REMIV
Remedial Planning Activities
at Selected Uncontrolled
Hazardous Waste Sites-Zone II
Environmental Protection Agency
Hazardous Site Control Division
Contract No. 68-O1-7251
Love Canal Emergency Declaration
Area Habitability Study
User's Guide to the Soil
Assessment for Indicator
Chemicals Integrated
Data Base
Black & Veatch
ICF
PRC
Ecology and Environment
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Love Canal Emergency Declaration
Area Habitability Study
User's Guide to the Soil
Assessment for Indicator
Chemicals Integrated
Data Base
Prepared for
U.S. EPA REGION II
26 Federal Plaza
New York. New York 10270
Prepared by
CH2M HILL SOUTHEAST, INC.
P.O. Box4400
Reston, Virgina 22090
(EPA Contract No. 68-01-7251)
and
Horizons System Corporation
423 Carlisle Drive
Herndon, Virginia 22070
(CH2M HILL REM IV Subcontract No. 3.00)
September V98'8
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Table of Contents
Section Page
1. 0 Introduction 1
1.1 Source Systems 2
1.2 Contents of Files 11
1. 3 The Structure of a SAS Data Set 15
1.4 Data Element Coding Standards 16
1.5 Detailed Description of Individual File Sections....18
2.0 Field Sample Master File and Ancillary File 21
2.1 Logical Record Description 21
2 . 2 Logical Subsets of the Files 23
2 . 3 Data Element Dictionaries 25
3.0 Initial Calibration Master File and Ancillary File..37
3 .1 Logical Record Description 37
3.2 Logical Subsets of the File - Special Screening 38
3 . 3 Data Element Dictionaries 39
4.0 Continuing Calibration Master File and Ancillary
File 47
4 .1 Logical Record Description 47
4.2 Logical Subsets of the File - Special Screening 48
4. 3 Data Element Dictionaries 48
5.0 Quality Control Sample Master File and Ancillary
File 57
5.1 Logical Record Description 57
5.2 Logical Subsets of the File - Special Screening 59
5. 3 Data Element Dictionaries 60
6.0 Form I Master File 69
6.1 Logical Record Description 71
6.2 Logical Subsets of the File - Special Screening 71
6.3 Data Element Dictionary 73
7.0 Blind Quality Control Spike Master File 79
7 .1 Logical Record Description 79
7.2 Logical Subsets of the File - Special Screening 79
7. 3 Data Element Dictionary 79
8 . 0 Combining Files 81
8.1 Form I with Detailed Data 81
8.2 Field Samples with Calibration Records ...81
8 . 3 Field Samples with Method Blanks 82
8.4 Blind QC Results with Spiking Levels 82
8.5 Native Field Sample MS/MSD Sets 83
8.6 Creating the Subset Used for Statistical Analysis...85
111
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Appendix Page
A Data Element Name Index A-l
B Names of Equivalent Data Elements Contained in
Multiple Files B-l
C Formulas for Computed Data Elements C-l
D Box Plot - A Graphic Representation of Analytical
Results D-l
Figure
1-1 Information Environment Data Flow Diagram 3
1-2 Integrated Data Base System Flow Chart 4
1-3 Information Management Systems 7
1-4 A SAS Data Set 15
6-1 Record Set Relationships 70
D-l Example of a Box Plot D-l
Table
l
1-1 Software Systems Developed and Used in the Soil
Assessment for Indicator Chemicals 5
1-2
Steps in the Load and Verification Process 8
IV
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1.0 Introduction
This document has been prepared to provide guidance to users of
the integrated data base created during the Love Canal Emergency
Declaration Area Habitability Study—Soil Assessment for
Indicator Chemicals. Approximately 1.8 million cells of data are
contained in the data base. The data base is a Statistical
Analysis System (SAS) relational data base, comprising ten
separate SAS data sets (i.e., files). The data base is available
from the U.S. Environmental Protection Agency (EPA) Region II.
A description of the study, including sampling, analytical
techniques, and the intended statistical use of the data, are
contained in Volume III, Soil Assessment—Indicator Chemicals, of
a five-volume series entitled Love Canal Emergency Declaration
Area Habitability Study. These documents are available through
NTIS, and the user is directed to Volume III for background on
the study intent and implementation.
The user is cautioned regarding the use of this data. The study
was designed for a very specific purpose, and the data was
collected and verified in accordance with that purpose. Other
uses of the data could lead to invalid and/or erroneous
conclusions. Careful consideration of the study design, as
documented in Volume III, Soil Assessment—Indicator Chemicals.
is required in any determination regarding the appropriate vs.
inappropriate uses of this data.
This user's guide is divided into eight sections and four
appendices:
The introduction, which gives an overview of the source
systems, file contents, and SAS data set structure;
- Six sections, each describing specific data sets in the
data base;
- An additional section on combining files, which describes
logical relationships between the data sets in the data
base;
Appendix A which lists the data elements in the data base
alphabetically;
Appendix B which lists equivalent data elements contained
in multiple data sets;
Appendix C which provides the formulas used in the
recomputation of final results; and
Appendix D which describes box plots, a statistical data
presentation technique used in the study.
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1.1 Source Systems
Development of the data and information systems was built on the
experience and software developed during a pilot soil study and
the soil assessment for dioxin. In addition, a functional
requirements analysis provided a software requirements summary
and a data flow diagram (see Figure 1-1).
Ten separate software systems were used: eight were implemented
on personal computers, and two were implemented on the EPA
mainframe system. Ease of use and the editing capabilities to
identify invalid data and prevent illogical functions were high
priorities in the development of virtually all of the systems. A
system flow chart depicting nine of these systems is presented in
Figure 1-2. The tenth system (not shown) was a model data base
implemented on the mainframe. The model data base was used to
design and test the statistical analyses performed for the study.
Each system is described in Table 1-1.
The construction of the Integrated Data Base incorporated many
automated data verification checks. The flow of this process is
shown in Figure 1-3. Table 1-2 lists the steps in the load and
verification processes.
The resulting Data Base is organized into ten interrelated files.
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W63394.T1(SA)
Ouamitation Resulis/Perlormance Check Chromatograms'
Vi'iiated Electronic Final Daia Package
D
Prccass
DM Fbw BowMn PHKMMI
OKI Stxai (CohOion of Dili Fb.)
SOKC« tec Oat Row or Oufflo* d Mi
Figure 1-1
INFORMATION ENVIRONMENT
DATA FLOW DIAGRAM
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W&3394.T1SA
Sample \ 'Includes data from
Tracking I i) Sample Collection System
Data* / 2) Sample Preparation System
LabData \ 'Each analysis shift
System ) from ead> laboratory is
Data* / a separate file
Migrate
i
Validation
Listing
r + -J
CCRLE f
(Containing [^ —*
(' ICFILE 7
(Initial U ,
^Calibrations) ^
NOTE;
Dashed lines (—) indicate an iterative process, i.e. the
output file becomes the input file for DM next iteration or
execution ol the program.
Figure 1-2
INTEGRATED DATA BASE
SYSTEM FLOW CHART
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Table 1-1
SOFTWARE SYSTEMS DEVELOPED AND USED IN THE
SOIL ASSESSMENT FOR INDICATOR CHEMICALS
System Name
Site Selection
Sample Collection
Sample Preparation
Sample Analysis
(LabData) I
Real-time QA/QC
Description
generates random selection sample
locations on EDA grid and comparison
area grid maps
generates forms and labels for field
sampling,
collects completed forms (via double-
data entry and comparison),
verifies data, and
produces reports on tracking/collection
status
generates and tracks sample preparation
forms,
automatically generates the project
sample identification number and
indicates sample splits and target
matrix spike/matrix spike duplicate
(MS/MSD) samples, and
edits and verifies data entered on forms
and produces labels and reports on
preparation data status
generates sample analysis data
reporting forms
performs chromatogram performance check
analyses
provides automatic interface with
project On-line QA/QC System
generates the electronic final data
package, and
provides automatic interface with the
project Data Validation System
produces QC reports on samples being
analyzed in the project laboratories on
a real-time basis, and
produces daily control charts for
selected QC data
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Data Validation
Form I Data Entry
Integrated Model Data
Base
Integrated Data Base
Project Bulletin Board -
interfaces with the project LabData
System and automatically displays
analytical results to be reviewed,
including shift files and calibration,
provides data entry for validation
checklists, and
provides error and status reports
collects and verifies the Form I's (data
reporting forms containing LCIC
concentrations) validated by U.S. EPA
Environmental Monitoring Systems
Laboratory in Las Vegas (EMSL-LV),
including the data validation and
usability flags assigned, and
generates a file for uploading to the
mainframe data base
creates a model SAS data base with
selected fields filled with data, using
distributions from the pilot study
integrates the data generated from the
LabData, Sample Collection, Sample
Preparation, Data Validation, and Form I
Data Entry systems into a mainframe SAS
data base,
recalculates all data reported on the
LabData forms,
checks for data consistency between the
systems where the same data were
available from more than one source, and
reports discrepancies and omissions
provides both file uploading and
downloading capabilities with full
security features for interfacing of
project systems, and
provides a message center for automated
transfer of information between
geographically dispersed project staff
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W63394.T1/S.A
PERSONAL COMPUTER SYSTEMS
QA/QC Results
Sample Collection
System
Sample Collection
Forms
Traffic Reports
Labels
I ognnri
Electronic System
Hard Copy
Q Diskette Containing
Eli
D
Electronic Info.
Integrated
Electronic Data
Disc
Sample Preparation
System
Sample Preparation
Forms
Traffic Control
Reports
Blind QC Results
Bulletin Board
System
Lab Data System
Laboratory
Analytical
Results
Data Validation
System
Forms II - X
Form I
Validated
Form Is
Form I Data
Entry System
Validation
Checklists
Real-time
QA/QC System
Audit Shift Lists
Init. Cal Checklists
Shift Checklists
Sample Checklists
QA/QC Results
Control Charts
Blind QC Results
Site Selection
System
.,,,,
'
'
• QA/QC Reports
• Verification
Reports
_*....
-
' " /'"'.'',-'
•
Data Base
Integration/
Verification System
,--•-- inirriMMr^
Integrated
DataBase
••;'•'
Target
Sample Sites
•• Includes:
11 Sample Collection Data "•
\ 2 Sample Preparation Data
.• 3. Laboratory Analytical Data
:; • Field Sample Results
| • Calfcration (Initial and Continuing) Results ''
'•;. • OC Sample Results Including 5
;' Blanks MS/MSD and Blind OC Samples -
" 4 Data Validation Results
MAINFRAME SYSTEMS
Figure 1-3
INFORMATION MANAGEMENT SYSTEMS
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Table 1-2
STEPS IN THE LOAD AND VERIFICATION PROCESS
Program Name
Validate LabData
(manual process)
Upload Final Data
Packages (manual
process)
MIGRATE
STMERGE
EDUPQC
Description
The lists prepared by EMSL-LV during
the data validation process were used
during visits to each laboratory to
verify that the laboratory's LabData
System data conformed to the list.
(This list, organized by analysis
shift, details all validated analyses,
including calibrations and field QC
analysis.) After completion of the
verification, final data packages for
all valid analyses shifts were then
generated.
The final data packages, contained
on diskettes, were uploaded to the
EPA mainframe computer. All files were
successfully uploaded.
The MIGRATE program, which separated
the LabData data into separate files to
be loaded into the integrated data
base, was then executed.
The program that merged the sample
tracking data with the field sample
data was executed. The validation
report from this program listed
records in sample tracking that did not
match to a field sample from the
LabData System and vice-versa. All
discrepancies were resolved.
This program processed the QC samples
and recomputed results fields, using
the original quantitation report data,
generated by LabData. Only results
fields requiring no data from other
quantitation reports (e.g., calibration
data) were recalculated. All
discrepancies were resolved in fields
used to join other table entries.
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EDUPIC
EDUPCC
8.
EDUPFS
9.
EDUPFIN
10.
FISTCOMP
QCSTCOMP
This program processed the 1C samples
and recomputed results fields using the
original quantitation report data
generated by LabData. All
discrepancies were resolved.
This program processed the CC samples
and recomputed results fields using the
original quantitation report data
generated by LabData. Only results
fields requiring no data from other
quantitation reports (e.g., 1C data)
were recalculated. All discrepancies
were resolved in fields used to join
other table entries.
This program processed the field
samples and recomputed selected results
fields using the original quantitation
report data generated by LabData. Only
results fields requiring no data from
other quantitation reports (e.g.,
calibration data) were recalculated.
Sample IDs were verified against the
sample tracking data. Edits were
performed to verify that the
calibration entry for the field sample
was in the data base and that QC
samples pointed to by the field sample
were also in the data base. All
discrepancies were resolved in fields
used to join other table entries.
This program processed the field
samples, verifying all fields that
require data from multiple sources; it
recomputed concentrations, recoveries,
etc., and all discrepancies were
resolved.
These programs performed a
three-level match between the Form I
data validated by EMSL-LV and the data
entered and the Form I data contained
on LabData. The initial match was on
the Lab Login identification for the
Form I. This was the unique key used
by the LabData System to track the
sample analysis. Any mismatches were
reported. Then, for those samples
whose identifications matched, two
additional levels were checked. The
sample identification (the project
identification), analysis date, and
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analysis time were matched and
mismatches reported. Then all LCIC
concentrations, percent moisture, and
dilution factors were compared.
Discrepancies between Lab Login IDs
were resolved, validated Form Irs were
linked to a valid LabData entry (which
contains all the raw data for the
analysis), and all LabData entries were
linked to a validated Form I.
11. SASBUILD This program loaded the validated data
files into the integrated data base.
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1.2 Contents of Files
The Integrated Data Base is composed of six master files and four
ancillary files, as follows:
- Field Sample Master File and Ancillary File,
- Initial Calibration Master File and Ancillary File,
- Continuing Calibration Master File and Ancillary File,
- Quality Control Sample Master File and Ancillary File,
- Forml Master File, and
- Blind Quality Control Spike Master File.
Prior to processing data files it is often useful to know how
many records they contain. Following are the record counts for
the master files:
Master File Records
FSFILE 58
ICFILE 239
CCFILE 1443
QCFILE 534
F1FILE 1564
BQFILE 293
Each of the master files is discussed below. Each ancillary file
corresponds to a master file and contains the original values for
GC/MS data corrected by the analyst via the LabData Corrections
subsystem. A record exists in an ancillary file only when one or
more of the Area/Scan Retention Time correction flags in the
master file are "on," indicating that a correction has been made.
For example, a value of "Y" in the FSCANAL data element
(correction flag for analyst) indicates that the Field Sample
Master File contains corrected data in the FSANLST data element.
It also indicates the existence of a record in the Field Sample
Ancillary File, containing the original (uncorrected) data.
An ancillary file has the same key field as its master file and,
except for the 1C and CC ancillary files, the same SAS data field
names. Note that the master files contain the corrected data
while the ancillary files contain the original data.
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The logical hierarchy of the data is as follows;
INITIAL CALIBRATION
CONTINUING CALIBRATION
FIELD SAMPLES
QC SAMPLES
CONTINUING CALIBRATION
FIELD SAMPLES
QC SAMPLES
INITIAL CALIBRATION
CONTINUING CALIBRATION
FIELD SAMPLES
QC SAMPLES
As can be seen, one Initial Calibration can have one or more
Continuing Calibrations associated with it; one Continuing
Calibration can have one or more Field and/or QC Samples
associated with it.
Field Sample Master File
A record in the Field Sample Master File contains all sample
collection, sample preparation, and GC/MS analysis data for all
field samples (HS), field splits (SPLIT), holding time samples
(HT), field handling blanks (FHB), preparation handling blanks
(PHB), and PHB splits. The GC/MS analysis data includes all
quantitation report data and computed data for the sample
analysis. Field samples are the soil samples actually taken from
the ramdomly selected locations in the various sampling areas.
Field splits are created by splitting a field sample in a manner
controlled to maintain representativeness. One half is treated
just as any other field sample, and the other receives a new
project sample ID (i.e., "HS" number). The results from the two
halves can then be used to assess inter- and intra-laboratory
variability.
Field handling blanks were "double blind" Quality Control (QC)
samples that were sent to the analytic laboratories just as field
samples were. The field handling blanks were samples of
uncomtaminated soil with an appearance similar to the field
sample soil. (The soil used for the blanks was taken from a
larger volume of soil that had been analyzed to verify that no
measurable concentrations of LCICs were present.) The field
handling blanks were used to measure whether cross-contamination
had occurred during the shipment, sampling, preparation, and
analytical processes. The field handling blanks were considered
"double blind" QC samples, because neither their identity nor the
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concentration of LCICs present was revealed to the analytical
laboratory.
Preparation handling blanks (PHB) and PHB splits were QC samples
that were sent to the analytic laboratories along with the field
samples. They were not analyzed unless contamination was
measured in the field handling blank.
Holding time samples were aliquots of soil samples used to study
the effects of extending the sample holding time on LCIC
concentrations in the samples.
Pointers, or keys, are present to join each sample's initial
calibration record, continuing calibration record, method blank
record, matrix spike (MS) and matrix spike duplicate (MSD)
records (if any), and Form I record.
Initial Calibration Master File
In the Initial Calibration Master File, a record contains all
quantitation report data and computed data for each five-point
initial calibration and/or EPA performance check analysis run on
the GC/MS. The performance check analysis could be run either in
the same analytic run (i.e., "shift") as the five-point or in a
later shift. Therefore some records contain the five-point data
and the performance check data; some records, only the five-point
data; and some records, only the performance check data.
Logically, this data represents the top of the data structure.
All continuing calibrations are associated with a five-point
initial calibration; thus one or more continuing calibration
records will point to a single initial calibration record.
