. If it is not, the problem must
be identified and corrected, and an acceptable
result must be obtained prior to sample analy-
sis.
-------
Section 9
Revision 2
Date: 2/87
Page 20 of 23
9.4.5 Reagent Blank
For methods that require sample prepa-
ration, a reagent blank for each group of
samples processed is prepared and analyzed.
A reagent blank is defined as a sample com-
posed of all the reagents, in the same quanti-
ties, used in preparing an actual sample for
analysis. The reagent blank undergoes the
same digestion and extraction procedures as
an actual sample. The concentration of the
reagent blank must be less than or equal to
the detection limit. If the concentration ex-
ceeds this limit, the source of contamination
must be investigated and eliminated. A new
reagent blank is then prepared and analyzed,
and the same criteria are applied. All samples
associated with the "high" blank must be
reprocessed and reanalyzed after the contami-
nation has been eliminated.
9.4.6 Preliminary Sample Analysis
Approximately seven samples and a
reagent blank are analyzed prior to matrix
spike and duplicate analyses so that approxi-
mate endogenous sample concentrations may
be determined.
9.4.7 Matrix Spike Analysis
One matrix spike sample is prepared for
each procedure, as specified.
9.4.7.1 Liquid Samples-
For liquid samples, a matrix spike sam-
ple is prepared by spiking an aliquot of a
solution with a known quantity of analyte prior
to analysis. The spike concentration must be
approximately equal to the endogenous level or
10 times the detection limit, whichever is
larger. Also, the volume of the added spike
must be negligible, i.e., less than or equal to
0.01 of the sample aliquot volume. The spike
recovery must be within 100 ± 15 percent to be
acceptable.
If the recovery is not acceptable, two
additional, different samples must be spiked
with the analyte in question and must be
analyzed. If the recovery for one or both
samples is not within 100 ± 15 percent, the
entire batch must be analyzed for the analyte
in question by the method of standard addi-
tions. The method of standard additions is
performed by analyzing the sample, analyzing
the sample plus a spike at about the endoge-
nous level, and analyzing the sample plus a
spike at about twice the endogenous level.
The concentration of the matrix spike sample
must not exceed the linear range of the instru-
ment. If it does, the spiked sample must be
diluted before analysis. The percent spike
recovery is calculated as follows:
value of sample - sample value
plus spike of unspiked
-x (100)
value of spike added
9.4.7.2 Solid Samples-
Matrix spikes for solid samples, e.g., for
analysis of total carbon and total nitrogen, are
prepared by adding a known weight of materi-
al containing the analyte of interest to a sam-
ple of known weight. The spike concentration
should be twice the endogenous level or 10
times the detection limit, whichever is larger.
The concentration of the matrix spike must not
exceed the linear range of the instrument.
Although it will not be negligible, the weight of
the spike material should be considered negli-
gible for the purposes of calculation.
The spike recovery must be within 100 ±
15 percent to be acceptable. If the recovery is
not acceptable, two additional, different sam-
ples must be spiked with the analyte in ques-
tion and must be analyzed. If the recovery for
one or both samples is not within 100 ± 15
percent, the entire batch must be analyzed for
that analyte by the method of standard addi-
tions.
9.4.8 Duplicate Sample Analysis
One sample per batch is prepared and
analyzed in duplicate for each parameter.
Some procedures require triplicate analysis.
-------
Section 9
Revision 2
Date: 2/87
Page 21 of 23
Refer to the specific method in Cappo et al.
(1987).
Calculate the percent relative standard
deviation (%RSD) as follows:
%RSD
where s
X 100
(HX-Xl')1/2
vn-v
The relative standard deviation is plotted
on a control chart, and 99 percent and 95
percent confidence intervals are established.
These confidence intervals represent control
and warning limits, respectively. Initial control
limits are set at the precision levels given in
Table 9-3. If duplicate values fall outside the
control limits, an explanation must be sought,
e.g., instrument malfunction or calibration drift.
A second, different sample must then be
analyzed in duplicate. No further samples
should be analyzed until duplicate sample
results are within the control limits.
Because %RSD is affected by concentra-
tion, this criterion is applied only when the
mean of duplicate analyses exceeds the detec-
tion limit by a factor of 10.
9.4.9 Ion Chromatography
Resolution Test
An ion chromatography resolution test is
performed once per analytical run by analyzing
a standard that contains concentrations of
approximately 1 mg/L for each of SO^1 PO^1
and N03'. If the resolution does not exceed 60
percent, the column should be replaced, and
the resolution test should be repeated.
9.4.10 Continuing Sample
Analysis
The remaining samples are analyzed if
the detection limit QC sample, QCCS, reagent
blank, matrix spike, and duplicate samples are
within the required limits. After every 10 or
fewer samples and after the last sample, a
QCCS is analyzed to periodically verify the
calibration curve. If the measured value of the
QCCS differs from the theoretical value by
more than the limits given in Table 9-3, the
instrument must be restandardized, and the
previous 10 samples must be reanalyzed.
9.5 Instrumental Detection
Limits
Instrumental detection limits (IDLs) are
determined and recorded monthly for each
parameter except pH. For this study, the
detection limit is defined as three times the
standard deviation of 10 nonconsecutive repli-
cate calibration blank analyses run on sepa-
rate days. In some analyses, such as ion
chromatography, a signal may or may not be
obtained for a blank analysts. If a signal is
not obtained for a blank analysis, the instru-
mental detection limit is defined as three times
the standard deviation of 10 nonconsecutive
replicate analyses of a standard whose con-
centration is four times the lesser of the
actual detection limit or the required detection
limit.
9.6 Reagent Blank Correction
for Spectrometric and Ion
Chromatographic
Procedures
For all spectrometric and ion chromato-
graphic procedures presented in Cappo et al.
-------
Section 9
Revision 2
Date: 2/87
Page 22 of 23
(1987), the equations presented in the calcula-
tions subsections assume that the concentra-
tion of the analyte in solution has been cor-
rected for the reagent blank. The reagent
blank, composed of all the reagents in the
same quantities used for actual samples,
undergoes the same manipulations as actual
samples and therefore should reflect any
analyte contamination from the sample matrix
or analytical procedure. Specifically, the actual
(corrected) solution concentration is equal to
the analyte concentration in the sample solu-
tion minus the analyte concentration in the
reagent blank.
9.7 Data Reporting
The data forms used by the analytical
laboratory are provided in Appendix B. The
raw data are recorded on forms 115,116, 303b,
306, and 308. The pH, moisture, and particle
size analysis results are summarized on forms
103a and 103b. Data that are corrected both
for blanks and dilutions are summarized on the
200-series forms. Data are annotated by
using the data qualifiers listed in Table 9-4, if
applicable. Results should be reported to the
same number of decimal places as listed in
Table 9-6; however, no more than four signifi-
cant figures should be reported. Forms 109
through 114 contain quality control data. After
a form is completed, the laboratory manager
must sign it to indicate that he or she has
reviewed the data and that the samples were
analyzed exactly as described in the procedure.
All deviations from the analytical protocol
must be documented. All original raw data
such as data system printouts, chromato-
grams, notebook, individual data sheets, QC
charts, and standard preparation data should
be retained.
9.8 Evaluation of Quality
Control Data
Each laboratory will make a report by
telephone to the QA manager or other autho-
rized representatives, as directed. The objec-
tive of these reports is to keep the QA manag-
er informed of the status of the internal QC
and external QA checks in the laboratory in
order to identify and solve problems that may
arise. The reports also allow the QA manager
to obtain preliminary results for the blanks,
duplicates, and audit samples. Otherwise,
these data would not be available for QA/QC
checks until the data packages are received
from the laboratories. During the telephone
contact, the QA manager or designer records
all interaction in a bound logbook.
-------
Section 9
Revision 2
Date: 2787
Page 23 of 23
Table 9-6. U«t of Decimal-Place Rtportlng
Requirements
Parameter Number of Decimal Places
In Reported Results*
Moisture content
Particle size
PH
Total C
Inorganic C
Total N
Total S
CEC
Na'
1C
Mg»
Ca"
AT
Fe"
NO,'
SO,"
SO," adsorption
Exchangeable acidity
Specific surface
3
1
2
3
3
3
2
3
3
3
3
3
3
3
2
2
3
2
4
After each day of analysis at the contractor
laboratory, control charts are updated and new
control and warning limits are calculated. The
contractor QA chemist then performs a QC
audit in which all the pertinent data are re-
viewed. Any values that lie outside the control
or warning limits are checked to verify that
they are not the result of a transcription error.
If bias is indicated by seven successive points
on one side of the cumulative mean, analysis
is stopped and an emanation is sought.
Copies of the plots are given to the contractor
analytical laboratory supervisor and to each
analyst.
*Report to a maximum of four decimal plaeee.
-------
Section 10
Revision 2
Date: 2/87
Page 1 of 2
Section 10
Performance and System Audits
10.1 Soil Samples to Estimate
Precision
Three kinds of paired quality assurance
samples are included in each batch of soil
samples submitted to an analytical laboratory:
(1) field duplicates, (2) preparation duplicates,
and (3) audit samples.
One horizon per crew, per day is sam-
pled in duplicate as specified in Blume et al.
(1987). The field duplicate undergoes all
preparation steps in order to estimate variation
in sampling a horizon.
One sample per batch is chosen by the
preparation laboratory to be split into two
subsamples. The preparation duplicates are
included to estimate the range in physical and
chemical characteristics for splits of the sam-
ple material.
Two audit samples that are replicates
from a homogenized bulk sample are sent to
the analytical laboratory via the preparation
laboratory. The audit samples do not undergo
further processing at the preparation labora-
tory. These samples are double-blind QA
samples, i.e., the analytical laboratory does not
recognize an audit sample as a QA sample
and does not know its predetermined composi-
tion. The audit samples are used to assess
analytical within-batch precision and to esti-
mate interlaboratory bias. Appendix C pres-
ents the plan for laboratory audit samples.
10.2 Field Sampling On-Site
Evaluation
Each field sampling crew can expect at
least one on-site evaluation during the course
of the sampling effort. This is an on-site
inspection to review site selection, profile
description, sampling procedures, and QA
efforts. The questionnaire given in Appendix D
is used to assist in the evaluation.
The QA auditor conducts an in-depth
review of all field operations for compliance
with the sampling protocols. This includes,
but is not limited to: (1) interviewing the
sampling crew, (2) accompanying the sampling
crew during a sampling excursion, and (3)
writing a summary report with results, obser-
vations, and recommendations. If there are
any problems, the evaluator must attempt to
correct them by reference to or interpretation
of the sampling protocols after the daily sam-
pling has been completed. All problems are
brought to the attention of the QA manager at
EMSL-LV within two working days. The QA
manager is responsible for conveying any
major problems to the technical monitor or
technical director.
10.3 Preparation Laboratory
On-Site Evaluation
Each preparation laboratory can expect
a minimum of two on-site evaluations. The
first on-site evaluation is performed before
samples are received. The purpose of this
evaluation is to assess the facilities, including
refrigerated storage and areas for soil drying
and for sample processing, i.e., crushing,
sieving, and splitting. The questionnaire in
Appendix E is used to assist in the evaluation.
The auditor brings any problems to the atten-
tion of the laboratory manager. All obser-
vations are summarized in an evaluation report
that is submitted to the QA manager at EMSL-
LV.
The second on-site evaluation is con-
ducted about a third of the way through sam-
ple processing. After reviewing the previous
evaluation report, any changes since the first
on-site evaluation are noted on the question-
naire. Also, any problems identified must be
corrected and brought to the attention of the
QA manager. A summary report is written for
this and any additional on-site evaluations and
is submitted to the QA manager at EMSL-LV.
-------
Section 10
Revision 2
Date: 2/87
Page 2 of 2
10.4 Analytical Laboratory
On-Site Evaluation
Each analytical laboratory can expect a
minimum of two on-site evaluations. The first
on-site evaluation is performed afterihe labo-
ratory has analyzed successfully a set of pre-
award performance evaluation (PE) samples
for the contract-required parameters, or during
the PE sample analyses (see Appendix F). The
PE samples contain up to the maximum num-
ber of required analytes in the expected analyt-
ical ranges. The pre-award scoring sheet
given in Appendix G is used to score the PE
sample results. Grading emphasizes analytical
accuracy, but a substantial portion of the
grade depends on meeting the QA, report-
ing, and deliverable requirements. The EPA
QA manager or an authorized representative
conducts an in-depth review of all laboratory
functions that are pertinent to the analyses.
The questionnaire in Appendix H is used to
assist in the on-site laboratory evaluation. The
auditor brings any problems to the attention of
the laboratory manager for corrective action.
All observations are summarized in an evalua-
tion report that is submitted to the QA manag-
er at EMSL-LV.
The second on-site evaluation is con-
ducted approximately a third of the way
through sample analyses. The evaluation
questionnaire is completed with emphasis on
all changes since the first on-site evaluation.
During the second on-site evaluation, audit
sample data and QC data received to date are
reviewed. An evaluation report is written for
this and any additional on-site evaluations and
is submitted to the QA manager at EMSL-LV.
-------
Section 11
Acceptance Criteria
Section 11
Revision 2
Date: 2/87
Page 1 of 2
11.1 Audit Sample Results
Acceptance windows for single values
from audit samples are based on previous
interlaboratory analyses of the same sample
material by the same protocols. The objective
of creating windows is to predict intervals for
acceptable single future values based on a
sample mean (X) and sample standard devia-
tion (s) computed from n previously observed
values. The limits of the windows are deter-
mined by using a t-statistic (t).
t -
_Z_ is a Student's t
where:
Z is the standard normal variate,
having a normal distribution with a
mean of 0 and a variance of 1;
fj is a variable with a chi-square
distribution with r degrees of freedom,
and Z and /J are independent.
The observed values X,, Xj, X.,, X,, are
independent and have a normal distribution
with a population mean (/j) and variance (a2).
A (1 - a) prediction interval for a single future
value y is needed. Let X equal sample mean
and s equal sample standard deviation. It is
known that:
y _ N (p. a ') and X ~ N y, \ n.
Therefore
y-X
z - v-y ~ N(o.i)
eforey \
~N (o, a'1+^rjl.
= n-1
- n-1.
~ X1 (n-1) and
Substituting,
y-X
y-X
The upper and lower limits of the win-
dow can be formalized as follows:
5? + (t)(sL/1 + J- = upper limit of the window
T n
X - (t)(s)*/1 + J_ = lower limit of the window
The Student's t-value has n-1 degrees of
freedom. The t-value is for a two-tailed test
with a cumulative probability of 0.95, i.e., 2.5
percent probability on either side.
For predicting future values, wider win-
dows than the standard 95 percent confidence
interval about the mean are desirable. As the
number of observed values increases, more
variance occurs because of chance alone.
Initially, there may not be sufficient data
(n < 10) available to provide good interval
estimates. Arbitrary criteria may be used until
10 or more values are available. The windows
should be updated periodically as more data
are accumulated.
To detect outliers, a statistical test, e.g.,
Grubbs' test (Grubbs, 1969), is applied to the
data before interval estimation. The outliers
are excluded from the computation of the
windows.
Windows for matrix spike analysis re-
sults are computationally identical to those for
audit sample results.
-------
Section 11
Revision 2
Date: 2/87
Page 2 of 2
11.2 Replicate Analysis Results
Acceptance criteria for the relative stan-
dard deviation (RSD) are based on the upper
95th percentile of observed values of RSD.
Because RSD is affected by concentration,
these criteria are applied only when the mean
of the duplicate or triplicate analyses exceeds
the contract-required detection limit (CRDL) by
a factor of 10.
Arbitrary acceptance criteria may be used
until sufficient (at least 10) RSD values have
been observed.
values have been observed. It is recom-
mended that no outlier test be applied until the
distribution has been estimated.
11.3 Corrective Action
Laboratories which fail to meet the
acceptance criteria for analysis of audit sam-
ples, matrix spikes, or replicates are required
to repeat the analysis that produced the
questionable results. If results from the
second analysis are still unacceptable, further
corrective action must be initiated.
The distribution of RSD values cannot be
estimated accurately until sufficient RSD
-------
Section 12
Revision 2
Date: 2/87
Page 1 of 3
Sect/on 12
Data Management System
The purpose of the data base manage-
ment system is to assemble and store data
generated as part of the DDRP, to provide
basic reports of the survey results, to perform
simple statistical analyses, and to provide
data security. The relationship of data base
management to the overall soil survey is
shown in Figure 12-1.
All data sets are protected from unautho-
rized or accidental access by individual, sys-
tem, and file password protection.
The data are stored in three major data
sets: (1) a raw data set, (2) a verified data
set, and (3) a validated data set.
12.1 Raw Data Base
At ORNL, the Statistical Analysis System
(SAS) is used to enter the field data, prepara-
tion laboratory data, and analytical laboratory
data (analytical results and data qualifiers, see
Table 9-5) into the raw data base. These data
are also sent to the EMSL-LV QA staff for
concurrent data analysis. The SAS full-screen
editor procedure is used to provide gross error
checking as data are entered. All data are
entered into two separate data sets by two
different operators. For the DDRP data base,
a comparison program is used to compare the
two data sets and to identify any inconsisten-
cies. This double entry and comparison pro-
cess allows typographical errors to be identi-
fied and removed from the data base.
12.2 Verified Data Base
data are reviewed. The analytical data are
processed by an on-line quality assurance
system being developed by EMSL-LV QA staff.
Problems with the data are flagged as deemed
necessary by the QA staff. Data are examined
for reporting errors and may be modified in the
data base. Also, reanalysis may be requested.
Old data values are maintained in the raw
data base as a historical file.
In addition to the standard QA analysis,
various printouts are supplied to the QA man-
ager to point out intralaboratory or inter-
laboratory bias as well as discrepancies in
blanks, audits, or other QA/QC samples. The
overall outcome is a verified data base in
which all values are either qualified or replaced
with missing value codes. EMSL-LV coordi-
nates with sampling crews, preparation labora-
tories, and the contractor laboratories to make
all appropriate corrections in the data.
12.3 Validated Data Base
A computer printout of the verified data
base is sent to ERL-C for data validation. The
validation procedure consists of a final review
of all data for internal and regional consisten-
cy and uses all the QA/QC information avail-
able.
The validation process compares data
for a set of variables against a much narrower
range established from internal chemical
relationships and data from each sampling
class.
As the field and analytical laboratory
data are received by EMSL-LV QA group, all
-------
Section 12
Revision 2
Date: 2/87
Page 2 of 3
SOIL SAMPLING
PREPARATION LABORATORIES
ANALYTICAL LABORATORIES
DATA ENTRY
BY ORNL
BATCH REPORTS,
RANGE CHECKS
VERIFICATION
BY EMSL-LV QA
DATA EDITING
(FLAGGING)
SITE REPORTS,
MAPS
VALIDATION BY
ERL-C AND EMSL-LV
DATA EDITING WITH
FLAGGING OF
QUESTIONABLE DATA
REPORTS, MAPS
STATISTICS
PRELIMINARY
ANALYSIS
ACCESS,
DISTRIBUTION,
ANALYSES
s DATA TRACKING SYSTEM
Figure 12-1. D«U mancgtmtnt for the DDRP Soil Survty.
-------
Section 12
Revision 2
Date: 2/87
Page 3 of 3
The validation step incorporates soil
chemistry to identify intrasite sample inconsis-
tencies. Sample data are checked by examin-
ing relationships between paired data, such as
pH H20 versus pH CaCI2 and cation exchange
capacity versus specific surface. Samples
flagged as questionable are subjected to
further review. Intersite validation consists of
comparing profile data for a single pedon with
profile data for all pedons in the sampling
class. Data that contrast with nearby sites
can be flagged for more detailed review. Data
from analytical replicates, audits, and other
paired QA samples are also reviewed . The
validation process increases the integrity of
the data base by using a systems approach to
determine that data are reasonable. After the
validated data are transferred to the validated
data base, the data base will be released by
EPA and will be made available to all data
users.
-------
Section 13
Revision 2
Date: 2787
Page 1 of 2
Section 13
Review of Data
As the field, preparation laboratory, and
analytical laboratory data are received by
EMSL-LV QA staff, all data are reviewed as
described in the following subsections.
13.1 Field Data Review
Field data forms are reviewed by:
• Checking the accuracy of the ID num-
bers.
• Reviewing all profile descriptions and
associated data.
• Contacting SCS or referring to field
notes to correct any errors.
• Notifying ORNL if the data base is
affected by any changes.
• Recording all interactions with ORNL,
EPA, and SCS in a bound logbook.
13.2 Preparation Laboratory
Batch Assignment and
Data Review
Form 101 is reviewed by:
• Checking all sample codes against ID
numbers on the field data forms.
• Checking for inclusion of duplicates
and audit samples.
• Recording identity of audit samples.
• Checking analytical data.
• Contacting preparation laboratory or
referring to the preparation laboratory
logbook for Label A to correct any
errors.
• Notifying ORNL if the data base is
affected by any changes.
• Notifying contractor analytical labora-
tory and Sample Management Office
(SMO) if any changes affect sample
analysis or data reporting.
• Recording all interactions with prepa-
ration laboratories, ORNL, SMO, and
contractor analytical laboratories in a
bound logbook.
Form 102 (shipping form) is reviewed by:
• Recording date that form is received
from contractor analytical laboratory.
• Checking Form 102 against Form 101
to verify analytical laboratory name
and number of samples.
• Verifying that prepared rock fragments
were shipped if organic carbon is to
be determined.
• Calling contractor analytical laboratory
to discuss condition of samples upon
receipt, and date and time of receipt.
• Calling other involved parties to cor-
rect any problems.
• Recording all interactions in a bound
logbook.
13.3 Analytical Laboratory Data
Review
13.3.1 Communications
Frequent communications, i.e., two or
three contacts each week, are maintained with
each contractor analytical laboratory to obtain
current sample data and to discuss any prob-
lems that may occur during analyses. Data
-------
Section 13
Revision 2
Date: 2/87
Page 2 of 2
may be available via electronic transfer. Data
that are received verbally are recorded in a
bound logbook. These preliminary data are
reviewed for anomalies. If a problem is identi-
fied, the laboratory is notified. Corrective
action or reanalysis may be suggested. All
interactions with each laboratory are recorded
in a bound logbook.
Contractual issues are referred to the QA
manager and to the contract officer. Major
technical issues are referred to the QA manag-
er.
13.3.2 Preliminary Data Package
Review
Each data package is reviewed by:
• Reviewing cover letter.
• Completing Data Package Complete-
ness Checklist (given in Appendix I) to
review internal QC data, data com-
pleteness, and data qualifiers used.
• Notifying the contractor laboratory of
any major discrepancies and recording
corrective action.
13.3.3 Computer Review of
Analytical Data
The National Computer Center (NCC),
Research Triangle Park, North Carolina, re-
ceives a magnetic tape from ORNL The
magnetic tape, containing all analytical data,
is accessed as follows:
(1)Each magnetic tape received by the
NCC tape library is given a volume
serial number and a BIN number. A
BIN number indicates the physical
location of the tape.
(2)EMSL-LV QA computer support con-
tacts the NCC tape library to obtain
the volume serial number and the BIN
number. Upon request from EMSL-LV
QA staff, the tape is loaded.
The QA staff runs the data through
programs that check laboratory QC, paired QA
data, and the internal consistency of data.
These programs generate lists of data that are
exceptions to predetermined criteria. These
exceptions are subject to the scrutiny of the
QA staff. Corrective action for exceptions
includes requests that the contractor analytical
laboratory confirm the data or reanalyze the
samples for which the data are anomalous.
-------
Section 14
Revision 2
Date: 2/87
Page 1 of 9
Section 14
Data Verification
14.1 Verification of Field Data
14.1.1 Verification of Sampling
Class and Vegetation
Class
This verification involves using the list of
sampling classes and corresponding vegeta-
tion classes as supplied by ERL-C to identify
the appropriate sampling class and vegetation
class for the specific pedon. Each field data
form lists the watershed ID, random point,
sampling class, and aspect on the first line of
the location description and free form site
notes. This information is checked against the
information from ERL-C.
14.1.2 Review of the Field Data
Forms for Completeness
and Misnomers
Each field data form is reviewed for:
• Left and right justification of letters
and numbers.
• Correctness of code values and cod-
ing, e.g., coding 0 as 0 and not as 0
or misplacing decimals.
• Completeness: many forms lack com-
plete information for certain parame-
ters; parameters not listed in Blume et
al. (1987) and missing data are con-
sidered incomplete.
Reference information used in the review
includes (1) instructions for using the SCS-232
field data form, (2) coding values found on the
SCS-232 form (see Appendix A), (3) Soil Survey
Manual, (4) National Handbook of Plant
Names, and (5) Land Resource Regions and
Major Land Resource Areas of the Northeast
United States U.S. Department of Agriculturel
Soil Conservation Service ([USDA/SCS], 1985).
After problems have been identified, a
discrepancy form describing these problems
will be sent to the SCS field crew. The form
consists of:
• Tracking number to identify the specif-
ic SCS-232 field data form, watershed
ID number.
• Soil series name.
• Pedon sample number.
• Description of problem, i.e., discrepan-
cy or missing data.
• Old value, i.e., value thought to be
incorrect or question mark if value is
missing.
• New value, i.e., value supplied if possi-
ble or to be filled in by SCS field crew.
• Signature of SCS personnel to ac-
knowledge the discrepancy and
change.
The SCS field crew checks the discrepan-
cy form against the SCS-232 forms, fills in the
appropriate areas, and returns the discrepancy
form. The form is rechecked by EMSL-LV QA
staff and is used to edit the local working
copy of the raw data base (see Section 14.1.4).
Discrepancy forms are sent to field
crews after review of approximately 40 data
forms, i.e., weekly. Copies of the discrepancy
forms are filed at EMSL-LV.
14.1.3 Verification of Soil
Descriptive Parameters
This step in verification of each soil
parameter on the field data form depends on
the type of information needed for verification.
Some parameters must be checked against
logbooks or analytical laboratory data; other
-------
Section 14
Revision 2
Date: 2/87
Page 2 of 9
parameters require comparison against soil
taxonomic criteria; field-observed parameters
may not be possible to verify.
Verification of the field data is accom-
plished with a computer program designed to
check every parameter on the 232 form. The
checks include:
• Appropriate coding.
• Missing information.
• Field parameter versus field parame-
ter, e.g., texture modifier versus per-
cent rock fragments.
• Field parameter versus analytical
parameter, e.g., field pH versus labo-
ratory pH.
The last two checks are exception pro-
grams that examine internal data consistency.
Page 1 of 4 of SCS-232 Field Form
NOTE: The following parameters are
found in sequence on the field
data form.
A. Soil Series Name-Verification de-
scribed in Section 14.1.1.
B. Sample Number-Verification against
logbook.
C. Major Land Resource Areas (MLRA)-
Verification against MLRA map
(USDA/SCS, 1985).
D. Latitude and Longitude-Verification
against watershed latitude and longi-
tude information supplied by ERL-C.
E. Date-Verification against logbook; set
ID from preparation laboratory log-
book.
F. Slope
1. % - field-observed: coding and
completeness check.
2. Shape (SHP) - field-observed: cod-
ing and completeness check.
3. Local Physiographic Component
(GM) - field-observed: coding and
completeness check.
4. Aspect (ASP) - field-observed:
coding and completeness check.
5. Microrelief - field-observed: coding
and completeness check
a. Kind (K)
b. Variation (A)
c. Pattern (P)
d. Position (POS)
G. Physiography
1. Regional (RG) - coding and com-
pleteness check.
2. Local (LOG) - coding and complete-
ness check.
H. Pedon Classification - (all parameters
in this category). Verification based
on taxonomic description of soil
series.
I. Precipitation - field crews not required
to describe parameter.
J. Water Table
1. Depth - field-observed: coding and
completeness check.
2. Month - verification against date.
3. Kind (KD) - field-observed: coding
and completeness check K. Land
Use (LU) Verification against MLRA,
vegetation class, and vegetation
species.
L Stoniness Class-field-observed:
coding and completeness check.
M. Estimated Permeability (PM)-verifica-
tion against texture for each horizon.
-------
Section 14
Revision 2
Date: 2/87
Page 3 of 9
N. Soil Drainage Class (DR)-verification
against sampling class description.
O. Elevation Meters-verification against
U.S. Geological Survey soil topographi-
cal map, if necessary. Otherwise
coding and completeness check.
P. Parent Material
1. Degree of weathering or bedding
inclination (w) field-observed:
coding and completeness check.
2. Mode of accumulation or deposition
(M) coding and completeness
check.
3. Origin or source of parent materi-
als (orig) verification against sam-
pling class description.
Q. Temperature-parameter not required to
be described by field crew.
R. Moisture Regime (MST RGE)-coding
and completeness check.
S. Weather Station Number-parameter
not required to be described by field
crew.
T. Control Section-coding and complete-
ness check.
U. Erosion (ERWA)-parameter not re-
quired to be described by field crew.
V. Runoff (RNOF)-coding and complete-
ness check.
W. Diagnostic Features
1. Depth- ) should correspond to
2. Kind (KND)> horizon description and
) relative taxonomy
X. Flooding
1. Frequency -Afield-observed (usually
2. Duration j not filled in)
Y. Vegetation-verification against Nation-
al Handbook of Plant Names (see
Section 14.1.2, Item 4) and vegetation
class specified by ERL-C (see Section
14.1.1)3.
Z. Location Description and Freeform
Site Notes-verification for watershed
ID, random site, sampling class, and
aspect against information from ERL-
C; must be coded in first 17 spaces.
Pace 2 of 4 of SCS 232
A. Depth Upper/Lower-codtng and com-
pleteness check.
B. Horizon Designation-coding and com-
pleteness check.
C. Thickness-Average thickness should
correspond approximately with differ-
ence of upper and lower depth param-
eters.
D. Moist Color
1. Location - field-observed: coding
and completeness check.
2. Percentage (%) - field-observed:
coding and completeness check.
3. Color - field-observed: coding and
completeness check.
4. Texture - verification against ana-
lytical data.
5. Texture modifier - coding and com-
pleteness check.
Page 3 of 4 of SCS 232
A. Structure
1. Grade (GRD)
2. Size (SZ)-field observed: coding
and completeness check
3. Shape (SHP)
-------
Section 14
Revision 2
Date: 2/87
Page 4 of 9
B. Consistence-Field-observed: coding
and completeness check.
C. Mottles-Field-observed: coding and
completeness check.
D. Boundary-Field-observed: coding and
completeness check.
E. Field Measured Properties
1. Kind - verification against horizon
designation and texture.
2. Amount - pH value may be corre-
lated to analytical data.
3. Soil Water - field-observed: coding
and completeness check.
Page 4 of 4 of SCS 232
A. Roots
1. Quantity (QT)
2. Size (SZ) -
3. Location (LOG)
field-observed:
coding and
completeness
check
B. Pores-Parameter not described by field
crew.
C. Concentrations-Parameter not de-
scribed by field crew.
D. Rock Fragments
1. Kind - verification against parent
material origin.
2. Percentage (%) - verification
against texture class and texture
modifier.
3. Size (SZ) - verification against
texture modifier.
14.1.4 Methods
Outliers
Used to Treat
In this section, the term outlier refers to:
• Information identified through discrep-
ancy forms.
• Codes input incorrectly.
• Exception program outliers.
• Computer program outliers.
Discrepancy form outliers and input
errors are corrected and other outliers are
flagged (see Table 14-1) through an editing
program. Editing is done on a working copy
of the official raw data base supplied from
ORNL via NCC (see Section 13.3.3). All editing
changes are made to this data base, thereby
-------
Section 14
Revision 2
Date: 2/87
Page 5 of 9
Table 14-1. Fl«g« for the Verification of fUld data
AO • miating valua
BO - invalid coda
CO • alpha character In numeric field
DO • numeric character in alpha field
EO - correlation outlier
FO - value inappropriate for state
GO - missing value; with explanation
HO - miscellaneous flag, for
unique problems
protecting the official raw data base. Upon
entering the editing program, a subset of the
field data is keyed in by the sample number,
state, and county. This subset is copied into
a temporary working file for manual editing.
When editing of the work file is finished, the
manual editing system is exited. The edited
information and the original field data are sent
automatically to a transaction file. The trans-
action file is printed and reviewed at the end
of an editing session.
After the edits have been checked, the
local master data base is updated. All edited
information in the transaction file is applied to
the local master data base, replacing the
original data. This information also enters the
history file, i.e., the record of all transactions
made to the local master data base. After the
process of correcting the local master data
base is completed, the data base becomes the
verified master data base.
Copies of the verified data base and a
hard copy of the history file are sent to ORNL
ORNL compares the official raw data base
with the verified master data base. Any anom-
alies between the data bases should corre-
spond to the history file. After both data
bases are proofed by ORNL, the official raw
data tape is stored, and the official verified
data tape becomes available for the next user.
14.2 Verification of Physical
and Chemical Data
14.2.1 Exceptions Programs for
Internal Consistency of
Data
data for each sample. For each relationship it
is expected that approximately 10 percent of
the data will not comply with these relation-
ships. These anomalous data are examined
by a soil chemist who qualifies them or as-
signs appropriate flags (see Appendix M). The
following relationships are examined in qualify-
ing the data:
(1) Laboratory-determined pH
should relate as follows:
values
pH H20 > pH 0.002 M CaCI2 > pH 0.01
M CaCI2
CaCI2 solution masks the effect of
soluble salts in soils. Ca2* ions
displace H+ ions from exchange sites;
the H+ ion concentration in solution
increases, and the result is the
measurement of a lower pH.
(2) Field pH should be greater than labo-
ratory-determined pH. Field pH is not
available for all samples; however,
when field pH is available, this com-
parison is made. This relationship
occurs because laboratory samples
are dried during sample processing,
whereas field pH is determined on a
field-moist sample.
(3) Phosphate-extractable sulfate should
be greater than water extractable
sulfate.
Phosphate-extractable sulfate approxi-
mates the total adsorbed sulfate;
water-extractable sulfate approximates
that which readily enters soil solution.
Simple mathematical relationships are
used to examine the internal consistency of
-------
Section 14
Revision 2
Date: 2/87
Page 6 of 9
(4) Cation exchange capacity (CEC)
should relate as follows:
NH4OAc CEC > NH4CI CEC.
A higher CEC is measured by using a
buffered (pH 7) NH4OAc saturating solution to
determine CEC in an acid soil. With an in-
crease in pH, HT ions are displaced. This
creates more exchange sites for retention of
NH4+. The NH4CI saturating solution is
unbuffered; therefore, cation exchange takes
place at the soil pH, resulting in the measure-
ment of a lower CEC.
(5) Exchangeable cations should relate
as follows:
Ca
2+
Mg
2+
K+ > Na+
except in the presence of illitic clays
where:
Ca2+ > K+ > Mg2+ > Na+.
The first relationship occurs because of
the natural abundance of the cations and
because of their hydrated radii. Illitic clays
provide an exception because they are potas-
sium rich.
(6) Exchangeable acidity should relate as
follows:
BaCI2-TEA acidity > KCI acidity
The BaCI2 -TEA solution is buffered to a
pH of 8, and this results in measurement of
total potential acidity. KCI is a neutral salt;
therefore, values obtained are more represen-
tative of natural exchangeable acidity in field
soils.
(7) The summation of sand, silt, and clay
should equal 100 percent. Also, the
sand and silt fractions should sum
to equal total sand and silt.
(8) The field-determined particle-size
estimates should be approximately
equivalent to particle-size data
measured in the laboratory.
(9) Soil permeability estimates should
compare to particle-size data.
(10) Each SO4 adsorption isotherm, in
adherence to the Langmuir Equa-
tion, should be linear up to the
point of surface saturation.
(11) Total carbon (C) should be greater
than total nitrogen (N). The ratio of
C to N should fall within a known
range.
(12) A plot of CEC versus percent clay
should display a proportional
relationship reflecting the relation-
ship of CEC to the amount of clay.
(13) Specific surface versus SO4 adsorp-
tion, CEC, and exchangeable cat-
ions are proportional relationships.
An increase in specific surface
should show a corresponding
increase in the other parameters.
(14) The summation of exchangeable
acidity and exchangeable basic
cations should be approximately
equal to CEC. In soils, Ca?+, Mg2+,
Na+, K+, AI3+, and H+ are the pre-
dominant cations; therefore, the
summation should be approximately
equal to the CEC. Some variation
occurs because of organic chela-
tion and the presence of organic
cations.
14.2.2 Other Exceptions Programs
Exceptions programs also check labora-
tory QC and paired QA data against predeter-
mined criteria. These programs generate lists
of data that are examined by the QA staff.
Corrective action includes requests for confir-
mation of data or reanalyses of batches for
which data are outside the criteria (see Ap-
pendix M).
-------
Section 14
Revision 2
Date: 2/87
Page 7 of 9
14.2.3 Methods Used to Treat produce the verified master data base, as
Outliers described in Section 14.1.4.
Misreported data and data from reanaly- 14-3 Reporting Scheme
ses are edited as described in Section 14.1.4
for field data. Outliers generated by excep- Lists of flagged data are hard-copied
tions programs are flagged according to and filed. Progress and major problems are
category (see Table 14-2). The edited files are reported to the EPA technical monitor at
applied to the local master data base to EMSL-LV.
Table 14-2. Flag* for the Verification of Analytical Data
Miscellaneous
AO* Value missing
Generated by Appropriate Blank Exception Program
B3* Internal (laboratory) calibration or reagent blanks are >2x CRDL and contribute >50% to the sample
concentrations in the batch.
B4" Potential negative sample bias based on internal (laboratory) blank data.
B5" Calibration blank >1.05 x reagent blank.
Generated by Duplicate Precision Exception Program
01** Field duplicate precision exceeded the maximum expected percent relative standard deviation (%RSD), and
either the routine or the duplicate value was >.10 x CRDL.
D2** Field duplicate precision exceeded the maximum expected %RSD, and both the routine and the duplicate
sample concentrations were >10 x CROL.
D3** Internal (laboratory) replicate precision exceeded the maximum contract required %RSD, and either the
routine or the duplicate sample concentration was >10 x CRDL
D4** Internal (laboratory) replicate precision exceeded the maximum contract required %RSD, and both the
routine and duplicate sample concentrations were >.10 x CRDL.
D5** Preparation duplicate precision exceeded the maximum expected %RSD, and either the routine or the
duplicate value was >.10 x CRDL.