Continuing Calibration Master File
In the Continuing Calibration Master File, a record contains all
quantitation report and computed data for each performance check
I/continuing calibration analysis and performance check 2
analysis run for an analytic shift on the GC/MS. This data
represents the second logical level in the data structure. Each
continuing calibration record will have one or more field sample
and/or QC sample records pointing to it.
Quality Control (QC) Sample Master File
In the QC Sample Master File, a record contains all quantitation
report and computed data for QC samples. Each analytic run, or
"shift," containing field samples was required to have certain QC
samples run as well. Depending upon various factors, one or more
types of QC samples were run in each shift. The QC samples
include the following types:
1) EMSL Blind QC samples - These were "single blind"
samples spiked with known concentrations of LCICs. The
samples are considered "single blind" to the laboratory
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because although the laboratory knows which samples are
Blind QC samples, the laboratory does not know the
spiked concentration of LCICS. A Blind QC sample was
extracted with each extraction batch of samples and
analyzed. If a given level of recovery was not
achieved in the Blind QC sample, then the laboratory
was directed to re-extract and re-analyze all the field
samples in the extraction batch.
2) Matrix Spike and Matrix Spike Duplicate - Approximately
every twentieth field sample was split into three
parts. One-third was treated as a normal field sample,
called the "native" sample in a native/MS/MSD set of
analyses. Each of the remaining thirds was then spiked
with a fixed amount of LCICs. One was called a Matrix
Spike (MS) and the other was called a Matrix Spike
Duplicate (MSD).
3) Method Blank - This was a blank sample, prepared by the
analytic laboratory from soil that had been analyzed to
verify that no measurable concentrations of LCICs were
present. The sample was used to measure any cross-
contamination during the analytical process. The
sample was extracted in a batch of field samples,
subjected to the same laboratory handling and storage
procedures, and analyzed with the field samples. If
significant levels of LCICs were found, the laboratory
re-extracted and re-analyzed the field samples in that
extraction batch.
4) Reagent Blank - This was a blank sample extract, made
from the solvents used during the sample extraction
process. The extract was analyzed to measure any LCIC
contamination introduced into the field samples during
the sample extraction process.
A pointer, or key, is present to link to each sample's continuing
calibration record.
Form I Master File
In the Form I Master File, a record contains Form I data
validated by EMSL-LV, along with flags indicating validation and
usability. The Form I document reports LCIC concentrations. The
Form I's were generated by the LabData system at the laboratory.
Both the electronic and the hardcopy results were transmitted by
the laboratory to EMSL-LV for cross-checking and for data
validation. The results of the cross-check and data validation
were incorporated in the Form I Master File.
The EMSL-LV data validation was an extensive review of the Form I
results, verifying that the concentrations on the Form I were
correctly reported. It included a review of both the data and
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supporting documentation produced by the analytic laboratories.
A series of flags was developed to characterize the data, and
from these flags, a summary usability flag was assigned. A
complete description of this process is contained in Appendix H
of Volume III. Because of this extensive review, the Form I data
contained in the Form I Master File are considered the "official"
results.
(The terms "Form I" and "Forml" are used interchangeably in this
document.)
Blind QC Spike Master File
In the Blind QC Spike Master File, each record contains analyte
spiking levels for the blind QC sample sent by EMSL-LV to the
analytical laboratory.
1.3 The Structure of a SAS Data Set
The Integrated Data Base is stored in a SAS data library. The
SAS System is a software system for data analysis. Each of the
"files" in the Integrated Data Base is a SAS data set within the
data library.
A SAS data set is a collection of data values arranged in a
rectangular form as shown in Figure 1-4. Each cell in the
rectangular table is a data value. The data values associated
with a single entity - a sample, a record - make up an
observation. In Figure 1-4, each row represents one observation.
The first observation represents all the data values associated
with the first sample whose data was recorded. The last
observation represents all the data values for the last sample.
In this document, the word "record" will often be used in place
of the SAS term "observation."
XXKEY XXY1 XXY2 XXY3 XXY4 XXY5 XXY6
A0001 1 .2 3 4 56
A0003 101 202 303 404 505 606
A0008 111 222 333 444 555 666
A0009 11 22 33 44 55 66
Figure 1-4: A SAS Data Set
The set of data values that describe a given characteristic make
up a "variable." Each observation in a SAS data set contains one
data value for each variable. In Figure 1-4, each column of data
values is a variable. For example, the first column makes up the
variable XXKEY and contains all the keys of the samples in the
data set, the second column makes up the variable XXY1 and
contains the sample's Yl's, and so on. The term "variable" has
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been replaced with "data element" in other sections of this
document.
There are two types of SAS variables: numeric and character. SAS
variables have a length attribute and a label attribute. The
length attribute of a variable is the number of bytes used to
store each of its values in a SAS data set. The label attribute
is a descriptive label that can be printed by certain SAS
procedures instead of the variable name. Labels have been stored
with the variables in the Integrated Data Base.
Many of the SAS data elements in the Integrated Data Base are
components of "arrays." The elements shown in Figure 1-4 called
XXY1 through XXY6 could be defined to SAS as a two-dimensional
array with two rows and three columns. This would be
accomplished by coding a SAS statement as follows:
ARRAY XXY{2,3} XXY1-XXY6;
One might visualize the first record's XXY array as follows:
column 1 column 2 column 3
row 112 3
row 24 5 6
The value of XXY(1,2) is 2, while the value of XXY(2,1) is 4.
For further discussion of SAS arrays please refer to the SAS
Users Guide; Basics. Version 5 Edition. Gary, NC: SAS Institute
Inc., 1985.
1.4 Data Element Coding Standards
The Integrated Data Base includes 1.8 million "cells" of data.
Many of the data elements are similar in the kind of data they
represent. The following data element coding standards were
adopted to make analysis of the data as easy as possible for the
user.
Flags
Flags that represent binary choices, such as yes/no, contain "*"
for yes-type responses and " " for no-type responses, except
where otherwise documented.
Validation Audit Failures
Data elements marked with an "*" in the "source" column of the
data elements descriptions have been recalculated during the data
base building process. The results were checked against the
output of LabData. Any record with a non-match between at least
one LabData captured value and its recalculated value was flagged
as a validation audit failure. The data element xxSTATUS was set
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to "E," where xx indicates the file (e.g., FSSTATUS was in the
Field Sample Master File).
Unique Key
The unique key in all files is the Analysis Lab Sample ID. This
data element is of the form xxANALID, where xx varies by file.
LCICs
When a data element occurs for each LCIC, the description says
"by 8 LCICs." The occurrences of the LCICs from 1 to 8 are as
follows:
Common
LCIC Abbreviation
1 = 1,2-Dichlorobenzene DCB
2 = 1,2,4-Trichlorobenzene TCB
3 = 1,2,3,4-Tetrachlorobenzene TeCB
4 = 2-Chloronaphthalene CNP
5 = Alpha-BHC A-BHC
6 = Delta-BHC D-BHC
7 = Beta-BHC B-BHC
8 = Gamma-BHC G-BHC
Surrogates
When a data element occurs for each surrogate, the description
says "by 3 surrogates." The occurrences from 1 to 3 are as
follows:
t Common
Surrogate Abbreviation
1 = 1,4-Dibromobenzene DBB
2 = 2,4,6-Tribromobiphenyl TBBP
3 = 1,2,4,5-Tetrabromobenzene QBE
Internal Standards
When a data element occurs for each internal standard, the
description says "by 5 Int Stds." The occurrences from 1 to 5
are as follows:
Common
Internal Standard Abbreviation
1 = D4-l,4-Dichlorobenzene IS1
2 = D8-Naphthalene IS2
3 = DIO-Acenaphthalene IS3
4 = DIO-Phenanthrene IS4
5 = DIO-Pyrene IS5
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SAS Dates
The dates in the Data Base are stored as SAS dates. Each date is
represented by the number of days between January 1, 1960 and
that date. The SAS language allows for flexibility in printing
dates in many recognizable forms.
1.5 Detailed Description of Individual File Sections
The remaining sections of this document provide detailed
descriptions of the files that compose the Integrated Data Base.
Each of these sections has three subsections, which contain the
following information:
n.l Logical Record Description - a narrative
description of the logical records in the file,
including counts, sort sequence, and data element
groupings
n.2 Logical Subsets of the File - a discussion of subsets
of the logical records in the file, including
illustrations of data elements to be used for typical
screening criteria
n.3 Data Element Dictionaries - detailed information about
every data element in the file, presented in subject-
related groupings. This information is given in
tabular form, with column heading as follows:
Data Element ID - ID of the form AA.Bnn, where:
AA is an abbreviation of the file,
FS = Field Sample Master File
FA = Field Sample Ancillary File
1C = Initial Calibration Master File
IA = Initial Calibration Ancillary File
CC = Continuing Calibration Master File
CA = Continuing Calibration Ancillary File
QC = Quality Control Master File
QA = Quality Control Ancillary File
Fl = Form 1 Master File
BQ = Blind Quality Control Master File
B is an alphabetical character assigned to a data
element group, and
nn is sequentially assigned within a data element
group
Name - SAS data element name
Type - type of data element:
CHAR for character, or
NUM for numeric
18
-------
Length - number of bytes used to store the data
element
Dimensions (for arrays) - shows the number of
dimensions for the data element array and the
number of elements in each dimension [e.g., (8,3)
is a two-dimensional array with 8 rows and 3
columns]
Description - text description of the data element,
including "by" phrase(s) to describe any array
dimensions (e.g., by eight LCICs)
Source System - identifies the system that provided
the data element values, either captured/reported
or computed (marked with a "*" prefix). Appendix
C contains the formulas that were used in the
computations.
19
-------
20
-------
2.0 Field Sample Master File and Ancillary File
A record in the Field Sample Master File contains all sample
collection, sample preparation, and GC/MS analysis data for all
field samples (HS), field splits (SPLIT), holding time samples
(HT), field handling blanks (FHB), preparation handling blanks
(PHB), and PHB splits.
Field samples were the soil samples actually taken from the
ramdomly selected locations in the various sampling areas.
Field splits were created at the preparation laboratory by
splitting a field sample in half. One half is treated just as
any other field sample, and the other receives a new project
sample ID (i.e., "HS" number). The results from the two halves
could then be linked for inter- or intra-laboratory comparisons.
Holding time samples were soil samples used to study the effects
of extending the sample holding time on LCIC concentration.
Field handling blanks were "blind" quality control (QC) samples
of uncontaminated soil. These samples were used to measure
cross-contamination of field samples throughout the shipping,
sampling, preparation, and analytical procedures.
Preparation handling blanks and PHB splits were QC samples of
uncontaminated soil that were sent to the analytic laboratories
along with the field samples. They were not analyzed unless
cross-contamination was measured in the field handling blanks.
Pointers, or keys, are present to join each sample's initial
calibration record, continuing calibration record, method blank
record, matrix spike (MS), and matrix spike duplicate (MSD)
records (if any), and Form I record.
2.1 Logical Record Description
A logical record in this file contains data for one sample. The
data elements are organized in groups, as follows:
- KEYS AND STATUS - the primary, unique identifier of each
record in the file, along with any other (perhaps
non-unique) keys, and the status flag.
- INTER-FILE LINKS/SECONDARY KEYS - Pointers, or keys,
providing linkage to the following records in
other files related to a sample: initial
calibration, continuing calibration,
method/holding blank, MS/MSD (if any), Form I, and
blind QC.
21
-------
INTRA-FILE LINKS/SECONDARY KEYS - Pointers, or keys,
providing linkage to records in this file related
to a sample.
CHRONOLOGY - dates and times of significant events during
the processing of the sample.
DATA TRANSFER TRACKING - system dates used for maintenance
of the data base.
FIELD SAMPLING DATA - data generated during the collection
of the sample in the field.
PREPARATION LAB DATA - data generated during the
preparation of the sample. The preparation
process consisted of removing the soil from the
sampling tube, homogenizing the soil, placing the
soil in a container for shipment, and shipping to
an analytical laboratory.
ANALYSIS LAB SAMPLE LOGIN DATA - data entered by the
analytic laboratory when the sample was logged
into their facility.
ANALYSIS LAB SAMPLE EXTRACTION DATA - data generated by
the analytic laboratory during the sample
extraction process. This process removes the
organic compounds from the solid soil material,
resulting in a liquid suitable for analysis on the
GC/MS.
ANALYSIS LAB INJECTION DATA - data entered by the lab
relating to injection of the sample in the GC/MS.
ANALYSIS LAB INTERPRETATION DATA - data identifying the
shift results file that the sample belonged to,
the quantitation method used for each analyte, and
the ion used for quantitation for each analyte.
This data also contains the results of the GC/MS
analysis when the peak height method of
quantitation was used.
CORRECTION FLAGS - flags used to indicate whether or not a
particular element has been corrected/updated. If
a flag is set "on" ("Y"), then the updated data is
contained in this file, and the original data
value is stored in the ancillary file record.
ANALYSIS RAW DATA - (after corrections, if any) raw data
generated by the GC/MS. This is essentially the
same data contained on the quantitation report
created by the GC/MS.
22
-------
- LABDATA COMPUTATIONS FOR FIELD SAMPLES - results
calculated by the LabData system using the raw
data generated by the GC/MS and additional data
entered by the laboratory. It includes the
concentration results after the identification
criteria (ID) have been applied, pre-criteria
concentrations, ID criteria results, and flags
indicating whether or not the criteria were met.
- LABDATA COMPUTATIONS FOR SURROGATE STANDARDS - results
computed by LabData for the surrogate recoveries
for the sample analysis. Included are the percent
recoveries, flags indicating whether or not the
recovery met the criteria, and the criteria.
- LABDATA COMPUTATIONS FOR INTERNAL STANDARDS - results
computed by LabData for the internal standards for
the sample analysis. Included are retention time
and area criteria check results.
- DATA VALIDATION FLAGS AND COMMENTS - results of the data
validation for the sample performed by EMSL-LV.
It includes data validation checklist responses,
comments, validation flags, and EMSL-LV usability
flags.
- INTEGRATED DATA BASE AUDIT SYSTEM FLAGS - results of the
automated audits and validations performed during
the data base building process.
The ancillary file consists of three groups: KEYS, CHRONOLOGY,
and DATA REPLACED BY CORRECTIONS. The last group corresponds to
the ANALYSIS RAW DATA group in terms of data elements, but
contains original data that has been replaced in the master file
by corrected data.
2.2 Logical Subsets of the File
The primary grouping of logical subsets in the Field Sample
Master File is based upon sample types. The table below describes
these sample types, along with sub-groups within each sample
type.
Sample
Type Code
(SAMPTYPE) Description
HS Original, randomly selected field sample. These
sample results were to be used for the comparison
analyses to determine if any differences in
contamination levels existed between the Love
Canal Emergency Declaration Area (EDA) and the
comparison areas.
23
-------
HS REP
SPLIT
FHB
PHB
HT
Replacement field sample for an uncollectable
original.
The field split half of a field sample was used to
measure inter- and intra-laboratory variability.
The field sample half retained the originally
assigned project sample ID. The field split half
was assigned a different project sample ID. Each
of these halves contains a data element (PLSID)
pointing to the other half.
Field handling blanks were "blind" Quality Control
(QC) samples of uncontaminated soil used to
measure whether cross-contamination had occurred.
Preparation handling blanks and PHB splits were QC
samples sent to the analytic laboratories along
with the field samples. They were not "blind" to
the analysis laboratory and were not analyzed
unless some contamination was measured in the
field handling blanks.
Holding time samples were soil samples used to
study the effects of extending the sample holding
time on LCIC concentration.
The first two sample types, "HS" and "HS REP," compose the group
of field samples used for comparison purposes. For most purposes
they are treated as a single group. Within the field sample
group there are several sub-groups, including:
Sub-group
Samples not
collected
Samples not
prepared
Samples not
analyzed
Description
Locations at which field
samples were planned, but
never were collected.
Some of the field samples
taken were not extrudable,
and no replacements were
able to be taken. These
samples have neither
preparation data nor
analysis data.
Some of the field samples
that were prepared but
could not be analyzed.
These samples have no
analysis data.
Selection Logic
(SITENBR not = 0
and HSID = blanks)
(SAMPTYPE="HS" or
"HS REP")
and FSFCDTE > 0
and FSPMDTE = 0
(SAMPTYPE="HS" or
"HS REP")
and FSFCDTE > 0
and FSPMDTE > 0
and FSAADTE = 0
24
-------
Analyzed The field samples that (SAMPTYPE="HSM or
Field were analyzed. Note "HS REP")
Samples that there are duplicate and FSAADTE > 0
analyses present for
some samples.
Field These were the field Same as above plus
Samples in sample results (numbering the deletion of the
Comparison 781) used in the 18 duplicates. See
Analysis statistical analyses. Section 8.6 for the
list.
When working with the analyzed field samples, it should be noted
that each sample was analyzed for the presence of eight analytes,
the LCICs. Any use of the concentration results in FSFILE
requires that the associated FORM1 file record (see Section 8) be
merged to obtain the data usability flags associated with the
results. Each analyte has its own data usability flag (LCICUSE1-
LCICUSE8), and the usability of each analyte should be examined
separately. For a description of the meaning of the usability
flags, refer to the field descriptions in Section 2.3. Careful
consideration should be exercised before using data not flagged
as "GOOD." Refer to Volume III, Soil Assessment—Indicator
Chemicals. Appendix H, CH2M HILL, 1988, for a complete
explanation of the validation flags associated with a usability
flag of "UNCERTAIN" or "BAD."
2 . 3 Data Element Dictionaries
The data element dictionaries for the Field Sample Master File
and the Field Sample Ancillary File follow this page.