D6** Preparation duplicate precision exceeded the maximum expected %RSD, and both the routine and the
duplicate sample concentrations were >10 x CRDL.
D7** Audit duplicate precision exceeded the maximum expected %RSD, and either of the audit sample
concentrations was >10 x CRDL.
08** Audit duplicate precision exceeded the maximum expected %RSD, and both audit pair concentrations were
>10 x CRDL
Generated for Known Relationships of Sulfur Isotherms
KO** Elemental parameter out of range; used for total C, N, and S only.
K1** Organic soil (total C 20-60%) and SO, • H,0 > 1.05 x SO, • POt.
K2** Mineral soil (total C 0-20%) and SO, - H,O > 1.05 x SO, - PO,.
(continued)
-------
Section 14
Revision 2
Date: 2/87
Page 8 of 9
Table 14-2. (Continued)
K3** Organic soil: 1,000 x Total S < SO. - PO. or SO, - H,O.
K4** Mineral soil: 3,000 x Total S < SO, - PO. or SO. - H,0.
Generated bv Detection Limit Exception Program
L1* Instrumental detection limit (IDL) exceeded contract required detection limit (CRDL) and sample
concentration was <10 x CRDL
Miscellaneous
MO* Value was obtained by using a method that Is unacceptable according to the contract.
D8** Audit duplicate precision exceeded the maximum expected %RSD, and both audit pair concentrations
were >10 x CRDL
Generated for Known Relationships of Sulfur Isotherms
KO** Elemental parameter out of range; used for total C, N, and S only.
K1** Organic soil (total C 20-60%) and SO. - H,0 > 1.05 x SO. - PO..
K2** Mineral soil (total C 0-20%) and SO. - H,0 > 1.05 x SO. - PO..
K3** Organic soil: 1,000 x Total S < SO. - PO. or SO. - H,0.
K4** Mineral soil: 3,000 x Total S < SO. - PO. or SO, - H,0.
Generated bv Detection Limit Exception Program
L1* Instrumental detection limit (IDL) exceeded contract required detection limit (CRDL) and sample
concentration was <10 x CRDL
Miscellaneous
MO* Value was obtained by using a method that is unacceptable according to the contract.
Generated bv Audit Check Program
NO** Audit sample value exceeded upper control limit.
N1** Audit sample value was below lower control limit.
N2** Audit sample value exceeded control limits; audit sample preparation procedure is suspect.
Generated bv QCCS Exception Program(s)
Q1** Quality control calibration sample (QCCS) was above contractual criteria.
Q2** QCCS was below contractual criteria.
Q3** Insufficient number of QCCSs were measured.
04** Detection limit QCCS was not 3 x CRDL and measured detection limit (DL) QCCS value was not within 20%
of the theoretical concentration.
Generated bv Matrix Spike Program
S1** Percent recovery of matrix spike was above contractual criteria (100115%).
S2** Percent recovery of matrix spike was below contractual criteria (100115%).
(continued)
-------
Section 14
Revision 2
Date: 2/87
Page 9 of 9
Table 14-2. (Continued)
Miscellaneous
WO* Air dry sample weight was not within contractual requirement.
Miscellaneous (flagged data not to be included In any statistical analyses)
XO* Invalid biA confirmed data based on QA/QC data review.
X1* Invalid b\A confirmed data - potential gross contamination of sample or parameter.
X2* Invalid ^\A confirmed data - potential sample switch.
* Sample Flag: Flag the affected parameter for the affected samples only.
** Parameter Flag: Flag the affected parameter for ALL samples in the batch (the assumption is that QA/QC
represents all samples in the batch).
-------
Section 15
Revision 2
Date: 2/87
Page 1 of 10
Section 15
Quality Assurance Plan for Mineralogy
15.1 Introduction
Mineralogical analyses are performed on
a subset of soil horizons studied during the
DDRP soil survey. The methods used for
mineralogical analyses include X-ray diffraction
spectrometry, wavelength-dispersive X-ray
spectrometry, and scanning electron miscro-
scopy/energy-dispersive X-ray spectrometry
(Cappo et al., 1987). To meet requirements for
data precision, accuracy, representativeness,
and completeness, specialized QA/QC proce-
dures are presented for use with these analyti-
cal methods.
15.2 Project Description
ERL-C designated a subset of the soil
samples for mineralogical analysis. The spe-
cific goals of the mineralogical study include:
• Identifying and quantifying the clay
minerals present in the soils.
• Identifying and quantifying the other
minerals present in the soils.
• Characterizing the chemistry of the
whole sample and of the clay fraction.
• Assessing the variability of the miner-
alogical and chemical characteristics.
• Establishing the chemical contribution
that mineral weathering makes to the
soil.
• Assessing the effect that clay content
and heavy-mineral content have on the
acid-neutralizing capacity of the soil.
15.3 Project Organization
Section 3.0 addresses project organiza-
tion.
15.4 Quality Assurance
Objectives
15.4.1 So/I Sampling
Section 4.1 addresses soil sampling.
15.4.2 Sample Preparation
15.4.2.1 Precision and Accuracy-
After processing, i.e., air-drying, disaggre-
gating, sieving, and homogenization, the prepa-
ration laboratory uses a Jones-type riffle
splitter to prepare 500-g subsamples from the
routine soil samples and special interest
watershed (SIW) samples designated by ERL-
C. Comparison of physical and chemical data
for these duplicates allows evaluation of the
subsampling procedure.
15.4.2.2 Representativeness-
After homogenization as described in
Section 4.2.2, each subsample is reduced to a
500-g aliquot by successive passes through a
Jones-type riffle splitter. This procedure main-
tains the representativeness of the sample.
15.4.2.3 Completeness-
Samples from mineral soil horizons
designated by ERL-C are analyzed for mineral-
ogy. Sample batches sent to each mineralogi-
cal laboratory include 23 percent QA/QC sam-
ples for the routine air-dry soil samples and
for the SIW samples. Each sample batch
consists of 20 routine or SIW samples, 3
duplicates, and 3 audit samples. One audit
sample in each batch is a synthetic sample.
-------
Section 15
Revision 2
Date: 2/87
Page 2 of 10
15.4.2.4 Comparability-
All preparation laboratories process bulk
samples according to protocols documented in
Bartz et al. (1987). Strict adherence to proto-
cols is required to ensure comparability among
preparation laboratories.
15.4.3 Laboratory Analysis
15.4.3.1 Precision and Accuracy-
The data quality objectives (DQOs) for
precision and accuracy of the analyses are
presented in Table 15-1. The structure of Table
15-1 is as follows:
Reporting Units - specifies the units in
which the laboratory data should be reported.
Reporting format - specified the signifi-
cant figures to which the data should be re-
ported.
Expected Range - specifies the range of
values expected to occur naturally in the soil
sampled, independent of measurement error.
Lower Reporting Limit - this value has
been extrapolated to that of the reporting unit;
if the sample values are lower than stated, the
"limit of reproducibility" is approached.
Table 16-1. Mlneraloglcal Data Quality Objective
Reported
Parameter Unit
1. Minerals
In <2-mm
fraction %
2. Minerals
<0.002-mm
fraction %
3. Reference
Intensity
Ratios D
4. Light
Minerals wt %
5. Heavy
Minerals wt %
6. Clay
Minerals wt %
7. Morpho- NA
logical
features
Wavelenath-disoersive and
Lower
Reported Expected Reporting
Format Range Limit
±1%
±1%
±0.01
units
±0.1%
±0.1%
±0.1%
Written
descrip-
tion with
photograph
Enerav-dlsoersive X-rav
8. Na %Na,0 ±0.1%
9. Mg %MgO ±0.1%
10. Ca %CaO ±0.1%
0-100%
0-100%
10,000 cps
0-80%
0-20%
0-100%
NA
Fluorescence
0-10%
0-5%
0-5%
2%
2%
0.0%
NA
NA
NA
NA
0.6%
1.0%
1.0%
Precision
at Lower
Limit
±0.1%
±0.1%
0.1%
NA
NA
NA
NA
1.0%
1.0%
1.0%
Precision
at Upper
Limit
±0.1%
±0.1%
0.1%
NA
NA
NA
NA
1.0%
1.0%
1.0%
D - Dimensionless number
NA - Not applicable
(continued)
-------
Section 15
Revision 2
Date: 2/87
Page 3 of 10
Tabla 15-1 (Continued)
Parameter
11. Al
12.81
13. P
14. Cl
15. K
16. Tl
17. Cr
18. Mn
19. Fe*
20. Co
21. Nl
22. Cu
23.Zn
24. Rb
28. Sr
26. Ba
27. La
28. Ca
29. Pb
30.Th
31. U
32. Zr
33.3
Reported Reported Expected
Unit Format Range
%AI,O,
%8IO,
ppm P.O,
ppm
%k,0
%T10,
ppm
ppm MnO,
*F«,0,
ppm
ppm
ppm
ppm
ppm
ppmSrO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
±0.1% 0-8%
±0.1% 0-20%
±1 ppm <1%
±1 ppm <1%
±0.1% 0-10%
±0.1% <1%
±1 ppm <1%
±1 ppm <1%
±0.1% 0-20%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
±1 ppm <1%
Lower
Reporting
Limit
1.0%
4.0%
100 ppm
120 ppm
0.8%
0.1%
400 ppm
300 ppm
0.6%
50 ppm
50 ppm
50 ppm
50 ppm
30 ppm
50 ppm
50 ppm
200 ppm
200 ppm
40 ppm
40 ppm
40 ppm
200 ppm
320 ppm
Precision
at Lower
Limit
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
Precision
at Upper
Limit
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
1.0%
*Fe represents both +2 and +3 oxidation atataa of Iron and is raportad aa %Fa,0,.
Precision at the Lower Limit • serves as
a guideline to define the acceptable absolute
percent standard deviation beyond which the
analytical reproducibility for low concentration
samples is questionable and often not attain-
able.
Precision at the Upper Limit • serves as
a guideline to define the acceptable percent
relative standard deviation beyond which the
analytical reproduclbilty for high concentration
samples la questionable.
15.4,3.2 Representativeness-
Section 4.3.2 addresses representative-
ness.
15.4.3.3 Completeness
Section 4.3.3 addresses completeness.
15.4.3.4 Comparability
Section 4.3.4 addresses comparability.
15.5 Strategy of Sample
Selection for Mlneraloglcal
Analysis
The strategy used to select specific
watersheds and sampling sites is described in
Section 5.0. This section details the sslsctlon
of a subsample of soil horizons for mlneralogi-
cal analysis from all horizons samplsd.
15.5.1 Constraints
A dBase III file Is used to index the
pedons sampled Into sampling classee, e.g.,
E2, and within each sampling class by lake ID,
e.g., 1A1-012. Histic soils, I.e., sampling
classes H1, H2, and H3, are not candidates for
-------
Section 15
Revision 2
Date: 2/87
Page 4 of 10
mineralogical analyses because they do not
have a significant mineral component; there-
fore, samples for mineralogical analyses are
selected randomly from the remaining pedons
within the sampling classes.
For the routine and special interest wa-
tersheds, samples were selected in pairs from
each mineral sampling class; one sample is
selected from the most weathered mineral
horizon, and one is selected from the least
weathered mineral horizon within a pedon.
Additional pairs of samples are selected from
the E2,12,133, S12, and 816 sampling classes.
The 133 sampling class (Inceptisol order)
represents the largest land surface area
studied, and the S12 sampling class (Spodosol
order) represents the next largest land area
studied. Additional mineralogical samples are
chosen from the E2, 12, and S16 sampling
classes because these classes are thought to
be regionally representative of the mineral soil
orders mapped.
For quality control, 15 percent of the
samples are collected in duplicate. These
duplicate samples are selected randomly.
15.5.2 Limitations to Selection
Criteria
The following situations disqualify a
specific horizon as a choice for mineralogical
analyses:
• LJthological discontinuity - A litholpgical
discontinuity within a pedon indicates
that the upper mineral horizons were
developed from a parent material other
than the one present in the C horizon.
In this situation, the mineralogical rela-
tionship between the upper horizons and
the C horizon is ambiguous. If a pedon
is disqualified for this reason, the selec-
tion procedure is repeated until a suit-
able pedon is selected.
• Horizon not sampled - Within a pedon, a
horizon described on the field data form
and assigned a sample code may not be
sampled if the quantity of soil is insuffi-
cient. When a pedon containing an
unsampled horizon is chosen randomly for
mineralogical analyses, the selection procedure
is repeated until a qualifying pedon is selected.
If a sampling class contains pedons
that have only one mineral horizon, it is diffi-
cult to study the extent of mineral weathering.
Therefore, rather than selecting paired samples
from the same pedon, two different pedons
are selected randomly from the sampling
class.
15.5.3 Selection Procedure
A random number, X was generated on
a Hewlett Packard-15C calculator, where 0 < X
< 1. Next, X was multiplied by the number of
pedons, N, within the specific sampling class.
The decimal portion of the resulting number
was truncated to give an integer. To this
integer, one (1) was added to result in a
random number, i, which ranged from one (1)
to N. Counting from the first pedon in each
indexed sampling class, the ith pedon was
selected for mineralogical analyses.
The procedure was repeated until one
unique pedon was selected from each of the
eligible sampling classes. For sampling
classes E2, 12, 133, S12, and S16, the proce-
dure was repeated to select a total of four
unique pedons from each sampling class.
Fifteen duplicate samples were chosen
from the first fifteen paired samples by the
toss of a coin. From each pair, either the
most weathered or the least weathered miner-
al horizon was selected as a duplicate sample.
This selection procedure was repeated
to select mineralogical samples from the spe-
cial interest watersheds.
15.6 Sampling Internal Quality
Control
Sampling internal quality control is
detailed in Section 7.0.
15.7 Preparation Laboratory
Internal Quality Control
-------
Section 15
Revision 2
Date: 2/87
Page 5 of 10
Preparation laboratory internal quality con-
trol is discussed in detail in Section 8.0.
One audit sample per batch is synthetic. It
is comprised of separate, naturally occurring
minerals which have been combined in known
weights. The other two audit samples are
taken from the audit samples prepared from
the C, Bs, and Bw horizons.
The preparation laboratory splits a 500-g
aliquot from each bulk soil sample. This is
stored in a 500-mL high-density polyethylene
bottle for shipment to EMSL-LV. EMSL-LV
prepares the sample batches and ships the
batches to the mineralogical laboratory. A
mineralogical batch of 26 samples consists of
20 routine or SIW samples, 3 duplicates, and
3 audit samples.
15.8 Laboratory Procedures
Analytical and mineralogical procedures are
detailed in Cappo et al. (1987). Table 15-2
summarizes the parameters determined and
the corresponding analytical techniques.
15.9 Mineralogical Laboratory
Internal Quality Control
15.9.1 Sample Receipt
Section 9.0 addresses sample receipt and
laboratory documentation for quality control.
15.9.2 X-ray Diffraction
Spectrometry
15.9.2.1 Sample Preparation and
Analysis-
Each sample must have a uniform
particle size (less than or equal to 0.002 mm)
prior to analysis to reduce the matrix adsorp-
tion effect. A titanium carbide ring-and-puck
pulverizer is recommended for initial particle-
size reduction to about 0.040 mm. For the
final particle-size reduction to £0.002 mm, an
automated mortar and pestle with the addition
of acetone is required. For the first five sam-
ples of the first batch, a check on the particle-
size distribution of the prepared sample is
required. Each batch of samples including a
duplicate sample is prepared by the same
technician.
15.9.2.2 Initial Alignment and
Continuing Calibration-
An initial alignment is performed with
National Bureau of Standards (NBS) standard
reference material (SRM) number 640A silicon
powder as required in the analytical method.
As a part of an on-going check on the align-
ment and intensity of the X-ray tube, the
silicon powder calibration standard is X-rayed
after half the samples are X-rayed and after
the last sample has been X-rayed. All three
patterns are included in the data package.
Table 15-2. Mlneraloglcal Parameters and Corresponding Analytical Techniques
Parameter
Method
Mineralogy of <2-mm and <0.002 mm
fractions
Elemental analysis of bulk sample and
of clay fraction
Mineralogy of heavy mineral fraction
Morphological features of samples
X-ray diffraction spectrometry
Wavelength-dispersive X-ray
spectrometery
Scanning electron microscopy/
energy dispersive X-ray
spectrometry
Scanning electron microscopy/
energy dispersive X-ray
spectrometry
-------
Section 15
Revision 2
Date: 2/87
Page 6 of 10
15.9.2.3 Instrumental Requirements-
Copper K,, radiation is required for these
analyses. The goniometer speed is determined
by the intensity of the X-rays generated and is
dependent upon the brand and age of the
diffractometer. Refer to Cappo et al. (1987) for
the requirements. The patterns are stored
digitally in the computer until they are printed
for the data package.
15.9.2.4 Determination of the
Reference Intensity Ratios-
Each diffractometer yields slightly different
patterns and reflection intensities. To estab-
lish the reference intensity ratios for the exter-
nal standard, pure corundum is mixed with
quartz, albite, orthoclase, hornblende,
montmorillonite, illite, and kaolinite in equal
amounts. This corundum reference standard
is X-rayed, the area under the strongest peak
of each mineral is integrated, and the refer-
ence intensity ratios are computed. As part of
the internal QC, the corundum-reference stan-
dard must be X-rayed after every 60 samples
for the <2-mm and <0.002-mm randomly
oriented powder mounts only. The calculation
of the reference intensity ratios is based on
the most recent analysis of the standard.
15.9.2.5 Data Reporting-
All required X-ray diffraction (XRD) patterns
are included with the data package. Each
pattern is indexed. Indexing includes marking
the °2Q in 1° increments, marking the °20 of
the starting and ending points of the pattern,
and labeling each peak with a °20 number, the
equivalent angstrom units, the mineral name,
and the number of the Joint Committee on
Powder Diffraction Standards (JCPDS) card
used to identify each mineral. On each pat-
tern, the sample number, size fraction, type of
mount (i.e., oriented or randomly oriented),
treatments, date of analysis, goniometer
speed, scale, and the millivolt (mV), milliam-
pere (mA), and time constant settings are
recorded.
15.9.3 Wavelength-dispersive
X-ray Spectrometry
15.9.3.1 Sample Preparation and
Analysis-
The <2-mm fraction and the <0.002-mm
fraction are palletized and analyzed as sepa-
rate samples. Half-batch lots are analyzed if
the X-ray fluorescence (XRF) carousel does not
accommodate a full batch of samples.
15.9.3.2 Background Signal
Corrections-
Background signals are determined and
subtracted by software developed at Oregon
State University. For each fixed channel, the
dependence of the background signal on the
average atomic number, Z, of the sample
matrix is established from measurements of 30
samples. These consist of pure-element
oxides, salts, and mixtures of salts and oxides,
which represent a Z range from 10 to 25. This
range accurately represents the Z range ex-
pected in naturally occurring samples such as
soils, rocks, and ocean sediments. The mea-
sured background signals (Bpeak) for the fixed
channel are related to measurements of the
scattered continuum (Bcont) obtained at one of
several 20° angles.
"B
cont
Bpeak
Plots of k versus Bcont permit calcula-
tion of k if Bcont is known. For routine sample
measurements, Bcont is measured, then the
software calculates k for each fixed channel.
The background is subtracted automatically
because Bpeak = k Bcont.
15.9.3.3 Spectral Interferences-
Spectral interferences are greatly mini-
mized through the inherently high resolution of
the wavelength-dispersive XRF. Some peak
overlaps do occur, however. For each overlap
situation, standards containing a fixed concen-
tration of analyte and a varying concentration
of the interfering element are prepared and
-------
Section 15
Revision 2
Date: 2/87
Page 7 of 10
analyzed. The appropriate functional relation-
ships are developed to permit software to
predict and subtract the contribution of an
interfering element to the measured analyte
signal.
15.9.3.4 Corrections for Interelement
Effects-
Interelement effects are dealt with through
software similar to that developed by Criss'
Software, Inc. The software is used to con-
vert from measured X-ray fluorescence line
intensities to chemical composition. The
software uses measured net intensities from
standards to establish a set of theoretical and
empirical coefficients that fit the concentration
versus intensity relationships over the range of
compositions represented by the standards.
15.9.3.5 Initial Calibration-
A suite of at least 25 certified standard rock
and sediment samples is analyzed by XRF,
according to the same measurement parame-
ters that are used for routine samples. Back-
ground signals are subtracted, and possible
spectral interferences are corrected for as
described in Section 15.10.3.2 and Section
15.10.3.3. Software described in Section
15.10.3.4 is used to establish data files which
contain the calibration information required to
convert the measured net intensities from
routine samples to elemental concentrations.
The calibration of the XRF using the software
requires entering the known elemental concen-
trations for the standards and their measured
net intensities. The measured intensities for
the standards may be scaled in any appropri-
ate manner as long as the scaling is applied
consistently. To ensure that the calibration is
not affected by differences in instrument
response due to such factors as replacement
of a detector, changing of a tank of detector
gas, or long-term drift, all sample and stan-
dard net element signals are divided by the
corresponding monitor net element signal. A
monitor sample is measured several times
during the analysis of each suite of samples,
and the same monitor sample is used for all
sample and standard runs. The instrument is
calibrated in terms of signal ratios.
15.9.3.6 Quality Control Calibration
Standards-
QCCSs are rock standards certified by
the United States Geological Survey (USGS).
The USGS standards are obtained already
ground, and the analyst at the contractor
laboratory pelletizes and analyzes the stan-
dards. Spectra are stored digitally for cross-
referencing by the software.
15.9.3.7 Dispersion Crystals-
The manufacturer sets the dispersion
crystals in the spectrometer for the simulta-
neous analysis of 25 elements. There are
three adjustable spectrometers available for
sequential analysis of elements that are not
among the 25 analyzed in the simultaneous
mode.
15.9.3.8 X-ray Target-
The manufacturer provides a rhodium
target in the X-ray tube.
15.9.3.9 Acquisition-
Spectral acquisition is 300 seconds.
15.9.3.10 Duplicate Sample Analysis-
Duplicate analysis is performed on a
separate portion of each thirteenth routine
sample.
15.9.3.11 Continuing Sample
Analysis-
A monitor standard is included in the
sample set. The monitor standard measures
instrument performance and must be analyzed
three times or more during the analysis of
each set of samples; the check standard is
treated as a normal sample so that its mea-
sured concentrations may be checked after
each set of samples has been analyzed. The
data is stored digitally for later printing.
-------
Section 15
Revision 2
Date: 2/87
Page 8 of 10
15.9.3.12 Instrumental Detection
Limit-
The instrumental detection limit is estab-
lished for each element. The concentration at
the detection limit, CL, is defined as that
amount of analyte which gives a net line
intensity equal to three times the square root
of the background intensity for a specified
counting time.
15.9.3.13 Data Reporting-
Results obtained from each kind of analysis
are recorded on the data forms in Appendix J.
After a sample is analyzed completely, the
results are summarized on the summary data
forms and are annotated by the data qualifiers
listed in Table 9.5, if applicable. Results should
be reported to the number of decimal places in
the current instrumental detection limit to a
maximum of three significant figures. The
laboratory manager must sign each completed
form to indicate that he or she has reviewed
the data and that the samples were analyzed
exactly as described in the protocol. Any
deviations from protocol require authorization
of the QA manager prior to sample analysis.
15.9.4 Scanning Electron Micro-
scopy/Energy-Dispersive
X-ray Spectrometry
(SEM/EDXRF)
15.9.4.1 Sample Preparation and
Analysis-
For this method, the light and heavy miner-
als of the very fine sand fraction (0.105-0.053
mm) and the clay fraction (less than or equal
to 0.002 mm) are studied. These procedures
are described in Cappo et al. (1987).
15.9.4.2 Quality Assurance Objectives
for Energy-Dispersive X-ray
Anaiysis-
15.9.4.2.1 Precision- Precision must be within
2 percent relative standard deviation when not
limited by counting statistics. Precision is
assessed by computing the standard deviation
of measurements from the QC calibration
standard. Individual standard deviations are
computed for each element in the standard.
An overall value is computed as the mean and
individual standard deviation.
15.9.4.2.2 Accuracy- Accuracy must be within
5 percent of true concentration when not
limited by counting statistics. As elemental
concentrations approach the detection limits,
precision and accuracy become poorer be-
cause of the effect of counting statistics.
15.9.4.2.3 Completeness - All samples sub-
mitted are analyzed. Data completeness is
computed by the following equation:
completeness, % = (100)
Number samples analyzed
Number samples received
15.9.4.2.4 Representativeness - The analysis
area is an elliptical spot about 10 by 12 mm
near the center of the pellet.
15.9.4.3 Calibration Procedures and
Frequency-
The instrument is calibrated with NBS-
certified or USGS-certified standard reference
materials. For each XRF analytical batch, a
multielement QC calibration standard is ana-
lyzed. Measured concentrations of the QC
calibration standard are compared with actual
concentrations. If the results show a trend or
drift, recalibration is required. The instrument
generally maintains calibration stability for 3 to
4 months.
15.9.4.4 Energy Dispersive X-ray
Fluorescence (XRF) Analyzer-
Atoms in the sample are excited from
their ground state to higher energy levels by
radiation from an X-ray tube. These excited
atoms emit X-rays of discrete energies as they
return to their normal ground-state energy
level. The energy of these X-rays is character-
istic of the emitting element and is used to
identify the element qualitatively. The number
of observed X-rays, which is proportional to
the number of atoms, is used to determine
-------
Section 15
Revision 2
Date: 2/87
Page 9 of 10
quantitatively the concentration of a specific
element through a direct comparison (by the
software) with certified reference standards.
There are potential spectral interferences
with the energy dispersive (ED) XRF method
because of its low resolution relative to the
number and spacing of possible X-ray lines.
Correction factors are determined by analyzing
single-element standards and by quantifying
their interference with other elements. Sam-
ples exhibiting chemical composition uncharac-
teristic of normal samples may require addi-
tional corrections. The software automatically
makes all the calculations and corrections.
15.9.4.5 Data Reduction, Validation,
and Reporting-
For each element measured, data in units of
ppm or percent are processed at the time of
analysis. These calculations are an integral
part of the analytical software. Results are
recorded in both floppy disk and hardcopy
formats. In addition, the raw spectra are
saved on floppy disk.
15.9.4.6 Internal Quality Control
A multielement standard is analyzed after
every batch of 15 samples. Results of that
analysis are compared with true concentra-
tions. If the deviation is greater than 2 per-
cent, all samples of that batch must be reana-
lyzed.
15.9.4.7 Preventive Maintenance-
The Si(Li) detector is cooled with liquid
nitrogen by filling the Dewar flask every week.
Routine cleaning and maintenance is perform-
ed semiannually.
15.10 Acceptance Criteria
The acceptance criterion for the relative
standard deviation (RSD) of duplicate sample
results is based on the upper 95th percentile
of observed values of RSD. Because the RSD
is affected by concentration, this criterion is
applied only when the mean of the duplicate
analyses exceeds the contract-required detec-
tion limit by a factor of 10. Arbitrary accep-
tance criteria are used until sufficient (at least
20) RSD values have been observed. No
outlier test is applied to the RSD values prior
to estimating the upper 95th percentile.
15.11 Data Management System
Section 12.0 describes the data man-
agement system.
15.12 Performance and System
Audits
15.12.1 QA/QC Samples
Reference standards are USGS-certified
rock samples for the XRF methods. Micro-
probe standards and the corundum used in the
semiquantitative X-ray diffraction (SQXRD)
method are certified by the manufacturers.
15.12.2 Laboratory On-Site
Evaluations
Each mineralogical laboratory can
expect two on-site evaluations. A QA repre-
sentative makes the first on-site evaluation
before analysis begins and makes another
during analysis. The questionnaire in Appendix
K is completed during this evaluation.
15.13 Review of Mineralogical
Data
15.13.1 Communications
Section 13.3.1 addresses communica-
tions.
15.13.2 Preliminary Data Package
Review
Each sample data package is reviewed
as described below:
-------
Section 15
Revision 2
Date: 2/87
Page 10 of 10
• Log sample data package into master
tracking notebook and indicate in note-
book if data package arrived late.
• Review cover letter.
• Complete Data Package Completeness
Checklist (given in Appendix L) to review
internal QC data, data completeness,
and data qualifiers used.
• Notify the contractor laboratory of any
major discrepancies, and record correc-
tive action.
15.13.3 Quality Assurance Reports
to Management
Results of precision, accuracy, and com-
pleteness are included in the final summary
report. Also included Is a discussion of data
quality and of all specific deviations from
protocol and from the QA plan.
15.14 Data Verification
The data package is reviewed for complete-
ness of the required patterns. The XRD pat-
terns from the routine samples are reviewed
for completeness of the required indexing
information. Each mineral in the pattern is
compared to the duplicates, audit samples,
and JCPDS card file that is the accepted
reference standard used to identify the mineral
for the qualitative portion of the SQXRD data
verification. Reference intensity ratios (RIR)
are checked against the corundum standard
for the quantitative portion of the SQXRD data
verification. The percent clay data from the
SQXRD analysis along with the chemical
composition (XRF), cation exchange capacity,
and specific surface data are used in a simul-
taneous linear equation clay analysis (SLECA)
computer program which refines the clay data.
The elemental analysis data for the
soils are reviewed for completeness as de-
scribed in Cappo et al. (1987). The elemental
data are compared against the duplicates,
audit sample, and reference standard data.
The SEM/EDXRF pictures and elemental
data are reviewed for completeness as de-
scribed in Cappo et al. (1987). The pictures
are reviewed and are compared with the
minerals identified by SQXRD and with the
elemental compositions identified by the
EDXRF analyses. The EDXRF elemental data
are compared with the data for the reference
standards.
-------
Section 16
Revision 2
Date: 2/87
Page 1 of 2
Section 16
References
Bartz, J. K., D. S. Coffey, and L J. Blume. 1987. Preparation Laboratory Manual for the
Direct/Delayed Response Project Soil Survey. U.S. Environmental Protection Agency, Las
Vegas, Nevada. Appendix A In: Direct/Delayed Response Project Southern Blue Ridge Province
Field Sampling Report: Vol. II Sample Preparation. EPA/600/4-87/041. U.S. Environmental
Protection Agency, Las Vegas, Nevada. 41 pp.
Blume, L J., M. L Papp, K. A. Cappo, J. K. Bartz, D. S. Coffey. 1987 Soil Sampling Manual for the
Direct/Delayed Response Project Soil Survey. U.S. Environmental Protection Agency, Las Vegas,
Nevada. Appendix A IQ: Direct/Delayed Response Project Southern Blue Ridge Province Field
Sampling Report: Vol. I Field Sampling. EPA/600/4-87/041. U.S. Environmental Protection
Agency, Las Vegas, Nevada. 71 pp.
Cappo, K A,, L J. Blume, Q. A, Raab, J. K. Bartz, and J. L Engels. 1987. Analytical Methods Manual
for the Direct/Delayed Response Project Soil Survey. EPA/600/8-87/020. U.S. Environmental
Protection Agency, Las Vegas, Nevada. 318 pp.
Costle, 0. M. May 30, 1979a. Administrator's Memorandum, EPA Quality Assurance Policy
Statement. U.S. Environmental Protection Agency, Washington, O.C.
Costle, D. M. May 30, 1979b. Administrator's Policy Statement, Quality Assurance Requirements
for all EPA Extramural Projects Involving Environmental Measurements. U.S. Environmental
Protection Agency, Washington, D.C.
Grubbs, F. E. 1969. Procedures for Detecting Outlying Observations in Samples. Technometrics,
TCMTA, v. 11, n. 4, pp 1-21.
Joint Committee for Powder Diffraction Standards. 1985/86. Powder Diffraction Files. International
Centre for Diffraction Data, Swarthmore, Pennsylvania.
U.S. Department of Agriculture/Soil Conservation Service. 1951. Supplement 1962. Soil Survey
Manual. Agriculture Handbook No. 18, U.S. Department of Agriculture, Washington, D.C.
U.S. Department of Agriculture/Soil Conservation Service. 1975. Soil Taxonomy. Agriculture
Handbook No. 436, U.S. Department of Agriculture, Washington, D.C.
U.S. Department of Agriculture/Soil Conservation Service. 1981. National Handbook of Plant Names.
Title Part 610, Plant Names List, U.S. Department of Agriculture, Washington, D.C.
U.S. Department of Agriculture/Soil Conservation Service. 1983a. National Soils Handbook. Title
430, U.S. Department of Agriculture, Washington, D.C.
U.S. Department of Agriculture/Soil Conservation Service. 1983b. Soils-Correlation-Glossary of
Landform and Geologic Terms. National Bulletin No. 430-3-1, U.S. Department of Agriculture,
Washington, D.C.
-------
Section 16
Revision 2
Date: 2/87
Page 2 of 2
U.S. Department of Agriculture/Soil Conservation Service. 1985. Land Resource Regions and Major
Land Resource Areas of the Northeast United States (map). U.S. Department of Agriculture,
Fort Worth, Texas.
U.S. Environmental Protection Agency. 1980. Interim Guidelines and Specifications for Preparing
Quality Assurance Project Plans. QAMS-005/80. U.S. Environmental Protection Agency,
Washington, D.C.
U.S. Environmental Protection Agency. 1985. Direct/Delayed Response Project Soil Survey Data
Quality Objectives (Draft). U.S. Environmental Protection Agency, Washington, D.C.
-------
Appendix A
Revision 2
Date: 2/87
Page 1 of 40
Appendix A
Forms and Legends for Reporting Field Data
Field data describing each sampled pedon are recorded on the SCS-232 form. This appendix
also includes specific information on the abbreviations used on this form, as well as the soil
description codes that are used in completing it.
-------
Appendix A
Revision 2
Date: 2/87
Page 2 of 40
FORM SCS-SOI-232
U S DEPARTMENT OF AGRICULTURE
SOIL CONSERVATION SERVICE
SOIL DESCRIPTION
SOU StftlfS KAMI
M M I I I I
i i
SAWn.1 NUMBf I
COUNT V
i i
4.ATITUDC
oca , WH
lOMGlTUDC
HI
S . MIC«0 , ,
itJTl1
N CLASSIFICATION
lil
WAU* 1
Df F>tM I I
1111 11 i
i i
PAFtfNl MAT
* | U OAKt
I t1
1 I i 3 It* !<•
I OHIO I M I MI OFttO I * I M I O*KJ I f
I Ul I i M I i I-
I WtNTf« 1 ANN
i i i i i i i i i i i i i i
CONTAOl SICllOW
i i I I I
l" i V
o
I I I I I
H00CHNG
FB) OU«
I I I
DC&CA4
1 1 1
[MS NAMES
I 1 I I
I I M 1 M I I I 1 I I
I I M I I I I I I I I I I I I I I I
CREW 10
.OCATIOM DCSCMIP1ION
I I I I I I I I I I I I I I I I I I I I I I I I M I I I I I I
I I I I I I I I I ! I I I I I
I I I I I I I I I I I I I I I I I I I I I I I I I I M I I I
fM[( fOMW 1lt| NOT 15
J_L
I I I M I I I M I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I
MM I I I M I I I I I I I I I I I I I I M I M I I I I I I I
I I M I I I I I I I I I I I I I I I I I I M I I I I I I I I I I I I I I I I I I I I I I I I I
SOM**t >
;t»c F(*iu*»t cooe^
OC Ctc
-------
FORM SCS-SOI-232 (Continued)
Appendix A
Revision 2
Date: 2/87
Page 3 of 40
1
2
3
4
5
6
7
8
9
10
DfPTM
u»»cri -f
^r\ty*4\ «
I I
I |
I I
1 |
l 1
I |
1 1
1 1
1
1
1 !
1 1
1
1 1
1 1
I
1
MQRi/o*«i*i
DtS*GN* 110*4
D
5 M»STIW
C. V»'M«» VJMl»
1 I 1 1 1 1 1
1 1 1 1 1 1 1
1 1 1 1 1 I 1
1 1 1 1 1 t
1 1 1 1 1 1 1
1 1 1 1 1
1 1 1 I I 1 1
1 1 1 1 1
1 1 1 1 ! 1 1
III! 1
tHICK
Nl&S
Avo
M*I
"'"
1 1
1 1
I |
1 1
1 1
1 1
1 1
| I
I |
I |
1 1
i :
L 1
t i
i i
i i
i i
i i
i i
i i
i i
i i
i i
i
i i
i i
i i
i i
i i
i i
onv C(XO"
v c
0 * M
C * MUI 1 H
|
|
|
|
|
|
|
|
|
|
|
|
|
|
I
|
|
1
|
|
1
|
|
1
|
|
1
|
|
1
1 1 1 1
1 1 1 I
1 t 1 1
till
till
1 1 1 1
1 1 1 1
1 I 1 1
1 1 1 1
1 1 1 1
1 1 1 1
i : i i
i i i i
1111
till
1111
i i i i
i i i i
i i i i
l i l i
1111
i i i
! 1 1 1
1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
III!
1111
MOIST CCKO*
L V C
O AH
C * MUI I «
|
|
|
|
|
|
|
|
|
|
|
|
|
|
1
|
|
1
|
|
1
|
|
1
|
|
1
1
|
1
1 1 I 1
1 1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
till
1 1 1 1
I 1 1 1
I 1 1 1
1111
1 1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
1 1 1 1
1 I 1 1
1 1 t 1
1 1 1 1
1 ! 1 1
1 1 I 1
1 1 i 1
1 1 1 1
1 1 1 1
1 1 1 1
lilt
1 i 1 1
1 1 1 1
1111
TllTU«
Ct «S5 *»OD
1 1 1
1 1 1
1 1 1
1 1 1
1 1 1
1 1 1
1 1 1
1 1 1
1 1 I
1 1 1
1 ,1 1
1 1 1
1 ,1 1
1 1 1
1 1 1
1 1 1
1 1 -J..
1 1 !
1 1 1
1 1
1 I
1 1
1 1
1 1
1 1
1 1
t I
1 1
1 1
1 1
1 1
1 1
1 I
1 1
1 1
-1..1
1 1
\ \
M |>,in«lK*(
<"> (><*—'
I COS ln»'"»
5 i«"rt
SCI i*»«iY l
S' Srii
5'CL S'i» cu
SI S»r.(*T 10*
V«V V»"» •-'
r,"* fi^M-">i
Cl O
SlRUClUMt SHAPt
page 2 of 4
-------
3
C
C
o
o
CM
CO
CM
I
*—t
o
I/O
J)
o
:si
I '«
U* «
< '
9
o -
• o
o «
*
4 K
I ^
A
§ ill
'
5
£
o a c
C\J
CO
m
CD
r-.
CO
c
J5
o
-
-
cMr«visctMCE *MN' coots r*'fN5'ON
M «c' HMwK-'imi r C"-> -.mm
• O MJO7 "3 *S] 0 &« 0"'"1 «"«*»
M t MC > , 1
•»
«
Ill 1'
iii!iH.i-:'
iiilfltijh
^ i
J ' ! ?
I ? 'jji'? ,!
! | Hi !§ -,l-,l;f|
giisii.-iiniin**
»
^
I
M iiiii .
t.ct I a "}l f*
s ? c - 1 r 4*
U?|*H
J i, iiijiif
>J| »,« — «
K t c ;
ifss 11
§'°u . ;;
8 ! lH,f
.ihitill
Jsliiliiiil
P J;444*i44«4
-------
Appendix A
Revision 2
Date: 2/87
Page 5 of 40
FOR SCS-SOI-232 (Continued)
SAME'S oon*
PKJO1S
O
o> a c
|
|
|
|
|
1
|
|
|
|
|
1
|
|
|
|
|
|
|
|
|
|
1
1
|
|
|
1
1
|
|
|
|
|
1
I
|
|
|
|
|
|
|
|
|
|
|
|
|
l
|
1
1
|
|
|
I
LOG
WEATMEP
SET ID
UNDE»S,0.v»tG
SLIDE S«s <»ED'AC6 OVERS7ORV
UNDEHSTOSV LANDSCAPE
5«" 0' SI
1
|
1
1
1
]
1
|
|
|
1
1
|
|
1
1
|
1
|
|
|
|
|
1
|
|
1
I
1
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
|
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
|
I
I
I
I
I
I
1
lOOTin** o« BOOTS
*
* "•""•"—"'
"""•;..';";:: '"-••••--
...
C (nmmnp
Wl •<•/•
**»IIKH ««ID P»t»-o> »«
PN fH . >w t*r j, \n.ttr.
,.•4 .«,.,. T. ,^ MMO-
v M.I--O
CONCCNTHATIONS
3
UNO OT f U
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
1
|
|
|
I
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
|
I
|
|
|
|
I
ncirj MCASuncD
MUD AMOUNT
P|
|
I
Pl
1
]
P|
1
I
P|
0|A
O |N
Pl
O^A,
O N
P 1
0|A
O |N
p 1
0(A
0 |N
pl
0|A
O |N
P |
0|A
O |N
P |
0|A
O|N
1 !
u
[
'flAOMCNTS
N
0 \
I I H
i i 1 1
i i 1 I
i i Mi
i i i 1
ill!
i i •
i i 1 1
i i 1 1
i i H
i i 1 1
i i 1 1
i i •
till
i i 1 1
i i •
i i I 1
i i 1 1
i t •
i i 1 1
iili
i i V
i
,
i i •
i t 1 1
i 1 1
i i
i i
SMBP1 Ot PO»f S r 1 *H«tl.» «M)<
IN lnl*.|M-l fj got r**\\f*
tn t»lt n«f»,IOil» ll!t»ltl' U1 PtftAnt-v-ll
Ts C*!"»l"f t«1 tutinl*- u? ^n*t «"M»»
II 1 i't"rt ••!* f 11,-lf rrnKfliml M4 U*a«l 1 «"
KINOOI CONCIMDA1IO
Rl lUntr t'vfll*f
97 So*l >w»u*t o< M"l»
•a v,.,..<—
D DMrt'-l
1* O CVMindrd
p P1«lr l.tr
1 V"t '"» *"1 <>i* C V^< n^lvt o< l>m*
*i"* wrt m C ''**' "^ '*"*•"» t^.'o.n.mr m!>M
1 fy^-v t W.-« «nd,,wt M **•""
4 f ,W»m-t, r.,» *P O i*(t IUt» S S«P"f
O lM'» i»«.>»'x>n% B "" "*r1
SOU MOr^liml COOIS 0* (—• «mi.*» ** *"XM1>
n (>•» 13 (*•*<*«.»» tone »t imt ^ «**won.i'-
|
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
s
1
2
3
1
2
3
1
2
3
1
2
3
\
2
3
1
2
3
1
2
3
1
j
3
1
2
3
1
?
3
»4*l.n«t In. «
>• ..r* ON
(NT
*»•
>O*1
m
ONS
Co" •"
1
?
8
4
h
H
7
H
9
10
S,-I
CM..
i rop*s
C f-afaqf
M M»rt,
1 S.^**
HOCK tpi*n
<<
pM rtuic(«hiM.,j >ri)
page 4 of 4
-------
Appendix A
Revision 2
Date: 2/87
Page 6 of 40
Left Justify letters and right Justify numbers. Use leading zeros to fill spaces where number entries
are used. Enter zero as "O/." All codes are on Form SCS-SOI-232 except for pedon classification
and parent material codes which are printed on another sheet. Metric units are specified for this
project.
Site Data
Tier Number 1
Series Name
So
IIS
eric
)3 1
Mar
ne
Sample Number
Sample Number S
St. County Unit u
.b
j_
J I
J I
St. - State alpha code
County - 3-digit FIPS county code
Unit - 3-digit number identify the pedon with a county
Sub - sub unit alpha code if needed
MLRA
Major Land Resource Areas
MLRA
s
u
b
J I
-------
Appendix A
Revision 2
Date: 2/87
Page 7 of 40
Latitude of Sample
Site
Latitude D
i
Deg Min Sec r
Longitude of Sample
Site
Longitude D
Deg Min Sec i
r
J I
I
Date
Mo
j
Date
Day
i
Yr
i
Date - Date pedon was described
Mo - 2-digit code for month
Day » 2-digits, 0 used in left column if one digit
Yr - last 2 digits of the year
-------
Appendix A
Revision 2
Date: 2/87
Page 8 of 40
Tier Number 2
Slope Characteristics
Slope
S
H
% P GM
I
I
A MICRO P
S
P K /
O
^ P S
% = Slope percent
SHP = Slope shape - The configuration of the slope
GM = Geomorphic position code - Specific part of a
hillslope or mountain slope, grading from
summit areas to lowlands
ASP = Slope aspect code - Direction slope is facing
MICRO = Microrelief codes
K = Kind - Kind, amount, and pattern of
microrelief that includes polypedon
described
A = Amount in elevation code
P = Pattern code - Pattern of the low parts
of the microrelief
POS = Pedon position on slope code - Placement
of the pedon site within the segment of
the Geomorphic Component
Physiography
PHYS
L
R O
G C
I
RG = Regional - Landform extending for kilometers
about the pedon site
LOC = Local • Landform in the immediate vicinity of
the pedon site
-------
Appendix A
Revision 2
Date: 2/87
Page 9 of 40
Pedon
Classification
PEDON CLASSIFICATION
O S O G G S GPSC MIN R X TMP OTH
1
1
1 1 1
1 1
1
1
1
1
O = Order
SO = Suborder
GG = Great group
SG = Subgroup
PSC = Particle size class
MIN = Mineralogy
RX = Reaction
TMP = Temperature
OTH = Other code
Precipitation
Not coded by field crews
PRECIP
CM
Water Table
(NSH p. 603-200)
Water
Depth
CM
i i
Table
K
D
Month
i
DEPTH - Depth to top of free water (NA used if no
water table observed)
KD - Kind code
MONTH = Month described
-------
Appendix A
Revision 2
Date: 2/87
Page 10 of 40
Miscellaneous
L
U
S
T
P
M
D
R
LU = Land use code - Current use of the land at
the pedon site (National Inventory and Moni-
toring Manual)
ST = Stoniness class - As defined in Soil Survey
Manual (NSH p. 602-60)
PM = Permeability code - Code for the least
permeable horizon excluding the surface
horizon (NSH p. 603-19)
DR = Drainage class code - As indicated in the
pedon description (SSM p. 4-32)
Tier Number 3
Elevation
ELEVATION
METERS
0 5 |2 0
Parent Material
(Glossary of Landform
and Geologic Terms)
Parent Material
12 3 4
W M ORIG W M ORIG W M ORIG W M ORIG
I
0
I
0
I (
0 I
I
W = Not coded by field crews, 0 in box
M = Mode of deposition code
ORIG = Origin of material code
BDRK = Bedrock fracturing
The Arabic numbers 1, 2, 3, and 4 are for separate types of material that may occur within the
profile. They correspond to lithologic discontinuities.
-------
Appendix A
Revision 2
Date: 2/87
Page 11 of 40
Tempera-
tures
Temperature C
Average Air Average Soil
ANN SUM WINTER ANN SUM WINTER
I I
I I
I I
I I
I I
I t
ANN = Annual
SUM = Summer
WINTER = Winter
Not coded by field crews
Moisture Regime
(MST RGE)
(Soil Taxonomy p. 51)
Weather station number
(not coded by field crews)
WEATHER STA
NUMBER
I l I I i
Tier Number 4
Control Section
CONTROL SECTION
C
l l
M
l
l
CONTROL SECTION = upper and lower limits of particle
size control section (Soil Taxonomy
p. 385)
Water erosion code (ERWA)
(not coded by field crew)
-------
Appendix A
Revision 2
Date: 2/87
Page 12 of 40
Runoff code (RNOF)
(SSM p. 4-34)
Diagnostic Features
DEPTH
CM
J L
K DEPTH
N CM
D
DIAGNOSTIC FEATURES
K
N
D
DEPTH
CM
_L_L
K
N
D
DEPTH
CM
J_L
K
N
D
DEPTH
CM
K
N
D
DEPTH = Upper and lower depths of feature
KND = Kind code
Coded in order of increased depth.
Flooding (NSH p. 603-40)
FLC
FRQ
I
XDDIf-
C
i
JG
)UR
i
FRQ = Frequency (times/yr)
DUR = Duration - months between which flooding occurs
-------
Tier Number 5
Vegetation-Scientific
plant name symbol for
dominant species
(National Handbook of
Plant Names)
MAJOR
i i i i i
VEGETATION
SPECIES
2nd
i i i i i I
3rd
i i i i i
Appendix A
Revision 2
Date: 2/87
Page 13 of 40
The major, 2nd, and 3rd fields should include the dominant tree
species by order of basal area. For areas that were clearcut since
mapping was conducted, use the code CC. Describe the dominant
vegetation types prior to the clearcut in the free-form site notes.
Describees' Names and Crew I.D.
DESCRIBERS' NAMES
J 1 I L-U I I I I I L.
_L
J I I L
I I I I I I I I I I
CREW I.D.
-------
Appendix A
Revision 2
Date: 2/87
Page 14 of 40
Tier Number 6
Location Description
Spaces 1 - 6 - Watershed I.D.
7 - Dash
8 = Site Number
9 - Dash
10 - 12 - Sampling class code. If class only has 2 characters, add a
zero (0) before the number, e.g., S9 becomes S09.
13 - Dash
14 - 16 - Aspect - Determined by the face of the pit described in a
perpendicular direction based on magnetic north. If azimuth
cannot readily be determined, as in Histosols, use N/A in
this field. Use leading zeros.
17 = Degree symbol
18 to end «• Location notes
LOCATION
. I . o
I I 1 I I I I I I I I I I I I I I
DESCR
i i
1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 II
IPTION
i i i i i
i i i i i
i
i
1111 j |_ j_ ]_
FREE FORM SITE NOTES
I 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
-------
HORIZON DATA
Depth
(SSM p. 4-50)
DEPTH
UPPER
LOWER
j I
j I
Appendix A
Revision 2
Date: 2/87
Page 15 of 40
Horizon Designation
(SSM p. 4-39)
HORIZON
DESIGNATION
D
I
S MASTER
C LETTER SUFFIX
i i
i i i
DISC = Discontinuity
(Arabic number)
MASTER LETTER - Master horizon
designation
SUFFIX = Subscript
Thickness (SSM p. 4-50)
AVE - Average thickness of horizon
MAX * Maximum thickness of horizon
MIN » Minumum thickness of horizon
THICK-
NESS
AVE
MAX
MIN
-------
COLORS (Dry and Moist)
Appendix A
Revision 2
Date: 2/87
Page 16 of 40
DRY COLOR
L
O
V
A
C % HUE L
i
i
i
I i
I i
i i
I i
I i
I i
C
H
R
There is space for three
matrix color entries. Enter
the dominant color on upper
line (SSM p. 4-62).
LOC = Location code
% = Percent of matrix (leave
blank if 100).
HUE = Hue (left justify; a
decimal requires a space).
VAL = Value
CHR = Chroma
Hues are coded as 0.
MOIST COLOR
L V C
O AH
C % HUE L R
i
,
i
i i i i
i i i i
itii
Texture
(SSM p. 4-52 and
NSH p. 603-198)
TEXTURE
CLASS MOD
i i i
i i
i i
i i
CLASS = Class code
MOD = Texture modifier
-------
Appendix A
Revision 2
Date: 2/87
Page 17 of 40
Structure
STRUCTURE
G
R
D
SZ SHP
i
i
i
i i
i i
i i
GRD = Grade code (SSM p. 4-72)
SZ = Size code (SSM p. 4-99)
SHP = Shape code (SSM p. 4-71)
Consistence
(SSM p. 4-81)
CONSISTENCE
DRY
MOIST
OTHER
i i
i i
1 |
ST/PL
i i
i i
C
E
DRY = Dry (1st line left side of field)
MOIST = Moist (2nd line left side of field)
OTHER = Other code (3rd line left side of field)
(SSM p. 4-83)
ST = Stickiness (1st line middle of the field)
PL = Plasticity (2nd line middle of the field)
CEM - Cementation code (lower right of field)
(SSM p. 4-79)
-------
Appendix A
Revision 2
Date: 2/87
Page 18 of 40
Mottles
(SSM p. 4-66)
MOTTLES
A
B
sz
i i
i i
,,
C V C
O AH
N L R
HUE
i i i
i i i
i i i
AB - Abundance code
SZ - Size code
CON = Contrast code
HUE - Hue (left justify)
VAL - Value
CHR » Chroma
Surface features
SURFACE FEATURES
K
N
D
A D L V C
M C S O AH
R N T C HUE L R
i
i
i
iiii
LA _L L
1111
KND = Kind code
AMT = Amount code
CN = Continuity
DST = Distinction code
LOC = Location code
HUE = Hue (left justify)
VAL = Value
CHR = Chroma
-------
Boundary
(SSM p. 4-51)
Distinctness-toft
Topography-right
BOUN-
DARY
Appendix A
Revision 2
Date: 2/87
Page 19 of 40
Effervescence
(SSM p. 4-91)
Not coded by field crews
EFFERVES-
CENCE
C A E
L G X
CL = Class code
AG = Agent code
EX = Extent code
Roots
(SSM p. 4-85)
ROOTS
L
0
QT SZ C
t I i
i I i
QT = Quantity code
SZ = Size code
LOC = Location code
-------
Pores
(SSM p. 4-84)
PORES
SHP QT SZ
i
i
i
1
I
i
i
i
SHP = Shape code
QT = Quantity code
SZ = Size code
Concentrations
(SSM p. 4-76)
CONCENTRATIONS
KND
i
i
i
S
H
QT P SZ
i
i
i
i
i
KND = Kind code
QT = Quantity code
SHP = Shape code
SZ = Size code
Appendix A
Revision 2
Date: 2/87
Page 20 of 40
-------
FIELD
MEASURED
PROPERTIES
KND
P
i
i
i
AMOUNT
i i
i i
P
E S
R 0
M I
L
-H4
i i
Appendix A
Revision 2
Date: 2/87
Page 21 of 40
KND = Kind code
pH = line one, all horizons
OA = % Clay, line two, horizon 4-10
ON = % Sand, line three, horizon 4-10
AMOUNT = Amount, no decimals
PERM - Permeabilility of horizon. Use same codes
as permeability on page one. Upper line.
SOIL = Soil moisture code. Lower line.
Rock Fragments
(SSM p. 4-97)
ROCK
FRAGMENTS
K
N
D
%
i
i
1 i
S
z
1
2
3
KND = Kind code
% = Percent by volume
SZ - Size code
-------
Appendix A
Revision 2
Date: 2/87
Page 22 of 40
Free
Form
Notes
Samp 1 e Codes
Clods
Sample Codes » Sample taken from particular horizon. Same
sample code that appears on Label A.
Clods » Number of clods taken from particular horizon
(if none, use 0)
LOG
1. Weather • Type of weather i.e., rainy, sunny, and average temperature.
2. Set I.D. - Unique numbers assigned to crews for each day in the field.
3. Understory vegetation
4. Slides - Number of slides corresponding to specific picture from film roll
LOG
WEATHER
SET I.D.
UNDERSTORY VEGETATION -
SLIDE NO.
pedon face
ove r s tory
unde r s tor y
Iandscape
-------
Appendix A
Revision 2
Date: 2/87
Page 23 of 40
2.0 Soil Description Codes for Form SCS-SOI-232
2.1 Slope Shape Codes
1 convex 2 plane 3 concave 4 undulating 5 complex
2.2 Geomorphic Position Codes
01 summit crested hills 11 summit interfluve
02 shoulder crested hills 12 shoulder interfluve
22 shoulder headslope 42 shoulder noseslope
03 backslope crested hills 23 backslope headslope
33 backslope sideslope 43 backslope noseslope
24 footslope headslope 34 footslope sideslope
44 footslope noseslope 05 toeslope crested hills
25 toeslope headslope 35 toeslope sideslope
04 footslope crested hills 00 not applicable
32 shoulder sideslope
2.3 Slope Aspect Codes
1 northeast 2 east 3 southeast 4 south
5 southwest 6 west 7 northwest 8 north
2.4 Microrelief (Micro) Codes
2.4.1 Kind (K)
B - micro depression M » mound
£ - tree-throw feature B " raised bog
F - frost polygon I - terracettes
S - gilgai Z - other (specify in notes)
i. * land leveled or smooth
2.4.2 Variation In elevation (A)
Q - minimal 2 - 20-50 cm
1 - <20 cm 4. - 50-100 cm
2.4.3 Pattern (P)
Q • none 2 = closed depressions
1 - linear £ = reticulate (net)
2.5 Pedon Position Codes
1 on the crest 2 on slope and crest 3 on upper third
4 on middle third 5 on lower third 6 on a slope
7 on a slope and depression 8 in a depression 9 in a drainageway
-------
Appendix A
Revision 2
Date: 2/87
Page 24 of 40
2.6 Regional Landform Codes
A coastal plains
E lake plains
G glaciated uplands
I bolson
L level or undulating uplands
N high hills
R hills
V mountain valleys or canyons
2.7 Local Landform Codes
A fan
C cuesta or hogback
E escarpment
Q crater
I hillside or mountainside
K kamef ield
M mesa or butte
P flood plain
R upland slope
T terrace—stream or lake
V pediment
X salt marsh
Z back barrier flat
2.8 Great Group Codes
ALFISOLS
AAQAL AJbaqualf
AAQNA Natraqualf
AAQPN Plinthaqualf
ABOCR Cryoboralf
ABOGL Glossoboralf
AUDAG Agrudalf
AUDFS Fraglossudalf
AUDNA Natrudalf
AUSDU Durustalf
ASUPA Paleustalf
AXEOU Durixeralf
AXENA Natrixeralf
AXERH Rhodoxeralf
AAQDU Duraqualf
AAQGL Glossaqualf
AAQTR Tropaqualf
ABOEU Eutroboralf
ABONA Natriboralf
AUDFE Ferrudalf
B intermountain basin
F river valley
H glaciofluvial landform
K karst
M mountains or deeply dissected plateaus
P piedmonts
U plateaus or tablelands
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
AUDGL Glossudalf
AUDPA Paleudalf
AUSHA Haplustalf
AUSPN Plinthustalf
AXEFR Fragixeral
AXEPA Palexeralf
AAQFR Fragiaqualf
AAQOC Ochraqualf
AAQUM Umbraqualf
ABOFR Fragiboralf
ABOPA Paleboralf
AUDFR Fragiudalf
AUDHA Hapludalf
AUDTR Tropudalf
AUSNA Natrustalf
AUSRH Rhodustalf
AXEHA Haploxeralf
AXEPN Plinthoxeralf
-------
Appendix A
Revision 2
Date: 2/87
Page 25 of 40
ARIDISOLS
DARDU Durargid
DARNT Natrargid
DORCM Camborthid
DORPA Paleorthid
DARHA Haplargid
DARPA Paleargid
ENTISOLS
EAQCR Cryaquent
EAQHY Hydraquent
EAQTR Tropaquent
EFLTO Torrifluvent
EFLUS Ustifluent
EORTO Torriorthent
EORUS Ustorthent
EPSQU Quartzipsamment
EPSUD Udipsamment
EAQFL Fluvaquent
EFLCR Cryofluvent
EFLUD Udifluvent
EORCR Cryorthent
HISTOSOLS
HFIBO Borofibrist
HFIME Medifibrist
HFOBO Borofolist
HHEBO Borohemist
HHEME Medihemist
HHETR Tropohemist
HSAME Medisaprist
HFICR Cryofibrist
HFISP Sphagnofibrist
HFOCR Cryofolist
INCEPTISOLS
IANCR Cryandept
IANEU Eutrandept
IANVI Vitrandepth
IAQFR Fragiaquept
IAQHU Humaquept
IAQSU Sulfaquept
IOCDU Durochrept
IOCFR Fragiochrept
IPLPL Plaggept
ITRHU Humitropept
IUMCR Cryumbrept
DORDU Durorthid
DORSA Salorthid
DARND Nadurargid
DORCL Calciorthid
DORGY Gypsiorthid
EAQPS Psammaquent
EARAR Arent
EFLTR Tropof luvent
EFLXE Xerofluvent
EORTR Troporthent
EORXE Xerorthent
EPSTO Torripsamment
EPSUS Ustipsamment
EAQHA Haplaquent
EAQSU Sulfaquent
EORUO Udorthent
EPSCR Cryopsamment
EPSTR Tropopsamment
EPSXE Xeropsammerit
HHECR Cryohemist
HHESI Sulfihemist
HSABO Borosaprist
HSATR Troposaprist
HFILU Luvifibrist
HFITR Tropofibrist
HFOTR Tropofolist
HHELU Luvihemist
HHESO Sulfohemist
HSACR Cryosaprist
IAQTR Tropaquept
IOCDY Dystrochrept
IOCUS Ustochrept
ITRDY Dystropept
ITRSO Sombritropept
IUMFR Fragiumbrept
IANDY Dystrandept
IANPK Placandept
IAQCR Cryaquept
IAQHP Haplaquept
IAQPN Plinthaquept
-------
Appendix A
Revision 2
Date: 2/87
Page 26 of 40
IUMXE Xerumbrept
IANDU Durandept
IANHY Hydrandept
IAQAN Andaquept
IAQHL Halaquept
IAQPK Palacaquept
MOLUSOLS
MALAR Argialboll
MAQCA Calciaquoll
MAQHA Haplaquoll
MBOCA Calciboroll
MBONA Natriboroll
MRERE Rendoll
MUDPA Paleudoll
MBOCR Cryoboroll
MBOPA Paleboroll
MUDAR Argiudoll
MUOVE Vermudoll
MUSDU Durustoll
MUSPA Paleustoll
MXECA Calcixeroll
MXENA Natrixeroll
MAQAR Argiaquoll
MAQDU Duraquoll
OXISOLS
OAQGI Giwsiaquox
OAQUM Umbr-:quox
OHUHA Haplohumox
OOREU Eutrorthox
OORSO Sombriorthox
OUSAC Acrustox
OUSHA Haplustox
OAQOC Ochraquox
OHUAC Acrohumox
OHUSO Sombrihumox
SPODOSOLS
SAQCR Cryaquod
SAQHA Haplaquod
SAQTR Tropaquod
SHUFR Fragihumod
SHUTR Tropohumod
SORHA Haplorthod
SAQDU Duraquod
SAQPK Placaquod
SFEFE Ferrod
IOCCR Cryochrept
IOCEU Eutrochrept
IOCXE Xerochrept
ITREU Eutropept
ITRUS Ustropept
IUMHA Haplumbrept
MUSCA Calciustoll
MUSNA Natrustoll
MXEAR Argixeroll
MXEHA Haploxeroll
MALNA Natralboll
MAQCR Cryaquoll
MAQNA Natraquoll
MBOAR Argiboroll
MBOHA Hapioboroll
MBOVE Vermiboroll
MUDHA Hapludoll
MUSAR Argiustoll
MUSHA Haplustoll
MUSVE Vermustoll
MXEOU Durixeroll
MXEPA Palexeroll
OORGI Gibbsiorthox
OORUM Umbriorthox
OUSEU Eutrustox
OUSSO Sombriustox
OAQPN Plinthaquox
OHUGI Gibbsihumox
OORAC Acrorthox
OORHA Haplorthox
OTOTO Torrox
SHUHA Haplohumod
SORCR Cryorthod
SORPK Placorthod
SAQFR Fragiaquod
SAQSI Sideraquod
SHUCR Cryohumod
SHUPK Placohumod
SORFR Fragiorthod
SORTR Troporthod
-------
Appendix A
Revision 2
Date: 2/87
Page 27 of 40
ULTISOLS
UAQAL AJbaquult
UAQPA Paleaquult
UAQUM Umbraquult
UHUPN Plinthohumult
UUDFR Fragiudult
UUDPN Plinthudult
UUSHA Haplustult
UUSRH Rhodustult
UAQFR Fragiaquult
UHUPA Palehumult
UHUTR Tropohumult
UUDPA Paleudult
VERTISOLS
VTOTO Torrert
VUSCH Chromustert
VXEPE Pelloxerert
VUDCH Chromudert
2.9 Subgroup Codes
AA Typic
ABO4 Abruptic aridic
AB10 Abruptic haplic
AB16 Abruptic xerollic
AE03 Aerie arenic
AE06 Aerie humic
AE09 Aerie tropic
AE12 Aerie xeric
AL02 Albaquultic
AL08 Albic glossic
AL13 Alfic andeptic
AL16 Alfic lithic
AN01 Andeptic
AN Andic
AN22 Andic ustic
AQ Aqualfic
AQ04 Aqueptic
AQ08 Aquic arenic
AQ16 Aquic duriorthidic
AQ24 Aquic haplic
AQ31 Aquic psammentic
AQ36 Aquultic
AR02 Arenic aridic
AR04 Arenic plinthaquic
AR08 Arenic rhodic
AR14 Arenic umbric
AR18 Arenic ustollic
AR24 Argiaquic xeric
UAQPN Plinthaquult
UHUHA Haplohumult
UHUSO Sombrihumult
UUDHA Hapludult
UUORH Rhodudult
UUSPA Paleustult
UXEHA Haploxerult
UAQOC Ochraquult
UAQTR Tropaquult
UUDTR Tropudult
UUSPN Plinthustult
UXEPA Palexerult
VUSPE Pellustert
VUDPE Pelludert
UXECH Chromxerert
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
AL12 Alfic arenic
AN24 Andaqueptic
AN11 Andeptic glossoboric
AN06 Andic Dystric
AN30 Anthropic
AQ02 Aquentic
AQ06 Aquic
AQ14 Aquic duric
AQ18 Aquic dystric
AQ26 Aquic lithic
AQ34 Aquollic
AR Arenic
AR03 Arenic orthoxic
AR06 Arenic plinthic
AR10 Arenic ultic
AR16 Arenic ustalfic
AR22 Argiaquic
AR26 Argic
-------
Appendix A
Revision 2
Date: 2/87
Page 28 of 40
AR28 Argic lithic
AR32 Argic vertic
AR36 Aridic calcic
AR50 Aridic pachic
AN03 Andaquic
BO02 Borolfic lithic
BO06 Borollic
BO10 Borollic lithic
CA Calcic
CA06 Calciorthidic
CA20 Cambic
CH06 Chromudic
CR10 Cryic lithic
CU Cumulic
CU04 Cumulic ultic
DU Durargidic
DUOS Durixerollic
DU11 Durochreptic
DU14 Durorthidic xeric
DY03 Dystric entic
DY06 Dystric lithic
AR30 Argic pachic
AR34 Aridic
AR42 Aridic duric
AR52 Aridic petrocalcic
BO Boralfic
BO04 Boroalfic udic
BOOS Borollic glossic
BO12 Borollic vertic
CA04 Calcic pachic
CA10 Calcixerollic
CH Chromic
CR Cryic
CR14 Cyric pachic
CU02 Cumulic udic
DU02 Duric
DU10 Durixerollic lithic
DU12 Durorthidic
DY02 Dystric
DY04 Dystric Fluventic
DY08 Dystropeptic
EN Entic
EN06 Entic ultic
EP10 Epiaquic orthoxic
EU02 Eutrochreptic
FE Ferrudalfic
FI02 Fibric terric
FL06 Fluventic
FR10 Fragiaquic
GL02 Glossaquic
GL10 Glossic udic
GL14 Glossoboralfic
GR Grossarenic
GR04 Grossarenic plinthic
HA01 Haplaquic
HA02 Haplic
HA07 Haploxerollic
HA12 Hapludollic
HE Hemic
HI Histic
HI06 Histic pergelic
HU Humic
HU05 Humic pergelic
HY Hydric
EN02 Entic lithic
EP Epiaquic
EU Eutric
EU04 Eutropeptic
FI Fibric
FL02 Fluvaquentic
FL12 Fluventic umbric
FR18 Fragic
GL04 Glossic
GL12 Glossic ustollic
GL16 Glossoboric
GR01 Grossarenic entic
HA Haplaquodic
HA05 Haplohumic
HA09 Hapludic
HA16 Haplustollic
HE02 Hemic terric
HI02 Histic lithic
HU10 Humaqueptic
HU02 Humic lithic
HU06 Humoxic
HY02 Hydric lithic
-------
Appendix A
Revision 2
Date: 2/87
Page 29 of 40
LE Leptic
LI01 LJthic
LI06 LJthic ruptic-alfic
LI09 Lithic ruptic-entic
LJ13 Lithic ruptic-ultic
L111 LJthic ruptic-xerorthentic
LI12 LJthic ultic
LI16 Lithic ustic
LI20 Lithic vertic
LI24 Lithic xerollic
MO Mollic
OC Ochreptic
OR Orthidic
OX Oxic
PA Pachic
PA04 Pachic ultic
PA08 Paleustollic
PA20 Paralithic vertic
PE01 Pergelic ruptic-histic
PE04 Petrocalcic
PE08 Petrocalcic ustollic
PE16 Petroferric
PK Placic
PK12 Plaggic
PL04 Plinthic
PS Psammaquentic
QU Quartzipsammentic
RE Rendollic
RU02 Ruptic-alfic
RU11 Ruptic-lithic-entic
RU17 Ruptic-ultic
SA Salorthidic
SA04 Sapric terric
SO04 Sombrihumic
SP02 Sphagnic terric
SU Suflic
AA Typic
TH04 Thapto-histic
TO Torrertic
TO04 Torriorthentic
TO10 Torroxic
TR02 Tropeptic
LI Limnic
LJ04 Lithic mollic
LI07 LJthic ruptic-argic
LJ08 Lithic ruptic-entic-xerollic
LJ15 Lithic ruptic-xerochreptic
LI10 Lithic udic
LI14 Lithic umbric
L118 Lithic ustollic
LI22 Lithic xeric
NA06 Natric
OR01 Orthic
OR02 Orthoxic
PA02 Pachic udic
PA06 Paleorthidic
PA10 Palexerollic
PE Pergelic
PE02 Pergelic sideric
PE06 Petrocalcic ustalfic
PE14 Petrocalcic xerollic
PE20 Petrogypsic
PK10 Plaggeptic
PL Plinthaquic
PL06 Plinthudic
PS02 Psammentic
RH Rhodic
RU09 Ruptic-lithic
RU15 Ruptic-lithic-xerochreptic
RU19 Ruptic-vertic
SA02 Sapric
SI Sideric
SP Sphagnic
SP04 Spodic
TE Terric
TH06 Thapto-histic tropic
TO02 Torrifluventic
T006 Torripsammentic
TR Tropaquodic
TR04 Tropic
-------
Appendix A
Revision 2
Date: 2/87
Page 30 of 40
UD01 Udalfic
U002 Udlc
UD05 Udorthentic
UL Ultic
UM02 Umbric
US02 Ustertic
US06 Ustochreptic
US12 Ustoxic
VE Vermic
XE Xeralfic
XE04 Xeric
2.10 Particle Size Codes
002 not used
005 ashy
008 ashy over loamy
019 ashy over medial
UD Udertic
UD03 Udollic
UD10 Udoxic
UM Umbreptic
US Ustalfic
US04 Ustic
US08 Ustollic
VE02 Vertio
XE02 Xerertic
XE08 Xerollic
003 cindery
015 skeletal-cindery over medial
004 cindery over sandy or sandy-
skeletal
114 clayey
116 clayey over fragmental
120 clayey over loamy-skeletal
118 skeletal-clayey over sandy or sandy
056 clayey-skeletal
080 coarse-loamy
082 coarse-loamy over fragmental
084 skeletal-coarse-loamy over sandy
or sandy
088 coarse-silty
090 coarse-silty over fragmental
092 skeletal-coarse-silty over sandy
or sandy
126 fine
102 fine-loamy over clayey
100 skeletal-fine-loamy over sandy
or sandy
106 fine-silty
108 fine-silty over fragmental
110 skeletal-fine-silty over sandy
or sandy
036 fragmental
072 skeletal-loamy over sandy
or sandy
007 ashy over cindery
013 ashy over loamy-skeletal
009 ashy-skeletal
006 cindery over loamy
122 clayey over fine-silty
124 clayey over loamy
058 clayey-skeletal over sandy
086 coarse-loamy overy clayey
094 coarse-silty over clayey
096 fine-loamy
098 fine-loamy over fragmental
112 fine-silty over clayey
068 loamy
050 loamy-skeletal
-------
Appendix A
Revision 2
Date: 2/87
Page 31 of 40
054 loamy-skeletal over clayey
052 loamy-skeletal over sand
010 medial
012 medial over cindery
016 medial over fragmental
020 medial over loamy-skeletal
022 skeletal-medial over sandy
or sandy
024 medial over thioxotropic
062 sandy
066 sandy over clayey
044 sandy-skeletal
026 thixotropic
034 thixotropic over loamy
030 thixotropic over sandy or
sandy-skeletal
027 thixotropic-skeletal
2.11 Mineralogy Codes
02 not used 04 calcareous
09 chloritic 07 clastic
10 dlatomaceous 12 ferrihumic
051 loamy-skeletal over fragmental
014 medial over clayey
018 medial over loamy
011 medial-skeletal
063 sandy or sandy-skeletal
063 sandy over loamy
046 sandy-skeletal over loamy
028 thixotropic over fragmental
032 thixotropic over loamy-skeletal
134 very fine
20 glauconitic
26 illitic
30 marly
35 mixed (calcareous)
18 gibbsitic
24 haltoysitic
28 kaolinitic
34 mixed
38 (calcareous)
montmorillonitic
40 oxidic 42 sepiolitic
46 siliceous 50 vermiculitic
2.12 Reaction Codes
05 carbonatic
08 coprogenous
14 ferritic
22 gypsic
27 illitic (calcareous)
32 micaceous
37 montmorillonitic
44 serpentinitic
02 not used
12 nonacid
04 acid
14 noncalcareous
08 dysic
10 euic
2.13 Temperature Regime Codes
02 not used
10 Isohyperthermic
18 thermic
04 frigid 06 hyperthermic 08 isofrigid
isomesic 14 isothermic 16 mesic
2.14 Other Family Codes
02 not used
08 micro
15 shallow and uncoated
16 sloping
04 coated 05 cracked 06 level
12 ortstein 14 shallow
17 shallow and coated
19 orstein shallow uncoated
-------
Appendix A
Revision 2
Date: 2/87
Page 32 of 40
2.15 Kind of Water Table Codes
no water table observed 1 flooded 2 perched
3 apparent 4 ground water 5 ponded
2.16 Landuse Codes
A abandoned cropland (>3 yrs) C cropland
E forest land grazed F forest land not grazed
G pasture land and native pasture H horticultural land
I cropland irrigated L waste disposal land
N barren land P rangeland grazed
Q wetlands drained R wetlands
S rangeland not grazed I tundra
U urban and built-up land
2.17 Stoniness Class Codes
0 class 0 2 class 2 4 class 4
1 class 1 3 class 3 5 class 5
2.18 Permeability Codes
1 very slow 2 slow 3 moderately slow 4 moderate
5 moderately rapid 6 rapid 7 very rapid
2.19 Drainage Codes
1 very poorly drained 2 poorly drained
3 somewhat poorly drained 4 moderately well drained
5 well drained 6 somewhat excessively drained
7 excessively drained
2.20 Parent Material Mode of Deposition Codes
A alluvium E eolian H volcanic ash W loess
S eolian-sand D glacial drift G glacial outwash T glacial till
L lacustrine M marine O organic Y solifluctate
V local colluvium R solid rock X residuum U unconsolidated
sediments
2.21 Parent Material Origin Codes
Mixed Lithology
YO mixed Y1 mixed-noncalcareous
Y2 mixed-calcareous Y3 mixed-lithology, unspecified
Y4 mixed-igeous-metamorphic and Y5 mixed-igneous and metamorphic
sedimentary Y7 mixed-metamorphic and
Y6 mixedigneous and sedimentary sedimentary
-------
Appendix A
Revision 2
Date: 2/87
Page 33 of 40
Conglomerate
CO conglomerate
C2 conglomerate-calcareous
Igneous
10 igneous
11 igneous-course
13 igneous-intermediate
15 igneous-fine
17 jgneous-andesite
19 igneous-ultrabasic
Metamorphic
MO metamorphic
M1 gneiss
M3 metamorphic-basic
MS schist and thyllite
M7 methamorphic-basic
M9 quartzite
Sedimentary
SO sedimentary
S1 marl
Interbedded Sedimentary
BO interbedded sedimentary
B2 limestone-sandstone
B4 limestone-siltstone
B6 sandstone-siltstone
Sandstone
AO sandstone
A2 arkosic-sandstone
A4 sandstone-calcareous
Shale
HO shale
H1 shale-noncalcareous
Siltstone
C1 conglomerate-noncalcareous
12 igneous-basic
14 igneous-granite
16 igneous-basalt
18 igneous-acid
M2 metamorphic-acidic
M4 serpentine
M6 metamorphic-acidic
MB slate
S2 glauconite
B1 limestone-sandstone-shale
B3 limestone-shale
B5 sandstone-shale
B7 shale-siltstone
A1 sandstone-noncalcareous
A3 other sandstone
H2 shale-calcareous
TO siltstone
T2 siltstone-calcareous
T1 siltstone-noncalcareous
-------
Appendix A
Revision 2
Date: 2/87
Page 34 of 40
Limestone
LO limestone
L1 chalk
L3 dolomite
L5 limestone-arenaceous
L7 limestone-cherty
Pyroclastic
PO pyroclastic
P1 tuff
P3 tuff-basic
P5 breccia-acidic
P7 tuff-breccia
P9 pahoehoe
Ejecta Material
EO ejecta-ash
E1 acidic-ash
E3 basaltic-ash
E5 cinders
E7 scoria
Organic Materials
KO organic
K2 herbaceous material
K4 wood fragments
K6 charcoal
K9 other organics
2.22 Bedrock Fracturing
1 10 cm between fractures
3 45 cm to 1 m between fractures
52m between fractures
2.23 Moisture Regime Codes
AR aridic moisture regime
US ustic moisture regime
AQ aquic moisture regime
XE xeric moisture regime
2.24 Erosion Codes
12 marble
L4 limestone-phosphatic
L6 limestone-argillaceous
P2 tuff-acidic
P4 volcanic breecia
P6 breccia-basic
P8 aa
E2 basic-ash
E4 andesitic-ash
E6 pumice
E8 volcanic bombs
K1 mossy material
K3 woody material
K5 logs and stumps
K7 coal
2 10 to 45 cm between fractures
4 1 to 2 m between fractures
UD udic moisture regime
TO torric moisture regime
PL) perudic moisture regime
0 none 1 slight
2 moderate
3 severe
-------
Appendix A
Revision 2
Date: 2/87
Page 35 of 40
2.25 Runoff Codes
1 none
5 moderate
2 ponded
6 rapid
3 very slow
7 very rapid
4 slow
2.26 Diagnostic Feature Codes
Epipedon
A anthropic
O ochric
Horizons
Q albic
C calcic
N natric
J petrogypsic
I sombric
Properties
H histic
P plaggen
R argic
B cambic
Xoxic
K placic
S spodic
mollic
U umbric
T argillic
G gypsic
E petrocalcic
Y salic
V sulfuric
L lithic contact
D durinodes Z duripan
W paralithic contact F fragipan
2.27 Horizon Codes
Color Location Codes
0 unspecified 1 ped interior 2 ped exterior
2.28 Texture Classes
C clay
CL clay loam
COSL coarse sandy loam
FM fragmental material
FSL fine sandy loam
L loam
LFS loamy fine sand
LVFS loamy very fine sand
SC sandy clay
SG sand and gravel
SIC silty clay
SIL silt loam
VFS very fine sand
ICE ice or frozen soil
VAR variable
DE diatomaceous earth
MARL marl
MUCK muck
3 rubbed or crushed
CINO cinders
COS coarse sand
CSCL coarse sandy clay loam
FS fine sand
G gravel
LCOS loamy coarse sand
LS loamy sand
S sand
SCL sandy clay loam
SI silt
SICL silty clay loam
SL sandy loam
VFSL very fine sandy loam
GYP gypsiferous earth
CE coprogenous earth
FB fibric material
MPT mucky peat
PDOM partially decomposed organics
-------
Appendix A
Revision 2
Date: 2/87
Page 36 of 40
UDOM undecomposed organics
SP sapric material
OPWD oxide-protected weathered bedrock
U unknown texture
WB weathered bedrock
PEAT peat
HM hemic material
UWB unweathered bedrock
IND indurated
GEM cemented
2.29 Texture Modifiers
BY bouldery
ST stony
CB cobbly
CBX extremely cobbly
CNX extremely channery
CRV very cherty
FLV very flaggy
GRF fine gravelly
GRX extremely gravelly
SHX extremely shaley
SYX extremely slaty
SR stratified
GY gritty
RB rubbly
BYV very bouldery
STV very stony
CBA angular cobbly
CN channery
CR cherty
CRX extremely cherty
FLX extremely flaggy
GRC coarse gravelly
SH shaley
SY slaty
CY cindery
MK mucky
GYV very gritty
BYX extremely bouldery
SIX extremely stony
CBV very cobbly
CNV very channery
CRC coarse cherty
FL flaggy
GR gravelly
GRV very gravelly
SHV very shaley
SYV very slaty
AY ashy
PT peaty
GYX extremely gritty
2.30 Grade of Structure
0 not used
3 strong
6 moderate and strong
2.31 Size of Structure
EF extremely fine
F fine
MC medium and coarse
CV coarse and very coarse
2.32 Structure Shape
PL platy
COL columnar
SBK subangular blocky
CR crumb
WEG wedge
1 weak
4 very strong
2 moderate
5 weak and moderate
VF very fine
FM fine and medium
CO coarse
LP lenticular
BK blocky
GR granular
MA massive
FF very fine and fine
M medium
VC very coarse
PR prismatic
BK angular blocky
CDY cloddy
SGR single grain
2.33 Dry Consistence
L loose S soft
H hard VH very hard
SH slightly hard
EH extremely hard
-------
Appendix A
Revision 2
Date: 2/87
Page 37 of 40
2.34 Moist Consistence
L loose VFR very friable
VFI very firm EFI extremely firm
FR friable
FI firm
2.35 Other Consistence
WSM weakly smeary
B brittle
CO uncemented
SC strongly cemented
VF very fluid
SM strongly smeary MS moderately smeary
R rigid VR very rigid
VWC very weakly cemented WC weakly cemented
I
indurated
SF slightly fluid
2.36 Stickiness
SO nonsticky SS slightly sticky
2.37 Plasticity
PO nonplastic SP slightly plastic
VP very plastic
S sticky VS very sticky
P plastic
2.38 Cementation Agent
H humus I iron L lime S silica
2.39 Mottle Abundance Codes
F few C common M many
2.40 Mottle Size Codes
X lime and silica
1 fine (5 mm) 2
12 fine to medium 13
medium (5 to 15 mm)
fine to coarse
3 coarse (>15 mm)
23 medium to coarse
2.41 Mottle Contrast Code
F faint D distinct
2.42 Surface Features
P prominent
U coats
B black stains
D clay bridging
I iron stains
Q nonintersecting slickensides
L lime or carbonate coats
M manganese or iron-manganese stains
S skeletans (sand or silt)
A skeletans over cutans
C chalcedony on opal
G gibbsite coats
K intersecting slickensides
P pressure faces
X oxide coats
O organic coats
T clay films
-------
Appendix A
Revision 2
Date: 2/87
Page 38 of 40
2.43 Surface Feature Amount Codes
V very few F few C common M many
2.44 Surface Feature Continuity Codes
P patchy D discontinuous C continuous
2.45 Surface Feature Distinctness Codes
F faint D distinct P prominent
2.46 Location of Surface Features
P on faces of peds M on bottoms of plates
H on horizontal faces of peds B between sand grains
V on vertical faces of peds I in root channels or pores
Z on vertical and horizontal faces of peds T throughout
U on upper surfaces of peds or stones R on rock fragments
L on lower surfaces of peds or stones F on faces of peds and in pores
C on tops of columns N on nodules
2.47 Boundary
A abrupt C clear G gradual 0 diffuse
2.48 Topography
S smooth W wavy I irregular B broken
2.49 Effervescence
1 slightly effervescent 2 stongly effervescent
3 violently effervescent 0 very slightly effervescent
2.50 Effervescence Agent Codes
H HCI (unspecified) I HCI (10%) P H202 (unspecified)
Q HA 0 to 4%)
-------
Appendix A
Revision 2
Date: 2/87
Page 39 of 40
2.51 Field Measured Property Kind Codes
2.51.1 For Organic Materials
Column 1 Column 2
F fiber B unrubbed R rubbed
H hemic W woody H herbacious
L Hmnic S sphagnum C coprogenous earth
S sapric D diatomaceous earth M marly
F ferrihumic U humilluvic
0 other L sulfidic
2.51.2 For Mineral Materials
ON sand OI silt OA clay
2.51.3 pH
pM pH meter (1:1 H20) pN pH (0.1 M CaCy pH Hellige-Truog
pL Lamotte-Morgan pB Bromthymol blue pC Cresol red
pP Phenol red pT Thymol blue pS soiltex
pY Ydrion pQ Bromcreso! green pR Chlorophenol red
2.52 Soil Moisture Codes
D dry M moist V very moist W wet
2.53 Quantity (Roots, Pores, Concretions)
VF very few FF very few to few F few FC few to common
CM common to many C common M many
2.54 Size (Roots, Pores, Concretions)
M micro Ml micro and fine V1 very fine
11 very fine and fine 1 fine 12 fine and medium
2 medium 23 medium and coarse 3 coarse
4 very coarse 5 extremely coarse 13 fine to coarse
2.55 Location of Roots
C In cracks M in mat at top of horizon
P between peds S matted around stones
T throughout
-------
Appendix A
Revision 2
Date: 2/87
Page 40 of 40
2.56 Shape of Pores
IR interstitial
IT interstitial and tubular
TU tubular
TO discontinuous tubular
TS constricted tubular
VT vesicular and tubular
IE filled with coarse material
IF void between rock fragment
TC continuous tubular
TE dendritic tubular
VS vesicular
TP total porosity
2.57 Kind of Concentrations
B1 barite crystals
K2 soft masses of carbonate
K4 carbonate nodules
C2 soft masses of lime
C4 lime nodules
13 insects casts
A2 clay bodies
D2 soft dark
D4 dark nodules
E4 gibbsite nodules
Q2 masses of gypsum
F2 soft masses of iron
F4 ironstone nodules
M2 soft masses of iron-manganese
M4 magnetic shot
H2 salt masses
S2 soft masses of silica
S4 durinodes
2.58 Shape of Concentrations
B2 soft masses of barite
K3 carbonate concretions
C1 calcite crystals
C3 lime concretions
T2 worm casts
T4 worm nodules
D1 mica flakes
D3 dark concretions
E3 gibbsite concretions
G1 gypsum crystals
F1 plinthite segregations
F3 iron concretions
M1 nonmagnetic shot
M3 iron-manganese concretions
H1 halite crystals
S1 opal crystals
S3 silica concretions
C cylindrical
T threads
0 dendritic
Z irregular
O rounded
P plate like
2.59 Rock Fragment Kind Codes
Y mixed lithology
S sedimentary rocks
A sandstone
H shale
K organic fragments
0 oxide-protected rock
I igneous rocks
F ironstone
M metamorphic rocks
B mixed sedimentary rocks L limestone
T siltstone
P pyroclastic rocks
E ejecta
R saprolite
2.60 Rock Fragment Size Codes
1. 20 to 76 mm
2. 76 to 250 mm
3. >250 mm
-------
Appendix B
Revision 2
Date: 2/87
Page 1 of 64
Appendix B
Forms for Reporting Analytical Laboratory Data
The following forms are used for recording raw data and results from the analytical
procedures detailed in Sections 3.0 through 16.0 of Analytical Methods Manual for the Direct/Delayed
Response Project Soil Survey by K. A. Cappo, L J. Blume, G. A. Raab, J. K. Bartz, and J. L Engels,
U.S. Environmental Protection Agency, Las Vegas, Nevada, 1987.