25
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
NAME
ARRAY TYPE
FS.A01 ALANALID CHAR
FS.A02
FS.B01
FS.B02
FS.B03
FS.B04
FS.B05
FS.B06
FS.B07
FS.B08
FS.C01
FS.C02
FS.C03
FS.C04
FS.C05
FS.C06
FS.C07
FS.D01
FS.D02
FS.D03
FS.D04
FS.D05
FS.D06
FS.D07
FS.D08
FS.D09
FS.D10
FS.D11
FS.D12
FS.D13
FSSTATUS
Inter- File
I CANAL ID
CCANALID
MSANALID
MDANALID
MBANALID
RBANALID
OCANALID
CLEANHS
Intra-File
HSID
FDUPID
FHBID
SSBIDF
SSBIDP
PHBID
PLSID
Chronology
FSFCDTE
FSFCTME
FSFSDTE
FSPLDTE
FSPMDTE
FSPMTME
FSPSDTE
FSALDTES
FSALDTEL
FSAEDTE
FSAADTE
FSAATME
FSDBDTE
CHAR
Links/Secondary
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
Links/Secondary
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
LENGTH
23
1
DESCRIPTION
Analysis Lab Sample Id (Lab Id + Lab Analysis Id)
Status Flag
Values:
E = Validation Audit Failure
blank = passed Validation Audit
KGVS *******************************************************
23 Initial Calibration Id (Lab Id + Lab Analysis Id of
23 Continuing Calibration/Performance Check Id
23
23
23
23
23
(Lab Id + Lab Analysis Id of CC/PC1)
Matrix Spike Id (Lab Id + Lab Analysis Id)
SOURCE
LabData
IntDBBld
IC1) LabData
LabData
LabData
Matrix Spike Duplicate Id (Lab Id + Lab Analysis Id) LabData
Lab Method Blank Id (Lab Id + Lab Analysis Id)
Reagent Blank Id (Lab Id + Lab Analysis Id)
Quality Control Id (Lab Id + Lab Analysis Id) not
LabData
LabData
currently used
8 Original Project Id (HS Number) IntDBBld
ICsvs *********************************************************************
6 Project Field Sample Id (HS #) SampTrac
6 Revised Site Id (of the form nnnn or nnnnR); SampTrac
6
6
6
6
CHAR 6
************************
NUM 8
NUM 8
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
8
8
8
8
if no R suffix, resampling not done
Field Handling Blank Id (HS #)
Field Group Ship/Store Blank Id (HS #)
Prep Group Ship/Store Blank Id (HS #)
Prep Lab Handling Blank Id (HS #)
Prep Lab Split Id (HS #)
Field Collection Date
Field Collection Time
Field Ship Date
Prep Lab Login Date
Prep Lab Mix Date
Prep Lab Mix Time
Prep Lab Ship Date
Analysis Lab Login Date (Sample Tracking)
Analysis Lab Login Date (LabData)
Analysis Lab Extract Date
Analysis Lab Analysis Date
Analysis Lab Analysis Time
Data Validation Date
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
LabData
LabData
LabData
LabData
DataVal
26
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE • DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
NAME
ARRAY
TYPE LENGTH DESCRIPTION
******* Data Transfer Tracking
FS.E01
FS.E02
FS.E03
FS.E04
FS.E05
FS.E06
FS.E07
FSGENDTE
FSGENTME
FSADDDTE
FSADDTME
FSUPDDTE
FSUPDTME
FSUPDCNT
SOURCE
NUM 8 LabData Gen Date
NUM 8 LabData Gen Time
NUM 8 DB Add Date
NUM 8 DB Add Time
NUM 8 DB Most Recent Update Date
NUM 8 DB Most Recent Update Time
NUM 8 DB Update Count
**************************************
LabData
LabData
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
******* Field Sampling Data *************
FS.F01 COLFORM CHAR 5
FS.F02 COLFORMR CHAR 5
FS.F03 SAMPTYPE CHAR 6
****************************************************
FS.F04
FS.F05
FS.F06
FS.F07
FS.F08
FS.F09
FS.F10
FS.F11
FS.F12
FS.F13
FS.F14
FS.F15
FS.F16
FS.F17
FS.F18
FS.F19
FS.F20
SITENBR
STREET
MEDIA
XCOORD
YCOORD
XACTUAL
YACTUAL
LOCDIFF
AREAID
NEIGHID
TEAMNBR
COLLECTR
SOILCOMP
TUBENBR
COLMLEN
DUPLICAT
FLDCOM
(3)
CHAR
CHAR
CHAR
NUM
NUM
NUM
NUM
NUM
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
NUM
CHAR
CHAR
4
70
1
8
8
8
8
8
1
2
2
20
80
4
8
1
80
Sample Collection Form # SampTrac
Sample Collection Replacement Form # SampTrac
Sample Type SampTrac
Values:
'HS ' = Field Sample
= Replacement Field Sample
= Field Sample Split
= Field Handling Blank
= Shipping & Storage Blank
= SSB Split
= Prep Lab Handling Blank
= Holding Time Blank
= Unable to classify, no Project Id assigned
'HS REP
•SPLIT1
'FHB'
'SSB1
•SSB SP
'PHB1
•HT '
'UNK'
Site Number
Street Address
Media (a constant of 'S')
Site X Coordinate
Site Y Coordinate
Site X Coordinate
Site Y Coordinate
Difference in feet between X/YCOORD & X/YACTUAL
Area Id
Values:
C = Cheektowaga
E = EDA (Emergency Declaration Area
I = Tonawanda
N = Niagara Falls (CT221 and CT225)
blank = no area (holding time blanks)
Neighborhood Id
Sampling Team Number
Sample Collector Name (text)
Soil Composition
Collection Tube Number
Length of Soil Column
Duplicate Flag
Field Comments (text 3X80)
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
IntDBBld
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
currently not used
SampTrac
27
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
FS.F21
FS.F22
FS.F23
FS.F24
FS.F25
FS.G01
FS.G02
FS.G03
FS.G04
FS.G05
FS.G06
FS.G07
FS.G08
FS.G09
FS.G10
FS.G11
FS.G12
FS.G13
FS.G14
FS.G15
FS.G16
FS.G17
FS.G18
FS.G19
FS.G20
NAME
FCOCFORM
FTRFFORM
FLFEDEX
FLSRMKS
FLPRVBLK
Preparation
PREPLAB
PREPCOND
PREPCOMM
PLRECBY
SPFORM
MIXRNAME
MIXTEAM
PREPCOM
TRAKCOM
SPLIT
PCOCFORM
PTRFFORM
MSFLAG
PLJARNBR
PLSPACE
PLPOSHI
PLSHMETH
PLFEDEX
PLSRMKS
PLPRVBLK
ARRAY TYPE
CHAR
CHAR
CHAR
CHAR
CHAR
Lab Data ******
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
(2) CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
NUM
NUM
CHAR
CHAR
CHAR
CHAR
CHAR
LENGTH
4
4
10
80
6
3
30
12
20
5
20
1
80
19
1
5
5
1
8
8
1
7
10
80
6
DESCRIPTION
Field Chain of Custody Form # (of the form Fnnn)
Traffic Report for Tubes Form # (of the form nnnn)
Fed Ex Airbill Number
Field Shipping Special Instructions
Field QC Samples Only Data
Previous Field Blank Id (HS #) currently
Prep Lab Id (a constant of 'CAA')
Condition on Receipt by Prep Lab (text)
Sampling Team Comment
Person Receiving in Prep Lab
Sample Preparation Form # (of the form Cnnnn)
Mixer Name (text)
Mixing Team
Values:
1 = Team 1
2 = Team 2
3 = Team 3
blank = unknown
Prep Comments (text 2X80)
Tracking Comment
Designated Split
Va I ues :
X = sample has been split; Id of split is
contained in field PLSID
blank = sample has not been split
Prep Lab Chain of Custody Form # (of the form 'Ennn ')
Traffic Report for Prepared Samples Form #
(of the form 'Dnnn ')
Matrix Spike Flag currently
Preparation Lab Jar Number
Head Space
Possible High Analysis Values
Values:
X = possible high concentration, subject to
screening analysis prior to GC/MS
blank = no screening analysis planned
Preparation Lab Shipping Method (a constant of 'FED EX1)
Fed Ex Airbill Number
Prep Lab Special Shipping Instructions
Prep Lab QC Samples Only
Previous Prep Lab Blank Id (HS #) currently
SOURCE
SampTrac
SampTrac
SampTrac
SampTrac
not used
1t1t1tit1t1t1tit
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampT rac
SampTrac
SampTrac
SampTrac
SampTrac
not used
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
SampTrac
not used
28
-------
DATA
ELEMENT
ID
FS.G21
NAME ARRAY
EXCPFLAG
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
TYPE LENGTH DESCRIPTION
SOURCE
NUM
FS.G22 FTTEMP
FS.G23 TRTEMP
NUM
NUM
Exception Flag SampTrac
Values:
0 = sent to analysis lab
1 = collected, but not prepped
2 = prepped, sent to analysis lab, but only screened
3 = sample not collected
Temperature inside cooler on arrival at preparation SampTrac
lab, in degrees Celsuis
Temperature inside cooler on arrival at analytic lab, SampTrac
in degrees Celsuis
******* Analysis Lab Sample Login Data **********************************************************************
FS.H01
FS.H02
FSSMPL
FSALID
FS.H03 FSALCOND
FS.H04 ALRECBY
FS.H05 FSRERUN
FS.H06 FSRRSTAT
FS.H07 FSORIG
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
10
3
30
20
2
1
1
Project Sample Id
Analytic Laboratory Id
Values:
AQI
CAA
CEC
EMS
MGM
NU2 = Contingency samples • for possible
replacement; prepped and stored but never
analyzed
NUS
VER
blanks = no analysis performed; therefore no Lab Id
LabOata
SampTrac
Condition on Receipt by Analysis Lab (text)
Person Receiving in Analysis Lab
Re-run Flag
Re-run Type
Orig. Found Flag
SampTrac
SampTrac
currently not used
currently not used
currently not used
FS.I01
FS.I02
FS.I03
FS.I04
FS.I05
Analysis Lab Sample Extraction Data *********************
FSTWTEXT
FSWTEXT
FSMOIST
FSCONCDF
FSEXTANL
NUM 8 Target Weight to Extract (gm)
NUM 8 Weight Extracted (gm)
NUM 8 Percent Moisture
NUM 8 Concentration Dilution Factor
CHAR 8 Extraction Analyst
LabOata
LabData
LabOata
LabOata
LabData
29
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
*******
FS
FS
FS
FS
.J01
.J02
.J03
.J04
*******
FS
FS
FS
FS
FS
FS
FS
FS
FS
FS
FS
FS
FS
FS
.K01
.K02
.K03
.K04
.K05
.K06
.K07
.K08
.K09
.K10
.K11
.K12
.K13
.K14
FS.K15
FS
FS
FS
FS
FS
FS
FS
.L01
.L02
.L03
.L04
.L05
.L06
.L07
NAME
Analysis Lab
FSINSTID
FSANLST
FSFILE
FSINJVOL
Analysis Lab
FSQFILE
FSQMTH
FSQION
FSLCPH
FSISPH
FSPYRPH
FSSSPH
FSHLCS
FSHLCR
FSHISS
FSHISR
FSHPYRS
FSHPYRR
FSHSSS
ARRAY
TYPE
Injection Data
CHAR
CHAR
CHAR
NUM
Interpretation
(8,3)
(8)
(8,3)
(5)
(3)
(8,3)
(8,3)
(5)
(5)
(3)
CHAR
CHAR
CHAR
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
LENGTH DESCRIPTION
SOURCE
*************************************************************************
15
8
15
8
Data
12
1
1
8
8
8
8
8
8
8
8
8
8
8
GC/MS Instrument Id
GC/MS Analyst
GC/MS Datafile Id
Injection Volume (ul)
LabOata
LabOata
LabOata
LabOata
********************************************************************
GC/MS Shift Results File Name
Quantisation Method Flag, by 8 LCICs, by 3 Ions
Values:
blank }
or } = GC/MS Automatic Area Quant i tat ion
A }
H = Peak Height Quant i tat ion
M = GC/MS Manual Quant i tat ion
0 = Computed using area by LabOata with correction
data
LCIC Quant i tat ion Ion Selection, by 8 LCICs
Values:
blank = primary ion used for quant i tat ion
S = secondary ion used for quant i tat ion
T = tertiary ion used for quant i tat ion
Peak Height, by 8 LCICs, by 3 Ions
Peak Height, by 5 Int. Stds. (Primary Ion)
Peak Height Pyrene-D10 (Secondary Ion)
Peak Height, by 3 Surrogates (Primary Ion)
Scan for Peak Height, by 8 LCICs, by 3 Ions
Retention Time for Peak Height, by 8 LCICs, by 3 Ions
Scan for Peak Height, by 5 Int. Stds.
Retention Time for Peak Height, by 5 Int. Stds.
Scan for Peak Height for Pyrene-D10
Retention Time for Peak Height for Pyrene-D10
Scan for Peak Height, by 3 Surrogates
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabOata
LabData
LabData
LabData
LabData
LabData
FSHSSR (3) HUM 8 Retention Time for Peak Height, by 3 Surrogates LabOata
Values:
Y = data corrected, original data stored in ancillary file
blank =
FSCDATE
FSCTIME
FSCANAL
FSCLCA
FSCLCS
FSCLCR
FSCISA
data not
(8,3)
(8,3)
(8,3)
(5)
corrected,
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
1
1
1
1
1
1
1
no data stored in ancillary file
Analysis Lab Analysis Date
Analysis Lab Analysis Time
Analyst Entering the Correction Data
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
LabData
LabData
LabData
LabData
LabData
LabData
LabData
30
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
FS.L08
FS.L09
FS.L10
FS.L11
FS.L12
FS.L13
FS.LU
FS.L15
*******
FS.M01
FS.M02
FS.M03
FS.M04
FS.M05
FS.M06
FS.M07
FS.M08
FS.M09
FS.M10
FS.M11
FS.M12
*******
FS.N01
FS.N02
FS.N03
FS.N04
FS.N05
FS.N06
FS.N07
FS.N08
FS.N09
FS.N10
FS.N11
FS.N12
NAME
FSCISS
FSCISR
FSCPYRA
FSCPYRS
FSCPYRR
FSCSSA
FSCSSS
FSCSSR
Analysis Raw
FSLCA
FSLCS
FSLCR
FSISA
FSPYRA
FSISS
FSPYRS
FSISR
FSPYRR
FSSSA
FSSSS
FSSSR
ARRAY
(5)
(5)
(3)
(3)
(3)
TYPE
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
LENGTH
1
1
1
1
1
1
1
1
DESCRIPTION
Scan, by 5 Int. Stds. (Primary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates (Primary Ion)
SOURCE
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
Data (After Corrections if any) ******************************************************
(8,3)
(8,3)
(8,3)
(5)
(5)
(5)
(3)
(3)
(3)
LabData Computations
FSRR
FSRRC
FSRRF
FSCONCB
FSCONCA
FSIRAT
FSIONF
FSMINS
FSMAXS
FSRANG
FSRANGF
FSIDEVT
(8)
(8)
(8)
•
(8)
(8)
(8)
(8)
(8)
(8)
(8)
(8)
(8)
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
8
8
8
8
8
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates (Primary Ion)
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
for Field Samples **************************************************************
NUM
NUM
CHAR
NUM
NUM
NUM
CHAR
NUM
NUM
NUM
CHAR
NUM
8
8
1
8
8
8
1
8
8
8
1
8
Relative Retention Time, by 8 LCICs (Quantitation Ion)
Relative Retention Time Criteria, by 8 LCICs
Flag for Rel. Ret. Time Out of Criteria, by 8 LCICs
Values:
* = Out of criteria
blank = Within criteria
PrelD-criteria Concentration, by 8 LCICs
(i.e. primary ion equivalent concentration)
Id Criteria applied Concentration, by 8 LCICs
Ion Ratio, by 8 LCICs
Flag for All Ions Being Present, by 8 LCICs
Values:
* = All ions present
blank = One or more ions not present
Minimum Scan Number of 3 Ions, by 8 LCICs
Maximum Scan Number of 3 Ions, by 8 LCICs
Scan Range (Max • Hin), by 8 LCICs
Flag for Scan range > 2, by 8 LCICs
Values:
* = Scan range greater than 2
blank = Scan range not greater than 2
Ion Ratio % Dev. from Theoretical Values, by 8 LCICs
*LabData
LabData
*LabOata
*LabOata
*LabOata
*LabData
*LabOata
LabData
LabData
•LabData
•LabData
•LabData
31
-------
DATA
ELEMENT
ID
FS.N13
NAME
FSIDEVF
ARRAY
(8)
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
TYPE LENGTH DESCRIPTION
CHAR
FS.N14 FSPRESCR
CHAR
FS.N15
FSSULFUR
CHAR
Flag for Ion ratio % Dev. Out of Criteria, by 8 LCICs
Values:
* = Ion ratio out of criteria; greater than 40%
+ = Ion ratio out of criteria; 20% < ratio <= 40%
blank = Ion ratio within criteria
Flag for Analysis Pre-screen
Values:
'MS ' = GC/MS pre-screening performed
'ECD1 = GC/ECD pre-screening performed
blanks = no pre-screening done
Flag for Sulphur Cleanup Performed
Values:
Y = sulphur cleanup performed
blank or N = no sulphur cleanup performed
SOURCE
*LabOata
LabOata
LabData
*******
FS.001
FS.002
FS.003
FS.004
FS.005
FS.006
FS.P01
FS.P02
FS.P03
FS.P04
FS.P05
FS.P06
FS.P07
FS.P08
LabData Computations
FSPR
FSPRF
FSSSADD
FSPRCL
FSPRCU
FSPROUT
(3)
(3)
(3)
(3)
(3)
LabData Computations
FSISADD
FSRD (5)
FSAD
FSRF
FSAF
FSRDC
FSADCL
FSADCU
(5)
(5)
(5)
(5)
(5)
(5)
for Surrogate
NUM
CHAR
NUM
NUM
NUM
NUM
8
1
8
8
8
8
for Internal
NUM 8
NUM 8
NUM
CHAR
CHAR
NUM
NUM
NUM
8
1
1
8
8
8
Standards ********************************************
% Recovery by 3 Surrogates
Flag for % Rec. Out of Criteria, by 3 Surrogates
Values:
* = Out of criteria
blank = Within criteria
Amount of Surrogate added (ng), by 3 Surrogates
% Recovery Criteria lower limit, by 3 Surrogates
% Recovery Criteria upper limit, by 3 Surrogates
Number of % Rec. Out of Criteria
Internal Standard Quantity Added (in nanograms)
Ret. Time Difference From CC Val, by 5 Int Stds
Area Difference % From CC Val, by 5 Int Stds
Flag for Ret. Time Out of Criteria, by 5 Int Stds
Values:
* = Out of criteria
blank = Within criteria
Flag for Area Out of Criteria, by 5 Int Stds
Values:
* = Out of criteria
blank = Within criteria
Retention Time Difference Criteria, by 5 Int Stds
Area % Diff. Crit. lower limit, by 5 Int Stds
Area % Diff. Crit. upper limit, by 5 Int Stds
•LabData
*LabData
LabOata
LabData
LabData
LabOata
LabOata
•LabOata
•LabOata
•LabData
•LabOata
LabData
LabData
LabData
32
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE • DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
FS.Q01
FS.Q02
FS.Q03
FS.Q04
FS.Q05
FS.Q06
FS.Q07
FS.Q08
FS.Q09
FS.Q10
FS.Q11
FS.Q12
FS.Q13
FS.Q14
FS.Q15
FS.Q16
FS.Q17
FS.Q18
FS.Q19
FS.Q20
FS.Q21
FS.Q22
FS.Q23
FS.Q24
*******
NAME ARRAY TYPE
LENGTH DESCRIPTION SOURCE
Values: (not currently available)
FSSURRA
FSSURRB
FSSURRC
FSSURCM
FSINTA
FSINTB
FSINTC
FSINTCM
FSIDA
FSIDB
FSIDC
FSIDD
FSIDE
FSIDCOM
FSQTA
FSQTB
FSQTC
FSQTCOM
FSGENA
FSGENB
FSGENC
FSGEND
FSGENCM
FSDQ
Integrated
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
CHAR
NUM
(3) CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
(8,5) CHAR
DB Audit System
1 Check surrogates spiked in all samples
1 Surrogates recoveries within criteria
1 Surrogates Miscellaneous
60 Surrogates Comments
1 Internal Standards RT Criteria
1 Internal Standards Area Criteria
2 Internal Standards Miscellaneous
60 Internal Standards Comments
1 Id All ions maximize simultaneously
1 Id Appropriate flags used.
1 Id All peaks reported that meet id criteria
2 Id Low level peaks examined
2 Id Miscellaneous
60 Id Comments
1 Quantitation appropriate RRF's used if nonstandard
1 Check integration parameters if manual quant, used
2 Quantitation Miscellaneous
60 Quantitation Comments
2 Review case narrative and address all problems
2 Examine SICPS
2 Examine quant i tat ion reports
2 General Miscellaneous
60 General Comments
2 Data Qualifier flags samples by analyte
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
Flags ********************************************************************
Values (except where indicated otherwise):
FS.R01
FS.R02
FS.R03
FS.R04
FS.R05
FS.R06
FS.R07
FS.R08
FS.R09
FS.R10
blank
1*1 -
FSTRACK
FSF1FLAG
FSICREF
FSCCREF
FSMSREF
FSMDREF
FSRBREF
FSMBREF
FSDUP
FSFHB
= record found /
record not found
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
no discrepancy / no difference
/ discrepancy / difference
1 Flag for Sample NOT Found in Sample Tracking
1 Flag for Sample Match to FORM1 Master File
Values:
1 = Found FORM1 and All data matches
2 = Found FORM1 and some data does not match
3 = No FORM1 found
blank = FORM1 match not attempted (sample tracking
records not matching field sample records)
1 Flag for 1C not found or date/time inconsistent
1 Flag for CC not found or date/time inconsistent
1 Flag for MS not found
1 Flag for MSD not found
1 Flag for RB not found
1 Flag for MB not found
1 Flag for Field Duplicate not found currently
1 Flag for Field Handling Blank not found currently
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
not used
not used
33
-------
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION ^SOURCE
FS.R11 FSSSBF CHAR 1 Flag for Shipping & Storage Blank not found currently not used
FS.R12 FSSSBP CHAR 1 Flag for Shipping & Storage Blank not found currently not used
FS.R13 FSPHB CHAR 1 Flag for Prep Lab Handling Blank not found currently not used
FS.R14 FSPLS CHAR 1 Flag for Prep Lab Split not found currently not used
FS.R15 FSRECALC CHAR 1 Flag for recalculation discrepancy on at least IntDBBld
one data element computed by LabData system
(within .2% tolerance)
FS.R16 FSDIFLAB CHAR 1 Flag for diff. lab between LabData & Samptrac currently not used
34
-------
DATA
ELEMENT
ID
***
FA.A01
NAME
ARRAY
LOVE CANAL HABITABILITY STUDY
FIELD SAMPLE ANCILLARY FILE - DATA ELEMENT DICTIONARY
TYPE LENGTH DESCRIPTION
SOURCE
Keys
************************************************************************************
ALANALID
CHAR
23 Analysis Lab Sample Id (Lab Id + Lab Analysis Id)
LabOata
******* Data Transfer Tracking ******************************************************************************
FA.B01
FA.B02
FA.B03
FA.B04
FA. BOS
FA.B06
FA.B07
*******
FA.C01
FA.C02
FA.C03
FA.C04
FA. COS
FA.C06
FA.C07
FA. COS
FA.C09
FA.C10
FA.C11
FA.C12
FSGENDTE
FSGENTME
FSADDDTE
FSADDTME
FSUPDDTE
FSUPDTME
FSUPDCNT
Data Replaced
FSLCA
FSLCS
FSLCR
FSISA
FSPYRA
FSISS
FSPYRS
FSISR
FSPYRR
FSSSA
FSSSS
FSSSR
by
(8,
(8,
(8,
(5)
(5)
(5)
(3)
(3)
(3)
NUM
NUM
NUM
NUM
NUM
NUM
NUM
Corrections
3) NUM
3) NUM
3) NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
***!
8
8
8
8
8
8
8
8
8
8
8
8
LabOata Gen Date
LabOata Gen Time
DB Add Date
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
DB Update Count
LabOata
LabData
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
************************************************************************
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates (Primary Ion)
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabOata
35
-------
36
-------
3.0 Initial Calibration Master File and Ancillary File
In the Initial Calibration Master File, a record contains all
quantitation report and computed data for each five-point initial
calibration and/or EPA performance check analysis run on the
GC/MS. The performance check analysis could be run either in the
same analytic run (i.e., "shift") as the five-point, or in a
later shift. Therefore some records contain the five-point data
and the performance check data; some records, only the five-point
data; and some records, only the performance check data.
Logically, this data represents the top of the data structure.
All continuing calibrations are associated with a five-point
initial calibration; thus one or many continuing calibration
records will point to a single initial calibration record.
3.1 Logical Record Description
A logical record in this file contains data for one five-point
initial calibration and/or EPA performance check. The data
elements are organized in groups, as follows:
- KEYS AND STATUS - the primary, unique identifier of each
record in the file, along with any other (perhaps
non-unique) keys, and the status flag.
- CHRONOLOGY - dates and times of significant events during
the processing of the sample.
- DATA TRANSFER TRACKING - system dates used for maintenance
of the data base.
- ANALYSIS LAB SAMPLE LOGIN DATA - data entered by the
analytic laboratory when the sample was logged
into their facility.
- ANALYSIS LAB INJECTION DATA - data entered by the lab
relating to injection of the sample in the GC/MS.
- ANALYSIS LAB INTERPRETATION DATA - data identifying the
shift results file that the sample belonged to,
the quantitation method used for each analyte, and
the ion used for quantitation for each analyte.
This data also contains the results of the GC/MS
analysis when the peak height method of
quantitation was used.
- CORRECTION FLAGS - flags used to indicate whether or not a
particular element has been corrected/updated. If
a flag is set "on" ("Y"), then the updated data is
contained in this file, and the original data
value is stored in the ancillary file record.
37
-------
- ANALYSIS RAW DATA - (after corrections, if any) raw data
generated by the GC/MS. This is essentially the
same data contained on the quantitation report
created by the GC/MS.
- LABDATA COMPUTATIONS FOR INITIAL CALIBRATION - results
calculated by the LabData system using the raw
data generated by the GC/MS. It includes the
initial calibration response factor results, the
QC criteria, and flags indicating whether or not
the criteria were met.
- LABDATA COMPUTATIONS FOR EMSL PERFORMANCE CHECK - results
calculated by the LabData system using the raw
data generated by the GC/MS. It includes the
initial calibration percent recovery results, the
QC criteria, and flags indicating whether or not
the criteria were met.
- DATA VALIDATION FLAGS AND COMMENTS - results of the data
validation for the sample performed by EMSL-LV.
It includes data validation checklist responses,
comments, validation flags, and EMSL-LV usability
flags.
- INTEGRATED DATA BASE AUDIT SYSTEM FLAGS - results of the
automated audits and validations performed during
the data base building process.
The ancillary file consists of three groups: KEYS, CHRONOLOGY,
and DATA REPLACED BY CORRECTIONS. The last group corresponds to
the ANALYSIS RAW DATA group in terms of data elements, but
contains original data that has been replaced in the master file
by corrected data.
3.2 Logical Subsets of the File - Special Screening
There are two primary groups of logical subsets in the Initial
Calibration (1C) Master File. Initially, the design of the data
base assumed that an EPA Performance Check Standard analysis
would be analyzed in the same analytic run as the five-point
initial calibration. Accordingly, a record in the 1C file was
designed to contain each five-point analysis and one EPA
Performance Check. Unfortunately, this did not turn out to
always be the case. In most cases, the EPA Performance Check was
run with the five-point analysis, and the 1C record contains all
six analyses. In some cases, the EPA Performance Check was run
in a later analysis shift and, as a result, is contained in a
separate 1C file record. Thus some 1C file records have only the
five-point analyses data, some have only the EPA Performance
Check data, and some have both. Since the data are typically
analyzed separately, this limitation should not be a problem. .
38
-------
To obtain those records containing five-point analyses, select
those records where the field ICSMPL1 = "IC1". To obtain those
records containing an EPA Performance Check, select those records
where the field ICSMPL6 = "EMPC" in the first four character
positions (in SAS use the SUBSTR command).
3.3 Data Element Dictionaries
The data element dictionaries for the Initial Calibration Master
File and the Initial Calibration Ancillary File follow this page.
39
-------
LOVE CANAL HABITABILITY STUDY
INITIAL CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION .SOURCE
***** KeyS and status ***************************************************************************************
IC.A01 I CANAL ID CHAR 23
IC.A02 ICANAL (4) CHAR 23
IC.A03 ICSTATUS CHAR 1
Initial Calibration Id LabOata
(Lab Id + Lab Analysis Id of the IC1 analysis)
Initial Calibration Id LabOata
(Lab Id + Lab Analysis Id of the IC2-IC5 analyses)
Status Flag IntDBBld
Values:
E = Validation Audit Failure
blank = Passed Validation Audit
Chronology
******************************************************************************************
IC.B01 ICAADTE (6) NUM
IC.B02 ICAATME (6) NUM
Analysis Lab Analysis Date,
by 5 Calibration Concentrations and EMSL PC
Analysis Lab Analysis Time
by 5 Calibration Concentrations and EMSL PC
LabData
LabData
******* Data Transfer Tracking
IC.C01
IC.C02
IC.C03
IC.C04
1C. COS
IC.C06
IC.C07
ICGENDTE
ICGENTME
ICADDDTE
ICADDTME
ICUPDDTE
ICUPDTME
ICUPDCNT
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
LabData Gen Date
LabData Gen Time
DB Add Date
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
DB Update Count
LabData
LabOata
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
***** Analysis Lab Sample Login Data **********************************************************************
IC.D01 ICSMPL (6) CHAR 10 Project Sample Id for Id thru IC5 and EMSL PC
Values for each of ICSMPL1 through ICSMPL5:
'ICn '= Initial calibration record generated
by a five-point initial calibration
(Where ICn takes the value of IC1 in ICSMPL1,
IC2 in ICSMPL2, etc. through IC5)
blank = Initial calibration record generated by a
stand-alone EMSL performance check
Values for ICSMPL6:
blank = no EMSL performance check data in this
record (only five-point calibration data)
'EMPC1 in the first four positions = EMSL
performance check data in this record
LabData
40
-------
DATA
ELEMENT
ID
IC.D02
NAME
ICALID
ARRAY
LOVE CANAL HABITABILITY STUDY
INITIAL CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
TYPE LENGTH DESCRIPTION
SOURCE
CHAR
Analytic Laboratory Id
Values:
AQI
CAA
CEC
EMS
MGM
NU2 = Contingency samples - for possible replacement;
prepped and stored but never analyzed
NUS
VER
blanks = no analysis performed; therefore no Lab Id
LabData
*******
IC.E01
IC.E02
IC.E03
IC.E04
1C. EOS
IC.E06
IC.E07
1C. EOS
IC.E09
IC.E10
IC.E11
IC.F01
IC.F02
Analysis Lab
ICINSTID
ICINSTMF
ICINSTMN
ICISCODE
ICSOLCD
ICCCCODE
ICCOLMMF
ICCOLMSN
ICANLST
ICFILE
ICINJVL
Analysis Lab
ICQFILE
ICQMTH
Injection
(5)
(6)
(6)
(6) >
Data
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
NUM
Interpretation
CHAR
(8,3) CHAR
****i
15
20
20
1
1
1
20
20
8
15
8
Data
12
1
Inj ect ion Data *************************************************************************
IC.F03
GC/MS Instrument Id
GC/MS Instrument Manufacturer
GC/MS Instrument Model Number
Internal Standard Solution Code
Initial Calibration Solution Codes (5)
Continuing Calibration Solution Code
Column Manufacturer
Column Serial Number
Analyst,
by 5 Calibration Concentrations and EMSL PC
Datafile Id,
by 5 Calibration Concentrations and EMSL PC
Injection Volume (ul),
by 5 Calibration Concentrations and EMSL PC
ICQION
(8)
CHAR
GC/MS Shift Results File Name
For IC2 ONLY:
Quantitat ion Method Flag, by 8 LCICs,
by 3 Ions
Values:
blank >
or > = GC/MS Automatic Area Quantitat ion
A >
H = Peak Height Quantitat ion
M = GC/MS Manual Quantitat ion
0 = Computed using area by LabData with correction
data
LCIC Quantitation Ion Selection, by 8 LCICs
Values:
blank = primary ion used for quantisation
S = secondary ion used for quantitation
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
*********
LabData
LabData
LabData
41
-------
LOVE CANAL HABITABILITY STUDY
INITIAL CALIBRATION MASTER FILE • DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
F04
F05
F06
F07
F08
F09
F10
F11
F12
F13
FU
F15
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
1C.
G01
G02
G03
G04
G05
G06
G07
G08
G09
G10
G11
G12
G13
G14
G15
*******
1C.
1C.
1C.
1C.
H01
H02
H03
H04
NAME
ICLCPH
ICISPH
ICPYRPH
ICSSPH
ICHLCS
ICHLCR
ICHISS
ICHISR
ICHPYRS
1CHPYRR
ICHSSS
ICHSSR
ARRAY
(8,3)
(5)
(3)
(8,3)
(8,3)
(5)
(5)
.
(3)
(3)
TYPE
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
LENGTH
8
8
8
8
8
8
8
8
8
8
8
8
DESCRIPTION
T = tertiary ion used for quant i tat ion
Peak Height, by 8 LCICs, by 3 ions
Peak Height, by 5 Int. Stds. (Primary Ion)
Peak Height Pyrene-D10 (Secondary Ion)
Peak Height, by 3 Surrogates (Primary Ion)
Scan for Peak Height, by 8 LCICs, by 3 Ions
Retention Time for Peak Height, by 8 LCICs,
by 3 Ions
Scan for Peak Height, by 5 Int. Stds.
Retention Time for Peak Height, by 5 Int.
Stds.