An index of data forms is presented on the following page. Form 101 summarizes data from
the preparation laboratory. Form 102 is a shipping form that is used to confirm sample shipment
and receipt. Forms 103a and 103b summarize pH, moisture, and particle size analysis results.
Forms 109 through 114 contain quality control data. The 200-series forms summarize data that are
corrected for both blanks and dilutions. Raw data are recorded on forms 115, 116, 303b, 306, and
308.
-------
Appendix B
Revision 2
Date: 2/87
Page 2 of 64
Index of Data Forms
Form Number
Title
101
102
103 (a,b)
109 (a.b.c)
110 (a.b.c)
111 (a through i)
112 (a through h)
113
114 (a.b.c)
115 (a through e)
116 (a through h)
204 (a,b,c,d)
205
206
207
208
303b
306
308
Preparation Laboratory Data
Shipping Form
Summary of pH and Particle Size Results
Quality Control: Detection Limits
Quality Control: Matrix Spikes
Quality Control: Replicates
Quality Control: Blanks and QCCS
Quality Control: Ion Chromatograph Resolution
Test
Quality Control: Standard Additions
Sample Weight in Grams
Dilution Factors and Dilution Blanks; Solution
Concentration; Titer and Normality
Summary of Exchangeable Bases and CEC
Results Blank Corrected
Summary of Iron- and Aluminum-Extraction
Data Blank Corrected
Summary of Extractable Nitrate and Sulfate,
Exchangeable Acidity, and Exchangeable
Aluminum Blank Corrected
Summary of Sulfate-Adsorption Isotherm Data
Blank Corrected
Summary of C, N, S, and Specific-Surface
Results Blank Corrected
Summary of Particle Size Analysts Raw Data
Summary or BaCI2 Exchangeable Acidity Raw
Data
Summary of C, N, S, and Specific Surface Raw
Data
-------
Appendix B
Revision 2
Date: 2/87
Page 3 of 64
DIRECT/DELAYED RESPONSE PROJECT (DORP) FORM 101
Bitch ID
Cre« ID
DATE RECEIVED
BY DATA MGT.
TT T~ TT TT
Bitch Sent to
Date Shipped
No. of Simples
Set ID
itte Stapled
Jtte Received
Dtle Prep Completed
Set ID
Dtte Sampled
Out Received
D«te Prep Completed
Staple
Mo.
01
02
03
04
05
06
07
06
05
10
11
12
13
14
IS
16
17
IB
19
20
21
22
23
24
Zi
26
27
26
29
30
31
32
33
34
35
36
37
36
3?
40
4]
Site ID
42
Staple Code
Set
ID
Signature of Preptrttlon Laboratory Mtnager
Cruar nts:
Rock
Frtgnents
weioht S
,
Air Dried
Hofslure
wfioht I
— — — —
__-_---_
Soil
Type
H • KIN
0 • ORG
Inorg
Ctrbon
(1C)
Y • Yei
N • NO
1
Bulk
Density
C/CC
WHITE - ORKl COPY
GOLD - ERL-C COPY ULLOW - PREPARATION LAB COPY PINK - EMSL-LV COPY
-------
Appendix B
Revision 2
Date: 2/87
Page 4 of 64
DIRECT/DELAYED RESPONSE PROJECT (ODRP) SOIL SURVEY
SHIPPING FORM 102
DATE RECEIVED
BY DATA MGT.
"IT ~tT ~W ~W ~R 7 T
Prep L
Batch
Analyt
Sample
Number
in
U2"
"133 '
~54
133 1
06 '
157
"58
~D~9
10
~n '
2
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
it> ID Date Received
D D M M M Y Y
ID Date Shipped
cal Lab ID
Sample
(Identify By Check)
Shipped Received
Soil Type
(Identify By Check)
Organic Mineral
Signature of Preparation laboratory Mane
Comments :
Inorganic
Carbon
Y - Yes
N - No
Rock
Fragments
Shipped
Check if Yes
ger:
Unite - SMO Canary - Analytical Pink - Analytical Gold - Analytical
with copy to SMO with copy to EMSL-LV Lab
-------
Appendix B
Revision 2
Date: 2/87
Page 5 of 64
SUMMARY OF pH AND MOISTURE DATA
DIRECT/DELAYED RESPONSE PROJECT (DDRP) SOIL SURVEY REPORT FORM 1033
Analytical Lab ID Lab Manager's Signature
Batch ID Date Form Completed
Prep Lab Name Date Batch Received
Remarks
Sample
Number
01
02
03
04
05
06
07
06
09 "•'
10
11
12
13
14
15
1C
17
'16
19
20
21
22
•23
?«•
25
U
27
•?8
"29
36
31
32
33
3*
35
U
37
36
34
40
41
42
PK
In H20
PH
in 0.01M
CiCl2
PH
in 0.002M
CaClj
Moisture,
height
:
-------
Appendix B
Revision 2
Date: 2/87
Page 6 of 64
PARTICLE SIZE ANALYSIS DATA
DIRECT/DELAYED RESPONSE PROJECT (ODRP) SOIL SURVEY REPORT FORM 103b
Analytical Lab 10 Lab Manager's Signature
Batch ID ~~~~"~~"~~~~~"~'~'~~
Prep Lab Name
Remarks ~~~~~~~"""""""""""~"~~
Date Form Completed
Date Batch Received
Particle Size Analysis, Weight J
Size Class and Particle Diameter (mm)
Sample
Number
01
02
03
04
05
06
07
06
09
10
11
12
13
14
15
16
17
16
19
20
21
22
23
24
25
26
27
28
29
30
31
32 '
33
34
35
36
37
38
39
40
41
42
Sand
(2.0-
0.05)
Silt
(0.05-
0.002}
Clay
(<0.002)
Sand
Very
Coarse
(2.0-
1.0}
• .
Coarse
(1.0-
0.5)
Medium
(0.5-
0.25)
Fine
(0.25-
0.1)
Very Fine
10.1-
0.05}
Si1 It
Coarse
(0.05-
0.02)
Fine
(0.02-
0.002}
-------
Direct/Delayed Response Project (DDRP) Soil Survey
Form 109a
Quality Control: Detection Limits
Appendix B
Revision 2
Date: 2/87
Page 7 of 64
i_ao Name
Lab Manager's
Parameter
Total S
Total N
Total C
Inorganic C
CEC (FIA)
CEC (titration)
Exchangeable
BaCI2-TEA
KCI
KCI-AI3*
Reporting
Units
wt. %
wt. %
wt. %
wt. %
meq/100 g
meq/100 g
Aclditv:
meq/100 g
meq/100 g
meq/100 g
Instrumental
Contract-Required Detection Date Determined
Detection Limit Limit (DD MMM YY)
0.010%
0.050%
0.050%
0.010%
0.140 mg N/L
0.010 meq NH4+*
0.40 meq*
0.25 meq*
0.10 mg/L
*For titrations, the instrumental detection limit is a calculated value based upon a minimum titration.
-------
Direct/Delayed Response Project (DORP) Soil Survey
Form 109b
Quality Control: Detection Limits
Appendix B
Revision 2
Date: 2/87
Page 8 of 64
i_au ixcn 1 10
Lab Manager's
Parameter
Calculated
Reporting
Units
NH,OAc Extract:
Ca2+ meq/100 g
Mg2+ meq/100 g
K+ meq/100 g
Na+ meq/100 g
NH.CI Extract:
Ca2+ meq/100 g
Mgz+ meq/100 g
K+ meq/100 g
Na+ meq/100 g
0.002 M CaCU Extract:
Ca2+ meq/100 g
Mg2+ meq/100 g
K+ meq/100 g
Na* meq/100 g
Fe3+ meq/100 g
AI3+ meq/100 g
Contract-Required Instrumental
Instrumental Detection Date Determined
Detection Limit Limit (DD MMM YY)
0.050 mg/L
0.020 mg/L
0.020 mg/L
0.020 mg/L
0.050 mg/L
0.020 mg/L
0.020 mg/L
0.020 mg/L
*
0.020 mg/L
0.020 mg/L
0.020 mg/L
0.050 mg/L
0.050 mg/L
'Report the standard deviation of 10 non-consecutive blank analyses.
-------
Appendix B
Revision 2
Date: 2/87
Page 9 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 109c
Quality Control: Detection Limits
Lab Name
Lab Manager's Signature -
-Batch ID
Parameter
Calculated Contract-Required Instrumental
Reporting Instrumental Detection
Units Detection Limit Limit
Date Determined
(DD MMM YY)
SO2"4 Adsorption mg S/L
SO2'4 (H2O extract) mg S/Kg
NO"3 (H2O extract) mg N/Kg
SO2-4 (PC-3", extract) mg S/Kg
Pvrophosphate Extract:
Fe3+ wt. %
AI3+ wt. %
Acid-Oxalate Extract:
Fe3+ wt. %
AI3+ wt. %
Citrate-Dithionite Extract:
Fe3+
AI3+
wt. %
wt. %
0.10 mg SO2VL
0.1 mg SCfJL
0.10 mg NOyL
0.10 mg
0.50 mg/L
0.50 mg/L
0.50 mg/L
0.50 mg/L
0.50 mg/L
0.50 mg/L
-------
Appendix B
Revision 2
Date: 2/87
Page 10 of 64
DIRECT/DELATED RESPONSE PROJECT (DORP) SOIL SURVEY
FORM 1104
QUALITY COHTROL: MATRIX SPlKLS
LAB NAME
LAB MANAGER'S SIGNATURE
BATCH ID
Extracting
Parameter
1.0 K HH40AC
Ca.
•g/L
"9.
•9/L
K.
•9/L
Na.
•9/L
1.0 M NHaCl
Ca.
«9/L
"9.
•9/1-
K.
•9/L
Na.
•9/L
0.002 M UC12
Ca.
ng/L
HS.
•S/L
K.
DS/L
Na,
•9/L
Fe.
•9/L
Al.
ng/L
NONE
CEC
Nh**.
First Matri«
Spike Sample ID:
Sample Result
Spike Result
Spike Added
1 Recovery
Second Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
I Recovery
Third M»trU
Spike Sample ID:
Sample Result
Spike Result
Spike Added
J Recovery
1
•CEC units »re instrument and method dependent: Fill 1n «g K/L for flow Injection *n»ly»1s or men for
distlllation/tltration.
-------
Appendix B
Revision 2
Date: 2/87
Page 11 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 11Ob
Quality Control: Matrix Spikes
Lab Name Batch ID
Lab Manager's signature
Extractant
Parameter
Pyrophosphate
Fe,
mg/L
Al,
mg/L
Acid-
Oxalate
Fe,
mg/L
Al,
mg/L
Citrate-
Dithionite
Fe,
mg/L
Al,
mg/L
KCl
Al,
mg/L
First Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
Second Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
Third Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
-------
Appendix B
Revision 2
Date: 2/87
Page 12 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form HObb
Quality Control: Matrix Spikes
Lab Name
Lab Manager's Signature
Batch ID
Extractant
Parameter
Deionized
H2°
NO-,
mg/L
S02-,
mg/L
S02-,
mg/L
500 mg P/L
First Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
Second Matrix
Spike sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
Third Matrix
Spike Sample ID:
sample Result
Spike Result
Spike Added
% Recovery
-------
Appendix B
Revision 2
Date: 2/87
Page 13 of 64
Direct/Delayed Response Project (DORP) Soil survey
Form llOc
Quality control: Matrix Spikes
Lab Name
Lab Manager's Signature
Batch ID
Parameter
Total S,
Weight %
Total N,
Weight %
Total C,
Weight %
Inorganic c,
Weight %
<2 mm
2 -2 Omm
First Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
second Matrix
Spike Sample ID:
Sample Result
Spike Result
Spike Added
% Recovery
Third Matrix
Spike sample ID:
Sample Result
spike Result
Spike Added
% Recovery
-------
Appendix B
Revision 2
Date: 2/87
Page 14 of 64
Direct/Delayed Response Project (DDRP) Soil survey
Form HOd
Quality Controlt Matrix spikes
Lab Name
Lab Manager's signature
Batch ID
Parameter
Sulfate remaining in solution, mg S/L
Initial solution concentration, mg S/L
0
2
4
8
16
32
First Matrix
Spike Sample ID:
Sample Result
spike Result
spike Added
% Recovery
second Matrix
Spike Sample ID:
sample Result
spike Result
spike Added
% Recovery
Third Matrix
spike Sample ID:
sample Result
Spike Result
spike Added
% Recovery
-------
Appendix B
Revision 2
Date: 2/87
Page 15 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form Ilia
Quality Controlt Replicates
Lab Name
Lab Manager's Signature
Batch ID
Parameter
Triplicate
sample IDs
First Replicate
Result
Second Replicate
Result
Third Replicate
Result
Average
Standard
Deviation
% RSD
pH
in H20
NA
pH
in 0.01 M
CaCl2
NA
PH
in 0.002 N
Cacl2
NA
specific
surface,
m2/g
NA
-------
Appendix B
Revision 2
Date: 2/87
Page 16 of 64
Lab Name
Lab Manager's
Direct/Delayed Response Project (DDRP) Soil Survey
Form lllb
Quality Control: Replicates
Batch ID
Signature
Particle Size Analysis, Weight t
Sice Class and Particle Diameter (mm)
Parameter
Sand
Sand
(2.0-
O.OS)
Silt
(0,05)-
0.002)
clay
(<0.002)
Very
Coarse
(2.0-1.0)
Coarse
(1.0-
0.5)
Medium
(0.5-
0.25)
Fine
(0.25-
0.1)
Very
Fine
(0.1-0.05)
Silt
Coarse
(0.05-
0.02)
Fine
(0.02-
0.002)
Duplicate
Sample ID:
Sample
Result
Duplicate
Results
t RSD
Second Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
Third Duplicate
Sample IDs
Sample
Result
Duplicate
Result
» RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 17 of 64
Direct/Delayed Response Project (DDRP) soil Survey
Form lllc
Quality Control: Replicates
Lab Name
Lab Manager's signature
Batch ID
Extractant
Parameter
1.0 M NH4OAc
Ca,
meq/100 g
Mg,
meq/100 g
K,
meq/100 g
Na,
meq/100 g
CEC,
meq/100 g
Duplicate
Sample ID:
Sample
Result
Duplicate
Results
% RSD
Second Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
Third Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 18 of 64
Direct/Delayed Response Project (DDRP) Soil survey
Form 11Id
Quality Control: Replicates
Lab Name
Batch ID
Lab Manager's signature
Extractant
Parameter
1.0 M NH4C1
Ca,
meq/100 g
Mg,
meq/100 g
*/
meq/100 g
Na,
meq/100 g
CEC,
meq/100 g
Duplicate
Sample ID:
Sample
Result
Duplicate
Results
» RSD
Second Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
Third Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 19 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form llle
Quality Control: Replicates
Lab Name
Lab Manager'a Signature
Batch ID
Extractant
Parameter
0.002 M CaCl2
Ca,
meq/100 g
Mg,
meq/100 g
K/
meg/100 g
Na,
meq/100 g
CEC,
meq/100 g
Duplicate
Sample IDi
Sample
Result
Duplicate
Results
* RSD
Second Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
Third Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 20 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 11If
Quality Control: Replicates
Lab Name
Lab Manager's Signature
Batch ID
Extract
Parameter
Polyphosphate
Fe,
Weight %
Al,
Weight %
Acid-Oxalate
Fe,
Weight %
Al,
Weight %
Citrate-Dithionite
Fe,
Weight %
Al,
Weight %
Duplicate
Sample IDi
Sample
Result
Duplicate
Results
% RSD
Second Duplicate
Sample ID:
Sample
Result
Duplicate
Result
% RSD
Third Duplicate
Sample ID:
Sample
Result
Duplicate
Result
t RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 21 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form lllg
Quality Control: Replicates
Lab Name
Lab Manager'a
Batch ID
Signature
Extract
Extractable Nitrate,
mg N/kg
H20
Extractable Sulfate,
mg S/kg
H20
P04
Exchangeable Acidity
meq/100 g
BaCl2
KC1
Extractable Al,
meq/100 g
KCl
Duplicate
Sample IDi
Sample Result
Duplicate
Result
% RSD
Second Duplicate
Sample IDi
Sample Result
Duplicate
Result
t RSD
Third Duplicate
Sample ID:
Sample Result
Duplicate
Result
t RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 22 of 64
Direct/Delayed Response Project (DDRP) Soil survey
Form 11In
Quality Controlt Replicates
Lab Name
Lab Manager's
Batch ID
Signature
Parameter
Sulfate remaining in aolution, mg 8/L
Initial tolution concentration, mg 8/L
0
2
4
a
i«
32
Duplicate
Sample IDi
Sample Reiult
Duplicate
Reiult
I RSD
Second Duplicate
Sample IDi
Sample Reault
Duplicate
Reiult
1 RSD
Third Duplicate
Sample IDi
Sample Reiult
Duplicate
Reiult
I RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 23 of 64
Direct/Delayed Response Project (DDRP) soil survey
Form llli
Quality Control: Replicates
Lab Name
Lab Manager's signature
Batch ID
Parameter
Duplicate
•ample IDs
Sample Reiult
Duplicate
Reault
I RSD
Seoond Duplicate
Sample IDI
Sample Result
Duplicate
Reiult
1 RSD
Total
s,
Height I
Total
at,
Height I
Total
c,
Height I
Inorganic C,
Height I
<2 mm
2-SOmm
Third Duplicate
Sample IDi
Sample Reiult
Duplicate
Reeult
I RSD
-------
Appendix B
Revision 2
Date: 2/87
Page 24 of 64
Direct/Delayed Response Project (DDRP) soil Survey
Form 112a
Quality Control: Blanks and QCCS
Lab Name
Lab Manager'a Signature
Batch ID
Parameter
Reagent Blank*
DL Theoretical
QCCS Measured
Low QCCS
True Value
Low QCCS
Upper Limit
Lower QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
pH
in H2O
HA
NA
pH
in 0.01M
CaCl2
NA
NA
pH
in 0.002M
CaCl2
NA
NA
•Reagent blank is the solution being added to the soil.
-------
Appendix B
Revision 2
Date: 2/87
Page 25 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 112b
Quality Control: Blanks and QCCS
Lab Name
Lab Manager's Signature
Batch ID
Particle Size Analysis, Weight %
Size Class and Particle Diameter (mm)
Sand
Parameter
Reagent
Blank
DL QCCS
Theoretical
Measured
Low QCCS
True Value
Low QCCS
Upper Limit
Low QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
Sand
(2.0-
0.05)
NA
NA
NA
Silt
(0.05-
0.002)
NA
NA
NA
Clay
(<0.002)
NA
NA
Very
Coarse
(1.0-
1.0)
NA
NA
NA
Coarse
(1.0-
0.5)
NA
NA
NA
Medium
(0.5-
0.25)
NA
NA
NA
Fine
(0.25-
0.1)
NA
NA
NA
Very
Fine
(0.1-
0.05)
NA
NA
NA
Silt
Coarse
(0.05-
0.02)
NA
NA
NA
Fine
(0.02-
0.002)
NA
NA
NA
-------
Appendix B
Revision 2
Date: 2/87
Page 26 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 112c
Quality Control: Blanks and O.CCS
Lab Name
Lab Manager's Signature
Batch ID
Extractant
Parameter
Calibration
Blank
Reagent Blank 1
Reagent Blank 2
Reagent Blank 3
DL Theoretical
QCCS Measured
Low QCCS
True Value
Low QCCS
Upper Limit
Lower QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
1.0 M NH4OAc
Ca,
mg/L
Mg,
mg/L
K,
mg/L
Na,
mg/L
CEC,
1.0 M NH4C1
Ca,
mg/L
Mg,
mg/L
K,
mg/L
Na,
mg/L
CEC,
*CEC reporting units are instrument and method dependent.
for distillation/titration.
Fill in mg N/L for flow injection analysis or meq
-------
Appendix B
Revision 2
Date: 2/87
Page 27 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 112d
Quality Control: Blanks and QCCS
Lab Name
Lab Manager's Signature
Batch ID
Extractant
Parameter
Calibration
Blank
Reagent Blank*
DL Theoretical
QCCS Measured
Low QCCS
True Value
Low QCCS
Upper Limit
Lower QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
0.002 H CaCl2
Ca,
mg/L
Mg,
mg/L
K,
mg/L
Na,
mg/L
Fe,
mg/L
Al,
mg/L
*Analyze 0.002 M CaCl2 solution that has been extracted through filter pulp.
-------
Appendix B
Revision 2
Date: 2/87
Page 28 of 64
Direct/Delayed Response Project (DDRP) Soil survey
Form 112e
Quality Control: Blanks and QCCS
Lab Name
Lab Manager's Signature
Batch ID
Extractant
Parameter
Calibration
Blank
Reagent Blank*
DL Theoretical
QCCS Measured
Low QCCS
True Value
Low QCCS
Upper Limit
Lower QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
Phosphate
Fe,
mg/L
Al,
mg/L
Acid-Oxalate
Fe,
mg/L
Al,
mg/L
Citrate-Dithionite
Fe,
mg/L
Al,
mg/L
-------
Appendix B
Revision 2
Date: 2/87
Page 29 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 112f
Quality Control: Blanks and QCCS
Lab Name
Lab Manager's signature
Batch ID
Parameter
Extract ant
Calibration
Blank
Reagent Blank 1
Reagent Blank 2
Reagent Blank 3
DL Theoretical
QCCS Measured
Low QCCS
True Value
Low QCCS
Upper Limit
Lower QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
Extractable Nitrate,
mg/L
H2O
Extractable Sulfate
mg/L
H20
Po3-
4
Extractable Acidity,
mg/L
Bad 2
KC1
Extractable Al,
mg/L
KCl
•Reagent blank is the extracting solution.
-------
Appendix B
Revision 2
Date: 2/87
Page 30 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 112g
Quality controlt Blanks and QCCS
Lab Name
Lab Manager's Signature
Batch ID
Parameter
Calibration
Blank
Reagent Blank*
DL Theoretical
QCCS Meaiured
Low QCCS
True Value
LOW QCCS
Upper Limit
Lower QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Upper Limit
High QCCS
Lower Limit
Initial
Continuing
Continuing
Final
Total
a,
Weight \
NA
Total
H,
Weight »
IF
X
Factor
pv/yg
NA
HA
Total
c,
Weight I
X
Factor
vv/yg
NA
NA
Inorganic C,
Weight t
<2 m 2-20mm
-------
Appendix B
Revision 2
Date: 2/87
Page 31 of 64
Direct/Delayed Response Project (DDRP Soil Survey
Form 112h
Quality Control: Blanks and O.CCS
Lab Name
Lab Manager's signature
Batch ID
Parameter
Low QCCS
True Value
Low QCC8
Upper Limit
Low QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High sees
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Final
Specific
Surface, nr/g
(at equilibrium)
Day*
0
1
2
3
4
5
6
7
a
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
2!
26
27
28
Weight of EGHZ in mg
Blank 1
Blank 2
Blank 3
*Mea«uremente may be taken leu frequently than daily, but record the reiulti on the day actually performed.
-------
Appendix B
Revision 2
Date: 2/87
Page 32 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 112i
Quality Control: Blanks and QCCS
Lab Name
Lab Manager's signature
Batch ID
Parameter
Reagent Blank
Low QCCS
True Value
Low QCCS
Upper Limit
Low QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Final
High QCCS
True Value
High QCCS
Lower Limit
Initial
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Continuing
Final
Sulfate remaining in solution, mg S/L
Initial solution concentration, mg S/L
0
2
N/A
4
N/A
8
N/A
16
N/A
32
N/A
-------
Appendix B
Revision 2
Date: 2/87
Page 33 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 113
Quality Control: Ion Chromatography Resolution Test
Lab Name Batch ID
Lab Manager's Signature
DateofAnalysisMM/DD/YR
1C Make and Model:-
Concentration „ Peak Area . . Peak Height
(mg/L) (integrator units) (cm)
SO%
PC-%
NO"3
Column Back Pressure (at max. of stroke): psi
Flow Rate: mL/min
Column Model: Date of Purchase:
Column Manufacturer:
Column Serial No:
Precolumn in system Yes No
*100 x 2(tr2-tr,)/(W1+WJ NO3 - PO4
Percentage Resolution: 100 x 2(tr2-tr1)/(W1+W2) PO4 - SO4
100x2*tr3-tr1)/(w1+W3) NO3-SO4 —
The resolution must be greater than 60%.
Test Chromatogram:
(FACSIMILE)
Calculations may change if order of elution is different from test chromatogram.
-------
Appendix B
Revision 2
Date: 2/87
Page 34 of 64
Direct/Delayed Response Project (DDRP) Soil survey
Form 114a
Quality Control: standard Additions
Lab Name
Batch ID
Lab Manager's signature
Extract
Parameter
1.0 M NH4OAC
Ca,
mg/L
Mg,
mg/L
K,
mg/L
r Na,
mg/L
1.0 M NH4C1
Ca,
mg/L
Mg,
mg/L
K,
mg/L
Na,
mg/L
Original
Sample ID:
Single
Response
Spike Added
Concentration
Sample Spike
1 Response
Spike 2
Concentration
Sample Spike
2 Response
Sample Con-
centration for
Original
Sample (calc. )
-------
Appendix B
Revision 2
Date: 2/87
Page 35 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 114b
Quality Control: Standard Additions
Lab Name
Batch ID
Lab Manager's signature
Extract
Parameter
1.0 M NH4OAC
Ca,
mg/L
Mg,
mg/L
K,
mg/L
Na,
mg/L
Fe,
mg/L
Al,
mg/L
Pyro-
phosphate
Fe,
mg/L
Al,
mg/L
Acid-
Oxalate
Fe,
mg/L
Al,
mg/L
Citrate
Dithionite
Fe,
mg/L
Al,
mg/L
Original
Sample ID:
Single
Response
spike Added
Concentration
Sample Spike
1 Response
Spike 2
Concentration
Sample Spike
2 Response
Sample Con-
centration for
Original
Sample (calc.)
-------
Appendix B
Revision 2
Date: 2/87
Page 36 of 64
Direct/Delayed Response Project (DDRP) Soil Survey
Form 114c
Quality Control: Standard Additions
Lab Name
Batch ID
Lab Manager's Signature
Extract
Parameter
H20
S02-
mg/L
PO3~
4
S02-
mg/L
KCL
Al,
mg/L
None
S02-
mg/L
Total
s,
wt %
Total
N,
wt %
Total
c,
wt %
Organic C,
wt %
<2mm
2 -2 Omm
Original
Sample ID:
Single
Response
Spike Added
concentration
Sample Spike
1 Response
Spike 2
Concentration
sample Spike
2 Response
Sample Con-
centration for
Original
Sample (calc. )
-------
Appendix B
Revision 2
Date: 2/87
Page 37 of 64
Air Dry Sample Weight in Grams
Direct/Delayed Response Project (DDRP) Soil Survey
Form 115a
Lab Name •
•Batch ID
Lab Manager's Signature
Sample
Number
01
0?