Scan for Peak Height for Pyrene-D10
Retention Time for Peak Height for
Pyrene-D10
Scan for Peak Height, by 3 Surrogates
Retention Time for Peak Height, by 3
SOURCE
LabData
LabOata
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
Surrogates
Values:
Y = data corrected, original data stored in ancillary file
blank
1CCDATE
ICCTIME
ICCANAL
ICCLCA
1CCLCS
ICCLCR
ICCISA
ICCISS
ICCISR
ICCPYRA
ICCPYRS
ICCPYRR
ICCSSA
ICCSSS
ICCSSR
= data not
(8,3)
(8,3)
(8,3)
(5)
(5)
(5)
(3)
(3)
(3)
Analysis Raw Data, By
(After
ICLCA
ICLCS
ICLCR
ICISA
corrected, no
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
5 Calibration
Corrections, if
(6,8,3)
(6,8,3)
(6,8,3)
(6,5)
NUM
NUM
NUM
NUM
any)
8
8
8
8
data stored in ancillary file
Analysis Lab Analysis Date
Analysis Lab Analysis Time
Analyst
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Retention Time,
by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time,
by 3 Surrogates (Primary Ion)
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabOata
LabData
LabData
LabData
LabData
Concentrations and EMSL Performance check************************
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
LabData
LabData
LabOata
LabOata
42
-------
LOVE CANAL HABITABILITY STUDY
INITIAL CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
IC.H05
IC.H06
IC.H07
1C. HOB
IC.H09
IC.H10
IC.H11
IC.H12
1C. 101
1C. 102
1C. 103
1C. 104
1C. 105
1C. 106
1C. 107
IC.J01
IC.J02
IC.J03
IC.J04
1C. JOS
IC.J06
IC.J07
1C. JOS
IC.J09
NAME
ICPYRA
ICISS
ICPYRS
ICISR
ICPYRR
ICSSA
ICSSS
ICSSR
ARRAY
(6)
(6,5)
(6)
(6,5)
(6)
(6,3)
(6,3)
(6,3)
LabOata Computations
ICMRF (11)
ICRSD (11)
ICRSDC
ICRSDF
ICRSDOUT
ICRF
ICCONC
(11)
(11)
(11,5)
(5)
LabData Computations
PCTCON (11)
PCPRLC
PCPRUC
PCPROUT
PCCONC
PCPR
PCPRF
PCISADD
PCVOLMCS
(11)
(11)
(11)
(11)
(11)
TYPE
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
LENGTH
8
8
8
8
8
8
8
8
DESCRIPTION
Area Pyrene-D10 (Secondary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-DIO (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
SOURCE
LabData
LabData
LabData
LabData
LabData
LabData
LabData
Retention Time, by 3 Surrogates (Primary Ion) LabData
NUM 8 Mean Response Factors, by 8 LCICs and 3 Surrogates *LabOata
NUM 8 % Relative Std. Dev., by 8 LCICs and 3 Surrogates *LabOata
NUM
CHAR
NUM
NUM
NUM
8
1
8
8
% Relative Std. Dev. criteria, by 8 LCICs
and 3 Surrogates
Flag for % Relative Std. Dev. out of criteria.
by 8 LCICs and 3 Surrogates
Values:
* = Out of criterin
blank = Within criteria
Number of % Relative Std. Dev. out of criteria
Response Factors, by 8 LCICs and 3 surrogates.
by 5 Calibration Concentrations
8 Concentrations, by 5 Calibration Concentrations
NUM 8 Theoretical Concentrations, by 8 LCICs
and 3 Surrogates
NUM
NUM
NUM
NUM
NUM
CHAR
NUM
NUM
8
8
8
8
8
1
8
8
% Recovery Lower Criteria, by 8 LCICs
and 3 Surrogates
% Recovery Upper Criteria, by 8 LCICs
and 3 Surrogates
Number of % Recovery Out of Criteria
Concentrations, by 8 LCICs and 3 Surrogates
% Recovery, by 8 LCICs and 3 Surrogates
Flag for % Recovery Within Criteria,
by 8 LCICs and 3 Surrogates
Values:
* = Out of criterin
blank = Within criteria
Amount of Internal Standard Added
Volume of Check Standard Solution
LabData
*LabData
LabData
*LabData
LabData
kit it it it it it it it it it it it it
LabData
LabData
LabData
LabData
•LabData
•LabData
•LabData
LabData
LabData
43
-------
LOVE CANAL HABITABILITY STUDY
INITIAL CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION SOURCE
******* Data Validation Flags and Cofments ******************************************************************
Values: (currently not available)
IC.K01 ICCALA CHAR 1 1C % RSD exceptions checked DataVal
IC.K02 ICCALB CHAR 2 1C check quantisation reports for evidence of editing DataVal
IC.K03 ICCALC CHAR 2 1C examine chromatograms DataVal
IC.K04 ICCALD CHAR 2 1C Miscellaneous DataVal
IC.K05 ICDVCOM (3) CHAR 60 1C Comments DataVal
******* integrated DB Audit System Results ******************************************************************
IC.L01 ICRECALC CHAR 1 Flag for calculation discrepancies IntDBBld
Values:
* = Discrepancy (could be a result of not having
all five-points plus performance check)
blank = No discrepancy
44
-------
LOVE CANAL HABITABILITY STUDY
INITIAL CALIBRATION ANCILLARY FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION SOURCE
***** Keys ************************************************************************************
IA.A01
I CANAL ID
CHAR 23 Initial Calibration Id
(Lab Id + Lab Analysis Id of the IC1 analysis)
LabData
******* Data Transfer Tracking ******************************************************************************
IA.B01
IA.B02
IA.B03
IA.B04
IA.B05
IA.B06
IA.B07
*******
IA.C01
IA.C02
IA.C03
IA.C04
IA.C05
IA.C06
IA.C07
IA.C08
IA.C09
IA.C10
IA.C11
IA.C12
ICGENDTE
ICGENTME
ICADDDTE
ICADDTME
ICUPDDTE
ICUPDTME
ICUPDCNT
Data Replaced
ICLCA
ICLCS
ICLCR
ICISA
ICPYRA
ICISS
ICPYRS
ICISR
ICPYRR
ICSSA
ICSSS
ICSSR
NUM
NUM
NUM
NUM
NUM
NUM
NUM
by Corrections
(6,8.3) NUM
(6,8,3) NUM
(6,8,3) NUM
(6,5) NUM
(6) NUM
(6,5) NUM
(6) NUM
(6,5) NUM
(6) NUM
(6,3) NUM
(6,3) NUM
(6,3) NUM
8
8
8
8
8
8
8
***1
8
8
8
8
8
8
8
8
8
8
8
8
LabData Gen Date
LabData Gen Time
DB Add Date
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
DB Update Count
LabData
LabData
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
************************************************************************
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Area Pyrene-DIO (Secondary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates (Primary Ion)
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
45
-------
46
-------
4.0 Continuing Calibration Master File and Ancillary File
In the Continuing Calibration Master File, a record contains all
guantitation report and computed data for each performance check
I/continuing calibration analysis and performance check 2
analysis run for an analytic shift on the GC/MS. This data
represents the second logical level in the data structure. Each
continuing calibration record will have one or more field sample
or QC sample records pointing to it.
4.1 Logical Record Description
A logical record in this file contains data for a performance
checkl/continuing calibration analysis and performance check 2
for an analytic shift. The data elements are organized in
groups, as follows:
- KEYS AND STATUS - the primary, unique identifier of each
record in the file, along with any other (perhaps
non-unique) keys, and the status flag.
- CHRONOLOGY - dates and times of significant events during
the processing of the sample.
- DATA TRANSFER TRACKING - system dates used for maintenance
of the data base.
- ANALYSIS LAB SAMPLE LOGIN DATA - data entered by the
analytic laboratory when the sample was logged
f into their facility.
- ANALYSIS LAB SAMPLE EXTRACTION DATA - data generated by
the analytic laboratory during the sample
extraction process. This process removes the
organic compounds from the solid soil material,
resulting in a liquid suitable for analysis on the
GC/MS.
- ANALYSIS LAB INJECTION DATA - data entered by the lab
relating to injection of the sample in the GC/MS.
- ANALYSIS LAB INTERPRETATION DATA - data identifying the
shift results file that the sample belonged to,
the quantitation method used for each analyte, and
the ion used for quantitation for each analyte.
This data also contains the results of the GC/MS
analysis when the peak height method of
quantitation was used.
- CORRECTION FLAGS - flags used to indicate whether or not a
particular element has been corrected/updated. If
47
-------
a flag is set "on" ("Y"), then the updated data is
contained in this file, and the original data
value is stored in the associated ancillary file
record.
- ANALYSIS RAW DATA FOR CC/PC1 (after corrections, if any)
AND PC2 - raw data generated by the GC/MS. This
is essentially the same data contained on the
quantitation report created by the GC/MS.
- LABDATA COMPUTATIONS FOR CONTINUING CALIBRATION - results
calculated by the LabData system using the raw
data generated by the GC/MS. It includes the
continuing calibration response factor results,
the QC criteria, and flags indicating whether or
not the criteria were met.
- LABDATA PERFORMANCE CHECK DATA - the performance check ion
ratios and the sensitivity results, the QC
criteria for each, and flags indicating whether or
not the criteria were met.
- DATA VALIDATION FLAGS AND COMMENTS - results of the data
validation for the sample performed by EMSL-LV.
It includes data validation checklist responses,
comments, validation flags, and EMSL-LV usability
flags.
- INTEGRATED DATA BASE AUDIT SYSTEM FLAGS - results of the
automated audits and validations performed during
the data base building process.
The ancillary file consists of three groups: KEYS, CHRONOLOGY,
and DATA REPLACED BY CORRECTIONS. The last group corresponds to
the ANALYSIS RAW DATA group in terms of data elements, but
contains original data that has been replaced in the master file
by corrected data.
4.2 Logical Subsets of the File - Special Screening
This file does not contain any data elements that define logical
subsetting of the records.
4.3 Data Element Dictionaries
The data element dictionaries for the Continuing Calibration
Master File and the Continuing Calibration Ancillary File follow
this page.
48
-------
LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
it it it it it it it
CC.A01
CC.A02
CC.A03
NAME ARRAY TYPE
CCANALID CHAR
CCPC2ID
CCSTATUS
CHAR
CHAR
LENGTH DESCRIPTION
23 Continuing Calibration/Performance Check 1 Id
(Lab Id + Lab Analysis Id of CC/PC1)
23
1
Performance Check 2 Id
(Lab Id + Lab Analysis Id of PC2)
Status Flag
Values:
E = Validation Audit Failure
SOURCE
LabData
LabData
LabData
blank = Passed Validation Audit
CC.B01
CC.B02
CC.B03
CC.B04
CC.C01
CC.C02
CC.C03
CC.C04
CC.C05
CC.C06
CC.C07
CC.D01
CC.D02
CCAADTE NUM 8 CC/PC1 Analysis Lab Analysis Date LabData
CCAATME NUM 8 CC/PC1 Analysis Lab Analysis Time LabData
PC2AADTE
PC2AATME
Data Transfer
CCGENDTE
CCGENTME
CCADDDTE
CCADDTME
CCUPDDTE
CCUPDTME
CCUPDCNT
Analysis Lab
CCSMPL
CCALID
NUM
8
NUM 8
NUM 8
NUM 8
NUM
NUM
NUM
NUM
NUM
Sample Login
(2) CHAR
CHAR
8
8
8
8
8
10
3
PC2 Analysis Lab Analysis Date
PC2 Analysis Lab Analysis Time
LabData Gen Date
LabData Gen Time
DB Add Date
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
DB Update Count
Sample Id for CC/PC1 and PC2
Analysis Lab Id
LabData
LabData
LabData
LabData
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
LabData
LabData
Values:
AQI
CAA
CEC
EMS
MGM
NU2 = Contingency samples - for possible
'replacement; prepped and stored but never
analyzed
NUS
VER
blanks = no analysis performed; therefore no Lab Id
******* Analysis Lab Injection Data (For CC/PC1 and PC2) ****************************************************
CC.E01 CCINSTID CHAR 15 GC/MS Instrument Id LabData
CC.E02 CCANLST (2) CHAR 8 GC/MS Analyst, by 2 Analyses LabData
49
-------
DATA
ELEMENT
ID
NAME
LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
ARRAY TYPE LENGTH DESCRIPTION
SOURCE
CC.E03 CCFILE (2) CHAR 15 GC/MS Datafile Id, by 2 Analyses
CC.E04 CCINJVL (2) NUM 8 Injection Volume (ul), by 2 Analyses
LabOata
LabOata
*******
CC.F01
CC.F02
CC.F03
Analysis Lab
CCQFILE
CCQMTH
CC.FU
CC.F15
CCOION
CCHSSS
CCHSSR
Interpretation Data ********************************************************************
CHAR
(8,3) CHAR
(8)
(3)
(3)
CHAR
NUM
NUM
12
CC.F04
CC.F05
CC.F06
CC.F07
CC.F08
CC.F09
CC.F10
CC.F11
CC.F12
CC.F13
CCLCPH
CCISPH
CCPYRPH
CCSSPH
CCHLCS
CCHLCR
CCHISS
CCHISR
CCHPYRS
CCHPYRR
(8,3)
(5)
(3)
(8,3)
(8,3)
(5)
(5)
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
8
8
8
GC/MS Shift Results File Name LabOata
For CC/PC1 ONLY:
Quantitat ion Method Flag, by 8 LCICs, LabData
by 3 Ions
Values:
blank }
or } = GC/MS Automatic Area Quantitat ion
A >
H = Peak Height Quantitat ion
M = GC/MS Manual Quantitat ion
0 = Computed using area by LabData with correction
data
LCIC Quant itat ion Ion Selection, By 8 LCICs LabOata
Values:
blank = Primary ion area used for quantitat ion
S = Secondary ion area used for quantitat ion
T = Tertiary ion'area used for quant i tat ion
Peak Height, by 8 LCICs, by 3 Ions LabOata
Peak Height, by 5 Int. Stds. (Primary Ion) LabData
Peak Height Pyrene-DIO (Secondary Ion) LabData
Peak Height, by 3 Surrogates (Primary Ion) LabData
Scan for Peak Height, by 8 LCICs, by 3 Ions LabData
Retention Time for Peak Height, by 8 LCICs, LabData
by 3 Ions
Scan for Peak Height, by 5 Int. Stds., LabData
Retention Time for Peak Height, by 5 Int. LabData
Stds.
Scan for Peak Height for Pyrene-D10 LabOata
Retention Time for Peak Height for LabOata
Pyrene-D10
Scan for Peak Height, by 3 Surrogates LabData
Values:
0 = Peak height scan not performed
nnnn = Scan number for peak height scan performed
Retention Time for Peak Height, by 3 LabData
Surrogates
******* Correction Flags (For CC/PC1 ONLY) ******************************************************************
Values:
Y = data corrected, original data stored in ancillary file
blank = data not corrected, no data stored in ancillary file
CC.G01 CCCDATE CHAR 1 Analysis Lab Analysis Date LabData
50
-------
LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
CC.G02
CC.G03
CC.G04
CC.G05
CC.G06
CC.G07
CC.G08
CC.G09
CC.G10
CC.G11
CC.G12
CC.G13
CC.GU
CC.G15
CC.H01
CC.H02
CC.H03
CC.H04
CC.H05
CC.H06
CC.H07
CC.H08
CC.H09
CC.H10
CC.H11
CC.H12
Ititititititlt
CC.I01
CC.I02
NAME
CCCTIME
CCCANAL
CCCLCA
CCCLCS
CCCLCR
CCCISA
CCCISS
CCCISR
CCCPYRA
CCCPYRS
CCCPYRR
CCCSSA
CCCSSS
CCCSSR
Analysis Raw
CCLCA
CCLCS
CCLCR
CCISA
CCPYRA
CCISS
CCPYRS
CCISR
CCPYRR
CCSSA
CCSSS
CCSSR
ARRAY TYPE
CHAR
CHAR
(8,3) CHAR
(8,3) CHAR
(8,3) CHAR
(5) CHAR
(5) CHAR
(5) CHAR
CHAR
CHAR
CHAR
(3) CHAR
(3) CHAR
(3) CHAR
Data For CC/PC1
(2,8,3) NUM
(2,8,3) NUM
(2,8,3) NUM
(2,5) NUM
(2) NUM
(2,5) NUM
(2) NUM
(2,5) NUM
(2) NUM
(2,3) NUM
(2,3) NUM
(2,3) NUM
LENGTH
1
1
1
1
1
1
1
1
1
1
1
1
1
1
(After
8
8
8
8
8
8
8
8
8
8
8
8
LabOata Computations for Continuing
CCRFA (11,3) NUM 8
CCRFPH
(11,3) NUM
8
DESCRIPTION
Analysis Lab Analysis Time
Analyst
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Retention Time,
by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time,
SOURCE
LabData
LabOata
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
by 3 Surrogates (Primary Ion)
Area, by 2 Analyses, by 8 LCICs, by 3 Ions LabOata
Scan, by 2 Analyses, by 8 LCICs, by 3 Ions LabOata
Retention Time, by 2 Analyses, by 8 LCICs,
by 3 Ions
Area, by 2 Analyses, by 5 Int. Stds.
(Primary Ion)
Area Pyrene-DIO (Secondary Ion),
by 2 Analyses
Scan, by 2 Analyses, by 5 Int. Stds.
(Primary Ion)
Scan Pyrene-D10 (Secondary Ion),
by 2 Analyses
Retention Time, by 2 Analyses,
by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-D10 (Secondary Ion),
by 2 Analyses
Area, by 2 Analyses, by 3 Surrogates
(Primary Ion)
Scan, by 2 Analyses, by 3 Surrogates
(Primary Ion)
Retention Time, by 2 Analyses,
by 3 Surrogates (Primary Ion)
Response Factors using Area, by 8 LCICs
and 3 Surrogates, by 3 Ions
Response Factors using Peak Height,
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
*LabData
*LabData
by 8 LCICs and 3 Surrogates, by 3 Ions
51
-------
DATA
ELEMENT
ID NAME
LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
ARRAY TYPE LENGTH DESCRIPTION
SOURCE
CC.I03 CCRIR
(11)
NUM
CC.I04
CC.I05
CC.I06
CCPDRF
CCPDC
CCPDF
(11)
(11)
(11)
NUM
NUM
CHAR
CC.I07 CCPDOUT
CC.I08 CCRR
NUM
(8,3) NUM
8
8
Target Ion Ratios for Id Criteria using LabOata
Theoretical Values, by 8 LCICs and
3 Surrogates
% Dev. From Mean of Response Factors, LabOata
by 8 LCICs and 3 Surrogates
% Dev. Criteria, by 8 LCICs LabOata
and 3 Surrogates
Flag for % Dev out of criteria, LabOata
by 8 LCICs and 3 Surrogates
Values:
* = % deviation out of criteria; greater than 40%
+ = % deviation out of criteria; 20% < % dev <= 40%
blank = % deviation within criteria
Number of % Dev Out of Criteria LabOata
Relative Retention Time, *LabData
by 8 LCICs, by 3 Ions
*******
CC.J01
CC.J02
CC.J03
CC.J04
LabData Performance Check I
PCIR
PCIRLC
PCIRUC
PCIRF
(2,9)
(2,9)
(2,9)
(2,9)
NUM
NUM
NUM
CHAR
**********************************************
CC.J05
CC.J06
CC.J07
CC.J08
CC.J09
CC.J10
PCI ROUT
PCBLSEP
PCPV
PCPVF
PCPVC
PCSNR
(2)
(3)
(3)
NUM
CHAR
NUM
CHAR
(3) NUM
(2,2) NUM
8
1
Ion Ratios, by 2 analyses (PC1, PC2), *LabOata
by 8 LCICs and Pyrene-010
Ion Criteria lower value, by 2 analyses LabData
(PC1, PC2), by 8 LCICs and Pyrene-D10
Ion Criteria upper value, by 2 analyses LabData
(PC1, PC2), by 8 LCICs and Pyrene-D10
Flag for Ion ratio Out of Criteria, *LabOata
by 2 analyses (PC1, PC2),
by 8 LCICs and Pyrene-D10
Values:
* = out of criteria
blank = within criteria
Number of PC Vals Out of Criteria, LabData
by 2 analyses (PC1, PC2)
Baseline Separation LabData
Values:
blank = no baseline separation
Y = baseline separation between CNP isomers
% valley (PC1/CNP, PC2/CNP, PC2/BHC) LabData
Flag for X valley (PC1/CNP, PC2/CNP, PC2/BHC) *LabData
Out of Criteria
Values:
* = % valley out of criteria; greater than 40%
+ = % valley out of criteria; 20% < % dev <= 40%
blank = % valley within criteria
% Valley Criteria (PC1/CNP, PC2/CNP, PC2/BHC) LabData
Signal to Noise Ratip(PC1/BHC,PC2/BHC,PC1/TeBB,PC2/TeBB) LabOata
52
-------
DATA
ELEMENT
ID NAME
LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION MASTER FILE • DATA ELEMENT DICTIONARY
ARRAY TYPE LENGTH DESCRIPTION
SOURCE
CC.J11 PCSNRF
(2,2) CHAR
CC.J12 PCSNRC
(2,2) NUM
Signal to Noise Ratio Out of Crit. Flag *LabOata
(PC1/BHC,PC2/BHC,PC1/TeBB,PC2/TeBB)
Values:
* = out of criteria
blank = within criteria
Signal to Noise Ratio(PC1/8HC,PC2/BHC,PC1/TeBB,PC2/TeBB) LabOata
Criteria
Values: (currently not available)
CC.K01
CC.K02
CC.K03
CC.K04
CC.K05
CC.K06
CC.K07
CC.K08
CC.K09
CC.K10
CC.K11
CC.K12
CC.K13
CC.K14
CC.K15
CC.K16
CC.K17
CC.K18
CC.K19
CC.K20
CC.K21
CC.K22
CC.K23
CC.K24
CC.K25
CC.K26
CC.K27
CC.K28
CC.K29
CC.K30
CC.K31
CC.K32
CC.K33
CC.K34
CC.K35
DVDELIV
DVMISS
DVRES
DVPC1A
DVPC1B
DVPC1C
DVPC1D
DVPC1E
DVPC1F
DVPC1DT
DVPC1TM
DVPCMDP
DVHALF
DVPC1CM
DVPC2A
DVPC2B
DVPC2C
DVPC2D
DVPC2E
DVPC2F
DVPC2DT
DVPC2TM
DVPC2CM
DVEPAA
DVEPAB
DVEPAC
DVEPAD
DVEPASMP
DVEPACM
DVCCCALA
DVCCCALB
DVCCCALC
DVCCDT
DVCCTM
DVCCCOM
CHAR
(7) CHAR
(7) CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
1 CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
1
40
8
1
1
1
2
2
2
8
8
1
12
60
1
1
1
2
2
2
8
8
60
2
2
2
2
10
60
1
1
2
8
8
60
Are all
Missing
Dates n
PC1 Com|
PC1 Comi
PC1 Chei
PC1 Chei
PC1 Chei
PC1 Misi
PC1 Dati
PC1 Timi
Is this
First hi
PC1 Com
PC2 Com]
PC2 Com|
PC2 Chei
PC2 Chei
PC2 Chei
PC2 Misi
PC2 Dati
PC2 Timi
PC2 Com
EPA Chk
EPA Chk
EPA Chk
EPA Chk
EPA Chk
EPA Com
Cont i nu
Continu
Continu
Cont i nu
Cont i nu
Cont i nu
***********************************************************
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
PC1 Compare percent valley SICPS
PC1 Compare signal to noise ratios with raw data
PC1 Check ion ratio criteria
PC1 Check chromatography
PC1 Check quantisation reports for evidence of editing
PC1 Miscellaneous
PC1 Date
PC1 Time
Is this a PC2 midpoint for 16 hour analytical run?
First half shift result file name if exists
PC1 Comments
PC2 Compare percent valley SICPS
PC2 Compare signal to noise ratios with raw data
PC2 Check ion ratio criteria
PC2 Check chromatography
PC2 Check quantisation reports for evidence of editing
illaneous
mts
Std. Recoveries within acceptance windows
Std. Check chromatography
Std. Check quantitat ion reports
Std. Miscellaneous
Std. Sample Id
nts
Continuing Calibration Internal standard areas
Continuing Calibration Check retention time differences
Continuing Calibration Miscellaneous
Continuing Calibration Date
Continuing Calibration Time
Continuing Calibration Comments
53
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LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION SOURCE
******* integrated DB Audit System Flags ********************************************************************
CC.L01 CCRECALC CHAR 1 Flag for calculation discrepancies IntDBBld
Values:
* = Discrepancy
blank = No discrepancy
54
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LOVE CANAL HABITABILITY STUDY
CONTINUING CALIBRATION ANCILLARY FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
CA.A01
CA.B01
CA.B02
CA.B03
CA.B04
CA.B05
CA.B06
CA.B07
CA.C01
CA.C02
CA.C03
CA.C04
CA.C05
CA.C06
CA.C07
CA.C08
CA.C09
CA.C10
CA.C11
CA.C12
NAME ARRAY TYPE
Keys *********
CCANALID
Data Transfer
CCGENDTE
CCGENTME
CCADDDTE
CCADDTME
CCUPDDTE
CCUPDTME
CCUPDCNT
Data Replaced
CCLCA
CCLCS
CCLCR
CCISA
CCPYRA
CCISS
CCPYRS
CCISR
CCPYRR
CCSSA
ccsss
CCSSR
CHAR
Tracking *****
NUM
NUM
NUM
NUM
NUM
NUM
NUM
by Corrections
(2,8,3) NUM
(2,8,3) NUM
(2,8,3) NUM
(2,5) NUM
(2) NUM
(2,5) NUM
(2) NUM
(2,5) NUM
(2) NUM
(2,3) NUM
(2,3) NUM
(2,3) NUM
LENGTH
23
8
8
8
8
8
8
DESCRIPTION
SOURCE
AAAAA^AAAAAAAAAAA
Continuing Calibration/Performance Check 1 Id LabData
(Lab Id + Lab Analysis Id of CC/PC1)
LabData Gen Date LabData
LabData Gen Time LabData
DB Add Date IntDBBld
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
8 DB Update Count
8 Area, by 2 Analyses, by 8 LCICs, by 3 Ions
8 Scan, by 2 Analyses, by 8 LCICs, by 3 Ions
8
8
8
8
8
8
8
8
8
8
Retention Time, by 2 Analyses, by 8 LCICs,
by 3 Ions
Area, by 2 Analyses, by 5 Int. Stds.
(Primary Ion)
Area Pyrene-DIO (Secondary Ion),
by 2 Analyses
Scan, by 2 Analyses, by 5 Int. Stds.
(Primary Ion)
Scan Pyrene-D10 (Secondary Ion),
by 2 Analyses
Retention Time, by 2 Analyses,
by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-D10 (Secondary Ion),
by 2 Analyses
Area, by 2 Analyses, by 3 Surrogates
(Primary Ion)
Scan, by 2 Analyses, by 3 Surrogates
(Primary Ion)
Retention Time, by 2 Analyses,
by 3 Surrogates (Primary Ion)
IntDBBld
IntDBBld
IntDBBld
IntDBBld
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
55
-------
56
-------
5.0 Quality Control (QC) Sample Master File and Ancillary File
In the QC Sample Master File, a record contains all quantitation
report and computed data for QC samples. Each analytic run, or
"shift," containing field samples was required to have certain QC
samples run as well. Depending upon various factors, one or more
different types of QC samples would be run in each shift.
A pointer, or key, is present to link to each sample's continuing
calibration record.
5.1 Logical Record Description
A logical record contains the data for one QC sample. The data
elements are organized in groups, as follows:
- KEYS AND STATUS - the primary, unique identifier of each
record in the file, along with any other (perhaps
non-unique) keys, and the status flag.
- CHRONOLOGY - dates and times of significant events during
the processing of the sample.
- DATA TRANSFER TRACKING - system dates used for maintenance
of the data base.
- FIELD SAMPLING DATA - data generated during the collection
of the sample in the field.
- PREPARATION LAB DATA - data generated during the
preparation of the sample. The preparation
process consisted of removing the soil from the
sampling tube, homogenizing the soil, placing the
soil in a container for shipment, and shipping it
to an analytical laboratory.
- ANALYSIS LAB SAMPLE LOGIN DATA - data entered by the
analytic laboratory when the sample was logged
into their facility.
- ANALYSIS LAB SAMPLE EXTRACTION DATA - data generated by
the analytic laboratory during the sample
extraction process. This process removes the
organic compounds from the solid soil material,
resulting in a liquid suitable for analysis on the
GC/MS.
- ANALYSIS LAB INJECTION DATA - data entered by the lab
relating to injection of the sample in the GC/MS.
- ANALYSIS LAB INTERPRETATION DATA - data identifying the
shift results file that the sample belonged to,
57
-------
the quantitation method used for each analyte, and
the ion used for quantitation for each analyte.
This data also contains the results of the GC/MS
analysis when the peak height method of
quantitation was used.
CORRECTION FLAGS - flags used to indicate whether or not a
particular element has been corrected/updated. If
a flag is set "on" ("Y"), then the updated data is
contained in this file, and the original data
value is stored in the associated ancillary file
record.
ANALYSIS RAW DATA - (after corrections, if any) raw data
generated by the GC/MS. This is essentially the
same data contained on the quantitation report
created by the GC/MS.
LABDATA COMPUTATIONS FOR QC SAMPLES - results calculated
by the LabData system using the raw data generated
by the GC/MS and additional data entered by the
laboratory. It includes the concentration results
after the identification criteria (ID) have been
applied, pre-criteria concentrations, ID criteria
results, and flags indicating whether or not the
criteria were met.
LABDATA COMPUTATIONS FOR SURROGATE STANDARDS - results
computed by LabData for the surrogate recoveries
for the sample analysis. Included are the percent
recoveries, flags indicating whether or not the
recovery met the criteria, and the criteria.
LABDATA COMPUTATIONS FOR INTERNAL STANDARDS - results
computed by LabData for the internal standards for
the sample analysis. Included are retention time
and area criteria check results.
LABDATA COMPUTATIONS FOR METHOD HOLDING BLANK -
concentrations for secondary and tertiary ions, QC
criteria results, and flags indicating whether or
not the criteria were met.
LABDATA MATRIX SPIKE DATA - quantity of the spike, percent
recovery, QC criteria results, and flags
indicating whether or not the criteria were met.
DATA VALIDATION FLAGS AND COMMENTS - results of the data
validation for the sample performed by EMSL-LV.
It includes data validation checklist responses,
comments, validation flags, and EMSL-LV usability
flags.
58
-------
- INTEGRATED DATA BASE AUDIT SYSTEM FLAGS - results of the
automated audits and validations performed during
the data base building process.
The ancillary file consists of three groups: KEYS, CHRONOLOGY,
and DATA REPLACED BY CORRECTIONS. The last group corresponds to
the ANALYSIS RAW DATA group in terms of data elements, but
contains original data that has been replaced in the master file
by corrected data.
5.2
Logical Subsets of the File - Special Screening
The primary grouping of logical subsets in the QC Sample Master
File is based upon sample types. The table below depicts these
sample types, and sub-groups within each sample type.
Sample
Type Code
(QCTYPE)
QCEMSL
MS
BLM
Description
EMSL Blind QC samples - samples spiked with known
concentrations of LCICs, but the levels were not
known by the analytic laboratory. A Blind QC
sample was extracted with each extraction batch of
samples and analyzed. If a given level of
recovery was not achieved in the Blind QC, then
the laboratory had to re-extract all the field
samples in the extraction batch.
The Matrix Spike and Matrix Spike Duplicate
samples MSD were created by splitting every
twentieth field sample into three parts. One
third was treated as a normal field sample (i.e.,
the "native" sample in a native/MS/MSD set of
analyses), one-third as an MS analysis, and one-
third as the MSD. Each MS and MSD was then spiked
with a fixed amount of LCICs. The results were
then used for QC purposes. See Section 8.5 for a
description of how to merge the native samples
with MS/MSD analyses.
The Method Blank was a blank sample, prepared by
the analytic laboratory, containing no known
levels of LCICs. This sample was then extracted
in a batch of field samples, subjected to the same
handling and storage, and analyzed with the field
samples. The results were not to indicate any
significant levels of LCICs. If significant
levels of LCICs were found, the laboratory had to
re-extract all field samples in that extraction
batch.
59
-------
BLR The Reagent Blank was also a blank sample, made up
from the solvents used during the sample
extraction process and analyzed to determine if
the analysis process was introducing LCIC
contamination into the field samples.
As was the case with the Field Samples in FSFILE, the data
usability flags associated with the sample results must be merged
in from the FORM I file. Section 8 contains directions for
combining files.
5.3 Data Element Dictionaries
The data element dictionaries for the Quality Control Sample
Master File and the Quality Control Sample Ancillary File follow
this page.