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
16
19
20
2;
22
23
24
25
26
27
26
29
30
31
32
33
3<
35
Moisture*
Dup 1
Air
36
37
36
39
4C
4]
42
Rep ic
Rep 2
her 3t
Oven
Dup 2
Air
1
NA
NA
Oven
NA
NA
NA NA
Particle Size
Analysis"
CLL andHfiTchangeaule
Cations
NH4OAc
1
1
NHaCl
'Moisture is performec In duplicate; place one sample weight in eacn column. First column
is air-dry weight, second column is oven-dry weight.
^Replicates are recorded here; the sample weight recorded by the sample number is repeated
as Rep 1.
cNot all methods require three replicates.
"Oven-dry weight after organic natter removal.
-------
Appendix B
Revision 2
Date: 2/87
Page 38 of 64
Air Dry Sample Weight in Grams
Direct/Delayed Response Project (DDRP) Soil Survey
Form 115b
Lab Name •
•Batch ID
Lab Manager's Signature
Simple
Number
01
02
03
00
05
06
07
oe
09
10
11
12
13
14
IS
16
17
16
19
20
21
22
23
24
25
26
27
26
29
30
31
32
33
3«
36
37
36
IB
«:
42
wi •
win
wpv-
Exchangeable Cations
in 0.002 H CaCl2
,
Exchangeable Acidity
Bid 2
KC1
'"fcepl kites
-------
Appendix B
Revision 2
Date: 2/87
Page 39 of 64
Air Dry Sample Weight in Grams
Direct/Delayed Response Project (DDRP) Soil Survey
Form 115c
Lab Name •
•Batch ID
Lab Manager's Signature
Simple
Number
01
0?
03
04
OS
06
07
08
09
10
11
1?
13
14
15
16
17
ie
19
20
21
22
23
2«
25
26
27
26
29
30
31
3?
3J
3«
36
36
37
36
39
tit
41
42
ReD 1*
we 2
Mt 3"
ExtricUble Fe »nd Al
Pyrophosphite
ACld-
Omlite
curate-
DUhionHe
i
K20 Cxtrictable
SOJ* «nd NOj
PO?" Utractilile
so«"
i
•RepiKives tre recoroeo here, the simple weight recorded oy the simple number is repeneo
as Rep 1.
••Not «11 methods require three replleites.
-------
Appendix B
Revision 2
Date: 2/87
Page 40 of 64
Air Dry Sample Weight in Grams
Direct/Delayed Response Project (DDRP) Soil Survey
Form 115d
Lab Name •
•Batch ID
Lab Manager's Signature
Sample
Number
01
02
03
01
05
06
07
08
09
10
11
1?
13
14
15
16
17
16
19
20
21
22
23
2t
2b
Zb
27
26
?§
30
31
32
33
3*
3, ,, ,
36
37
36
39
40
41
J-f - '
Rep V
Keo 2
Rep 3*«
SuHate Adsorption Isotherm
Initial bolution Concentration, mg b/L
0
2
4
e
1
i
I
16
32
I
number is repeated as Rep 1.
"Not all methods require three replicates.
-------
Appendix B
Revision 2
Date: 2/87
Page 41 of 64
Air Dry Sample Weight in Grams
Direct/Delayed Response Project (DDRP) Soil Survey
Form 115e
Lab Name •
-Batch ID
Lab Manager's Signature
Sample
Number
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
IB
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
36
39
40
41
42
Rep ifc
kec 2
ker 3C
Total S,
mg
Total N,
mg
Specific
Surface,4
9
7ota1 C.
mg
1
i
t
Inorganic C,
<2 mil.
2-20 mm
i
1
i
!
P.Ur • ory weight.
cates are recorded here; the sample weight recoroed b> the sample number
is repeated as Rep 1.
all methods require three replicates.
-------
Exchangeable Basic Cations in NH4OAc
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116a
Appendix B
Revision 2
Date: 2/87
Page 42 of 64
Lab Name -
-Batch ID
Lab Manager's Signature
Sample
Number
01
0?
03
04
Ob
06
07
06
09
10
1 1
12
13
14
Ib
16
17
16
19
20
21
22
2~
24
25
26
27
2fi
2°
3C1
Solution
Recovered
in
Syringe ImL
Aliquot Volume (mL)*
Ca
Mg
i
31 !
32
3.'
34
3S
36
37
3f
39
40
41
4/
K
Na
1
!
Exchangeable Basic Cations in Nh^OAc
Total Dilution Volume (mL)*
Ca
Mg
1
|
K
1
1
Na
1
Solution Concentration (mg/L)
Ca
Mg
I
|
K
|
NO
|
|
I i
1
Blank
D-Blank
D-Blank
Total Volume
in Sample (ml)
D-Blank 1
D-Blank
Aliquot Volume
in Dilution (ml)
Total Volume
ef Di lution (mL)
i
D-Riank i |
D-Blank i
Ui lution Blank
Concentrations (mg/L)
Ca
Mg
]
1
K
Na
•Enter u if no dilution is made.
-------
Exchangeable Basic Cations in NH4CI
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116b
Appendix B
Revision 2
Date: 2/87
Page 43 of 64
Lab Name •
-Batch ID
Lab Manager's Signature
Sample
Number
01
02'"
03
'04
K
Of
07
-OB
09
1C
1
1?
3
\i
15
U
7
16
19
26
21
2?
"23
24
25
2£
~T>
26
2'
3P
Exchangeable Basic Cations in Nh/iCl
Solution
Recovered
in
Syringe (mi'.
32
33
34
35
. t>
37
3E
39
it)
41
4'
AUauot Volume (ml)*
Ca
Mg
K
Na
Total Dilution Volume (mU*
U
Mg
i
K
Ka
Solution Concentration (mg/L)
Ca
Hg
K
i
Ka
I
Blank
D-Blank
)-Biank
D-Elant
(-B1an.
^-Blank
D-Biank
Total Volume
in Sample (ml.)
Al iquot Volume
in Dilution (ml)
Total Volume
of Dilution (ml)
1
In lution 81 ahl
Concentrations (mg/L)
Ca
Mg
K
ha
•Enter u if no dilution is made.
-------
Appendix B
Revision 2
Date: 2/87
Page 44 of 64
Cation Exchange Capacity
Dilution Factors and Dilution Reagent Blank Values; Titer and Normality
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116c
Lab Name •
-Batch ID
Lab Manager's Signature
Blank
D-Blani
D-Bianik
[-Blank
Cation Exchange Capacity (F1A)
lolal
Volume in
Sample (ml)
Aliquot
Volume
(ml)
l
Dilution
Volume
(ml.)
Di lution
Cone, (mg N/L)
Kn^UAc
Nn^Ll
1
1
Sample
Number
cn
nj
"A3
c<
OS
ne
d?
06
09
10
u
\t
13
]<
Ii
ie
17
1 8
1«
?0
21
2?
73
?4
?s
?t
7 '
2s
21
3d
31
3?
33
?4
35
~36
37
3F
Cation txchange Capacity (F1A)
Total
Volume in
Sample (ml)
Al iquot
Volume (ml)*
NH^OAc
I
i
KH^Cl
!
i
!
3* ! !
*P
41
«?
Total Dilution
Volume (mil*
NH^OAc
NH4C1
i
Sol ution
Cone, ma K7L)
NH4OAc
NH4C1
i
•
1
Lation Lxciidngc-
Capacity duration]
NHaOAc
Titer
(Volume
in ml )
i
Normal i ly
of
Titrant
Sh4Cl
Ti ter
(Volume
in ml )
1
formality
ot
Titrant
i
1
•Enter U if no additional is made.
-------
Appendix B
Revision 2
Date: 2/87
Page 45 of 64
KCI-Exchangeable Acidity and Extractable Aluminum
Dilution Factors and Dilution Reagent Blank Values; Titer and Normality
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116cc
Lab Name
•Batch ID
Lab Manager's Signature
Sample
Number
01
02
03
04
05
06
6}
08
09
10
11
12
13
14
15
16
17
16
19
20
21
22
J3
?<
25
2i
27
•7fi
20
3fl
31
3?
33
3i
35
36
37
3S
39
4&
il
Solution
Recovered
in Syringe
(ml)
12 1
KCl-[xtractable Al
Aliquot
Volume
ImD"
Total Dilution
Volume (ml)*
Solution
Cone. (mg/L)
1
KLI-L*changeoUle
Acidi Vy
T1 ter
(Volume
in ml)
Normal i ly
of
Ti trant
Blank
D-Bl»nk
D-Blank
D-Blank
Total
Volume in
Sample (nL)
KCl-Extractable Al
Aliquot
Volume
(mL)
Total
Dilution
Volume (ml)
Dilution
Cone. (mc/L)
KC1
•Inter U it no dilution li IMOE.
-------
Exchangeable Basic Cations in CaCI2
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116d
Appendix B
Revision 2
Date: 2/87
Page 46 of 64
Lab Name •
•Batch ID
Lab Manager's Signature
Sample
Number
Ol
Tl?
TJ3 '"
04
-IJ5 '
T)6
07
Tip" '
"W
IS
-II "•
•'1?
"'13 '
"If '
""15
-TZ
Total
Volume In
Sample (ml)'
-7
'»
"1?
"2fl "
-?! '"•
-jj
-?«• -
T5
11 V
-?{•"""
no1 "•
•5 •
IT
-jr
TS1 ""
-36 ""
~37
"T5
"39 ' '
•*o "
-J]
1
Aliquot Volume (ml)1'
C«
Mg
K
N4
Uctiongsable Basic Cauoni in CaClj
Totil Pilution Volume (mL)b
Ca
Mg
K
Na
Solution Concentration
Ca
1
Mg
K
Img/L)
Ka
I
Blank
"B=Trr»h"H
|"B-81ani( |
1-61 ink
T-Blinl
•&-r«nk
Total Volume
Al iQuot Volume
1n DUutlon ImL)
Total Volume
of Dilution (ml)
Concentrations (mg/L)
Ca
HS
K
Ka
'Volume adoed for extraction,
6[nt«r U
-------
Exchangeable Fe and Al In CaCI2
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116e
Appendix B
Revision 2
Date: 2/87
Page 47 of 64
Lab Name •
•Batch ID •
Lab Manager's Signature
Simple
Number
01
0?
Oi
04
Oh
06
07
OB
09
10
1J
?
3
I
&
6
7
8
1
1
3
t,
$
6
7
8
9
, 0
~~I 1
, 2
, A
. 5
""IT"
37
"T?
3*
— n 1
[urteubli Ft ind Al In CtClj
Tout
Volume In
Umplo
lnL)«
~~n
All QUO t
Volum* |nL)b
Fl
Al
To til Dilution
Veluw lffiL)l>
Fl
Al
Solution
Cone. Img/l)
Fl
Al
Soli T»p«
Mlniril IM)
or
Org.
'Soil to solution ritlo Is ixpressed «i 1:«; enter
the vilue of «.
-------
Exchangeable Fe and Al in Pyrophosphate
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116ee
Appendix B
Revision 2
Date: 2/87
Page 48 of 64
Lab Name •
Batch ID
Lab Manager's Signature
Sample
K umber
01
2
03
04
'5
55
17
06
53
10
n i
13
TE 1
n
TB
R
JiT
21 1
22
?3
?<:
25
26
n
JB
30
31
3?~
31
3«
3?
36
37
36
3?
40
4;
-------
Exchangeable Fe and Al in Acid-Oxalate
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116f
Appendix B
Revision 2
Date: 2/87
Page 49 of 64
Lab Name
•Batch ID
Lab Manager's Signature
Sample
Nuntoer
01
02
03
P4
Ob
06
07
08
09
10
11
12
13
U
IS
16
17
18
19
20
21
22
23
24
25
26
27
26
29
30
31
32
33
34
3S
J(-
Extractablc Fe and Al in Acid-Oxalate
Total
Vo 1 ume
in Sample
(mil*
Al iquot
Volume (mL)11
Fe
1
1
37 |
36
39
Al
Total Dilution
Volume (ml)lJ
Fe
Al
Solution
Cone. (rog/L)
Fe
1
1
Al
1
1
i
40
41
42 1
BUnk
D-Bisnt
[>-Blank
D-Blank
p-Blank
D-Blank
D-Blank
£xtractable Fe and Al in Acid-Oxalate
Total
Volume in
Sample (ml)
Al iquot
Volume
(ml)
Di lution
Vo 1 ume
(ml)
Di lution
Cone. (mg/L)
re
i
A!
'Volume adced for extraction.
bE.nter U if no dilution is made.
-------
Extratable Fe and Al in Citrate-Dithionite
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116ff
Appendix B
Revision 2
Date: 2/87
Page 50 of 64
Lab Name
-Batch ID
Lab Manager's Signature
Sample
Number
01
2
03
fw
U5
06
7
55
9
TP
n
7
n
U"
15
ITS
n
19
0
ZT
2
S
Total
Vo 1 ume
in Sample
Extracuble Fe and Al in Ci trate-Di thioni te
Al iquot
Volume (mL)b
Fe
1
Al
Total Dilution
Volume (mL)b
Fe
0
7
6
3o
31
32
33
34
35
36
37
36
39
-------
Appendix B
Revision 2
Date: 2/87
Page 51 of 64
Water Extratable Sulfate and Nitrate
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116g
Lab Name •
-Batch ID
Lab Manager's Signature
Sample
Kumber
01
0?
03
04
05
06
07
OE
09
10
J]
1? 1
Ij
14
15
16
17
16
19
20
21
22
23
2<
2J
26
27
26
2?
30
31
3?
33
34
3S
36
Si
3e
39
HzO ExtracUble Nitrate
Total
Volume
in Sample
(mU»
Al iquot
Volume
lmL)b
1
I
40
41
4?
Total
Dilution
Vo 1 umc
(ml)"
1
Solution
Concentration
(mg/L)
H^O Extractable Sultate
Al iquot
Vo 1 unie
InL)"
Total
Dilution
Volume
(mL)b
i
i
Solution
Concentration
(mg/L)
Blank
D-BIank
0-Blani,
D-Blani,
Total Volume
in Sample (ml)
Aliquot Volume
in Dilution (ml)
Total Volume
of Dilution (ml)
Dilution Blank
Concentrations
N03
soj-
'Volume adoeo for extraction.
Hnter U if no dilution is made.
-------
Appendix B
Revision 2
Date: 2/87
Page 52 of 64
Lab Name •
Phosphate Extratable Sulfate
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116gg
Batch ID —
Lab Manager's Signature
Sample
Number
01
0?
03
04
05
06
07
OS
09
10
1]
12
13
14
15
16
17
16
19
20
21
22
23
24
25
PO^" Utractable Sulfate
Total
Volume
in Sample
(«L)»
26 1
Z7
28
29
30
31
32
33
3'
35
3c
37
36
39
40
41
42
A) iquot
Volume
(ml)b
!
Total
Oi lution
Volume (mL)b
Solution
Concentration
Img/L)
1
!
i
1
Blank
[(-Blank
p-Biank
Total volume
in Sample
ImL)
fi-Blank
Aliquot Volume
in Dilution
ImL)
Total Volume
of Dilution
(ml)
i
!
1
Dilution Blink.
Concentration
(mg/L)
a Volume adaec tor extraction.
DEnter u if no dilution is mane.
-------
Sulfate Adsorption Isotherms
Dilution Factors and Dilution Reagent Blank Values
Direct/Delayed Response Project (DDRP) Soil Survey
Form 116h
Appendix B
Revision 2
Date: 2/87
Page 53 of 64
Lab Name •
Batch ID
Lab Manager's Signature
Simple
NumOer
0!
(12
03
04
K
06
Ofe
09
1 10 I
'11
I?
!"
]i "
15
16
7
Sulfale Adsorption Isotherm
Total
Volume
in Sample
(ml)4
Al iQuol
Volume (mL)b
0
1 1* 1
2
20
-jn ' J"
23
?4
Jf
~7T
r?p
~7^ —
3('
32
35 "
35
Sf
37
3f
34
1 •»!
«
4
8
'Volume aooec for aasorp
''Enier U 1 f no dilution
16
33
Total
Dilution Volume (mL)b
0
2
1
4
B
16
1
1
32
Solution
Concentration (mo/L)
U
2
1
1
1 1 1
4
b
lo
32
i
1 !.!..!
1
1 ,
lor. .
is made.
-------
Appendix B
Revision 2
Date: 2/87
Page 54 of 64
Summary of Exchangeable Cations in NH4OAc
Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 204a
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Simple
Number
01
02
UJ
04
OS
06
07
Of!
09
1(1
11
u
13
14
15
16
17
18
19
20
21
22
2}
?4
25
26
27
J8
?9
35
31
32
"T!
Cuchtngeable Citlont in NH^OAc,
meq/lOug
U
34
'"35 '
35
37
3*
39" "
46
41
4?
M;
1
K
ha
-------
Appendix B
Revision 2
Date: 2/87
Page 55 of 64
Summary of Exchangeable Cations in NH4CI
Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 204b
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Simple
Number
01
0?
OJ
01
05
Ub
07
08
09
10
11
12
13
14
IS
16
17
18
19
20
Zl
Z2
23
Z4
25
Z6
27
26
2?
3P
31
32
33
3«
31
3C
37
36
39
<0
41
42
Exchangeable Cations In NH^Cl,
•eq/lOOg
Ca
M9
K
|
1
Ha
-------
Appendix B
Revision 2
Date: 2/87
Page 56 of 64
Summary of Exchangeable Cations in 0.002 M CaCI2
Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 204c
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Simple
Nimber
01
0?
03
0<
05
06
0'
0£
10
n
12
13
14
15
16
n
)6
15
20
21
22
ZJ
24
2B
Z6
21
28
ZS
30
31
$e
33
3<
35
36
37
38
39
40
41
42
Exchangeable Cations in 0.002 M Cad2,
meq/lOOg
Ca*
M9
1
K
Na
Fe
i
|
i
Al
1
i
i
i
•Reported oata may be negative.
-------
Appendix B
Revision 2
Date: 2/87
Page 57 of 64
Summary of Cations Exchange Capacity (CEC)
Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 204d
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Sample
Number
01
02
03
04
05
06
07
08
0$
10
11
12
13
14
15
16
17
18
19
20
21
CEC,
meq/lOOg
NH4OAc
NH4C1
CEC,
meq/lOOg
NH4OAc
22
23
24
2b
26
21
28
29
30
31
32
33
34
3b
36
3/
38
39
4U
41
42
NH4C1
-------
Appendix B
Revision 2
Date: 2/87
Page 58 of 64
Summary of Extractable Iron and Aluminum Data
Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 205
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Sample
Number
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
30
31
32
33
34
35
36
37
38
39
40
41
42
Pyrophosphate
Extractable,
Weight 1
Fe
Al
Acid-Oxalate
Extractable,
Weight 1
Fe
Al
Ci trate-Di thioni te
Extractable.
Weight 1
Fe
Al
-------
Appendix B
Revision 2
Date: 2/87
Page 59 of 64
Summary of Extractable Sulfate, Exchangeable Acidity, and
Extractable Aluminum Data, Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 206
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Sample
Kuraber
Extract
01
02
03
04
05
06
07
06
09
10
11
12
13
14
15
16
17
If
15
20
21
22
23
24
2-:
26
?7
2f
29
30
31
3?
33
34
35
3f
3'
38
39
40
41
42
Extractable
Nitrate
mg N/kg
HZO
ExtractaMe Sulfate,
mg SAg
HjO
POj"
1
I
1
1
I
Exchangeable Acidity,
meq/lUOg
Bad 2
KC1
Extractable
Al , meq/lOug
KC1
1
!
1
|
1
1
I
1
1
-------
Appendix B
Revision 2
Date: 2/87
Page 60 of 64
Summary of Sulfate-Adsorption Isotherm Data
Corrected for Blanks* and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 207
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Sample
Number
01
02
03
04
05
06
07
08
09
15
11
12
13
14
IS
16
17
16
15
20
21
22
23
24
X
26
27
26
29
30
31
32
35
34
35
36
37
36
39
10
4i
42
Sul tate Remaining in Solution, mg S/L
Initial Solution Concentration, mg S/L
0
2
4
e
16
32
i
*Blanks are oouDie-deiomzed water.
-------
Appendix B
Revision 2
Date: 2/87
Page 61 of 64
Summary of Total C, N, S, Specific Surface, and Inorganic Carbon Data
Corrected for Blanks and Dilutions
Direct/Delayed Response Project (DDRP) Soil Survey Form 203
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name —
Lab Manager's Signature
Remarks
Sample
Number
01
02
03
04
05
06
07
08
09
10
1]
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
Total
S,
Weight I
Total
N,
Weight J
Speci fie
Surface,
m2/g
.
Total
C,
Weight %
Inorg
Wei
-------
Appendix B
Revision 2
Date: 2/87
Page 62 of 64
Particle Size Analysis Raw Data
Direct/Delayed Response Project (DDRP) Soil Survey Form 303b
Analytical Lab ID
Date Form Completed
Date Batch Received -
Batch ID
Prep Lab Name
Lab Manager's Signature
Remarks
Cylinder Volume (mL)
Pipet Volume (mL)
Height of Fraction, grams
Size Class and Particle Diameter (mm)
Sample
Number
~6J
03
04
05
Ub
07
OB
09
10
11
1 2
13
14
15
16
17
18
19
20
11
22
23
24
2$
26
27
26
29
30
31
32
33
34
35
36
37
38
39
40
41
42
sand
Sand
(2.0-
O.OS)
Clay and
Fine S1lt
(<0.02)
Clay
U0.002)
Very
Coarse
(2.0-
1.0)
Coarse
(1.0-
0.5)
Medium
(0.5-
0.25)
Fine
(0.25-
0.1)
Very Fine
(0,1-
0.05)
-------
Appendix B
Revision 2
Date: 2/87
Page 63 of 64
Summary of BaCI2 - Exchangeable Acidity Raw Data
Direct/Delayed Response Project (DORP) Soil Survey Form 306
Analytical Lab 10
Date Form Completed
Date Batch Received -
Lab Manager's Signature
Remarks
Batch ID
Prep Lab Name
Sample
Number
Extract
0!
02
03
0<
05
06
07
08
09
10
1)
1?
lj
14
15
16
17
Ifc
19
20
21
22
23
2t
25
26
27
Zl>
29
30
Jl
32
33
J«
3b
Bad; - ^changeable Acidity
THer
(Volume
In ml)
36 1
37
36
39
«0
41
«2
1
Normality
of THrant
-------
Appendix B
Revision 2
Date: 2/87
Page 64 of 64
Summary of Total C, N, S, Specific Surface, and Inorganic Carbon Data
Direct/Delayed Response Project (DDRP) Soil Survey Form 308
Analytical Lab ID
Date
Batch ID
Date Batch Received
Prep Lab Name
Lab Manager's Signature ••—
Remarks —
Sample
Number
01
"TJ^ZZZj
Ol
04
~DT
-jjg—
"B7 — ~
-w—
09
10
11
__2 _
~n— <
~rr™ —
~TT~
16
IT
16 '
19
20
21
22
2j
~2T
25
26
27
28
29
~W 1
31
~32
33
_3___™
3s
36
"3^
'IS
~1<)
40'
"41
-ft ~
Total
S,
M9
Total
N,
M9
|
_.. j
.„ i
Specific Surface,
mg EGME
added
retained
Total
C.
P9
Inorganic C,
M9
<2 mm
2-20 mm
1
-------
Appendix C
Revision 2
Date: 3/87
Page 1 of 2
Appendix C
Plan for Laboratory Audit Samples
1.0 Introduction
Natural audit samples are used for monitoring the analytical laboratories of the Direct/De-
layed Response Project (DDRP) Soil Survey. Synthetic audit samples of known composition are not
used in this project. The purpose of natural audit samples is to determine within-batch precision
and relative intralaboratory and interlaboratory bias and to assure that each laboratory is
maintaining the capability to analyze samples satisfactorily. Every effort is made to ensure that
the analytical laboratory does not recognize an audit sample as different from a routine sample.
Therefore, an audit sample is a double-blind quality assurance (QA) sample; that is, the analytical
laboratory does not recognize an audit sample as a QA sample and does not know its composition.
2.0 Source of Laboratory Audit Samples
Because audit samples should have properties similar to those samples undergoing physical,
chemical, and mineralogical characterization, six soil samples were chosen to serve as natural audit
samples for the soil survey. Four samples from New York were derived from horizons of an
Inceptisol, a Histosol, and two Spodosols; these are representative of soils sampled in the
northeastern United States. The two samples from Georgia are Ultisols, representative of soils
from the southeastern United States.
Specific descriptions below include series name, soil taxonomic class, interval from which the
sample was taken, vegetative cover, geomorphic position, and geographic location:
1. Bw - Bice series; Typic Dystrochrept, coarse loamy, mixed, frigid; depth 38 to 96 cm; sugar
maple - yellow birch - cherry; convex glacial till upland; Ava (Oneida County), New York;
West Avenue Road, 90 m west of cemetery.
2. Oa - Palms series; Terric Medisaprists; depth 25 to 140 cm; open wetland, sphagnum;
kettle position; Rome (Oneida County), New York; Tannery Road.
3. Bs - Allagash series; Typic Haplorthod, coarse loamy over sandy, mixed, frigid; depth 36
to 64 cm; sugar maple - beech - yellow birch with balsam inclusions; convex high terrace;
Webb (Herkimer County), New York; along upper end of Independence Lake water line.
4. C - Adams series; Typic Haplorthod, sandy, mixed, frigid; depth 0.9 to 9.1 m; sugar maple -
beech with black cherry inclusions; terrace; Webb (Herkimer County), New York; 305 m
east of Old Forge Airport.
5. A - Hayesville series; Typic Hapludult, clayey, oxidic, mesic; depth 0 to 20 cm; mixed forest;
upland, 10 to 25 percent slopes; near Blue Ridge (Fannin County), Georgia.
6. B2t - Hayesville series, Typic Hapludult, clayey, oxidic, mesic; depth 38 to 119 cm; mixed
forest; upland, 10 to 25 percent slopes; near Blue Ridge (Fannin County), Georgia.
-------
Appendix C
Revision 2
Date: 3/87
Page 2 of 2
Bulk soil sample and descriptive information were provided by the Soil Conservation Service
in New York and Georgia.
3.0 Characterization of Laboratory Audit Samples
The audit samples are used to monitor laboratories providing physical and chemical data, as
well as laboratories providing mineralogical data.
The initial referee laboratories responsible for characterizing the chemical and physical
parameters according to the analytical procedures set forth in their contracts with EPA were the
Soil Conservation Service National Soil Survey Laboratory in Lincoln, Nebraska, and the
Weyerhaeuser Technology Center Analytical Laboratory in Federal Way, Washington.
The referee laboratory responsible for mineralogical characterization was the Soil Conserva-
tion Service National Soil Survey Laboratory in Lincoln, Nebraska.
The data obtained from referee laboratories are used to set acceptance windows for single-
parameter values reported by analytical laboratories over the course of the soil survey (see Section
12.1).
4.0 Stability of Laboratory Audit Samples
Data generated by the contractor analytical laboratories will be examined to assess possible
changes in the chemical parameters of the audit samples with respect to time.
5.0 Logistics
Audit samples prepared at the QA laboratory are packaged to resemble routine samples:
audit samples for physical and chemical parameters, in 1-kg lots; those for mineralogical analyses,
in 500-g lots. Audit samples are supplied to each preparation laboratory. Without additional
processing of the samples, the preparation laboratory inserts the audit samples into batches that
are sent to the analytical laboratories.
For physical and chemical parameters, two audit samples of the same type are included in
each analytical batch. These are specified by the QA manager or designee. Each analytical batch
of up to 39 routine samples and field duplicates also includes one preparation duplicate.
The use of audit samples for mineralogical laboratories is specified in Section 15.0 of this
document.
-------
Appendix D
Revision 1
Date: 7/86
Page 1 of 31
Appendix D
Field Sampling On-Site Evaluation Questionnaires
This appendix contains questionnaires for evaluation of sampling crews in the Northeastern
Soil Survey (Fall, 1985) and in the Southern Blue Ridge Province Soil Survey (Spring, 1986).
-------
Appendix D
Revision 1
Date: 7/86
Page 2 of 31
Field Sampling On-Site Evaluation Questionnaire
Northeastern DDRP Soil Survey
Date: Crew ID:
State:
Reviewers
Name Title Education Experience
I. Equipment Yes No Comments
1. Munsell color book
(condition)
2. Clinometer
(type)
3. Camera
(type)
4. Film
(type, expiration date)
5. Lens
(type)
6. Spades
(type)
-------
7. Augers
(type)
What is used to
sample Histosols?
8. Sieves
(size, brand)
9. Compass
(type, declination)
10. Measuring tape
11. SCS-232 Form
How is it kept dry?
12. Marking pens
13. Saran
Ratio
Quantity
How often is it used?
When is it used?
14. Coolers
15. Gel packs
16. Thermometers
17. Maps
18. Aerial photographs
19. Flagging
20. Marker flags
21. Staplers or twist ties
22. Clod boxes
(type, condition)
Appendix D
Revision 1
Date: 7/86
Page 3 of 31
I.
Equipment (continued)
Yes No
Comments
-------
Appendix D
Revision 1
Date: 7/86
Page 4 of 31
I. Equipment (continued)
23. Clod wire
24. Clod labels
II. Site Selection
1. Does the crew have a list of
sampling classes to be
sampled in each watershed?
2. Does the crew have a map with the
five (5) random points marked?
3. How are distances measured?
If pacing is used, is pacing
standardized?
4. What does the crew use for the
starting point or control site?
5. Does the crew mark the initial
random point with a marker flag?
6. Does the crew leader stay within
a 100 square yard area when
assessing sampling class?
7. Does the crew understand
vegetation class?
8. How does the crew decide if the
soil type is of the desired
sampling class?
9. On what area is vegetation
class determined?
10. Does the crew have a clear under
standing of basal area?
-------
Appendix D
Revision 1
Date: 7/86
Page 5 of 31
II. Site Selection (continued)
11. Does the crew leader proceed at
20-foot intervals from the
initial random point?
12. Does the crew leader use a
compass to determine cardinal
direction?
13. Does the crew understand which
direction corresponds to the
random numbers from 1 to 8?
14. Does the crew have enough
copies of the field sampling
manual?
15. Are the criteria used in
selection of each site
entered in the logbook?
16. Is the field logbook neat and
legible?
17. Is a pen used for all entries
in the logbook?
18. Are entries in the logbook
reviewed or checked by
other members of the crew?
III. Sampling and Pedon Description
1. Is the pit large enough for
description, i.e., 1 meter
vertical face?
2. Is loose soil material cleaned
from the sides of the pit
prior to profile description?
3. Are pit faces examined from the
top downward?
-------
Appendix D
Revision 1
Date: 7/86
Page 6 of 31
III. Sampling and Pedon Description (continued)
4. Are horizon boundaries marked
before identification?
5. Are photographs taken after
horizons are identified?
6. Is each horizon studied in
the horizontal exposure?
7. Are the following parameters
determined for each horizon?
a) Type
b) Depth
c) Boundary
d) Color
e) Texture
f) Structure
g) Consistence
h) Presence of mottles:
(1) abundance
(2) size
(3) contrast
8. Are the following parameters
determined for each pedon?
a) Surface vegetation
b) Rock fragments
c) Presence of roots,
pores, etc.
d) Slope and aspect
e) Physiographic region
and location
f) Azimuth perpendicular to
pedon face
-------
Appendix D
Revision 1
Date: 7/86
Page 7 of 31
III. Sampling and Pedon Description (continued)
g) Drainage class
h) Permeability
i) Pedon position
j) Water table
k) Depth to bedrock
I) Diagnostic features
m) Taxonomic classification
n) Bulk density
9. How are photographs taken
(distance, angle, scale)?
By whom?
10. In sampling for bulk density:
a) Is an attempt made to obtain
clods from all horizons?
b) Are clods fist-sized?
c) Are clods taken in
triplicate?
d) How are clods dried?
e) Are clods sufficiently
dipped in the Saran resin?
f) Are clods labeled correctly?
(1) Sample code
(2) Horizon
(3) Replicate number
g) Are clods packed carefully?
11. Is NADSS LABEL A filled out
correctly and neatly?
12. Is one field duplicate
sampled per day?
-------
Appendix D
Revision 1
Date: 7/86
Page 8 of 31
III. Sampling and Pedon Description (continued)
13. How is the field duplicate
sampled?
14. Are both plastic and canvas
bags labeled?
15. Are two sample bags completely
filled for organic horizons?
16. Is mineral soil sieved through a
19-mm sieve onto plastic or into
a 1-gallon bucket?
17. Is excess water drained from
Histosols?
18. Are precautions taken to
prevent contamination from
above and below horizon?
19. Are sieves and sampling tools
cleaned sufficiently between
samples?
20. On SCS Form 232:
a) Is the day added under
sampling date?
b) Is vegetation correctly
described in order of tree
basal area?
c) Is the CREW ID written in
the lower right hand corner
of box labeled "DESCRIBERS
NAMES"?
d) Are digits 1 through 17
of "LOCATION DESCRIPTION
AND FREE FORM SITE NOTES"
correct?
1-6 = site ID
8 = random point
10-12 = sampling class
14-17 = azimuth
-------
III. Sampling and Pedon Description (continued)
e) Are volume estimates of coarse
fragments correctly recorded?
2-75 mm
75 - 250 mm
>250 mm
f) Are horizon descriptions
legible?
Appendix D
Revision 1
Date: 7/86
Page 9 of 31
-------
Appendix D
Revision 1
Date: 7/86
Page 10 of 31
Field Sampling On-Site Evaluation Questionnaire
Southern Blue Ridge Province DDRP Soil Survey
General (Page 1 of 1)
Date: State:
Crew ID: Site Number:
Time of arrival at site: Time of departure:
Field Crew:
Name
Audit Team:
Name Representing
Notes or Comments:
-------
Appendix D
Revision 1
Date: 7/86
Page 11 of 31
Site Selection (Page 1 of 3)
Used in Field?
Item
Screw auger
Bucket auger
Aerial photographs
Stereoscope
Compass
Punch probe
Spade
Topographic site map
Sampling site map
Random number table
Yes
No
Other site selection equipment used:
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 12 of 31
Site Selection (Page 2 of 3)
item
Does the field crew have the
watershed soil map with
prioritized starting points?
Are the procedures detailed
in Section 3 . 0 of the
sampling maual followed?
If no - note deviations:
Is the starting point
marked?
HOW?
How many compass directions
were attempted?
What were the total number
of points necessary to
arrive at an acceptable
site?
Were the number of points
and the compass direction
recorded properly on 232
Form?
How are the 10-m intervals
measured?
How is the sampling class
assessed at each site?
How is the vegetation class
assessed at each site?
Used in Field?
Yes
No
Comments
-------
Appendix D
Revision 1
Date: 7/86
Page 13 of 31
Site selection (Page 3 of 3)
Used in Field?
Item
Was this site a paired
pedon?
If yes, describe how the
second pedon was chosen.
If yes, is the pedon of the
same series?
If yes, is the pedon of the
same sampling class?
How far was the paired
pedon from the routine
pedon?
Are the slope and elevation
the same as that of the
routine pedon?
Yes
No
Comments t
-------
Appendix D
Revision 1
Date: 7/86
Page 14 of 31
Pedon Excavation (Page 1 of 2)
Used in Field?
Item
Shovels
Spades (sharpshooters)
Picks/Bars
Hand pump
(Beckenson Gusher*, 16 GPM)
Posthole digger
Backhoe
Yes
No
Other pedon excavation equipment used:
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 15 of 31
Pedon Excavation (Page 2 of 2)
Used in Field?
Item
Is the excavated pit of
suitable size (1m x 2M)?
Does this pit have any water
table problems?
If yes, what was done to
control sample
contamination?
Is this an organic soil?
If yes, how was the soil
excavated?
If yes, what was used to
excavate?
Yes
No
Comments:
-------
Appendix D
Revision 1
Date: 7/86
Page 16 of 31
Photographic Documentation (Page 1 of 2)
Used in Field?
item
3 5 -mm camera, automated
with flash*
If the camera is supplied by
the crew, what type is it?
Slide film
R^R
Photogray cards*
Khaki measuring tape
Yes
No
Other photographic equipment used:
'Supplied by EMSL-Las Vegas
tSupplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 17 of 31
Photographic Documentation (Page 2 of 2)
Item
Are the photos taken before
destructive profile
description is begun?
Are the horizons delineated
with golf tees?
Is the khaki measuring tape
included in the photo?
Is the photogray card placed
at the top of the profile?
Is it correctly filled out?
Are slides recorded in the
field notebook?
Are slides recorded on the
232 Form?
Are the 4 required (minimum)
photographs taken:
pedon face?
tree canopy?
understory vegetation?
landscape /landform?
Used in Field?
Yes
No
Comments:
-------
Appendix D
Revision 1
Date: 7/86
Page 18 of 31
Pedon Description (Page 1 of 3)
Item
SCS-232 Form*
Tablet/form holder
Munsell color chart
Condition:
Clinometers
Compass
Set for declination?
What was local declination?
Hard lens
Knife, ice pick, or equi-
valent
pH kit
Kind-
Indicators-
Is the indicator fresh
(<3 months old)?
Peat sampler (Histosols)
Flagging*
Used in Field?
Yes
No
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 19 of 31
Pedon Description (Page 2 of 3)
Item
Yellow flag markers*
Labeling pens* indelible?
Golf tees
Other soil description
equipment used?
List
Is the pit face cleaned
before horizons are
delineated?
Is spatial variability
assessed not only horizon-
tally but also in three
dimensions?
How?
Is horizon depth measured
from an accurate zero-point
at the top of the profile?
Specifically where?
over what horizontal range
is horizon thickness
determined?
who determines color?
Describer?
Used in Field?
Yes
No
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 20 of 31
Pedon Description (Page 2 of 3) Continued
Used in Field?
item
Recorder?
other?
Yes
NO
'Supplied by EMSL-Las Vegas
•(•Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 21 of 31
Pedon Description (Page 3 of 3)
Item
Is the 232 Form filled in
completely?
Is the 232 Form filled in
legibly?
Who recorded 232 form data?
la the compass used for
azimuth determination
corrected for declination?
What is the declination?
How was the declination
value determined?
Is the azimuth determined
perpendicular to the pedon
face?
Are the codes adequate for
all situations encountered
for this pedon?
Were the codes adequate for
other pedons?
Was any of the 232 form
filled out before arrival in
field?
Used in Field?