60
-------
LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION
SOURCE
******* Keys and status**************************************************************************************
QC.A01 QCANALID CHAR 23 OC Lab Analysis Id - LabData
(Lab Id + Lab Analysis Id)
QC.A02 QCSTATUS CHAR 1 Status Flag IntDBBld
Values:
E = Validation Audit Failure
blank = Passed Validation Audit
QC.A03 CLEANHS CHAR 8 Original Project Id (HS Number) IntDBBld
******* chronology ******************************************************************************************
QC.B01 QCALDTE NUM 8 Analysis Lab Login Date LabData
OC.B02 QCAEDTE NUM 8 Analysis Lab Extract Date LabData
QC.B03 QCAADTE NUM 8 Analysis Lab Analysis Date LabData
QC.B04 QCAATME NUM 8 Analysis Lab Analysis Time LabData
QC.B05 OCDBDTE NUM 8 Data Validation Date DataVal
******* Qata Transfer Tracking *****************************************************************************
QC.C01
QC.C02
QC.C03
OC.C04
QC.C05
QC.C06
QC.C07
QCGENDTE
QCGENTME
QCADDDTE
OCADDTME
QCUPDDTE
QCUPDTME
QCUPDCNT
NUM 8 LabData Gen Date
NUM 8 LabData Gen Time
NUM 8 DB Add Date
NUM 8 DB Add Time
NUM 8 DB Most Recent Update Date
NUM 8 DB Most Recent Update Time
NUM 8 DB Update Count
LabData
LabData
IntDBBld
IntDBBld
IntDBBld
IntDBBld
IntDBBld
******* Analysis Lab Sample Login Data *****************
************
**************
QC.D01
QC .D02
QC.D03
QC.D04
QC.D05
QCSMPL
OCALID
QCRERUN
QCRRSTAT
QCORIG
(the Project Sample Id)
LabData
LabData
CHAR 8 QC Sample Id from LabData
CHAR 3 Analytic Laboratory Id
Values:
AQI
CAA
CEC
EMS
MGM
NU2 = Contingency samples - for possible
replacement; prepped and stored but never
analyzed
NUS
VER
blanks = no analysis performed; therefore no Lab Id
CHAR 2 Re-run Flag currently not used
CHAR 1 Re-run Type currently not used
CHAR 1 Orig. Found Flag currently not used
61
-------
DATA
ELEMENT
ID
QC.D06
LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL MASTER FILE - DATA ELEMENT DICTIONARY
NAME ARRAY TYPE LENGTH DESCRIPTION
QCTYPE CHAR 6 QC Sample Type
Values:
MS = Matrix Spike
MSD = Matrix Spike Duplicate
BLM = Method Blank
BLR = Reagent Blank
QCEMSL = EMSL Blind QC Sample
SOURCE
LabData
QC.E01
QC.E02
QC.E03
QC.E04
QC.F01
QC.F02
QC.F03
QC.F04
*******
QC.G01
QC.G02
Analysis Lab
QCTWTEXT
QCWTEXT
QCMOIST
QCCONCDF
Analysis Lab
QCINSTID
QCANLST
QCFILE
QCINJVOL
Analysis Lab
QCOFILE
QCQMTH
Sample Extraction Data *****************************************************************
NUM
NUM
NUM
NUM
Injection Data
CHAR
CHAR
CHAR
NUM
Interpretation
CHAR
(8,3) CHAR
8
8
8
8
15
8
15
8
Data
12
1
Target Weight to Extract (gm)
Weight Extracted (gm)
Percent Moisture
Concentration Dilution Factor
GC/MS Instrument Id
GC/MS Analyst
GC/MS Datafile Id
Injection Volume (ul)
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
********************************************************************
GC/MS Shift Results File Name
Quant i tat ion Method Flag, by 8 LCI Cs, by 3 Ions
LabData
LabData
QC.G03
QCQION
(8)
CHAR
QC.G04
QC.G05
QC.G06
QC.G07
QC.G08
QC.G09
QC.G10
QC.G11
QC.G12
QCLCPH
QCISPH
QCPYRPH
QCSSPH
QCHLCS
QCHLCR
QCHISS
QCHISR
QCHPYRS
(8,3)
(5)
(3)
(8,3)
(8,3)
(5)
(5)
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
8
8
Values:
blank }
or > = GC/MS Automatic Area Quantitat ion
A >
H = Peak Height Quantisation
M = GC/MS Manual Quantitat ion
0 = Computed using area by LabData with correction
data
LCIC Quantitat ion Ion Selection, by 8 LCICs LabData
Values:
blank = Primary ion used for quant Station
S = Secondary ion used for quantitat ion
T = Tertiary ion used for quantiat ion
Peak Height, by 8 LCICs, by 3 Ions LabData
Peak Height, by 5 Int. Stds. (Primary Ion) LabData
Peak Height Pyrene-DIO (Secondary Ion) LabData
Peak Height, by 3 Surrogates (Primary Ion) LabData
Scan for Peak Height, by 8 LCICs, by 3 Ions LabData
Retention Time for Peak Height, by 8 LCICs, by 3 Ions LabData
Scan for Peak Height, by 5 Int. Stds. LabData
Retention Time for Peak Height, by 5 Int. Stds. LabData
Scan for Peak Height for Pyrene-D10 LabData
62
-------
LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL MASTER FILE • DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
QC.G13
QC.GH
QC.G15
NAME
QCHPYRR
QCHSSS
QCHSSR
ARRAY
(3)
TYPE LENGTH DESCRIPTION SOURCE
NUM 8 Retention Time for Peak Height for Pyrene-D10 LabData
NUM 8 Scan for Peak Height, by 3 Surrogates LabData
NUM 8 Retention Time for Peak Height, by 3 Surrogates LabData
Values:
blank = data has not been corrected
"Y" = data has been corrected; original data in ancillary file
QC.H01
QC.H02
QC.H03
QC.H04
QC.H05
QC.H06
QC.H07
QC.H08
QC.H09
QC.H10
QC.H11
QC.H12
QC.H13
QC.H14
QC.H15
QC.I01
QC.I02
QC.103
QC.I04
QC.I05
QC.I06
QC.I07
QC.I08
QC.I09
QC.I10
QC.I11
QC.I12
*******
QCCDATE
QCCTIME
QCCANAL
QCCLCA
QCCLCS
QCCLCR
QCCISA
QCCISS
QCCISR
QCCPYRA
QCCPYRS
QCCPYRR
QCCSSA
QCCSSS
QCCSSR
Analysis Raw
QCLCA
QCLCS
QCLCR
QCISA
QCPYRA
QCISS
QCPYRS
QCISR
QCPYRR
QCSSA
QCSSS
QCSSR
(8,3)
(8,3)
(8,3)
(5)
(5)
(5)
(3)
(3)
(3)
Data
(8,3)
(8,3)
(8,3)
(5)
(5)
(5)
(3)
(3)
(3)
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
Analysis Lab Analysis Date
Analysis Lab Analysis Time
Analyst
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates
(Primary Ion)
NUM 8 Area, by 8 LCICs, by 3 Ions
NUM 8 Scan, by 8 LCICs, by 3 Ions
NUM 8 Retention Time, by 8 LCICs, by 3 Ions
NUM 8 Area, by 5 Int. Stds. (Primary Ion)
NUM 8 Area Pyrene-D10 (Secondary Ion)
NUM 8 Scan, by 5 Int. Stds. (Primary Ion)
NUM 8 Scan Pyrene-D10 (Secondary Ion)
NUM 8 Retention Time, by 5 Int. Stds. (Primary Ion)
NUM 8 Retention Time Pyrene-D10 (Secondary Ion)
NUM 8 Area, by 3 Surrogates (Primary Ion)
NUM 8 Scan, by 3 Surrogates (Primary Ion)
NUM 8 Retention Time, by 3 Surrogates
(Primary Ion)
f l*tl~ rtr C^mnl^^ *******************************************************
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
QC.J01 QCRR (8) NUM 8 Relative Retention Time, by 8 LCICs
(Quantitat ion Ion)
QC.J02 QCRRC (8) NUM 8 Relative Retention Time Criteria, by 8 LCICs
•LabOata
LabData
63
-------
DATA
ELEMENT
ID
QC.J03
QC.J04
QC.J05
QC.J06
QC.J07
QC.J08
QC.J09
QC.J10
OC.J11
QC.J12
OC.J13
NAME
QCRRF
QCCONCB
QCCONCA
QCIRAT
QCIONF
OCMINS
QCMAXS
QCRANG
GCRANGF
QCIDEVT
QCIDEVF
ARRAY
(8)
(8)
(8)
(8)
(8)
(8)
(8)
(8)
(8)
(8)
(8)
TYPE 1
CHAR
NUM
NUM
NUM
CHAR
NUM
NUM
NUM
CHAR
NUM
CHAR
.ENG-
1
8
8
8
1
8
8
8
1
8
1
QC.J14
QCPRESCR
QC.J15 QCSULFUR
LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL MASTER FILE - DATA ELEMENT DICTIONARY
DESCRIPTION SOURCE
Flag for Rel. Ret. Time Out of Criteria, by 8 LCICs *LabOata
Values:
* = Out of criteria
blank = Within criteria
PrelD-criteria Concentration, by 8 LCICs *LabOata
(i.e.,primary ion equivalent concentration)
Id Criteria applied Concentration, by 8 LCICs *LabOata
Ion Ratio, by 8 LCICs *LabOata
Flag for All Ions Being Present, by 8 LCICs "LabOata
Values':
* = All ions present
blank = One or more ions not present
Minimum Scan Number of 3 Ions, by 8 LCICs LabOata
Maximum Scan Number of 3 Ions, LabData
by 8 LCICs
Scan Range (Max - Min), by 8 LCICs *LabOata
Flag for Scan range >2, by 8 LCICs *LabOata
VaIues:
* = scan range greater than 2
blank = scan range less than or equal to 2
Ion Ratio % Dev. from Theoretical Values, by 8 LCICs *LabData
Flag for Ion ratio % Dev. Out of Criteria, by 8 LCICs *LabData
Values:
* = % dev. out of criteria; greater than 40%
+ = % dev. out of criteria; 20% < % dev <= 40%
blank = % dev. within criteria
Flag for Analysis Pre-screen LabData
VaIues:
'MS ' = GC/MS pre-screening performed
'ECD1 = GC/ECD pre-screening performed
blanks = no pre-screening done
Flag for Sulphur Cleanup Performed LabData
Values:
Y = sulphur cleanup performed
blank or N = no sulphur cleanup performed
CHAR
CHAR
******* LabData Computations for Surrogate Standards ********************************************************
QC.K01
QC.K02
OCPR
QCPRF
QC.K03 QCSSADD
QC.K04 OCPRCL
QC.K05 QCPRCU
QC.K06 QCPROUT
(3) NUM 8 % Recovery by 3 Surrogates ' *LabOata
(3) CHAR 1 Flag for % Rec. Out of Criteria, by 3 Surrogates *LabData
Values:
* = Out of criteria
blank = Within criteria
(3) NUM 8 Amount of added(ng), by 3 Surrogates LabData
(3) NUM 8 % Recovery Criteria lower limit, by 3 Surrogates LabData
(3) NUM 8 % Recovery Criteria upper limit, by 3 Surrogates LabData
NUM 8 Number of % Rec. Out of Criteria *LabData
64
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LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
QC.L01
QC.L02
QC.L03
QC.L04
QC.L05
QC.L06
QC.L07
OC.L08
*******
QC.M01
QC.M02
QC.M03
QC.M04
*******
QC.N01
OC.N02
QC.N03
QC.N04
QC.N05
QC.N06
QC.N07
*******
QC.001
QC.002
QC.003
OC.004
QC.005
QC.006
NAME
ARRAY
LabOata Computations
QCISADD
QCRD (5)
QCAD
QCRF
QCAF
QCRDC
QCADCL
QCADCU
(5)
(5)
(5)
(5)
(5)
(5)
LabOata Computations
QCSICON
QCTICON
OCMAXCON
QCCONF
(8)
(8)
(8,3)
TYPE
LENGTH
DESCRIPTION
NUM 8 Internal Standard Quantity Added (in nanograms)
NUM 8 Ret. Time Difference From CC Val, by 5 Int Stds
NUM
CHAR
CHAR
NUM
NUM
NUM
8
1
1
8
8
8
Area Difference % From CC Val, by 5 Int Stds
Flag for Ret. Time Out of Criteria, by 5 Int Stds
Values:
* = Out of criteria
blank = Within criteria
Flag for Area Out of Criteria, by 5 Int Stds
Values:
* = Out of criteria
blank = Within criteria
Retention Time Difference Criteria, by 5 Int Stds
Area % Diff. Crit. lower limit, by 5 Int Stds
Area % Diff. Crit. upper limit, by 5 Int Stds
SOURCE
LabOata
*LabOata
*LabData
•LabOata
*LabData
LabOata
LabOata
LabData
for Method Holding Blank *******************************************************
NUM
NUM
NUM
CHAR
8
8
8
1
Concentration, by 8 LCICs (secondary ion)
Concentration, by 8 LCICs (tertiary ion)
Maximum Cone. Criteria
Concentration Out of Criteria Flag,
by 8 LCICs, by 3 Ions
Va I ues :
* = Out of criteria
blank = Within criteria
*LabOata
*LabData
LabOata
•LabOata
LabOata Matrix Spike Data ***************************************************************************
QCSADDED
QCSRECV
QCSPRCU
QCSPRCL
QCSPRL
QCSPR
QCSPDD
(8)
(8)
(8)
(8)
(8)
(8)
Data Validation Flags
Values:
DVCHKA
DVCHKB
DVCHKC
DVCHKD
DVSAMP
DVCOM
(currently
(3)
NUM
NUM
NUM
NUM
NUM
NUM
NUM
8
8
8
8
8
8
8
Amount of Spike Added (ng)
Amount of Spike Recovered (ng), by 8 LCICs
% Recovery Upper Limit Criteria, by 8 LCICs
% Recovery Lower Limit Criteria, by 8 LCICs
% Recovery Relative % Dev. Limit, by 8 LCICs
% Recovery, by 8 LCICs
Relative % Dev. of MS/MSD % Recoveries,
by 8 LCICs
LabOata
•LabData
LabData
LabOata
LabOata
•LabData
''LabOata
and Comments ******************************************************************
not available)
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
2
2
2
2
10
60
Recoveries within acceptance criteria
Check chromatography
Check quant i tat ion reports
Blind QC Samples Miscellaneous
Sample Id
Blind QC comments
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
65
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LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
QC.009
QC.010
QC.011
QC.012
QC.015
QC.016
QC.017
OC.018
QC.021
QC.022
QC.023
QC.024
QC.025
QC.026
OC.029
OC.030
QC.031
QC.032
QC.035
QC.036
QC.037
QC.038
QC.039
QC.042
NAME
QCSURRA
QCSURRB
QCSURRC
QCSURCM
QCINTA
QCINTB
QCINTC
QCINTCM
QCIDA
OCIDB
QCIDC
QCIDD
QCIDE
QCIDCOM
QCQTA
QCOTB
QCQTC
QCQTCOM
QCGENA
QCGENB
QCGENC
QCGEND
QCGENCM
QCDQ
ARRAY TYPE
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
(3) CHAR
CHAR
CHAR
CHAR
CHAR
(3) CHAR
(8,5) CHAR
LENGTH
1
1
1
60
1
1
1
60
1
1
1
2
2
60
1
1
2
60
2
2
2
2
60
2
DESCRIPTION
Check surrogates spiked into all samples
Recoveries within criteria
Miscellaneous
Surrogates Comments
Internal Standards RT Criteria
Internal Standards Area Criteria
Internal Standards Miscellaneous
Internal Standards Comments
Id All ions maximize simultaneously
Id Appropriate flags used
Id All peaks reported that meet Id criteria
Id Low level peaks examined
Id Miscellaneous
Id Comments
Quant it at ion Appropriate RRF's used if nonstandard
Quantitation Check integration parameters if manual
Quantitation Miscellaneous
Quantitation Comments
General Review case narrative and address all problems
Examine SICPS
Examine quant i tat ion reports
Miscellaneous
General Comments
Data Qualifiers 8 Analytes by 5 samples
SOURCE
DataVal
DataVal'
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
DataVal
******* integrated DB Audit System Flags ********************************************************************
QC.P01
QCF1FLAG
QC.P02 QCRECALC
CHAR 1 Flag for Forml Match Results IntDBBld
Values:
1 = Found Forml and all data matches
2 = Found Forml and some data does not match
3 = Forml not found
CHAR 1 Flag for calculation descrepancies IntDBBld
Values:
* = descrepancy found in calculation
blank = no descrepancy found in calculation
66
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LOVE CANAL HABITABILITY STUDY
QUALITY CONTROL ANCILLARY FILE • DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
QA.A01
QA.B01
QA.B02
QA.B03
QA.B04
QA.B05
QA.B06
QA.B07
*******
QA.C01
QA.C02
QA.C03
QA.C04
OA.C05
QA.C06
QA.C07
QA.C08
QA.C09
QA.C10
QA.C11
QA.C12
NAME ARRAY TYPE LENGTH DESCRIPTION SOURCE
QC ANAL ID
Data Transfer
QCGENDTE
QCGENTME
QCADDDTE
OCADDTME
QCUPDDTE
QCUPDTME
QCUPDCNT
Data Replaced
QCLCA
QCLCS
OCLCR
QCISA
QCPYRA
QCISS
QCPYRS
QCISR
OCPYRR
QCSSA
QCSSS
QCSSR
CHAR 23 QC Lab Analysis Id • LabOata
NUM
NUM
NUM
by
(8,
(8,
(8,
(5)
(5)
(5)
(3)
(3)
(3)
NUM
NUM
NUM
NUM
Corrections
3) NUM
3) NUM
3) NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
NUM
(Lab Id + Lab Analysis Id)
8
8
8
8
8
8
8
LabOata Gen Date LabOata
LabData Gen Time LabData
DB Add Date IntDBBld
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
DB Update Count
IntDBBld
IntDBBld
IntDBBld
IntDBBld
************************************************************************
8
8
8
8
8
8
8
8
8
8
8
8
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs, by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Area Pyrene-D10 (Secondary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Scan Pyrene-D10 (Secondary Ion)
Retention Time, by 5 Int. Stds. (Primary Ion)
Retention Time Pyrene-D10 (Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates
(Primary Ion)
LabData
LabData
LabData
LabData
LabData
LabOata
LabData
LabData
LabData
LabData
LabData
LabData
67
-------
68
-------
6.0 Form I Master File
The FORM I Master File contains a record for each validated Form
I generated by the analytic laboratories. A Form I was generated
for each QC sample and for each field sample that was collected,
prepared, and sent to the analytic laboratories. Figure 6-1
depicts the record set relationship among the Field Sample, QC
Sample, and Form I Master Files.
The data on the Form I, plus the validation results generated by
EMSL-LV, were separately keyed, verified, and loaded into this
file. As such, these are the "official, approved, validated"
results. The "same" data was also loaded into the other master
files in the data base from the LabData Systems in each analytic
laboratory. Along with the concentrations, all the background
and QC data that go into computing the concentration results were
loaded. Since there were changes and re-submissions required of
the analysis laboratories during the validation process, some
discrepancies resulted between the Form I data that were keyed
and loaded into the FORM I file and the data taken from the
LabData System and loaded into the other files. The
discrepancies appear to be the result of earlier versions of the
quantitation report data being included in the data taken from
the LabData systems in the laboratories. During the data
validation process, there was a substantial number of re-
submissions generated by the laboratories. The resulting
occurrence of multiple versions of data seems to have caused the
problem. In all cases, where a discrepancy exists between the
data from LabData and the data from the Form I, the Form I data
is correct. The audit results fields should be referred to in
order to determine if any discrepancies exist.
When working with the analysis results, it should be noted that
each sample was analyzed for the presence of eight analytes,
i.e., the LCICs. Data usability flags are assigned to each
analyte within a sample (LCICUSE1- LCICUSE8). Thus, the
usability of each analyte must be examined separately. For the
meaning of the usability flags, refer to the field descriptions
in Section 6.3. Refer to Volume III, Soil Assessment—Indicator
Chemicals, Appendix H, CH2M HILL, 1988, for a complete
explanation of validation flags associated with a usability flag
Of "UNCERTAIN" or "BAD."
It should also be noted that there are duplicate field sample
analyses present. The statistical analyses were performed using
only the analysis selected by the project chemists as the most
appropriate. For information on creating the data subset used
for the primary statistical comparisons, see Section 8.6.
69
-------
FSFUJB
1
1
1
1,
- - _ -
mm mm mm mm mm mm mm m
mm
\
\
1
••
• PIFILE '
Figure 6-1
Record Set Relationships
70
-------
6.1 Logical Record Description
A logical record in this file contains data for each Form I
validated by EMSL-LV. The data elements are organized in groups,
as follows:
- KEYS AND STATUS - the primary, unique identifier of each
record in the file, along with any other (perhaps
non-unique) keys, and the status flag.