Yes
No
Comments:
-------
Appendix 0
Revision 1
Date: 7/86
Page 22 of 31
Soil sampling (Page 1 of 4)
Item
20-mm sieve*
1-gallon plastic bucket
How many?
Plastic sheet*
Brush for cleaning sieve
What is used to clean the
pedon face?
Plastic inner bags*
Canvas outer bags*
Label A*
Staplers*
Dust pan
Hand trowel
Post hole digger
(Histosols only)
Spatula or putty knife
Used in Field?
Yes
No
Other sampling equiment used:
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 23 of 31
Soil sampling (Page 2 of 4)
Used in Field?
item
Are all important horizons
sampled?
Was adequate amount of
organic horizon material
collected?
Was adequate mineral
material collected for each
horizon?
If no, was there a limiting
factor?
what?
How was the pedon sampled?
State the order of horizon
Yes
No
-------
Appendix D
Revision 1
Date: 7/86
Page 24 of 31
Soil Sampling (Page 3 of 4)
Item
Was the pedon sampled in
such a way as to avoid
contamination?
If no, give a detailed
explanantion:
Was each horizon sampled
into a dustpan
Was the sampled sieved
according to proctocol?
Were any horizons split for
sampling?
Specify:
Were they >30 cm thick
( above 1m )
Were they >60 cm thick?
(below 1m)
Were the sample bags labeled
correctly?
Were the canvas bags labeled
correctly?
How were the sample bags
closed?
Used in Field?
Yes
No
-------
Appendix D
Revision 1
Date: 7/86
Page 25 of 31
soil Sampling (Page 4 of 4)
Used in Field?
Item
Were any problems or
concerns identified in the
field sampling methods?
If yes, provide a detailed
explanantion:
Was the field duplicate
taken?
Was the field duplicate
properly labeled?
How was the field duplicate
taken?
How were the two samples for
paired pedons collected?
Were alternate trowelsful
used?
Were rock fragment size
classes determined
correctly?
Yes
No
Comments:
-------
Clod Sampling (Page 1 of 2)
Appendix D
Revision 1
Date: 7/86
Page 26 of 31
used in Field?
Item
Saran*
Mixture ratio
acetone for thinning?
What is the Saran stored in?
Hairnets*
Plastic bags*
Clod box*
Labels*
on the clod
on the box
Describe system for drying
clods.
Comments :
Yes
NA
NA
NA
NO
NA
NA
NA
Other clod sampling equipment used:
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 27 of 31
clod Sampling (Page 2 of 2)
Item
Were 3 clods obtained from
each horizon sampled?
If no, which horizons had no
corresponding clod samples?
Why?
Were clods fist sized?
If no, is there any
explanation?
Are clods dipped once in
Saran?
If more dips are required,
is it noted?
Is the clod-drying set-up
adequate?
If no, explain
Are clods labeled correctly?
Were clods placed correctly
in the clod box (i.e., No. 1
in upper left, etc.)
Are replicate numbers
assigned?
Used in Field?
Yes
No
Comments:
-------
Appendix D
Revision 1
Date: 7/86
Page 28 of 31
Sample Transport (Page 1 of 3)
Used in Field?
Item
Backpacks
Styrofoam coolers*
Gel-packs*
Are there any leaking
problems?
Thermometers*
Yes
NO
Other sample transport equipment used?
* Supplied by EMSL-Las Vegas
t Supplied by ERL-Corvallis
-------
Appendix D
Revision 1
Date: 7/86
Page 29 of 31
Sample Transport (Page 2 of 3)
item
How are samples carried from
the site to the vehicle?
How are clod boxes carried?
Were all samples accounted
for upon arrival at the
vehicle?
Were coolers available?
with gel-pacs?
What was the temperature in
the cooler?
Were samples to be trans-
ported to the preparation
laboratory that evening?
If not, how were they kept
cool until delivery?
Were there any problems in
the past with sample bags
breaking?
Were there any problems
with contamination due to
gel-pack leakage?
Were there any problmes with
sample cross-contamination?
Used in Field?
Yes
No
-------
Sample Transport (Page 3 of 3)
Appendix D
Revision 1
Date: 7/86
Page 30 of 31
Used in Field?
Item
Was all field equipment
accounted for at the end of
sampling?
Was the pit closed?
Was the pit marked?
Was the field notebook
filled in?
Was the field notebook
legible?
Yes
No
Comments:
-------
Appendix D
Revision 1
Date: 7/86
Page 31 of 31
Summary (Page 1 of 1)
Summary Comments:
Areas of Concern:
Concerns that should be reported to sampling task leader (with suggested resolution, if
appropriate):
-------
Appendix E
Revision 2
Date: 3/87
Page 1 of 17
Appendix E
Preparation Laboratory On-Site
Evaluation Questionnaire
The following questionnaire is completed to provide documentation of an on-site evaluation.
Generally, a preparation laboratory is evaluated prior to receiving samples to assess the ability of
the laboratory, in terms of personnel, facilities, and equipment, to process soil samples
successfully. A second evaluation is made after sample processing is underway. At the time of
the second evaluation, adherence to protocol is evaluated, and specific problems are addressed.
-------
Appendix E
Revision 2
Date: 3/87
Page 2 of 17
Preparation Laboratory On-Site
Evaluation Questionnaire
DDRP Soil Survey
General (Page 1 of 2)
Date
Laboratory:
Street Address:
Mailing Address (if different from above):
City:
State:
Laboratory Telephone Number: ( )
Laboratory Director:
Laboratory Quality Assurance Officer:
Type of Evaluation:
Contract Number:
Contract Title:
-------
Appendix E
Revision 2
Date: 3/87
Page 3 of 17
General (Page 2 of 2)
Personnel Contacted:
Name Tjtte
Laboratory Evaluation Team:
Name Title
-------
Appendix E
Revision 2
Date: 3/87
Page 4 of 17
-------
Organization and Personnel (Page 2 of 3)
Laboratory Personnel
Position Name Academic Training* Special Training Years Experiencet
*List highest degree obtained and specialty. Also list years toward a degree.
Hist only experience directly relevant to task to be performed.
-------
Appendix E
Revision 2
Date: 3/87
Page 6 of 17
Organization and Personnel (Page 3 of 3)
Item
Yes No Comments
Do personnel assigned to this project have the ap-
propriate educational background to successfully ac-
complish the objectives of the program?
Do personnel assigned to this project have the
appropriate level and type of experience to
successfully accomplish the objectives of this program?
Is the organization adequately staffed to meet project
commitments in a timely manner?
Was the Laboratory Manager available during the
evaluation?
Was the Quality Assurance supervisor available during
the evaluation?
Do the laboratory personnel observe safety regulations?
Are the following available:
Lab coats?
Goggles?
Gloves?
Aspirators?
is there a laboratory dress code?
If there is a dress code, is it enforced?
Who will be responsible for splitting preparation duplicate samples?
Who will be responsible for receiving audit samples?
-------
Appendix E
Revision 2
Date: 3/87
Page 7 of 17
Laboratory Manager (Page 1 of 1)
Item
Yes No
Comments
Does the laboratory manager have his/her own
copy of the Field Sampling Manual and the Labo-
ratory Methods Manual?
Before filling out Form 102, does the laboratory
manager :
Review data values on Form 101?
Review raw data in lab notebooks?
Check for adequate and accurate ID of QC sample?
Does the laboratory manager have forms 101 and 102
on file?
Procedural Questions:
Who is responsible for assuring that Form 102 is contained in each box shipped
to the analytical laboratory?
How many copies of the forms are filed by the preparation laboratory?
-------
Appendix E
Revision 2
Date: 3/87
Page 8 of 17
standard Operating Procedures (Page 1 of 1)
Item Yes No Comments
Does the laboratory have a standard operating
procedures (SOP) manual?
Is the SOP manual followed in detail?
Does the SOP manual contain quality control
practices?
Does each analyst/technician have a copy of the
SOP manual?
Does the SOP manual deviate from the procedures
required by this project?
If the SOP manual does deviate, are the deviations
documented in written form?
Does each analyst/technician have a copy of all
methods and procedures required by this project?
Comments:
-------
Appendix E
Revision 2
Date: 3/87
Page 9 of 17
Laboratory Facilities (Page 1 of 3)
When touring the facilities, give special attention to (1) the overall
appearance of organization and neatness, (2) the proper maintenance of facilities
and instrumentation, and (3) the general adequacy of the facilities to accomplish
the required work.
Item
Does the laboratory appear to have adequate work-
space for sample drying?
Does the laboratory appear to have adequate work-
space for sample preparation (sieving, crushing)?
Does the laboratory have a source of distilled/
deionized/demineralized water?
Is the analytical balance located away from draft
and areas subject to rapid temperature changes?
Has the balance been calibrated within the past
year by a certified technician?
Is the balance checked with a class s standard
weight before each use, and is the result
recorded in a logbook?
Are exhaust hoods provided that allow adequate
workspace within?
Is the laboratory clean and organized?
Are contamination-free work areas provided?
Are adequate cold storage facilities provided for
sample storage?
Are all samples stored in cold storage (4 °C)
when not in use?
Yes
No
-------
Appendix E
Revision 2
Date: 3/87
Page 10 of 17
Laboratory Facilities (Page 2 of. 3)
Item
Yes No
Comment
Is the temperature of the cold storage facilities
recorded daily in a logbook?
Is there a temperature gauge on the outside of
each cold storage unit that measures the temper-
ature of that unit?
Are the stored samples tightly closed?
Are there any open samples stored in the storage
units?
Is there any food stored in the units?
Are there any reagents stored in the units?
Are all chemicals dated upon receipt and thrown
away when shelf life is exceeded?
Are chemical waste disposal procedures/policies
adequate?
Is the laboratory secure?
-------
Appendix E
Revision 2
Date: 3/87
Page 11 of 17
Laboratory Facilities (Page 3 of 3)
Available
Item
Gas
Lighting
compressed air
Electrical services
Hot and cold water
Laboratory sink
Ventilation system
Hood space
Cabinet space
storage space (m2)
shared space
Yes
NO
Comments
Comments:
-------
Appendix E
Revision 2
Date: 3/87
Page 12 of 17
General Equipment (Page 1 of 1)
Item
Equipment
Condition/Age
Balance, analytical
Balance, top-loading
Class "S" weights
Balance table
DBS-calibrated
thermometer
Distilled/Deionized
water
Drying oven
Drying surfaces
Drying containers/
trays
Riffle splitter
Quantity
Make
Model
Good
Fair
Poor
comments
Comments:
-------
Appendix E
Revision 2
Date: 3/87
Page 13 of 17
soil Preparation Process (Page 1 of 1)
Equipment
Available
Yes No
Comments
Drying surfaces
Wooden rolling pin
Crushing tray or surface
2 -nun sieve, US 10 std.
mesh, sq. hole
Jones-type riffle
splitter (or comparable
equipment)
Procedural Questions:
How is cross-contamination between samples in the drying area avoided?
Are there separate workspaces for sample drying and for sample preparation?
How are riffle splitters and sieves cleaned between samples?
Is drying area removed from reagent storage?
reagent use?
How?
Are labels kept with drying samples?
How is the moisture-content sample removed?
Is the moisture-content sample returned to the bulk sample?
-------
Appendix E
Revision 2
Date: 3/87
Page 14 of 17
Qualitative Test for Inorganic Carbon and Handling of Rock Fragments
(Page 1 of 1)
Equipment
Available
Yes No
Comments
Porcelain spot plate
DI water in squeeze
bottle or eyedropper
Microscope (10X or
higher power)
4 N HCL
Test soil spiked with 5%
CaCO3
Test soil spiked with 5%
CaMg ( CO3 ) 2
Procedural Questions:
How are rock fragments saved from the sieving process?
Is this analysis physically removed from the sieving and soil-drying processes?
How are rock fragments from a positive test labeled?
stored?
How are rock fragments from a negative test disposed of?
Comments:
-------
Appendix E
Revision 2
Date: 3/87
Page 15 of 17
Sample Archiving and Shipping (Page 1 of 1)
How are archived samples labeled?
stored?
Is there a systematic storage procedure? Explain.
Is a map or key showing the location of archived samples readily available?
Are archived samples easily retrieved?
Are sample identifications permanent and legible?
Is there a designated sample custodian? If yes, name.
Are the sample custodian's procedures and responsibilities documented? If yes,
where?
Are sample numbers cross-referenced with field data and filed?
where?
Comments:
-------
Appendix E
Revision 2
Date: 3/87
Page 16 of 17
Summary (Page 1 of 2)
Item
Yes No
Comments
Do responses to the evaluation indicate that
project and supervisory personnel are aware
of QA and its application to the project?
Do project and supervisory personnel place
positive emphasis on QA/QC?
Has responses with respect to QA/QC aspects
of the project been open and direct?
Has a cooperative attitude been displayed by
all project and supervisory personnel?
Have any QA/QC deficiencies been discussed
during evaluation?
Is the overall QA adequate to accomplish the
objectives of the project?
Have corrective actions recommended during
previous evaluations been implemented?
Are any corrective actions required? If so,
list in detail below and on following page.
-------
Appendix E
Revision 2
Date: 3/87
Page 17 of 17
Summary (Page 2 of 2)
Summary comments and corrective actions:
-------
Appendix F
Revision 2
Date: 3/87
Page 1 of 2
Appendix F
Facsimile of
Instructions for Pre-Award Performance
Evaluation Samples
Instructions accompany the pre-award performance evaluation samples that are sent to
potential contractor laboratories.
In the instructions, three references are made to exhibits of the Invitation for Bid (IFB). The
corresponding references are indicated below:
1) "Exhibit B" is Appendix B of this document.
2) "Exhibit D" is derived from the Analytical Methods Manual for the Direct/Delayed
Response Project Soil Survey by K. A. Cappo, L J. Blume, G. A. Raab, J. K. Bartz, and
J. L. Engels, U.S. Environmental Protection Agency, Las Vegas, Nevada, 1987.
3) "Exhibit P is Section 10.0 (Internal Quality Control) of this document and Section 2.0 of
Cappo et al. (1987).
-------
Appendix F
Revision 2
Date: 3/87
Page 2 of 2
2.0 Direct/Delayed Response Project Soil Survey
Pre-Award Performance Evaluation Samples
Instructions
Enclosed are two 1-kg soil samples to be used In the evaluation of contractor laboratories
Interested In participating in the Direct/Delayed Response Project Soil Survey, sponsored and
conducted by the U.S. Environmental Protection Agency.
Upon receipt, check the contents of this package to ensure that both containers are present
and intact. Call the Quality Assurance Manager immediately In case of missing items, spillage, or
questionable condition of the pre-award samples.
Each sample is to be analyzed for all parameters according to the methods described In
Exhibit D. All quality control (QC) procedures specified in Exhibit E must be followed. Duplicate
sample analyses are required for each parameter, with the exception that triplicate samples are
required for surface. Matrix spike analyses are required for all parameters except particle size, pH,
and specific surface. Replicate and matrix spike analyses may be performed on either soil sample.
Initial, continuing, and final quality control calibration samples, as well as reagent and calibration
blanks, are required for the parameters indicated on forms 112 a through g. Instrumental
detection limits must be determined and reported for each parameter as indicated on forms 109a
through c.
Sample data and QC results must be submitted on enlarged copies of DDRP forms 103 through
113 as specified in Exhibit B. Copies of associated raw data and documentation of instrumental
detection limits must be submitted. The complete data package must be received by both data
recipients within 25 calendar day? of sample receipt.
On-site evaluations will be scheduled immediately after successful completion and scoring of the
pre-award performance evaluation samples. Prior to the on-site evaluation, a preliminary
questionnaire will be sent. This will include a request for fully documented standard operating
procedures. This questionnaire must be completed before the on-site evaluation and will be
discussed at that time.
Data Recipients:
Lockheed-EMSCO Attn: DDRP QA Manager
Flamingo Executive Park, Suite 200
1050 East Flamingo Road
Las Vegas, NV 89119
U.S. Environmental Protection Agency
Contract Laboratory Program
Sample Management Office Attn: DDRP
300 North Lee Street
Alexandria, VA 22314
-------
Appendix Q
Revision 1
Date: 7/86
Page 1 of 5
Appendix G
Pro-Award Performance Evaluation Scoring Sheet
Data from bidding laboratories are evaluated according to the criteria described on the scoring
sheet. A successful laboratory scores at least 80 percent overall for the categories of quanitifi-
cation, quality assurance, and reporting and deliverables.
-------
Direct/Delayed Response Project Soil Survey
Pre-Award Performance Evaluation Scoring Sheet
Appendix G
Revision 1
Date: 7/86
Page 2 of 5
Laboratory:.
Date:
Quantitation:.
Sample 1:
QA/QC:.
Deliverables:
Sample 2:_
Sample 3:.
Sample 4:_
Note: Samples will be two of 1, 2, 3, or 4.
Total Score
(Maximum = 200 points)
Part I. Quantitation
A Parameters
1) pH in 0.01 M CaCla and 01 H2O:
number of parameters within
acceptance criteria x 10/2*.
2) CEC (NH4OAc): number of
parameters within acceptance
criteria x 20/5*.
3) CEC (NH4CI): number of
parameters within acceptance
criteria x 20/5*.
4) Fe and Al (in oxalate, citrate-
dithionite, and pyrophosphate
extracts): number of parameters
within acceptance criteria x 18/6*.
5) Lime and Aluminum Potentials
(pH, K, Na, Mg, Ca, Fe, Al in
0.002 M CaCy: number of
parameters within acceptance
criteria x 21/7*.
Possible
Points
10
20
20
18
21
Points
Awarded
(Samples)
1
2
3
4
Total
Score
'Number of parameters analyzed.
(continued)
-------
Laboratory:.
Part I. Quantitation (continued)
Date:
Appendix G
Revision 1
Date: 7/86
Page 3 of 5
6) Specific surface: number of
parameters within acceptance
criteria x 8/1*.
7) Particle Size (percent sand,
silt, and clay): number of
parameters within acceptance
criteria x 6/3*.
8) Exchangeable Acidity (BaCI2-
TEA and HCL): number of
parameters within acceptance
criteria x 8/2*.
9) Extractable Sulfate (DI water
and PO3^ soluble): number of
parameters within acceptance
criteria x 12/2*.
10) Sulfate Adsorption (6 point iso-
therm): number of parameters
within acceptance criteria 30/6*.
11) Total Sulphur: number of para-
meters within acceptance criteria
x 4/1*.
12) Total Organic Carbon: number of
parameters within acceptance
criteria x 4/1*.
13) Inorganic Carbon: number of
parameters within acceptance
criteria x 4/1*.
14) Total Nitrogen: number of para-
meters within acceptance criteria
x 4/1*.
15) Extractable Al (in KCL): number
of parameters within acceptance
criteria x 5/1*.
Possible
Points
8
6
8
12
30
4
4
1
4
5
Points
Awarded
(Samples)
1
2
3
4
Total
Score
*Number of parameters analyzed.
-------
Appendix G
Revision 1
Date: 7/86
Page 4 of 5
Laboratory:.
Date:
Part II. Quality Assurance
A. Reagent Blank Analyses:
1. All parameters less than IDL.
2. One parameter at more than IDL
3. Two parameters at more than IDL.
4. Three or more parameters at more
than IDL
B. Quality Control Check Sample:
1. All verifications within
acceptance criteria.
2. One or more verifications
outside acceptance criteria.
C. Matrix Spike Analyses:
1. All percent recoveries within
acceptance criteria or analyzed
by Method of Standard Additions.
2. Percent recoveries outside
acceptance criteria and not
corrected by Method of
Standard Additions.
D. Duplicate Sample Analyses:
1. All RSD within acceptance criteria.
2. One or two parameters outside
acceptance criteria.
3. Three or four parameters outside
acceptance criteria.
4. Five or more parameters outside
acceptance criteria.
Possible
Points
3
2
1
0
5
0
2
0
3
2
1
0
Points
Awarded
(Samples)
1
2
3
4
Total
Score
(continued)
-------
Laboratory:.
Part II. Quality Assurance (continued)
Date:
Appendix G
Revision 1
Date: 7/86
Page 5 of 5
E. Detection Limits:
1. All instrumental detection limits
within acceptance criteria.
2. One or more outside acceptance
criteria.
3. Two of more outside acceptance
criteria.
Possible
Points
4
2
0
Points
Awarded
(Samples)
1
2
3
4
Total
Score
Part III. Reporting and Deliverables
A. Data results submitted in acceptance format
on standard forms.
B. Quality assurance/quality control data
supplied in acceptable format.
C. Raw data supplied.
D. Tabulated instrument detection limits and
associated blank data supplied.
E. Validation of results submitted with signature
of Laboratory Manager.
Possible Points
4
2
2
2
2
-------
Appendix H
Revision 2
Date: 3/87
Page 1 of 80
Appendix H
Analytical Laboratory On-Site Evaluation Questionnaire
The following questionnaire is completed to provide documentation of an on-site evaluation.
An analytical laboratory is evaluated prior to the award of a contract to assess the ability of the
laboratory, in terms of personnel, facilities, and equipment, to analyze soil samples successfully.
A second evaluation is made after sample analysis is under way. At the time of the second
evaluation, adherence to protocol is evaluated, and specific problems are addressed.
-------
Appendix H
Revision 2
Date: 3/87
Page 2 of 80
Analytical Laboratory On-Site
Evaluation Questionnaire
DDRP Soil Survey
General (Page 1 of 2)
Date
Laboratory:
Street Address:
Mailing Address (if different from above):
City:
State: Zip:.
Laboratory Telephone Number: ( )
Laboratory Director:
Laboratory Quality Assurance Officer:
(Quality Control Chemist)
Type of Evaluation:
Contract Number:
Contract Title:
-------
Appendix H
Revision 2
Date: 3/87
Page 3 of 80
General (Page 2 of 2)
Personnel Contacted:
Name Title
Laboratory Evaluation Team:
Name Title
-------
Appendix H
Revision 2
Date: 3/87
Page 4 of 80
£
.Q
•*-•
§ .§
" i
i«
.1
I 1
(0
o>
6
-------
Organization and Personnel (Page 2 of 3)
Laboratory Personnel
Position Name Academic Training* Special Training Years Experiencet
*IJst highest degree obtained and specialty. Also list years toward a degree.
tLJst only experience directly relevant to task to be performed.
-------
Appendix H
Revision 2
Date: 3/87
Page 6 of 80
Organization and Personnel (Page 3 of 3)
Item
Yes No
Comment
Do personnel assigned to this project have the
appropriate educational background to successfully
accomplish the objectives of the program?
Do personnel assigned to this project have the ap-
propriate level and type of experience to success-
fully accomplish the objectives of this program?
Is the organization adequately staffed to meet
project commitments in a timely manner?
Does the laboratory Quality Assurance Supervisor
report to senior management levels?
Was the Project Manager available during the
evaluation?
Were chemists and technicians available during the]
evaluation?
Was the Quality Assurance Supervisor available
during the evaluation?
-------
Laboratory Manager (Page 1 of 1)
Appendix H
Revision 2
Date: 3/87
Page 7 of 80
Item
Yes No
Comment
Does the laboratory manager have his/her own copy
of the standard operating procedures?
Does the laboratory manager have.his/her own copy
of the instrument performance data?
Does the laboratory manager have his/her own copy
of the latest monthly QC plots?
Is the laboratory manager aware of the most recent
control limits?
Does the laboratory manager review the following
before reporting data:
a. The data itself?
b. The quality control data sheet with analyst
notes?
c. The general instrument performance and
routine maintenance reports?
-------
Appendix H
Revision 2
Date: 3/87
Page 8 of 80
Standard Operating Procedures (SOP) (Page 1 of 1)
Item
Does the laboratory have a standard operating
procedure (SOP) manual?
Is the SOP manual followed in detail?
Does the SOP manual contain quality control
practices?
Does each analyst/technichian have a copy of the
SOP manual?
Does the SOP manual deviate from the procedures
required by the project?
If the SOP manual does deviate, are the deviations
documented in written form?
Does each analyst/technician have a copy of all
methods and procedures required by this project?
Are plots of instumental accuracy and precision
available for every analysis?
Are detection limit data tabulated for each
analysis?
Yes
No
Comment
J I I
-------
Appendix H
Revision 2
Date: 3/87
Page 9 of 80
Laboratory Facilities (Page 1 of 4)
When touring the facilities, give special attention to: (1) the overall
appearance of organization and neatness, (2) the proper maintenance of facilities
and instrumentation, (3) the general adequacy of the facilities to accomplish
the required work.
Item
I Yes
Comment
Does the laboratory appear to have adequate work- J
I
space (6 linear meters of unencumbered bench space j
]
per analyst)? j
Does the laboratory have a source of distilled/
demineralized water?
Is the specific conductance of distilled/deminer-
alized water routinely checked and recorded?
Are the analytical balances located away from
draft and areas subject to rapid temperature
changes?
1
Has the balance been calibrated within one year by|
a certified technician?
Is the balance checked with a class S standard
before each use and recorded in a logbook? Have
technician demonstrate how this is done.
Are exhaust hoods provided to allow efficient work
with volatile materials?
Have the hoods been checked for operating effi-
ciency? How often is this done?
I I
I I
H h
Is the laboratory maintained in a clean and
organized manner?
J L
-------
Appendix H
Revision 2
Date: 3/87
Page 10 of I
Laboratory Facilities (Page 2 of 4)
Item
Are contamination- free work areas provided for the
handling of toxic materials?
Are adequate facilities provided for separate
storage of samples, extracts, and standards,
including cold storage?
Is the temperature of the cold storage units
recorded daily in logbooks?
Are chemical waste disposal policies /procedures
adequate?
Are contamination-free areas provided for trace
level analytical work?
Can the laboratory supervisor document that trace-
free water is available for preparation of
standards and blanks?
Do adequate procedures exist for disposal of waste
liquids for the ICP and AA spectrometers?
Do adequate procedures exist for disposing of
liquid and solid wastes?
Is the laboratory secure?
Are all chemicals dated on receipt and thrown away
when shelf life is exceeded?
Are all samples stored in the refrigerator between
analyses?
Are acids and bases stored in separate areas?
Are hazardous, combustible, and toxic material!
stored safely?
Yes
No
Comment
-------
Appendix H
Revision 2
Date: 3/87
Page 11 of 80
Laboratory Facilities (Page 3 of 4)
Item
Gas
Lighting
Compressed air
vacuum system
Electrical services
Hot and cold water
Distilled water
Laboratory sink
Ventilation system
Hood space
Cabinet space
storage space (m2)
Refrigerated storage (4°C)
Available
Yes No
Comments
(where applicable, cite system,
QC check, adequacy of space)
-------
Laboratory Facilities (Page 4 of 4)
Appendix H
Revision 2
Date: 3/87
Page 12 of 80
Comments on Laboratory Facilities
-------
Appendix H
Revision 2
Date: 3/87
Page 13 of 80
Equipment General (Page 1 of 2)
Item
Equipment
i i
# of | |
units | Make | Model
i i
Condition/Age |
i i 1
1 1 1
Good | Fair | Poor |
i i i
Comments
Balance, analytical)
1
2
3
Balance, top loader
Class "S- weights
Balance table
NBS-calibrated
thermometer
Desiccator
Distilled water
Double deionized,
distilled/deion-
ized, or double
distilled water
Glassware
1 Beakers
2 Erlenmeyer flasks
3 Sedimentation
cylinders
4 Graduated
cylinders
-------
Appendix H
Revision 2
Date: 3/87
Page 14 of 80
Equipment General (Page 1 of 2)
Equipment
Item
Condition/Age
Glassware (cont.)
5 Fleakers
6 other
Drying ovens
Hot plates
Water bath
Centrifuge
vortex mixer
Eppendorf pipets
(or equivalent)
Reciprocating
shaker
# of
units
Hake
Model
Good
Fair
Poor
Comments
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 15 of 80
Moisture Content
Item
Manufacturer
| installation
Model | Date
Comments
Balance, ±0.01 g
Convection ovens j
Item
Available
Quantity j Type
Comments
Thermometers
0 to 200 °C
I Weighing
containers
Desiccant
I Desiccator
Comments:
-------
Moisture Content (Page 2 oJ
Question
Is the balance calibrated weekly?
Do the thermometers have a range of -20 to 200 °c?
Are thermometers calibrated (with barometric
correction) at the boiling and freezing points at
least once every 3 months?
Is the oven temperature checked and recorded
daily?
Is the oven temperature calibrated at least
monthly?
Are organic soil samples dried at the specified
temperature?
Are replicates of each sample prepared and run?
Are mineral soil samples dried at the specified
temperature ?
Are two separately calibrated ovens used, one for
organic and one for mineral soils?
If only one oven is used, is at least 24 hours
allowed for the oven to stabilize at the new
temperature?
Is sample-drying time extended as specified in the
procedure?
Are calculations correctly performed, and are at
least 5% (or 2 per batch) checked by hand?
: 2)
Yes
No
NA
Appendix H
Revision 2
Date: 3/87
Page 16 of 80
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 17 of 80
Partical size Analysis
Item
Hot plate or block
digester
Analytical balance,
0. 1 ing
Shaker, horizontal
reciprocating (120
oscillations /min. )
Sieve shaker, 1.25 cm
vertical and lateral
movement )
Complete sieve set
with receiving pan
Automatic pipets
Shaw pipet rack
Motor-driven stirrer
Manufacturer
Model
Installation Date
t.
Comments
!
-------
Appendix H
Revision 2
Date: 3/87
Page 18 of 80
Partical size Analysis (Page 2 of 5)
Item
Thermometer 10
to 50 °c
Erlenmeyer flask
or Fleaker 300ml
Pasteur-
Chamberlain
filter candles
(fineness "F")
1-L sedimenta-
tion cylinders
Insulation
covering
Hand-driven
stirrer
Shaw pipet rack
equivalent
Ringstand
Clamp
Volumetric
pipet, 25 itiL
Evaporating
dishes
Waterproof
marker or paint-
pen
Weighing bottles
90-mL wide-mouth
Desiccator
Available
Quantity
Type
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 19 of 80
Partical Size Analysis (Page 3 of 5)
Chemical
Hydrogen peroxide
(H202) 30 to 35%
Dessicant: Phosphorus
pentoxide (P2<>5)
Sodium carbonate
(Na2C03)
sodium Hexameta
phosphate ( NaPOa ) 6
Quantity
Grade
Expiration Date
Comments
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 20 of 80
Particle size Analysis (Page 4 of 5)
Question
Is analysis performed on mineral horizons only?
Is the organic matter removed as specified before
proceeding?
Are chemicals reagent grade or better?
Is heat applied after organic matter is visibly
destroyed to remove excess H2O2?
Is reciprocating shaker calibrated once every 6
months if no gauge is included (every year with
gauge ) ?
Is the 500 stroke per minute (1.25 cm vertical and
lateral oscillator) shaker calibrated once every 6
months ?
Are pipets calibrated monthly, gravimetric ally on
a calibrated balance?
Are the specified methods used for separating
sand, silt, and clay?
Is a standard sand, silt, clay "soil" used as a
control?
Is the water temperature checked during sedimen-
tation to determine when to take a sample?
Are the specified procedures followed during
sedimentation?
Is note made of which sedimentation table is used
to determine sampling depth and time?
Yes
No
NA
Comments
1 I
-------
Appendix H
Revision 2
Date: 3/87
Page 21 of 80
Particle size Analysis (Page 5 of 5)
Question
Yes I No INAI Comments
Are weights for each mineral fraction correctly
recorded and calculated?
Are calculations correctly performed, and are at
least 5% (or 2 per batch) checked by hand?
i i i
-------
Appendix H
Revision 2
Date: 3/87
Page 22 of 80
pH Determination
Item
Digital pH meter
Combination
Manufacturer
Model
Installation Date
Comments
(electrodes, non-gel
I type
Item
Available
Quantity
Type
Comments
Thermometer
Beakers, 50 mL
stirrers
QCCS standard
Chemical
j Quantity
Grade
Expiration Date | Comments
Calcium chloride
(CaCl2)
Calcium hydroxide
(Ca(OH)2)
chloroform (CHCls) orj
I I
|Thymol
|Hydrochloric
I
|acid (HCL)
|National Bureau of
I
|Standards (MBS)
buffers
Potassium Biphthalate
(KHC8H404)
(Potassium chloride
(KCl)
L
-------
Appendix H
Revision 2
Date: 3/87
Page 23 of 80
pH Determination (Page 2 of 3)
Question
|Yes|No|NA| Comments
Are chemicals reagent grade or better?
Is the air-dried soil stored in sealed containers?]
Is the pH meter digital to ±0.01 (and ±1 mv)?
Does the pH meter have internal temperature j
compensation to ±0.5 °C?
Is the combination electrode a non-gel type?
Is the combination electrode of the recommended |
style with retractable sleeve junction?
Are the buffers calibrated daily to ±.01 pH units?
Is the pH meter:
calibrated before samples are analyzed
checked every batch as stated in methods
Is the temperature compensation manual or
internal?
Are equilibrium times required for standards
checked, to see if electrode response is slowing?
Is a spare combination electrode available and
properly stored?
Is manufacturer recommended warm-up time allowed
before samples are run?
i i i
-------
Appendix H
Revision 2
Date: 3/87
Page 24 of 80
pH Determination (Page 3 of 3)
Question
Are pH meters placed away from drafts and areas of
rapid temperature change?
Are the specified between-sample procedures
followed?
Are pH units equipped with programmable sampling
times?
If yes above, are they used in this analysis?
Are electrodes properly stored and maintained?
Are the QC results plotted in real time?
What is the QCCS sample?
Is the QCCS solution analyzed first and thereafter
as called for in the methods?
Are a QCCS and duplicate sample included in each
run?
Is the quality control data reviewed by the
analyst before deciding whether to release the
data for reporting?
Yes
No
NA
Comments
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 25 of 80
Total Carbon and Total Nitrogen
Item
CHN analyzer
Mill - Hammer,
|ball or other
Thermal
detector
Recording
system
60-mesh sieve
Balance ( . Img)
Convection oven
Desiccator
Heat resistant
vials
Item
Natural gas
Helium gas
(He) 99.995+%
Oxygen gas (02)
99.99+%
Air source
(pressurized)
Acetanilide
NBS standard
Manufacturer
Available
Model /Grade
Quantity
Installation Date
Type
Comments
Comments
1
-------
Appendix H
Revision 2
Date: 3/87
Page 26 of 80
Total Carbon and Total Nitrogen (Page 2 of 4)
Item
Alumina wool (blank)
Forceps
Bunsen burner
Tamping device
Available
Quantity
Type
Comments
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 27 of 80
Total carbon and Total Nitrogen (Page 3 of 4)
Question
Are compressed gases of required purity?
Is the pressure in each gas cylinder checked
before each use?
Is the gas flow periodically checked and recorded
during operation?
Are extra cylinders of gas available in the
laboratory?
Is one- or two-day delivery of compressed gas
available?
IB distributor willing/able to replace contami-
nated gas IMMEDIATELY?
Has contaminated gas ever been delivered by this
distributor previously?
Are balances away from drafts and areas of sudden
temperature changes?
Is the hammermill properly maintained?
is the acetanilide of MBS origin?
is alumina wool of sufficient purity?
Is alumina wool pretreated according to the
procedures?
Are specified procedures followed while working
with the alumina wool?
is the thermal conductor properly calibrated
with the acetanilide standard, an alumina wool
blank, and one or more in-house soil standards?
Do the in-house standards meet the specifications
of the procedure for 10% relative standard
deviation?
Yes
No
NA
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 28 of 80
Total Carbon and Total Nitrogen (Page 4 of 4)
Question
Is the instrument recalibrated whenever the system
is opened?
Is the instrument recalibrated whenever traps,
scrubbers, or combustion or reduction tubes are
changed the oxygen or helium is changed, or gas
system otherwise modified?
Are vials properly handled during a run?
Are most components left on to prevent warm-up
problems?
If not, is the manufacturer specified warm-up time
allowed before samples are run?
Are at least 5% (2 per batch) of the calculations
check manually?
Are calculations performed correctly?
Yes
No
NA
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 29 of 80
Inorganic Carbon
Item
Coulometer
Mineral carbon
apparatus
Item
Acid dispenser auto-
matic repipet adjus-
table to 2 mL
Weighing boats
mineral carbon free
Heating unit
Coulometer accesso-
ries, manufacturers
recommended
Chemical
Sulfuric acid
(H2S04)
Calcium carbonate
(CaCO3)
Manufacturer
Available
Quantity
Model
Quantity
Grade
Installation Date
Type
Expiration Date
Comments
Comments
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 30 of 80
Inorganic Carbon (Page 2 of 4)
Chemical
Hydrochloric acid
|(HC1)
Potassium hydroxide
(KOH)
Silver sulfate
(Ag2S04)
Hydrogen peroxide
(H2O2-30%)
Potassium iodide (KI)
Stannous chloride
(Sncl2)
Ferrous sulfate
(FeSO4)
Anti-foam agents
Quantity
Grade
Expiration Date
Comments
i
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 31 of 80
Inorganic Carbon (Page 3 of 4)
Question
Yes
No
NA
Comments
Is the inorganic carbon (1C) test run only if a
positive test for carbonates is found?
Is the 1C test run on both the soil (<2nun) and
rock fragment (2 to 20mm) fractions?
Are duplicates of each sample used?
Is sample weight based on the expected carbonate
content?
Is the amount of soil used equivalent to 1 to 3 mg j
of mineral carbon?
Are samples weighed into a weighing boat before
being placed into the sample tube?
I I
If the sample is placed directly into the sample |
I
tube, is the tube first cleared of residual acid?
Are all accessory tubes and materials inspected
daily?
Is the acid dispenser calibrated daily so that
approximately 2 mL of acid are delivered?
Are standards containing a known weight of
carbonate (QCCS) used with each run?
Is the system checked daily for leaks?
Is the temperature of the heating unit checked
daily?
i i
-------
Appendix H
Revision 2
Date: 3/87
Page 32 of 80
Inorganic Carbon (Page 4 of 4)
Question
Is the temperature low enough so the scrubber is
not overloaded?
Is the sample allowed to purge until the
coulometer gives a relatively steady reading?
Are the times required for the reaction recorded
for blanks, samples, and standards?
Are calculations performed correctly, and are at
least 5% (2 per batch) checked by hand?
Yes
No|NA
Comments
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 33 of 80
Total Sulfur
Item
|Manufacturer| Model Installation Date | Comments
JS<>2 Analyzer
Detector
I Temperature regulator
Recorder
|Analytical balance
Item
Available
Quantity j Type
Comments
I Crucibles
|Gas trap
|Dust trap
I Moisture trap
(catalytic oxidants
|Forceps
I standards
|Oxygen
Chemical
Quantity
Grade Expiration Date
Comments
Chemicals as called
|for in manufacturer's
j method
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 34 of 80
Total Sulfur (Page 2 of 4)
Question
la the detector checked and calibrated at least
weekly?
Is the temperature regulator on the detector unit
stable to ±0.5 °c?
Is the instrument checked at least weekly for both
correct temperature and stability?
Are the crucibles used able to withstand heat
repeatedly?
Are crucibles handled according to manufacturer's
specifications in order to avoid contamination?
Do the crucibles produce low blank values (based
on manufacturer's ratings)?
Are all traps checked before each run to see if
they are working properly?
Are the traps changed on a scheduled basis and
more frequently if needed?
Is the S02 analyzer away from drafts and areas of
rapid temperature changes?
Is the purity of the oxygen gas equal or greater
than specified by the manufacturer?
Hill the distributor replace contaminated gas or
deliver new gas within one day?
Is an extra cylinder of oxygen available?
Is the oxygen pressure monitored periodically
during a run?
Yes
No
NA
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 35 of 80
Total sulfur (Page 3 of 4)
Question
If used, are catalytic oxidizers of sufficient
purity?
Are standards NBS-traceable?
Are standards used before, during, and after each
run?
Is the balance away from drafts and areas of rapid
temperature change?
Are soil samples adequately ground?
Is the required amount of soil used for the
expected values of sulfur?
Have manufacturer's recommendations or other
procedural modifications been approved by the QA
Yes
No
NA
Comments
manager or designee?
If the titration method of detection is used:
-Is the buret checked for accuracy gravimetrically
at least monthly?
-Are reagents of a quality equal to or exceeding
manufacturer's specifications?
-Are sufficient quantities of chemicals available?
-Are manufacturer's specified or recommended
standards used before, during, and after a run to
assure accuracy?
_L
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 36 of 80
Total Sulfur {Page 4 of 4)
Question
|Yes|No|NA| Comments
Is a QC sample run with each batch?
Is the titrator restandardized when any changes
are made in the system, or when irreproducible
results occur?
Are detection limits tested before and after each
run?
Is the detection limit determined according to
protocol?
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 37 of 80
cation Exchange Capacity
Item
|Manufacturer| Model (installation Date Comments
Mechanical extractor
Flow injection
analyzer
JTitration apparatus
|Reciprocating shaker
Item
Available
Quantity|
Type
Comments
(steam distillation
(unit
Digestion tubes 250mL
Kjeldahl flasks SOOmL
(Analytical filter
1
I pulp
Disposable syringes
60 mL
Rubber tubing
connectors
Linear polyethylene
bottles, 25 mL
-------
Appendix H
Revision 2
Date: 3/87
Page 38 of 80
Cation Exchange capacity (Page 2 of 5)
Chemical
Quantity
Grade | Expiration Date
Comments
Glacial acid
(HC2H302)
Ammonium hydroxide
(NH4OH)
Ammonium acetate
(NH4OAC)
Ammonium chloride
(NH4C1)
|Ethanol
Nessler's reagent
(Potassium iodide (Kl)
(Mercuric iodide
I
l(Hgi2)
Sodium hydroxide
(NaOH)
I Sodium chloride
| (Mad)
I Antifcam
|Hydrochloric acid
I
l(HCl)
-------
Appendix H
Revision 2
Date: 3/87
Page 39 of 80
Cation Exchange Capacity (Page 3 of 5)
Chemical
Quantity
Grade
Expiration Date | Comments
sodium carbonate
(NA2C03)
Methyl orange
indicator
Boric acid
Zinc, granular
jPhenol (CgHgO)
{Potassium sodium
I
Itartrate
| Sodium citrat
|(Na3C6H507» 2H2O)
|Sodium nitroferricya-
I
jnide
I
|2H20
Sodium hypochlorite
j(NaOCl)
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 40 of 80
Cation Exchange Capacity (Page 4 of 5)
Question
Are the chemicals reagent grade or better?
Are dilute standards prepared and calibrated
daily?
Are working standards prepared and calibrated at
least weekly?
Are reagents stored properly to prevent premature
decomposition?
Are hazardous chemicals used strictly under the
hood?
Is an antifoam agent available for use?
Is all glassware cleaned and stored as specified?
Does the flow injection analyzer (FIA) have the
correct interference filter?
Are the pump lines inspected for wear before
each run?
is the heat bath of the FIA calibrated monthly and
checked before each run?
Are the pump tubes all of the correct type for the
reagents and method in use?
Yes
„
No
NA
Comments
Are all peripherals such as printer, plotter, and
disk drives functional and, in the case of re-
corders and plotters, calibrated before each run?
Is the shaker used for organic samples calibrated
every six months or less along with general
maintenance?
i i i
-------
Appendix H
Revision 2
Date: 3/87
Page 41 of 80
Cation Exchange Capacity (Page 5 of 5)
Question
I Yes I No
NA Comments
Is the auto analyzer (distillation/titration)
calibrated for titration before each run?
H 1-
Are the condensation facilities of the distil-
lation apparatus inspected before each run?
Are all calculations performed correctly, and are
at least 5% being checked by hand?
Is the mechanical extractor calibrated for extrac-
tion time?
Is the calibration of the mechanical extractor
checked at least monthly?
Are the specified size, type, and grade of dis-
posable syringes used with the extractor?
Is the tubing checked frequently and replaced when
needed?
Is the filter pulp washed before the extraction isj
performed?
Are all procedures involving the extraction |
followed precisely according to the statement of (
I
work? I
Are three blanks carried through to record mean
and standard deviation?
i i i
-------
Appendix H
Revision 2
Date: 3/87
Page 42 of 80
Exchangeable Basic Cations
Item
Flame atomic
absorption
spectrometer
Inductively
coupled plasma
emission
spectrometer
Chemical
Argon
Acetylene gas
(C2H4)
Natural gas
(CH4)
Hydrochloric
acid (HCl)
Nitric acid
(HN03)
Calcium carbo-
nate (CaCO3)
Magnesium oxide
(MgO)
Potassium
chloride (KCl)
Sodium chloride
(NaCl)
Lanthanum
oxide (L32O3)
Manufacturer
Quantity
-
Model /Grade
Grade
Installation Date
Expiration Date
Comments
Comments
1
-------
Appendix H
Revision 2
Date: 3/87
Page 43 of 60
Exchangeable Basic cations (Page 2 of 3)
Chemical
cesium chloride
(CSCl)
Lithium
chloride (Lid)
Lithium nitrate
(LiNOa)
QCCS
Calcium (Ca2+)
Magnesium
(Mg2+)
Potassium (X+)
Sodium (Na+)
Quantity
Grade
Expiration Date
Comments
i
Comments t
-------
Appendix H
Revision 2
Date: 3/87
Page 44 of 80
Extractable Bases (Page 3 of 3)
Question
Is the analytical instrument cleaned and adjusted
before and after each run?
Is the power source secure, that is, protected
against line fluctuation?
Are standards made in a matrix as close as
possible to that of the extract?
If the lantham oxide method is used, is the La2O3
Yes
NO|NA
Comments
added to the samples and standards?
Are the pHs of the samples and standards approxi-
mately identical?
Are all chemicals of analytical reagent grade or
better?
Are chemicals used for standards traceable to NBS
standards?
Does the laboratory have copies of Methods for
Chemical Analysis of Water and Wastes, and
Standard Methods 14th edition or access to them?
Are all calculations performed correctly, and are
at least 5% (2 per batch) checked manually?
i i i
Fill out pertinent section in back of appendix:
Flame atomic absorption spectrometer
Inductively coupled plasma spectrometer
Flame photometer
I I
-------
Appendix H
Revision 2
Date: 3/87
Page 45 of 80
Lime and Aluminum Potential
Item
Manufacturer I Model/Grade I Installation Date
Comments
Flame atomic
absorption
| spectrometer
h
|Inductively
I
| coupled plasma
I
I emission
spectrometer
Flame atomic
(emission
spectrometer
Mechanical
extractor
Item
Reciprocating
shaker
Disposable
syringes, 60 mL
Rubber tubing
connectors
Analytical
filter pulp
Linear poly-
ethylene bottle
(25 and 50 mL)
Available
Quantity
Type
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 46 of 80
Lime and Aluminum Potential (Page 2 of 4)
Chemical
Calcium chlo-
ride (CaCl2)
Hydrochloric
acid (HCl)
NBS traceable
standards:
Calcium (Ca2+)
Magnesium
-------
Appendix H
Revision 2
Date: 3/87
Page 47 of 80
Lime and Aluminum Potential (Page 3 of 4)
Question
Is the reciprocating shaker calibrated every six
months or less in addition to general maintenance?
what is the QC source?
Is the QC solution analyzed first and as called
for in the methods?
Are the QC results plotted in real time?
Is the quality control data reviewed by the
analyst before deciding whether to release the
data for reporting?
Are the results for Ca reported after adjusting
for the CaCl2 extraction solution?
Are results reported based on oven-dry soil
weight?
Are all calculations correctly performed, and are
5% (2 per batch) checked manually?
Yes
No
NA
Comments
J I L
Fill out the pertinent section(s) in back of
appendix:
Flame atomic absorption
Inductively coupled plasma
Flame photometry
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 48 of 80
Lime and Aluminum Potential (Page 4 of 4)
Question
Is the mechanical extractor calibrated for
extraction time?
Is the calibration of the mechanical extractor
checked at least monthly?
Are the specified size, type, and grade of dispos-
able syringes used with the extractor?
Is the tubing checked frequently and replaced when
needed?
Is the filter pulp washed before the extraction is
performed?
Are all procedures involving the extraction
followed precisely according to the statement of
work?
Are three blanks carried through to record mean
and standard deviation?
Yes
No
~
NA
Comments
J L
-------
Appendix H
Revision 2
Date: 3/87
Page 49 of 80
Extractable Iron and Aluminum
Item
Manufacturer
Model/Grade | Installation Date
Comments
Flame atomic
absorption
spectrometer
Inductively
coupled plasma
emission
spectrometer
Centrifuge
Mechanical
extractor
Item
Available
Quantity
Type
Comments
Reciprocating
shaker
Repipet
Automatic pipet
Buret
|60 mL polypro-
jpylene syringes
I Filter pulp
I 250 mL polypro-
jpylene centri-
|fuge bottles
iFleakers
Volumetric
pipet
Volumetric
flasks
L
-------
Appendix H
Revision 2
Date: 3/87
Page 50 of 80
Extractable iron and Aluminum (Continued)
Chemicals
Sodium pyro-
phoephate
(Na4P2<>7«10H20)
Sodium hydrox-
ide (NaOH)
pH buffers, pH
• 7 and 10
Phosphoric acid
(H3P04)
Superfloc 16
Sodium Dithio-
nite (Na2S204)
Sodium citrate
(Na3C6Hs07«xH20
Ammonium
oxalate
(NH4)2C2O4»H2O
Oxalic acid
(H2C204.H20)
pH buffers,
pH - 4 and 2
Nitric acid
(HN03)
Quantity
Grade
Expiration Date
Comment 8
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 51 of 80
Extractable Iron and Aluminum (Page 3 of 5)
Question
Sodium Pyrophosphate and Citrate-Dithionite Method
Are the proper type of polypropylene 250 mL cen-
trifuge tubes used?
IB the reciprocating shaker calibrated yearly if
it possesses a speed gauge, every 6 months if not?
Is the centrifuge calibrated yearly if it pos-
sesses a speed gauge, every 6 months if not?
Are standards made up in the same expected matrix
as are the extracts?
Are the chemicals reagent grade or better?
Is the extract promptly stored at 4 °C?
Is analysis performed for Fa and Al within 24
hours of extraction?
Are the calculations carried out correctly and are
at least 5% (2 per batch) checked by hand?
Yes
No
NA
Comments
Fill out pertinent section in back of appendix:
Flame atomic absorption
Inductively coupled plasma
-•-
-------
Extractable Iron and Aluminum (Pa
Question
Acid-Oxalate Extraction
Is the shaker used for organic samples calibrated
every six months or less along with general
maintenance?
Is an ant if cam agent available for use?
Are component reagents properly mixed to provide
the final reagent?
Is the correct filter pulp used?
Is the extractor covered for the overnight
extraction?
is the extract promptly stored at 4 °c?
-
Is analysis performed for Fe and Al within 48
hours of extraction?
Are the calculations carried out correctly and are
at least 5% (2 per batch) checked by hand?
Fill out pertinent section in back of appendix:
Flame atomic absorption
Inductively coupled plasma
ge 4
Yes
of
No
~
5)
NA
Appendix H
Revision 2
Date: 3/87
Page 52 of 80
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 53 of 80
Extractable Iron and Aluminum (Page 5 of 5)
Question
Is the mechanical extractor calibrated for
extraction time?
Is the calibration of the mechanical extractor
checked at least monthly?
Are the specified size, type, and grade of dispos-
able syringes used with the extractor?
Is the tubing checked frequently and replaced when
needed?
Are all procedures involving the extraction
followed precisely according to the statement of
work?
Are three blanks carried through to record mean
and standard deviation?
Yes
No
NA
Comments
j I
-------
Appendix H
Revision 2
Date: 3/87
Page 54 of 80
Extractable Sulfate and Nitrate
Item
|Manufacturer| Model |Installation Date | comments
Balance, ±0.01 g
Ion chromatograph
Automated injection
system
Filtration apparatus
Centrifuge
••
Vortex mixer
Reciprocating shaker
_ 1
Item
100-mL centrifuge
tubes with screw caps
• • "
Volumetric flasks
0.20 m pore size
membrane filters
| Volumetric pipets
Available
Quantity
Type
L , _ ,_
• " " " "
_ -
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 55 of 80
Extractable Sulfate and Nitrate (Page 2 of 4)
Chemicals Quantity
Monobasic so-
jdium phosphate
(NaH2PO4«H2O)
Sodium carbon-
1
|ate (N32CO3)
Sodium hydrox-
ide (NaOH)
r
Sulfuric acid
|(H2S04)
i
Magnesium sul-
fate (mg2S<>4)
Sodium nitrate
(NaN03)
Grade
Expiration Date
Comments
-------
Extractable Sulfate and Nitrate (P
Question
Is the ion chromotograph maintained according to
manufacturer's specifications?
Are manufacturer recommendations for optimum 1C
sensitivity used?
Are chemicals reagent grade or better?
Are the phosophate and sulfate concentrations low
enough so they elute separately? Are dilutions
made if not?
Are all the proper accessories maintained on the
1C?
-anion separation column?
-micro-membrane suppressor (anion separation)
column?
is the optional automatic injection system used?
Are all soutions made fresh when needed?
age
Yes
3 o
No
f 4
NA
Appendix H
Revision 2
Date: 3/87
Page 56 of 80
)
Comments
-0.40M NaC03
-0.0020M N32CO3/0.002M NaOH
-other
-stock resolution standard
-working resolution standard
-sulfate and nitrate calibration
— "— —
J L
-------
Appendix H
Revision 2
Date: 3/87
Page 57 of 80
Extractable Sulfate and Nitrate (Page 4 of 4)
Question
|Yes|No|NA| Comments
Are conversion operations performed correctly for:
-meq/L to mg/L 804? (1 meq = 48.0288 mg)
-mg/L to meq/L 804? (1 meq = 0.02082 meq)
-804 to S? (1 mg 304 = .3338 mg 3)
-S to 304? ( 1 mg S = 2.9962 mg 304)
Are recording instruments calibrated before each
use?
Is a pump stroke noise supressor or pressure gauge
used to stabilize pressure?
Is resolution high enough so no startover is
required?
Are peak heights /areas recorded in a logbook?
If peaks are not sharp and symmetric, is an
approved method for peak area determination used?
Is peak area determined by microprocessor? If
yes, which methods and formulas does it use?
Are calibration curves constructed according to
manufacturer ' s recommendations ?
Is the flow rate checked gravimetrically with
time for consistency of flow?
Is the rate of flow calibrated before each
batch is run?
1
1
1
1
J L
-------
Appendix H
Revision 2
Date: 3/87
Page 58 of 80
Sulfate Adsorption Isotherms
Item.
Balance, ±0.01 g
Ion chromatograph
Filtration apparatus
Centrifuge
Reciprocating shaker
Item
Centrifuge tubes with
screw caps, 100 or
SOmL
0.20 m pore size
membrane filters
volumetric pipets
50mL
Chemical
Magnesium sulfate
(Mgso4)
Manufacturer
Available
Quantity
Model
Quantity
Grade
Installation Date
Type
Expiration Date
1
Comments
Comments
Comments
Commentsi
-------
Appendix H
Revision 2
Date: 3/87
Page 59 of 80
Sulfate Adsorption Isotherms (Page 2 of 2)
Question
Are Mgs04 adsorption solutions correctly prepared?
Are the adsorption solutions calibrated for accu-
racy before being used in the run?
Are the working standards made fresh daily?
Is the deionized water sent through the 0.20 m
membrane filter?
Is the correct amount of soil (oven-dried weight)
used?
Are methods of analysis by ion chromatography the
same as used in extractable sulfate procedure?
Are the correct conversion factors used as in the
extractable sulfate procedure?
Are all calculations performed correctly, and are
at least 5% (2 per batch) checked?
Yes
No
NA
comments
-------
Appendix H
Revision 2
Date: 3/87
Page 60 of 80
Exchangeable Acidity
item
Manufacturer I Model (installation Date Comments
Mechanical extractor
pH meter
IAutomatic titrator
pH electrode
Reciprocating shaker
Item
Available Quantity
Type
Comments
jpipettors, adjustable
I
I to 25 ml.
Eppendorf pipets, 5
mL and 5 L
Titration (Erlen- |
meyer) 250 and 125 mLj
(Linear polyethylene
(bottles 25 mL
I Volumetric flasks
Drying tube
Diluter
Tubes, 25 mL glass
(stirring rods
(Syringes 60 mL
-------
Appendix H
Revision 2
Date: 3/87
Page 61 of 80
Exchangeable Acidity (Page 2 of 5)
Chemicals
Ascarite
Barium chloride
(BaCl2»2H2O)
Triethanolamine
(N(CH2CH2OH) 3)
Sodium hydrox-
ide ( NaOH )
Sulfuric acid
(H2S04)
Hydrochloric
acid (HCl)
Potassium
chloride (KCl)
Methyl orange
indicator
Nitric acid
(HN03)
Phenolphthalein
NBS-traceable
buffers, pH=4,
7, and 10
Primary alumi-
num standard
Quantity
Grade
Expiration Date
Comments
Comments:
-------
Appendix H
Revision 2
Date: 3/87
Page 62 of 80
Exchangeable Acidity (Page 3 of 5)
Question
BaCl2 - TEA Extraction
Is the buffer solution protected from CO2?
Are the syringes prepared according to protocol?
Is the pH calibration the same as for the pH
procedure ( comment on any exceptions ) ?
Is the automatic titrator calibrated gravimetri-
cally before each batch?
Is the pH endpoint of the automatic titrator
calibrated to 4.60?
Are at least 5% of the calculations checked
manually?
Yes
No
NA
Comments
Are
calculations
performed
1
correctly?
, . _., .
KCl Extraction
Are the prepared solutions 002 free?
Are the solutions protected against atmospheric
C02?
Are syringes prepared according to protocol?
Is the titrator calibrated gravimetrically
before each batch?
Are all samples titrated to the same color (or
pH = 8.4) endpoint?
Is aliquot for aluminum determination acidified
immediately?
Is aluminum determined by ICP?
I I I
-------
Exchangeable Acidity (Page 4
Question
Are all aspects of aluminum determination correct
according to Lime and Aluminum Potential
procedure?
Common
Is the reciprocating shaker calibrated every six
months or less in addition to general maintenance?
Is the auto analyzer (distillation/titration)
calibrated for titration before each run?
Are titration results calculated, and are 5% hand
checked?
Is the 25-mL pipetter calibrated gravimetrically
daily (if the adjustible type) and at least weekly
if a fixed volume?
Is the dilutor calibrated and checked gravimetri-
cally before each run?
is the same amount of filter pulp used with each
sample?
Is the filter pulp washed before use?
1
1
Is the specified number of blanks run for each
batch? |
of
Yes
5)
No
— 1
NA
Appendix H
Revision 2
Date: 3/87
Page 63 of 80
Comments
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 64 of 80
Exchangeable Acidity (Page 5 of 5)
Question
Common (Continued)
Are chemicals of reagent grade or better?
Fill out pertinent section in back or appendix:
Is the mechanical extractor calibrated for
extraction time?
Is the calibration of the mechanical extractor
checked at least monthly?
Are the specified size, type, and grade of dispos-
able syringes used with the extractor?
Is the tubing checked frequently and replaced when
needed?
Are all procedures involving the extraction
followed precisely according to the statement of
work?
Are three blanks carried through to record mean
and standard deviation?
Yes
NO
NA
Comments
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 65 of 80
Specific Surface
Item
Analytical balance
±0.1 mg
Vacuum desiccator
Item
Vacuum pump
Drying tube for EGME
trap
Syringe, 1 mL
Chemical
Calcium chloride
( CaCl2 ) anhydrous
Ethylene glycol mono-
ethyl ether (EGME)
reagent grade
Phosphorus pentoxide
(P205)
Item
Quality control cali-
bration samples
Manufacturer
Available
Quantity
Manufacturer
Model
Quantity
Grade
Type
Installation Date
Type
Expiration Date
Grade
Comments
Comments
Comments
1
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 66 of 80
Specific Surface (Page 2 of 2)
Question
IB specific surface determined only on mineral
soils?
Is the balance calibrated at least weekly?
is the balance located away from areas of sudden
temperature changes and drafts?
is the soil sufficiently dried by vacuum over
P205?
is sufficient EGME used to cover and coat all
surfaces of the soil samples?
is the standard surface area material suitable for
the EGME method?
Are weighings performed daily until three
successive daily weights are within 1 rog EGME /gram
soil?
Are calculations performed correctly, and are at
least 5% (2 per batch) checked manually?
Yes
Mo
NA
Comments
I I I
-------
Appendix H
Revision 2
Date: 3/87
Page 67 of 80
Flame Atomic Absorption Spectroscopy
Question
For which methods is this instrument used?
Is the burner head cleaned and adjusted for each
run?
Is the burner head cleaned frequently when
solutions of high ionic strength are analyzed?
Is DI water or cleaning solution aspirated both
before and after a run?
Is the nebulizer cleaned at least weekly?
Is the correct flame type used for determination
of each element?
Is the acetylene of specified purity?
is gas pressure monitored during a run?
Are filters used to remove water and oil from the
compressed air?
is constant air pressure maintained? How?
IB the wavelength optimized before a run?
Is the slit width correctly set for the desired
element?
is the optical system aligned at least every 6
months? With a major realignment every 12 months?
Yes
No
NA
Comments
J I , 1
-------
Appendix H
Revision 2
Date: 3/87
Page 68 of 80
Flame Atomic Absorption Spectroscopy (Continued)
Question
Are the lamp and instrument allowed adequate
time to warm up before use?
-Lamp time (30-60+ minutes)?
-Instrument time (constant if possible)?
-Flame time (5+ minutes)
Is the unit adequately vented?
Is tubing inspected before each run?
Yes
No|NA| Comments
J I
-------
Appendix H
Revision 2
Date: 3/87
Page 69 of 80
Inductively Coupled Plasma Emission Spectroscopy
Question | Yes |No
1 1
For which methods is this instrument used? | |
1 1
is the tubing inspected before each run? | |
1 1
Are the electrodes replaced as instructed by the | |
manufacturer or more frequently?
NA
Comments
manufacturer or more frequently?
Is the instrument adequately vented?
is the instrument in a temperature controlled
room?
Is ample time allowed for the instument to warm
up?
Are standards calibrated both alone and as part of
a multi-element matrix?
Is the UV-IR shielding in place?
Is an adequate supply of the carrier gas present?
Are manufacturer operating procedures followed?
On multi-element units, are alternate wavelengths
used when necessary to avoid interference?
-------
Appendix H
Revision 2
Date: 3/87
Page 70 of 80
Flame Photometry (Flame Atomic Emission)
Question
For which methods is this instrument used?
Are the correct filters used for each element?
Is the pressure of the gases monitored during a
run?
Is the oxygen supply of 99.95% purity or higher?
Is the fuel supply of sufficient purity and of
constant pressure?
Is the aspirator cleaned before and after each
run?
Is a rinse solution of DI water (or wash solution)
used between samples to prevent salting-up of the
aspirator?
Is the unit given adequate time to warm up before
use?
Is the unit calibrated before use?
Is the aspirator/nebulizer unit inspected daily
for proper seating and function?
Is the unit placed away from areas of drafts and
sudden temperature changes?
Yes
No
NA
Comments
I I I
-------
Documentation/Tracking ( Page ]
Item
Is a sample custodian designated? If yes, name of
Are the sample custodian's procedures and respon-
sibilities documented? If yes, where are these
doc ume n t e d ?
Is sample tracking performed via paper or
computer?
Are written standard operating procedures (SOPs)
developed for receipt of samples? If yes, where
are they documented?
Are written standard operating procedures (SOPs)
developed for compiling and maintaining sample
document files? If yes, where are they documented?
Are samples stored under refrigeration? At what
temperature?
After completion of the analysis are the samples
properly stored for six months or until laboratory
personnel are told otherwise?
Are magnetic tapes stored in a secure area?
L of
Yes
1)
No
Appendix H
Revision 2
Date: 3/87
Page 71 of 80
Comments
J L
-------
Appendix H
Revision 2
Date: 3/87
Page 72 of 80
Analytical Methodology (Page 1 of 2)
Item
Are the required methods used?
Is there any unauthorized deviation from contract
methodology?
Are written analytical procedures provided to the
analyst?
Are reagent grade or higher purity chemicals used
to prepare standards?
Are fresh analytical standards prepared at a
frequency consistent with good QA?
Are reference materials properly labeled with con-
centrations, date of preparations, and the
identity of the person preparing the sample?
Is a standard preparation and tracking logbook
maintained?
Do the analysts record bench data in a neat and
accurate manner?
Is the appropriate instrumentation used in
accordance with the required protocol(s)?
Yes
No
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 73 of 80
Analytical Methodology (Page 2 of 2)
Comments on Analytical Methods and Practices
-------
Appendix H
Revision 2
Date: 3/87
Page 74 of 80
Quality Control (Page 1 of 3)
Item
Does the laboratory maintain a quality control
manual?
Does the manual address the important elements of
a QC program, including the following:
a. Personnel?
b. Facilities and equipment?
c. Operation of instruments?
d. Documentation of procedures?
e. Procurement and inventory practices?
f. Preventive maintenance?
g. Reliability of data?
h. Data validation?
i. Feedback and corrective action?
j. Instrument calibration?
k. Record keeping?
1. Internal audits?
Yes
No
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 75 of 80
Quality control (Page 2 of 3)
Item
Are QC responsibilities and reporting relation-
ships clearly defined?
Have standard curves been adequately documented?
Are laboratory standards traceable?
Are quality control charts maintained for each
routine analysis?
Do QC records show corrective action when
analytical results fail to meed QC criteria?
Do supervisory personnel review the data and QC
results?
Does the QC chemist have a copy of the standard
operating procedures?
Does the QC chemist have a copy of the instrument
performance data?
Does the chemist have a copy of the latest QC
plots?
Is the QC chemist aware of the most recent control
limits?
Does the QC chemist prepare a blind audit sample
once per week?
Does the QC chemist routinely review and report
blank audit data to the laboratory manager?
Yes
No
Comments
-------
Appendix H
Revision 2
Date: 3/87
Page 76 of 80
Quality Control (Page 3 of 3)
Item
|Yes|No|
Comments
Does the QC chemist update control limits and
obtain new control charts once per batch?
Are all QC data (e.g., control charts, regression
charts, QC data bases) up to date and accessible?
Are minimum detection limits calculated as
specified?
Is QC data sheet information reported to the
analyst?
-------
Data Handling (Page 1 of
Item
Does data clerk check all input to the computer
for accuracy?
Are calculations checked by another person?
Are calculations documented?
Does strip chart reduction by on-line electronic
digitization receive at least 5% manual spot
checking?
Are data from manually interpreted strip charts
spot-checked after initial entry?
Do the laboratory records include the following
information:
Sample identification number
Sample type
Date sample received in laboratory
Date of analysis
Analyst
Result of analysis (including raw analytical
data)
Recipient of the analytical data
2)
Yes
No
Appendix H
Revision 2
Date: 3/87
Page 77 of 80
Comments
J L
-------
Appendix H
Revision 2
Date: 3/87
Page 78 of 80
Data Handling (Page 2 of. 2)
Item
I Yes I No I
Comments
Does the laboratory follow required sample
tracking procedures from sample receipt to
discard?
Does the data clerk routinely report quality
control data sheet information to the analyst?
Does the data clerk submit quality control data
sheet information to the laboratory manager, along
with the analytical data to be reported?
Do records indicate corrective action taken?
Are provisions made for data storage for all raw
data, calculations, quality control data, and
reports?
Are all data and records retained for the required
amount of time?
Are computer printouts and reports routinely
spot-checked against laboratory records before
data are released?
1 1
1 1
-------
summary (Page 1 of 2)
Appendix H
Revision 2
Date: 3/87
Page 79 of 80
Item
Yes
No
Comments
Do responses to the evaluation indicate that
project and supervisory personnel are aware of QA
and its application to the project?
Do project and supervisory personnel place
positive emphasis on QA/QC?
Have responses with respect to QA/QC aspects of
the project been open and direct?
Has a cooperative attitude been displayed by all
project and supervisory personnel?
Does the organization place the proper emphasis on
quality assurance?
Have any QA/QC deficiencies been discussed before
leaving?
Is the overall quality assurance adequate to ac-
complish the objectives of the project?
Have corrective actions recommended during
previous evaluations been implemented?
Are any corrective actions required? If so, list
the necessary actions below.
-------
Appendix H
Revision 2
Date: 3/87
Page 80 of 80
Summary (Page 2 of 2)
Summary Comments and Corrective Actions
-------
Appendix I
Revision 2
Date: 3/87
Page 1 of 3
Appendix I
Facsimile of the Data Package Completeness Checklist
The Data Package Completeness Checklist was developed to serve three related functions:
• To give the contractor analytical laboratory a concise listing of what is required in the data
package.
• To give the data recipients a check-off listing to inventory the contents of the data
package.
• To serve as an index to the handwritten data file.
Two references are made to the invitation for bid (IFB). The corresponding references in this
document are indicated below:
(1) "Ex C, pg. C-2" is Table 9-3, Required Minimum Detection Limits, Expected Ranges, and
Intralaboratory Relative Precision Goal.
(2) "Ex E, Table 1" is Table 9-4, Summary of Internal Quality Control.
-------
Appendix I
Revision 2
Date: 3/87
Page 2 of 3
Data Package Completeness Checklist
Lab Number:
Initials:
Batch ID:
Date: —
1. Any major difficulties during analysis have been
discussed with the QA Manager or designee.
2. a, Required forms (102-108) are submitted.
b. lab name, batch ID, prep lab name, Lab Manager's
signature, date form completed, and date batch
received are recorded on all forms.
c. Correct number of samples were analyzed and the
results for each parameter are tabulated.
d. Data qualifiers (J, L, M, or U) are reported when results
are missing.
e. The data qualifier R is reported when a sample is
reanalyzed for QC purposes.
f. F is reported as a data qualifier when a result is
outside of criteria with consent of QA Manager.
g. G is reported as a data qualifier when the method of
standard additions is used and Form 114 is submitted.
3. Required Forms (109-114) are submitted.
a. Lab name, batch ID, and Lab Manager's signature are
on all forms.
4. Form 109
a. Instrumental detection limits and associated dates of
determination are tabulated.
b. Instrumental detection limits are less than or equal to
the contract-required detection limit (IFB, Ex C, pg.
C-2).
5. Form 110
a. Percent recovery on matrix spikes is reported for each
required parameter.
b. Percent recovery is within ±15% of 100.
6. Form 111
a. Duplicate precision results are reported for each
parameter.
b. Duplicate precision results are less than or equal to
the maximum % relative standard deviation (% RSD)
(IFB, Ex E, Tablel).
Yes Partial No
(continued)
-------
Appendix I
Revision 2
Date: 3/87
Page 3 of 3
(continued)
7. Form 112
a. Calibration blanks, reagent blanks, and detection-limit
quality control (QC) calibration samples are reported
where required.
b. Calibration blank values are less than 2 times the
contract-required detection limit (CRDL).
c. Reagent blank values are less than CRDL.
d. Detection-limit QC calibration samples are approxi-
mately 2-3 times the CRDL and the measured values
are within 20% of the theoretical values.
e. True values of QC calibration samples are in the
midrange of sample values.
f. Any problems encountered are addressed in cover
letter.
8. Form 113
a. 1C resolution test results are reported.
b. Resolution value exceeds 60%.
9. Form 114
a. Standard additions are performed and results are
reported when matrix spike results do not meet
contract requirements.
yes Partial No
Note: Checklist must be included in the data package.
-------
Appendix J
Revision 2
Date: 2187
Page 1 of 8
Appendix J
Forms for Reporting Mineralogical Laboratory Data
The following forms are used for recording data from the mineralogical procedures.
-------
Appendix J
Revision 2
Date: 2/87
Page 2 of 8
Direct/Delayed Response Project (DDRP) Soil Survey Form 400
Data from Randomly Oriented Powder Mounts
Analytical Lab ID:
Analyst:
Batch No.:
Date Received:
Date Completed:
Lab Manager's Signature:
Sample Number:
Size Fraction: <2-mm <0.002-mm
(circle one)
520
d(A)
I/Ii
Mineral
Name
JCPDS|
Card j
Number| hkl
Integrated|
Area I RIR
Half-Height
Peak Width
Minerals (in order
of highest to
least abundance)
Major Peaks
i m i \
1 I 2 I
I confirming j
-I Peak I
Degree
Of
Match
1
2
3
|4
|5
|6
|7
|8
19
-------
Appendix J
Revision 2
Date: 2/87
Page 3 of 8
Direct/Delayed Response Project (DDRP) Soil Survey Form 401
Data from Oriented Pipet Mounts
Analytical Lab ID:
Analyst:
Batch No.:
Date Received:
Date Completed:
Lab Manager's Signature:
Treatment: (circle one)
Mg - sat. A D GLY
K - sat. A D 110°C 350°C 550°C
°20
d(A)
I/Ii
Mineral
| Name
JCPDS
Card
Number
| hkl
Response
to treatment
1
1
Weight from Section 17.10.5
_g freeze-dried <0.002-mm material.
-------
Appendix J
Revision 2
Date: 2/87
Page 4 of 8
Direct/Delayed Response Project (DDRP) Soil survey Form 402a
Chemical Composition of Materials by Wavelength-dispersive XRF
Analytical Lab ID: Batch No.:
Analyst: Date Received:
Date Analyzed:
Lab Manager's Signature:
Sample Number:
Elements
Major oxide
sodium Na2O
Potassium K2O
Rubidium Rb2O
Magnesium MgO
Calcium CaO
strontium sro
Aluminum A12O3
Silicon SiO2
Phosphorus P2Os
Iron* F©2O3
Manganese MnO2
Titanium TiC>2
| Total
Conceni
Elemental,
wt%
NA
;ration
Oxide ,
wt%
2o
error
NA
l/I(b)
NA
Detection
Limit
1
1
NA
* The iron value represents both the +2 and +3 states of iron.
Comments:
-------
Appendix J
Revision 2
Date: 2/87
Page 5 of 8
Direct/Delayed Response Project (DDRP) Soil Survey Form 402b
Chemical Composition of Materials by Wavelength-Dispersive XRF
Analytical Lab ID: Batch No.:
Analyst: Date Received:
Date Analyzed:
Lab Manager's Signature:
Sample Number:
1
Minor and Trace
Elements
Sulfur S
Chloride Cl
Barium Ba
Lead Pb
Nickel Ni
Copper Cu
Cobalt Co
Chromium Cr
Zinc Zn
Uranium u
Thorium Th
Zirconium Zr
Niobium Nb
Cerium Ce
Concenl
Elemental,
wt% or ppm
tration
Oxide,
wt% or ppm
2a
error
l/i(b)
Detection
Limit
-------
Appendix J
Revision 2
Date: 2/87
Page 6 of 8
Direct/Delayed Response Project (DDRP) Soil Survey Form 403
Pertinent Geometry and Instrument Settings Specific to the System
Analytical Lab ID:.
SEM Machine Name:
Operator: EDXRF Machine Name:.
Lab Manager's Signature:
1. X-ray detector to specimen fixed angle and azimuth.
2. X-ray detector to specimen distance
3. X-ray detector active area
4. X-ray detector window
5. Specimen tilt angle and tilt azimuth.
6. Specimen to SEM pole piece working distance (adjusted on the electron beam axis to the
main constant for every spectral collection).
7. SEM operating voltage:
8. SEM beam current (±10%):
9. SEM spot size:
10. SEM scan rate (preferred as fast as possible):
11. Specimen area fluoresced: ; volume excited:.
12. Magnification: ; full frame or partial field:.
13. Spectral acquisition time (dead-time corrected):
14. Spectrometer pulse shaping time constant:
electron volts/channel:
15. Average absorbed current:.
16. Average input count rate:_
-------
Appendix J
Revision 2
Date: 2/87
Page 7 of 8
Direct/Delayed Response Project (DDRP) Soil Survey Form 404
Comments on Observations, Photographs, and Areas of Analysis
Analytical Lab ID: Batch No:.
Analyst: Date Received:.
Date Completed.
Lab Manager's Signature:
-------
Appendix J
Revision 2
Date: 2/87
Page 8 of 8
Direct/Delayed Response Project (DDRP) Soil Survey Form 405
SEM Photograph and Chemical Composition of Minerals
Analytical Lab ID:
Analyst:
Lab Manager's Signature:
Clay Mineral:
Light Mineral:
Heavy Mineral:
Wt % Heavy Minerals.
Sample Number:
yes
yes
yes
no
no
no
Batch No.:
Date Received:
Date Completed:
(circle one)
(circle one)
(circle one) If yes, include:
Wt % Light Minerals
Mineral Name:
Magnification:.
Composition: (Attach spectrum to the back of this sheet.)
-------
Appendix K
Revision 2
Date: 3/87
Page 1 of 29
Appendix K
Mineralogical Laboratory On-Site Evaluation Questionnaire
The following questionnaire is completed to provide documentation of an on-site evaluation.
A mineralogical laboratory is evaluated prior to the award of a contract to assess the ability of the
laboratory, in terms of personnel, facilities, and equipment, to analyze soil samples successfully.
A second evaluation is made after sample analysis is underway. At the time of the second
evaluation, adherence to protocol is evaluated, and specific problems are addressed.
-------
Appendix K
Revision 2
Date: 3/87
Page 2 of 29
Mineralogical Laboratory On-Site
Evaluation Questionnaire
DORP Soil Survey
General (Page 1 of 2)
Date.
Laboratory:
Street Address:
Mailing Address (if different from above):
City:.
State: Zip_
Laboratory Telephone Number ( ):
Laboratory Director:
Laboratory Quality Assurance Officer:.
Type of Evaluation:
Contract Number:
Contract Title:
-------
Appendix K
Revision 2
Date: 3/87
Page 3 of 29
General (Page 2 of 2)
Personnel Contacted:
Name Title
Laboratory Evaluation Team:
Name Title
-------
Appendix K
Revision 2
Date: 3/87
Page 4 of 29
CO
"o
§>
(0
To
I
(0
o
•*-*
a
(0
s
(Q
.Q
(Q
E
o
I
(Q
I
(0
-------
Organization and Personnel (Page 2 of 3)
Laboratory Personnel
Position Name Academic Training* Special Training Years Experiencet
0)
*List highest degree obtained and specialty. Also list years toward a degree.
tList only experience directly relevant to task to be performed.
-------
Organization and Personnel (Page 3 of 3)
Appendix K
Revision 2
Date: 3/87
Page 6 of 29
Item
Yes No Commenta
Do personnel assigned to this project have the ap-
propriate educational background to successfully ac-
complish the objectives of the program?
Do personnel assigned to this project have the
appropriate level and type of experience to
successfully accomplish the objectives of this program?
Is the organization adequately staffed to meet project
commitments in a timely manner?
Was the project manager available during the
evaluation?
Was the Quality Assurance Supervisor available during
the evaluation?
Does the laboratory QA supervisor report to senior
management levels?
Were chemists and technicians available during the
evaluation?
-------
Appendix K
Revision 2
Date: 3/87
Page 7 of 29
Laboratory Manager (Page 1 of 1)
Item Yes No Comments
Does the laboratory manager have his/her own copy of
the standard operating procedures?
Does the laboratory manager have his/her own copy of
the instrument performance data?
Does the laboratory manager have his/her own copy of
the latest monthly QC plots?
Is the laboratory manager aware of the most recent
control limits?
Does the laboratory manager review the following before
reporting data:
a. The data itself?
b. The quality control data sheet with analyst's
notes?
c. The general instrument performance and routine
maintenance reports?
-------
Appendix K
Revision 2
Date: 3/87
Page 8 of 29
Standard operating Procedures (Page 1 of 1)
Item Yes No Comments
Does the laboratory have a standard operating
procedure (SOP) manual?
Is the SOP manual followed in detail?
Does the SOP manual contain quality control
practices?
Does each analyst/technician have a copy of the
SOP manual?
Does the SOP manual deviate from the procedures
required by this project?
If the SOP manual does deviate, are the deviations
approved for this project and documented in written
form?
Does each analyst/technician have a copy of all
methods and procedures required by this project?
Are plots of instrument accuracy and precision
available for every analysis?
Are detection limit data tabulated for each
analysis?
-------
Appendix K
Revision 2
Date: 3/87
Page 9 of 29
Laboratory Facilities (Page 1 of 3)
When touring the facilities, give special attention to (1) the overall
appearance of organization and neatness, (2) the proper maintenance of facilities
and instrumentation, and (3) the general adequacy of the facilities to accomplish
the required work.
Item
Yes No
Comment
Does the laboratory appear to have adequate work-
space ( 6 linear meters of unencumbered bench
space per analyst)?
Is the specific conductance of deionized water
routinely checked and recorded?
Have the hoods been checked for operating
efficiency? How often is this done?
Are the analytical balances located away from
draft and areas subject to rapid temperature
changes?
Has the balance been calibrated within one year
by a certified technician?
Is the balance checked with a class s standard
weight before each use, and is the result of the
check recorded in a logbook? (Have technician
demonstrate how this is done.)
Are exhaust hoods provided that allow efficient
work with volatile materials?
Is the laboratory clean and well organized?
-------
Appendix K
Revision 2
Date: 3/87
Page 10 of 29
Laboratory Facilities (Page 2 of 3)
Item
Yes No
Comment
Are contamination-free work areas provided for the
handling of toxic materials?
Are adequate facilities provided for separate
storage of samples, extracts, and standards,
including cold storage?
Is the temperature of the cold storage units
recorded daily in logbooks?
Are chemical-waste disposal policies /procedures
adequate?
Are contamination-free areas provided for trace-
level analytical work?
Can the laboratory supervisor document that water
is used for preparation of standards and blanks?
Are all chemicals dated upon receipt and thrown
away when shelf life is exceeded?
Do adequate procedures exist for disposal of waste
liquids from the ICP and AA spectrometers?
Do adequate procedures exist for disposal of
liquid and solid wastes?
Is the laboratory secure?
Are all samples stored in the refrigerator between
analyses?
Are acids and bases stored in separate areas?
Are hazardous, combustible, and toxic materials
stored safely?
-------
Appendix K
Revision 2
Date: 3/87
Page 11 of 29
Laboratory Facilities (Page 1 of 3)
Item
Available Comments
(where applicable, cite system, QC check,
Yes No adequacy of space)
Gas
Lighting
Compressed air
Electrical services
Hot and cold water
Laboratory sink
Ventilation system
Hood space
Cabinet space
Storage space (m2)
Vacuum system
Deionized water
Refrigerated storage
(4°C)
-------
Laboratory Facilities (Page 4 of 4)
Appendix K
Revision 2
Date: 3/87
Page 12 of 29
Comments on Laboratory Facilities
-------
Appendix K
Revision 2
Date: 3/87
Page 13 of 29
Equipment, General (Page 1 of 2)
Equipment
Condition/Age
item
Balance, analytical
(1)
(2)
(3)
Balance, top-loader
Class "S" weights
Balance table
NBS-calibrated
thermometer
Double-deionized
(DDI) water source
or equivalent system
Desiccator
Glassware
(1) Beakers
(2) Vacuum flasks
(3) Fritter funnels
( 4 ) Graduated
cylinders
Quantity
Make
Model
Good
Fair
Poor
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 14 of 29
Equipment, General (Page 2 of 2)
Equipment
Condition/Age
Item
Glassware (cent.)
(5) Fleakers
(6) Other
Riffle-splitter,
Jones-type
Muffle Furnace
(Oe-600°C)
Wiggle bug mixer
Ultrasound water
bath
Automated mortar and
pestle
Pulverizer
Reciprocating shaker
Quantity
Make
Model
Good
Fair
Poor
Comments
Comments t
-------
Appendix K
Revision 2
Date: 3/87
Page 15 of 29
Equipment for SQXRD
Item
International No. 2
centrifuge with a
No. 240 head, or
equivalent
Centrifuge tubes,
plastic, lOOmL
centrifuge tubes,
glass, 50 mL
X-ray powder dif-
fraction unit with
Cu-radiation tube,
an x-, y- plotter,
solid state pulse
height analyzer,
peak area inte-
gration capability,
rotating and oscil-
lating stage, dif-
fraction pattern
library, and data
analysis software
Eye dropper or pipet
Desiccator
Freeze-dryer
Ring-and-puck pul-
verizer, titanium
carbide, or equiva-
lent equipment
convection oven
Syringes, plastic,
10 mL
Screen, 80-mesh
Manufacturer
Mode
Installation
Date
comments
-------
Appendix K
Revision 2
Date: 3/87
Page 16 of 29
Reagents and Consumables for SQXRD
Chemical
Scribe
Reference minerals
(list those used)
Calibration standard
(specify)
Sodium Hexameta-
phosphate [Na(PO3)6]
Magnesium chloride
(Mgcl2)
Ethanol (C2HsOH)
Methanol (CH3OH)
Silver nitrate
(AgNC-3)
Potassium chloride
(KCL)
Ethylene glycol
(CH2OHCH20H)
Linde semiconductor
grade a-Al2O3,
corundum, 1 micron
Cation exchange resin
Rexyn 101 (H) or
equivalent
Silica gel
Hydrogen peroxide
(H202)
Quantity
Grade
Expiration Date
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 17 of 29
Reagents and Consumables for SQXRD
Chemical
Dialysis tubing
Sodium acetate
(NaC2H302)
Quantity
Grade
Expiration Date
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 18 of 29
Equipment for XRF
Item
Simultaneous wave-
length-dispersive
X-ray fluorescence
spectrometer
Hydraulic press
capable of producing
pressure of 5 T/in^
Pellet die
Desiccator
Manufacturer
Mode
Installation
Date
Comments
Reagents and consumables for XRD
chemical
Microcellulose powder
Desiccant
Calibration standards
made from CCRMP-, NBS-,
or USGS-certified rock
standards
Quantity
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 19 of 29
Equipment for SEM/EDXW
Item
Scanning electron
microscope with 200-
to 300-angstrom re-
solution in the
secondary electron
mode
Gold/palladium sput-
ter coater with argon
diffusion chamber
Energy-dispersive
X-ray fluorescence
analytical unit and
software (or equiva-
lent) which can
interface with SEM
Separatory funnel,
250 mL
Fritted funnel, 50 mL
sieves, 60-mesh and
270-mesh
Polaroid camera
Manufacturer
Mode
Installation
Date
Comments
Comments:
-------
Appendix K
Revision 2
Date: 3/87
Page 20 of 29
Reagents and Consumables for SEM/EDXFR
Chemical
Gold/palladium wire,
metal for coating
specimens
Film, 35-mm or 4x5-
inch format
Film, Polaroid Type
55
Certified microprobe
mineral and rock
standards
Sodium polytungstate,
reagent grade,
density = 2.95
Filter paper, Whatman
No. 1
Carbon specimen mount
Silver conducting
paint
Quantity
Grade
Expiration Date
Comments
Comments:
-------
Appendix K
Revision 2
Date: 3787
Page 21 of 29
Documentation/Tracking (Page 1 of 1)
Item
Is a sample custodian designated? If yes, name of
Are the sample custodian's procedures and respon-
sibilities documented? If yes, where are these
documented?
Is sample tracking performed via paper or
computer?
Are written standard operating procedures (SOPs)
developed for receipt of samples? If yes, where
are they documented (e.g., laboratory manual,
written instructions)?
Are written standard operating procedures (SOPs)
developed for compiling and maintaining sample
document files? If yes, where are they
documented?
After completion of the analysis, are the samples
correctly stored for 6 months or until laboratory
personnel are told otherwise?
Are magnetic tapes stored in a secure area?
Yes
No
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 22 of 29
Analytical Methodology (Page 1 of 2)
Item
Are the specified methods used?
Za there any unauthorized deviation from contract
methodology?
Are written analytical procedures provided to the
analyst?
Are reagent grade or higher purity chemicals used
to prepare standards?
Are fresh analytical standards prepared at a
frequency as specified in the methods manual?
Are reference materials properly labeled with con-
centrations, date of preparations, and the
identity of the person preparing the sample?
Is a standard preparation and tracking logbook
maintained?
Do the analysts record bench data in a neat and
accurate manner?
Is the appropriate instrumentation used in
accordance with the required protocol(s)?
Yes
NO
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 23 of 29
Analytical Methodology (Page 2 of 2)
Commenta on Analytical Methods and Practices
-------
Appendix K
Revision 2
Date: 3/87
Page 24 of 29
Quality Control (Page 1 of 2)
Item
Does the laboratory maintain a quality control
manual?
Does the manual address the important elements of
a QC program, including the following:
a. Personnel?
b. Facilities and equipment?
c. operation of instruments?
d. Documentation of procedures?
e. Procurement and inventory practices?
f. Preventive maintenance?
g. Reliability of data?
h. Data validation?
i. Feedback and corrective action?
j . Instrument calibration?
k. Record keeping?
1. Internal audits?
Yes
No
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 25 of 29
Quality Control (Page 2 of 2)
Item
Are QC responsibilities and reporting relation-
ships clearly defined?
Are laboratory standards traceable?
Are quality control charts maintained for each
routine analysis?
Do QC records show corrective action when
analytical results fail to meet QC criteria?
Do supervisory personnel review the data and QC
results?
Does the QC analyst have his/her own copy of the
standard operating procedures?
Does the QC officer have his/her own copy of the
instrument performance data?
Does the QC officer have his/her own copy of the
latest QC plots?
Is the QC officer aware of the most recent control
limits?
Does the QC officer obtain control limits and
obtain new control chart plots once per batch?
Are all QC data (e.g., control charts, regression
charts, QC data bases) up to date and accessible?
Are minimum detection limits calculated as
specified?
Is information on QC data sheet reported to the
analyst?
Yes
No
Comments
\
-------
Appendix K
Revision 2
Date: 3/87
Page 26 of 29
Data Handling (Page 1 of 2)
Item
After data are input into the computer, does data
clerk check all data for accuracy?
Are calculations checked by another person?
Are calculations documented?
Does strip chart reduction by on-line electronic
digitization receive at least 5% manual spot
checking?
Are data from manually interpreted strip charts
spot-checked after initial entry?
Do the laboratory records include the following
information:
Sample identification number
Sample type
Date sample received in laboratory
Date of analysis
Analyst
Result of analysis (including raw analytical
data)
Recipient of the analytical data
Yes
No
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 27 of 29
Data Handling (Page 2 of 2)
Item
Does the laboratory follow required sample
tracking procedures from sample receipt to
discard?
Does the data clerk routinely report quality
control data sheet information to the analyst?
Does the data clerk submit quality control data
sheet information to the laboratory manager, along
with the analytical data to be reported?
Do records indicate corrective action taken?
Are provisions made for data storage for all raw
data, calculations, quality control data, and
reports?
Are all data and records retained for the required
amount of time?
Are computer printouts and reports routinely
spot-checked against laboratory records before
data are released?
Yes
No
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 28 of 29
Summary (Page 1 of 2)
Item
Do responses to the evaluation indicate that
project and supervisory personnel are aware of QA
and its application to the project?
Do project and supervisory personnel place
positive emphasis on QA/QC?
Have responses with respect to QA/QC aspects of
the project been open and direct?
Has a cooperative attitude been displayed by all
project and supervisory personnel?
Does the organization place the proper emphasis on
quality assurance?
Have any QA/QC deficiencies been discussed (before
the audit team leaves)?
Is the overall quality assurance adequate to ac-
complish the objectives of the project?
Have corrective actions that were recommended
during previous evaluations been implemented?
Are any corrective actions required? If so, list
the necessary actions below.
Yes
No
Comments
-------
Appendix K
Revision 2
Date: 3/87
Page 29 of 29
Summary (Page 2 of 2)
summary Comments and Corrective Actions
-------
Appendix L
Revision 1
Date: 7/86
Page 1 of 2
Appendix L
Mfneraloglcal Data Package Completeness Checklist
The mlneralogical data package completeness checklist that follows was developed to (1) give
the contractor mlneralogical laboratory a concise listing of what Is required In the data package;
(2) give the data recipients a check-off listing to Inventory the contents of the data package; and
(3) to serve as an Index to the handwritten data file.
-------
Appendix L
Revision 1
Date: 7/86
Page 2 of 2
Mineralogical Data Package Completeness Checklist
Lab Name:
Batch ID:
Lab Manager's Signature:
Date:
1. Any major difficulties during analysis have been discussed
with the QA Manager or designee.
2. a. For SQXRD the patterns obtained according to the
procedures described in the methods manual are included:
• NBS silicon powder standards, 3 patterns
• Randomly oriented powder mount of the multiphase
standard; one for every batch of samples
• Randomly oriented powder mount of <2-mm fraction
with standard
• Oriented Mg-sat. AD
• Oriented Mg-sat. gly
• Oriented K-sat. AD
• Oriented K-sat. 110 °C
• Oriented K-sat. 350 °C
• Oriented K-sat. 550 °C
• Randomly oriented powder mount of <0.002-mm
fraction with standard.
b. Required forms (400-405) are submitted.
c. Lab name, batch number, prep lab name, lab manager's
signature, date form completed, and date batch received
are recorded on all forms.
d. Correct number of samples were analyzed and the results for each parameter are
tabulated.
Yes
I
I
Partial
No
I
Note: Checklist must be included in the data package.
-------
Appendix M
Revision 0
Date: 3/87
Page 1 of 28
Appendix M
Example Verification Report
The verification report summarizes the review of the data for each analytical batch. It also
documents the required actions, e.g., confirmation and reanalysis requests and flagging of data.
-------
Batch ID:
Analytical Laboratory:
Preparation Laboratory:
Audit Horizon Type(s): _
Audit Pair(s):
Preparation Pair(s):
Field (Sampling) Pair(s):
Organic Samples:
Missing Samples:
Northeastern DDRP Soil Survey
Verification Report
Appendix M
Revision 0
Date: 3/87
Page 2 of 28
Date Data Package Received:
Date Data Package Evaluated (Initial):
Date Evaluation Letter Sent:
Date Laboratory Response Received:
Date Reanalysis Request Sent:
Date Verified (First Pass):
Date Verification Tape Sent to
ORNL (First Pass):
Date Verified (Final):
Date Verification Tape Sent to
ORNL (Final):
By:
By:
By:
By:
By:
By:
By:
By:
-------
Appendix M
Revision 0
Date: 3/87
Page 3 of 28
I. Outstanding Issues - Contractor Analytical Laboratory
The following items that are identified as missing should be resubmitted and problems should
be resolved before verification is completed:
A. General (forms 102-108)
1. Required forms have been submitted.
2. Laboratory name, batch 10, preparation laboratory name, laboratory manager's
signature, date form completed, and date batch received are included on all forms.
3. Correct data qualifiers (tags) were used as needed (see Table 1).
B. Data examination (forms 103-108)
1. Check that audit pairs are within established control criteria.
2. Estimate %RSD for all paired QA samples for each parameter, and record in Table 3.
3. Check the internal consistency of the data.
a. Form 103a: pH, H2O > 0.002 > 0.01.
b. Form 103b: sand + silt + clay = 100 ± 0.2.
c. Form 104d: CEC NH4OAc > CEC NH4CI.
d. Form 106: Ext. Sulfate, H2O < PO4.
e. Form 106: Exch. Acidity, BaCI2 > KCI.
f. Form 107: Sulfate Isotherms are 0 < 2 < 4 < 8 < 16 < 32. Adsorption solution
is within 5% of the theoretical value.
g. Form 104c: Extraction ratio is 1:2 for mineral samples and 1:10 or 1:25 for organic
samples.
h. Forms 103b and 108: For particle size analysis and specific surface, organic
samples are reported as a U.
C. General (forms 109-116)
1. Required forms have been submitted.
2. Laboratory name, batch ID, and laboratory manager's signature are included on all
forms.
D. Data examination (forms 109-116)
1. Forms 109a-c: Detection Limits
a. Check that instrumental detection limits (IDL) and associated dates of
determination are tabulated. IDL should be updated monthly for each parameter.
b. IDL should be less than or equal to the contract-required detection limit (CRDL)
for each parameter.
2. Form 110a-c: Matrix Spikes
a. Identify samples used for spiking.
b. Check that percent recovery for matrix spikes is reported for each parameter
required.
-------
Appendix M
Revision 0
Date: 3/87
Page 4 of 28
c. Check that percent recovery is calculated correctly (recalculate at least three per
page).
d. Check that percent recovery is 100 ± 15% for each parameter; if it is not, then
spiking must be repeated on two different samples.
e. Verify that the level of spike is 10 times the CRDL or equal to the endogenous
level, whichever is greater.
f. Check that the sample used for Total S, N, and C is not an organic sample for
each batch.
3. Form 111a-i: Replicates
a. Replicate precision results are reported for each parameter. For pH and specific
surface, triplicates are determined.
b. Correct equation is used to calculate %RSD (degrees of freedom equal n-1).
c. %RSDs are 0-10% (except on fractionated sand and silt).
4. Forms 112a-h: Blanks and QCCS
a. Calibration blanks, reagent blanks, and detection limit (DL) QCCS are reported
where required.
b. Calibration and reagent blanks should be less than or equal to the CRDL
c. Form 112g: K-factors are reported correctly.
d. Form 112h: Three high EGME blanks are reported correctly.
e. DL QCCS theoretical values are approximately 2 to 3 times the CRDL, and the
measured values are within 20% of the theoretical value.
f. QCCS true values are approximately in the midrange of the reported sample
values or of the calibration curve.
g. Initial, continuing, and final QCCS values are within upper and lower control limits.
5. Form 113: Ion Chromatography
a. 1C resolution test results are reported.
b. Resolution value exceeds 60%.
c. Peaks are clean on chromatogram(s).
d. At least one chromatogram is provided for each day of operation for each
instrument.
6. Form 114: Standard Additions
a. Standard additions are performed and results are reported when matrix spike
results do not meet contractual requirements.
7. Forms 115a-e: Air Dry Sample Weights
a. The air-dried soil weight is reported for each parameter, except for particle-size.
analysis (oven dried) and specific surface (P2 Os wt. = oven dried).
b. Weights are reported correctly (see Table 2).
c. Form 115a: One sample is determined in triplicate for moisture and specific
surface.
d. Duplicates are reported correctly.
8. Forms 116a-h: Dilution Factors
a. Total sample volume, aliquot volume, total dilution volume, dilution concentrations,
and dilution blanks are recorded for each sample.
-------
Appendix M
Revision 0
Date: 3/87
Page 5 of 28
E. Forms 200: Blank-corrected data
1. Required forms 204-208 have been submitted.
2. Laboratory name, batch ID, preparation laboratory name, manager's signature, and date
batch received are included on all forms.
3. Correct number of samples were analyzed, and the results for each parameter are
tabulated.
F. Forms 300: Raw Data
1. Required forms 303b-308 have been submitted.
2. Laboratory name, batch ID, preparation laboratory name, laboratory manager's
signature, and date batch received are included on all forms.
3. Correct number of samples were analyzed, and the results for each parameter are
tabulated.
G. Reporting units are correct on the following forms (see Table 4):
1. 103-108
2. 109: Detection Limits
3. 110: Matrix Spikes
4. 111: Replicates
5. 112: Blanks and QCCS
6. 115: Air Dry Sample Weights
7. 116: Dilution Factors/Concentration
8. 200: Blank-Corrected Data
9. 300: Raw Data
-------
Appendix M
Revision 0
Date: 3/87
Page 6 of 28
Table 1. Analytical Laboratory/Field Data Qualifiers (TAGS)
Data Qualifier Indicates
A Instrument unstable.
B Redone, first reading not acceptable.
F Result outside criteria with consent of QA Manager.
Q Result obtained from method of standard additions.
J Result not available; insufficient sample volume shipped to
laboratory.
L Results not available due to interference.
M Result not available; sample lost or destroyed by laboratory.
N Result outside QA criteria.
P Result outside criteria, but Insufficient volume for reanalysis.
R Result from reanalysis.
S Contamination suspected.
T Container broken.
U Result not required by procedure; unnecessary.
X No sample.
Y Available for miscellaneous comments.
Z Result from approved alternate method.
-------
Appendix M
Revision 0
Date: 3/87
Page 7 of 28
\\
98 8 959
CM
CM
CM CM CM
CMCM CM CM CM CM
CM
3
ri
«
UJ
-------
Appendix M
Revision 0
Date: 3/87
Page 8 of 28
Table 3. %RSD chart for Replicate QA Samples
Key: A - Audit Pair
P - Preparation Pair
F - Field Pair
pHH20
pHOlCaCl2
pH002CaCl2
Sand
Silt
Clay
VCSand
CSand
MS and
FSand
VFSand
CSilt
FSilt
Exchangeable Bases:
Ca, NH40AC
Mg, NH40AC
K, NH4OAC
Na, NH4OAC
Ca, NH4C1
Mg, NH4C1
K, NH4C1
Na, NH4C1
Ca, CaCl2
Mg, CaCl2
K, CaCl2
Na, CaCl2
Fe, CaCl2
Al, CaCl2
CEC, NH4OAC
CEC, NH4C1
Fe, Pyro
Al , Pyro
Al
A2
P
Fl
F2
F3
F4
F5
F6
F7
F8
F9
(continued)
-------
Appendix M
Revision 0
Date: 3/87
Page 9 of 28
Table 3. (Continued)
Key: A - Audit Pair
P - Preparation Pair
F - Field Pair
Al, Acid-ox
Fe, cit-Dith
Al, cit-Dith
XSulf, H2O
xsulf, P04
Exchangeable Acidity
BaCl2
KCl
Extractable Al
Al, KCl, Ext.
Sulfate Isotherms
Sulf iso, 0
Sulf iso, 2
Sulf Iso, 4
Sulf Iso, 8
Sulf Iso, 16
Sulf iso, 32
S, Total
N, Total
SpecSurf
c, Total
Al
A2
P
Fl
F2
F3
F4
F5
F6
F7
F8
F9
-------
Table 4. Required DDRP Soil Reporting Units
Direct/Delayed Response Project Soil Reporting Units
Data Type
Forms 103-108 Form 109 Form 110
Reporting Detection Matrix
Parameter Forms Limits Spikes
Radical Size
Exchangeable
Cations
Cation Exchange
Capacity
FIA
Titration
Extractable
Fe and Al
Extractable SO.
Exchangeable
Acidity
KCI-Extractable
Al
SO. Isotherms
Total S, N, and
C
Specific Surface
wt% NA NA
meq/100 g mg/L mg/L
meq/100 g mg N-NH./L mg N-NH./L
meq/100 g meq NH./L meq NH./L
wt% mg/L mg/L
mg S/kg mg SO./L mg SO./L
meq/100 g meq/L NA
meq/100 g NA NA
mg S/L mg SO./L NA
wt% wt% wt%
rn'/g NA NA
Form 111
Replicates
wt%
meq/100 g
meq/100 g
meq/100 g
wt%
mg S/kg
meq/100 g
meq/100 g
mg S/L
wt%
m'/g
Form 112 Form 115 Form 116
Blanks and Air-Dry Dilution
QCCS Sample wt. Concent.
wt% grams NA
mg/L grams mg/L
meq/L grams mg N-NH./L
meq NH./Lgrams meq NH./L
mg/L grams mg/L
mg S/L grams mg S/L
meq grams NA
mg/L grams mg/L
mg S/L grams mg S/L
wt% grams NA
mg EGME grams NA
(blanks)
m'/g
(QCCS)
Form 200
Blank Form 300
Corrected Raw Data
NA grams
meq/100 mg/L
meq/100 g mg N-NH
meq/100 g meq NH.
wt% mg/L
mg S/kg mg SO./L
meq/100 g meq
meq/100 g mg/L
mg S/L mg S/L
wt* ug
m'/g mg EGME
T>o:p^>
(D (D (/)* (5
ocoi'l
2-2j0e
£
-------
Appendix M
Revision 0
Date: 3/87
Page 11 of 28
II. Sample Data Review
A. The reported sample data (were, were not) complete. The following suspect sample
results should be confirmed by the contractor analytical laboratory:
Sample Form Date Date Reason for
Parameter Number Number Requested Confirmed Confirmation
B. Sample analysis (was, was not) complete based on data submitted. Reanalysis is
recommended for the following suspect samples:
Sample Date Date Reason for
Parameter Number Requested Submitted Reanalvsis
-------
Appendix M
Revision 0
Date: 3/87
Page 12 of 28
III. QA Data Review
Data for the following parameters and samples were not acceptable based on the following:
A. For a routine/field pair, a preparation pair, or an audit pair with one or both concentrations
greater than 10 times the CRDL, the duplicate precision was not within the expected
criteria. The maximum expected %RSD was exceeded for the following parameters:
Replicate Reported Contract-Required
Parameter Sample Type %RSD Maximum %RSD Explanation
NOTE: All samples in the batch for the affected parameters listed above should be flagged with
the appropriate parameter flag 01, D2, or D5-D8.
-------
Appendix M
Revision 0
Date: 3/87
Page 13 of 28
B. Audit sample data were not within the expected performance range of the audit windows.
The following audit samples were outside the expected range:
Audit Horizon Reported Expected
Parameter Type Value Range Explanation
NOTE: All samples in the batch for the affected parameters listed above should be flagged using
the appropriate parameter flag NO/, N1, or N2.
-------
Appendix M
Revision 0
Date: 3/87
Page 14 of 28
IV. QC Data Review
A. If the instrumental detection limit (IDL) reported on Form 109 exceeded the CRDL, the
integrity of the following sample values that are reported at less than 10 times the CROL
could be In question:
Sample Reported Reported
Parameter Number Concentration IDL CRDL Explanation
NOTE: Only samples with concentrations less than 10 times the CRDL for the affected
parameters listed above should be flagged with the sample flag L1.
-------
Appendix M
Revision 0
Date: 3/87
Page 15 of 28
B. Matrix spike recovery reported on Form 110 should be 100 ± 15%. If It Is not, two different
samples should be run. If the recovery for one or both samples Is not within 100 115%,
standard additions must be performed. Spike concentrations must be equal to 10 times
the CRDL or equal to the endogenous level, whichever Is greater.
Contract-
Sample Spike 10 Times Required Percent
Parameter Result Level CRDL Spike Level Recovery
NOTE: All samples In the batch for the affected parameters listed above should be flagged with
the appropriate parameter flag SO/ or S1.
-------
Appendix M
Revision 0
Date: 3/87
Page 16 of 28
C. Replicate precision data reported on Form 111 should be 10% or less. If initial replicate
precision was outside the criterion, an additional replicate must be analyzed as required
by the contract. The 10% RSD criterion is applicable only when the mean of the duplicate
analyses exceeds the CRDL by a factor of 10.
Program
Reported Calculated
Parameter %RSD %RSD Explanation
NOTE: All samples in the batch for the affected parameters listed above should be flagged with
the appropriate parameter flag D3 or 04.
-------
Appendix M
Revision 0
Date: 3/87
Page 17 of 28
D. Blanks and QCCS reported on Form 112:
1. Calibration and reagent blanks: If either blank was greater than the CRDL and
contributed more than 50% to the sample concentrations, then list contaminated
samples:
Parameter Sample Number % Concentration Explanation
NOTE: All samples in the batch for the affected parameters listed above should be flagged with
the sample flag B3 or the appropriate parameter flag B4, B5, or B7.
-------
Appendix M
Revision 0
Date: 3/87
Page 18 of 28
2. Quality control calibration sample (QCCS) analyses: List those QCCSs not within
contractual requirements. Were sufficient QCCS run?
Number of Number of
Reported Required QCCS Runs QCCS Runs
Parameter Value Range Performed Required Explanation
3. Detection Limit (DL) QCCS (DL QCCS) analyses: for those theoretical DL QCCS
concentrations that exceeded 2 to 3 times the CRDL, the measured concentration of DL
QCCS should be within 20% of the theoretical concentration.
Theoretical Measured
Parameter Value Concentration CRDL Explanation
NOTE: All samples in the batch for the affected parameters listed above should be flagged with
the appropriate parameter flags Q1-Q4.
-------
Appendix M
Revision 0
Date: 3/87
Page 19 of 28
E. The following air-dry sample weights reported on Form 115 were not within contractual
requirements:
Reported Contract-Required
Parameter Value Sample Weight Explanation
NOTE: Only samples affected for the parameters listed above should be flagged with the sampling
flag WO.
-------
Appendix M
Revision 0
Date: 3/87
Page 20 of 28
F. The following dilution factors, total sample volumes, aliquot volumes, total dilution
concentrations were not reported correctly on Form 116:
Reported Contract-
Parameter Value Required Value Explanation
G. Summarize requests for confirmation of data or reanalysis of samples on Form 500 (see
page 21).
-------
Appendix M
Revision 0
Date: 3/87
Page 21 of 28
V. Summary of Flagged Data
All QC data (matrix spikes, replicates, calibration blanks, reagent blanks, QCCS, IDL, air-dry
sample weights, and dilution factors) and paired QA data (preparation duplicates, field duplicates,
and audits) were not within contractual or expected criteria for the samples and the associated
parameters listed below:
(Parameter Flags: B4-B7, D1-D8, KO-K4, NO, N1, N2, Q1-Q4, SO, and S1) (Sample Flags: AO,
B3, L1, MO, WO, XO, X1, and X2)
List parameter flags and the affected parameters for this batch:
-------
Round
Page:_
of
Pre-veri fication
Post-verification
VI. summary of Modifications
(Additions/Deletions of Numerical/Flag Transactions)
To be applied to the Raw Data Set by Lockheed-EMSCO QA Staff
Batch
ID
Sample
ID
Parameter
Name
Date-Type
Subtype*
Old
Flag
New
Flag
Old
Value
New
Value
Init:
Edi1
Lai
t
By
Init.
Edi1
Lai
b
By
Fin<
Edi1
il
b
By
Final
Review
By
*See Table 4
8
-------
Table 4. Datatype
Datatype
1
2
3
M
M
M
M
R
R
R
R
R
W
and Subtype Definitions
Subtype
Blank
Blank
Blank
SPR
SPA
REG
SAR
REP1
REP2
REP3
AV1
RSD
Blank
Spike result
Spike added
Recovery, percent
Sample result
Replicate 1
Replicate 2
Replicate 3 (not required for
Average
Weights
Appendix M
Revision 0
Date: 3/87
Page 23 of 28
all parameters)
-------
VII. Modifications (Additions and Deletions) to be made to a copy of the Raw Data
Set by ORNL Staff
Batch
ID
Form
Number
Sample
ID
Watershed
ID
Variable
Name
Original
Value
New
Value
Comments
Date Change.
Applied at (
5
DRNL
By
TJO
! 9:
^°s
-------
VIII. Summary of Outstanding Issues Addressed to Sample Management Office
Regarding 15% Withholding
Batch ID:
Sample
Number
Parameter
Flag
Used
Cause of Exception
Reason For
Recommendation of
Penalty or Waiver
Lockheed-
EMSCO
Recommen-
dation*
EPA
Approval
*Possible recommendations: P = Penalty or W = Waiver
-------
Appendix M
Revision 0
Date: 3/87
Page 26 of 28
Table 5. Data Qualifiers for the Verification of Analytical Data (FLAGS)
Miscellaneous
AO* Value missing
Generated by Appropriate Blank Exception Program
B3* Internal (laboratory) calibration or reagent blanks are >2x CRDL and contribute >50%
to the sample concentrations in the batch.
B4** Potential negative sample bias based on internal (laboratory) blank data.
B5** Calibration blank >1.05 x reagent blank.
Generated bv Duplicate Precision Exception Program
D1** Field duplicate precision exceeded the maximum expected percent relative standard
deviation (%RSD), and either the routine or the duplicate value was >.10 x CRDL.
D2** Field duplicate precision exceeded the maximum expected %RSD, and both the routine
and duplicate sample concentration was >.10 x CRDL.
D3** Internal (laboratory) replicate precision exceeded the maximum contract required %RSD,
and either the routine or the duplicate sample concentration was >_10 x CRDL.
04** internal (laboratory) replicate precision exceeded the maximum contract required both
the routine and duplicate sample concentrations were >_10 x CRDL
D5** Preparation duplicate precision exceeded the maximum expected %RSD and either
routine or the duplicate value was >.10 x CRDL.
D6** Preparation duplicate precision exceeded the maximum expected %RSD and both the
routine and the duplicate sample concentrations were >_10 x CRDL.
D7** Audit duplicate precision exceeded the maximum expected %RSD, and either of the audit
sample concentrations was >.10 x CRDL
D8** Audit duplicate precision exceeded the maximum expected %RSD, and both audit pair
concentrations were >10 x CRDL
(continued)
-------
Appendix M
Revision 0
Date: 3/87
Page 27 of 28
Table 5. (Continued)
Generated for Known Relationships of Sulfur Isotherms
KO** Elemental parameter out of range; used for total C, N, and S only.
K1** Organic soil (total C 20-60%) and SO^HjO > 1.05 x SO^PO,.
K2** Mineral soil (total C 0-20%) and SO«_H20 > 1.05 x SOJ>04.
K3** Organic soil: 1,000 x Total S < SO^PO, or SO^H-A
K4** Mineral soil: 3,000 x Total S < SO^PO, or SO^HjO.
Generated by Detection Limit Exception Program
L1* Instrumental detection limit (IDL) exceeded contract-required detection limit (CRDL) and
sample concentration was <10 x CROL
Miscellaneous
MO* Value was obtained by using a method that is unacceptable according to the contract.
Generated by Audit Check Program
NO** Audit sample value exceeded upper control limit.
N1** Audit sample value was below lower control limit.
N2** Audit sample value exceeded control limits; and sample preparation procedure is
suspect.
Generated by QCCS Exception Program(s)
01** Quality control calibration sample (QCCS) was above contractual criteria.
Q2** QCCS was below contractual criteria.
Q3** Insufficient number of QCCSs were measured.
Q4** Detection limit QCCS was not 3 CRDL and measured DL QCCS value was not within
20% of the theoretical concentration.
Generated by Matrix Spike Program
S1** Percent recovery of matrix spike was above contractual criteria (100 t 15%).
S2** Percent recovery of matrix spike was below contractual criteria (100 ± 15%).
-------
Appendix M
Revision 0
Date: 3/87
Page 28 of 28
Table 5. (Continued)
Miscellaneous
WO* Air dry sample weight was not within contractual requirement.
Miscellaneous (not to be included in any statistical analyses!
XO* Invalid but confirmed data based on QA/QC data review.
X1* Invalid but confirmed data - potential gross contamination of sample or parameter.
X2* Invalid but confirmed data - potential sample switch.
* Sample Flag: Flag the affected parameter for the affected samples only.
** Parameter Flag: Flag the affected parameter for ALL samples in the batch (the assumption
is that QA/QC represents all samples in the batch).
•fr US GOVERNMENT PRINTING OFFICE 1990 — 7 >t 8 - 1 5 9 / 0 0 >t ^ 7
------- |