- SAMPLE INFORMATION - the data related to samples login,
sample extraction, and GC/MS injection.
- SUMMARY SAMPLE DATA VALIDATION QUALIFIERS - flags that
summarize, by analyte, the data usability flags
assigned by EMSL-LV (these flags were assigned at
either the sample level or the analyte level). If
a sample was flagged as "UNCERTAIN" solely based
on holding time, it was re-classified as "GOOD."
- SAMPLE SPECIFIC DATA VALIDATION QUALIFIERS - qualifiers at
the sample level, denoting data validation
deficiencies.
- ANALYTE SPECIFIC LABDATA AND LABORATORY QUALIFIERS -
qualifiers at the analyte level, denoting
anomalies in the data and identifying data quality
deficiencies.
- ANALYTE SPECIFIC FLAGS - flags relating to presence of
ions, scan range, ion ratio, and relative
retention time.
- FORM 1 COMMENTS - textual explanation of any modifications
made to the quantitation results using the LabData
system.
- INTEGRATED DATA BASE AUDIT SYSTEM FLAGS - results of the
automated audits and validations performed during
the data base building process.
6.2 Logical Subsets of the File - Special Screening
The primary grouping of logical subsets in the FORM I Master File
is based upon sample types. The table below presents these
sample types and discusses sub-groups within each sample type.
Sample
Type Code
(F1TYPE) Description
HS The field samples. These samples' results were
used for the comparison analyses to determine if
71
-------
any differences in contamination levels existed
between the Love Canal Emergency Declaration Area
(EDA) and the comparison areas. The actual
statistical analyses were performed using the
"GOOD," non-duplicate subset of this data.
SPLIT The field split half of a field sample was
separated for inter- and intra-laboratory
comparison of performance. The field sample half
retained the originally assigned project sample
ID, and the field split half was assigned a
different project sample ID.
FHB Field handling blanks were actually Quality
Control (QC) samples that were sent to the
analytic laboratories just as field samples were
(i.e., they were "blind"). They had a similar
appearance and soil composition as field samples
but were known to contain no detectable
concentrations of LCICs. They were analyzed and
handled just as field samples were, and the
results indicated whether or not any contamination
had been introduced by the analytic laboratory.
PHB Preparation Handling Blanks were actually QC
samples introduced at the sample preparation
laboratory and sent to analytic laboratories just
as field samples were sent (i.e., they were
"blind"). They were analyzed and reported just as
field samples were, and the results indicated
whether any contamination was introduced by the
preparation laboratory.
HT Holding time samples were soil samples used to
study the effects of extending the holding time on
LCIC concentrations in the sample. QCEMSL EMSL
Blind QC samples were samples spiked with known
concentrations of LCICs, but the levels were not
known by the analytic laboratory. A Blind QC
sample was extracted with each extraction batch of
samples and analyzed. If a given level of
recovery was not achieved in the Blind QC, then
the laboratory re-extracted and re-analyzed the
field samples in the extraction batch.
MS The Matrix Spike and Matrix Spike Duplicate
samples (MSD) were created by splitting every
twentieth field sample into three parts. One-
third was treated as a normal field sample (i.e.,
the "native" sample in a native/MS/MSD set of
analyses), one-third as an MS analysis, and one-
third as the MSD. Each MS and MSD was then spiked
with a fixed amount of LCICs. The results were
then used for QC purposes. See Section 8.5 for a
72
-------
description of how to merge the native samples,
with MS/MSD analyses.
BL This group includes both Reagent or Instrument
blanks as well as Method Blanks. The Method Blank
is a blank sample, prepared by the analytic
laboratory, containing no known levels of LCICs.
This sample was then extracted in a batch of field
samples, subjected to the same handling and
storage and analyzed with the field samples. The
Reagent Blank is also a blank sample, made from
the solvents used during the sample extraction
process and analyzed to determine if the analysis
process was introducing LCIC contamination into
the field samples.
6.3 Data Element Dictionary
The data element dictionary for the Form I Master File follows
this page.
73
-------
LOVE CANAL HABITABILITY STUDY
FORM I MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION SOURCE
******* Keys and Status *************************************************************************************
F1.A01
F1.A02
F1ANALID
CLEANHS
CHAR 20 Analysis Lab Sample Id
(Lab Id + Lab Analysis Id)
CHAR 10 Original Project ID (HS Number)
LabOata
LabOata
*******
F1.B01
F1.B02
Sample Information
F1SMPL
F1TYPE
************************************************************************
F1.B08 F1SULFUR
CHAR
CHAR
CHAR
10
6
F1.B03
F1.B04
F1.B05
F1.B06
F1.B07
F1GENDTE
F1GENTME
F1LDVER
F1MOIST '
F1PRESCR
CHAR
CHAR
CHAR
NUM
CHAR
8
8
5
8
3
F1.B09
F1.B10
F1.B11
F1.B12
F1.B13
F1.BU
F1.B15
F1ANLST
F1WTEXT
F1AADTE
F1AATME
F1CONCD
F1QFILE
F1DFILE
CHAR
NUM
CHAR
CHAR
NUM
CHAR
CHAR
8
8
8
8
8
12
15
Project Sample Field Id (HS #)
Type of sample
Values:
MS = Matrix Spike
MSD = Matrix Spike Duplicate
BL = Method Blank or Reagent Blank
QCEMSL = EMSL Blind QC Sample
HS = Field Sample
HS REP= Field Sample Replacement
HT = Holding Time Blank
FHB = Field Handling Blank
PHB = Prep Lab Handling Blank
SPLIT = Field Split
SSB = Shipping and Storage Blank
SSB SP = Shipping and Storage Blank Split
LabData Generation Date
LabData Generation Time
LabData Software Version
Percent Moisture
Flag for Analysis Pre-screen
Values:
MS = GC/MS pre-screen performed
ECD = GC/ECD pre-screen performed
blank = pre-screen not performed
Flag for Sulphur Cleanup Performed
Values:
blank or N = sulphur cleanup not performed
Y = sulphur cleanup performed
GC/MS Analyst
Weight Extracted
Analysis Date
Analysis Time
Concentration Dilution Factor
GC/MS Shift Results File Name
GC/MS Data File Id
LabOata
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
LabData
74
-------
DATA
ELEMENT
ID
NAME
ARRAY
LOVE CANAL HABITABILITY STUDY
FORM I MASTER FILE • DATA ELEMENT DICTIONARY
TYPE LENGTH DESCRIPTION
SOURCE
******* Summary Sample Data Validation Qualifiers
F1.C01 LCICUSE (8) CHAR 2 Data validation usability flags, by 8 LCICs IntDBBld
Values: 'G ' = Good; no QC flaws.
'U ' = Uncertain; minor QC flaws,-may or may not
be usable, depending on application.
"B ' = Bad; major QC flaws; data unusable.
******* EMSL-LV Sample Specific Data Validation Qualifiers ******
F1.D01
S FLAG
(4)
CHAR
F1.D05 S FLAGS
CHAR
***********************************
FormlDE
Sample specific qualifiers (1 through 4)
Values:
E1-E8 M1-M4 12-15 B1-B4 Q1-Q8 QA Z1-Z9 ZA-ZJ
H1-H4 K2
(See Volume III, Soil Assessment Indicator Chemicals,
Appendix H, CH2M Hill 1988 for a full description of
these qualifiers.)
Sample specific qualifier 5 - EMSL-LV data validation FormlDE
rating
Values:
blank = usability is flagged on an analyte basis
(see next data group)
>G ' = Good; no QC flaws.
'U ' = Uncertain; minor OC flaws,-may or may not
be usable, depending on application.
>B ' = Bad; major QC flaws; data unusable.
Analyte Specific LabData and Laboratory Qualifiers ********************
Values for E_FLAGnA through E_FLAGnD:
E1-E8 M1-M4 12-15 B1-B4 Q1-Q8 QA Z1-Z9 ZA-ZJ H1-H4 K2
Values for E_FLAGnE (analyte usability):
'G ' = Good; no QC flaws.
'U ' = Uncertain; minor QC flaws,-may or may not
be usable, depending on application.
'B ' = Bad; major QC flaws; data unusable.
blank = this flag slot not used
(See Volume III, Soil Assessment Indicator Chemicals,
Appendix H, CH2M Hill 1988 for a full description of
these qualifiers.)
1,2-Dichlorobenzene qualifier A
1,2-Dichlorobenzene qualifier B
1,2-Dichlorobenzene qualifier C
1,2-Dichlorobenzene qualifier D
1,2-Dichlorobenzene qualifier E
1,2,4-Trichlorobenzene qualifier A
1,2,4-Trichlorobenzene qualifier B
1,2,4-Trichlorobenzene qualifier C
1,2,4-Trichlorobenzene qualifier D
F1.E01
F1.E02
F1.E03
F1.E04
F1.E05
F1.E06
F1.E07
F1.E08
F1.E09
E_FLAG1A
E_FLAG1B
E_FLAG1C
E_FLAG1D
E_FLAG1E
E_FLAG2A
E_FLAG2B
E_FLAG2C
E FLAG2D
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
2
2
2
2
2
2
2
2
2
1
1
1
1
1
1
1
1
1
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
75
-------
LOVE CANAL HABITABILITY STUDY
FORM 1 MASTER FILE - DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID
F1.E10
F1.E11
F1.E12
F1.E13
F1.EU
F1.E15
F1.E16
F1.E17
F1.E18
F1.E19
F1.E20
F1.E21
F1.E22
F1.E23
F1.E24
F1.E25
F1.E26
F1.E27
F1.E28
F1.E29
F1.E30
F1.E31
F1.E32
F1.E33
F1.E34
F1.E35
F1.E36
F1.E37
F1.E38
F1.E39
F1.E40
F1.E41
F1.E42
NAME ARRAY
E_FLAG2E
E_FLAG3A
E_FLAG3B
E_FLAG3C
E_FLAG3D
E_FLAG3E
E_FLAG4A
E_FLAG4B
E_FLAG4C
E_FLAG4D
E_FLAG4E
E_FLAG5A
E_FLAG5B
E_FLAG5C
E_FLAG5D
E_FLAG5E
E_FLAG6A
E_FLAG6B
E_FLAG6C
E_FLAG6D
E_FLAG6E
E_FLAG7A
E_FLAG7B
E_FLAG7C
E_FLAG7D
E_FLAG7E
E_FLAG8A
E_FLAG8B
E_FLAG8C
E_FLAG8D
E_FLAG8E
CONC (8)
EXT_DATE
TYPE
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
CHAR
NUM
CHAR
LENGTH
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
8
8
DESCRIPTION
1,2,4-Trichlorobenzene qualifier E
1,2,3,4-Tetrachlorobenzene qualifier
1,2,3,4-Tetrachlorobenzene qualifier
1,2,3,4-Tetrachlorobenzene qualifier
1,2,3,4-Tetrachlorobenzene qualifier
1,2,3,4-Tetrachlorobenzene qualifier
2-Chtoronaphthalene qualifier A
2-Chloronaphthalene qualifier B
2-Chloronaphthalene qualifier C
2-Chloronaphthalene qualifier D
2-Chloronaphthalene qualifier E
Alpha-BHC qualifier A
Alpha-BHC qualifier B
Alpha-BHC qualifier C
Alpha-BHC qualifier D
Alpha-BHC qualifier E
Delta-BHC qualifier A
Delta-BHC qualifier B
Delta-BHC qualifier C
Delta-BHC qualifier D
Delta-BHC qualifier E
Beta-BHC qualifier A
Beta-BHC qualifier B
Beta-BHC qualifier C
Beta-BHC qualifier D
Beta-BHC qualifier E
Gamma- BHC qualifier A
Gamma -BHC qualifier B
Gamma-BHC qualifier C
Gamma -BHC qualifier D
Gamma-BHC qualifier E
Concentrations, by LCIC
Order of the LCICs:
1 , 2 -D i ch I orobenzene
1,2,4-Trichlorobenzene
1,2,3,4- Tet rachorobenzene
2-Chloronaphthalene
Alpha-BHC
Delta-BHC
Beta-BHC
Gamma-BHC
Date Sample Extracted
A
B
C
D
E
SOURCE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
FormlDE
LabOata
FormlDE
76
-------
DATA
ELEMENT
ID
NAME
ARRAY
LOVE CANAL HABITABILITY STUDY
FORM I MASTER FILE - DATA ELEMENT DICTIONARY
TYPE LENGTH DESCRIPTION
SOURCE
******* Analyte Specific Flags
F1.F01 ALLIONS
F1.F02
F1.F03
F1.F04
SCANRNG
IONRATI
RRT
*********************************************************************
(8) CHAR 1 All Ions Flags, by 8 LCICs LabData
Values:
blank = all three ions present
'*' = one or more ions missing
(8) CHAR 1 Scan Range Flags, by 8 LCICs LabData
Values:
blank = scan range less than or equal to 2
'*' = scan range greater than 2
(8) CHAR 1 Ion Ratio Flags LabData
Values:
blank = ion ratio within 20% of theoretical
'*' = ion ratio greater than 40 % from theoretical
'+' = ion ratio between 20% and 40% from theoretical
(8) CHAR 1 Relative Retention Time Flags LabData
Values:
blank = within the relative retention time window
'*' = outside of relative retention time window
*******************************
******* porm 1 Comments **************************************************
F1.G01 COMM (10) CHAR 80 Form 1 Comments • containing explanation of manual
LabData quantitation override
LabData
******* Integrated DB Audit System Results
F1.H01 F1TRACK CHAR 1 Sample not found in Sample Tracking
Values:
* = not found in Sample Tracking
blank = found in Sample Tracking
***
IntDBBld
77
-------
78
-------
7.0 Blind Quality Control (QC) Spike Master File
In the Blind QC Spike Master File, a record contains analyte
spiking levels for a blind QC sample sent by EMSL-LV to an
analytical laboratory.
7.1 Logical Record Description
The data elements in a logical record are organized in data
groups, as follows:
- KEYS - the primary, unique identifier of each record in
the file.
- BLIND QUALITY CONTROL SPIKE INFORMATION - information on
spike levels, by analyte, along with the specific
bottle number.
7.2 Logical Subsets of the File - Special Screening
This file does not contain any data elements that define logical
subsetting.
7.3 Data Element Dictionary
The data element dictionary for the Blind Quality Control Master
File follows this page.
79
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LOVE CANAL HABITABILITY STUDY
BLIND QUALITY CONTROL MASTER FILE • DATA ELEMENT DICTIONARY
DATA
ELEMENT
ID NAME ARRAY TYPE LENGTH DESCRIPTION SOURCE
******* Key *************************************************************************************************
BQ.A01 QCSMPL CHAR 8 Sample Id BlindQC
******* Analyte Spiking Level Data **************************************************************************
BQ.B01 QCBOTTLE CHAR 3 Bottle Number BlindQC
BQ.B02 OCSPIKE (8) NUM 8 Spike Levels, by 8 LCICs in ppb BlindQC
80
-------
8.0 Combining Files
Since the Data Base is composed of ten files, some data analyses
may require combining two or more of these files. This is
accomplished through SAS by a series of steps that usually
involves sorting the records and then combining or merging the
files based on one of the keys they contain.
The first four subsections present outlines of the basic steps
needed to complete some common file combinations. The last two
subsections contain the actual SAS code used during two of the
data analyses.
8.1 Form I with Detailed Data
To combine the "official" analytical results in the Form I
records (F1FILE) with detail data in the sample master files
(FSFILE and QCFILE), the following steps must be taken:
1. sort F1FILE on F1ANALID
2. concatenate F1FILE and QCFILE, renaming QCANALID and
ALANALID to F1ANALID
3. sort output of step 2. by F1ANALID
4. merge F1FILE and output of step 3. by F1ANALID,
retaining only observations that are in both files
8.2 Field Samples with Calibration Records
To combine field samples (FSFILE) with continuing calibration
(CCFILE)and initial calibration (ICFILE) records, the following
steps must be taken:
1. select desired FSFILE records (by FSTYPE or other
criteria, if any)
2. sort output of step 1. by CCANALID
3. sort CCFILE by CCANALID
4. merge the output of step 2. and step 3. by CCANALID,
retaining only observations that are in both files
5. sort ICFILE by ICANALID
6. merge output of step 4. with output of step 5. by
ICANALID, retaining only observations that are in both
files
81
-------
8.3 Field Samples with Method Blanks
To combine field samples with their associated method blanks, the
following steps must be taken:
1. select QCFILE records with QCTYPE = "BLM", renaming
QCANALID to MBANALID
2. sort output of step 1. on MBANALID
3. select FSFILE records (as desired)
4. sort output of step 3. on MBANALID
5. merge output of step 2. and output of step 4. by
MBANALID, retaining only observations that are in both
files
8.4 Blind QC Results with Spiking Levels
The merging of blind QC results with blind QC spiking levels is
accomplished by doing the following:
1. select F1FILE records whose F1TYPE = "QCEM"
2. sort output of step 1. on F1ANALID
3. select QCFILE records whose QCTYPE = "QCEM", renaming
QCANALID to F1ANALID
4. sort output of step 3. on F1ANALID
5. merge output of step 2. and output of step 4. by
F1ANALID, retaining only observations that are in both
files
6. sort output of step 5. by CLEANHS
7. read BQFILE, renaming QCSMPL to CLEANHS
8. sort output of step 7. by CLEANHS
9. merge the output of step 6. and the output of step 8.
by CLEANHS, retaining only observations that are in
both files
82
-------
8.5 Native Field Sample MS/MSD Sets
An example of the SAS code necessary to create the native field
sample MS/MSD sets is as follows:
DATA FS;
SET VAXDB1.F1FSFILE;
LENGTH MSSAMP $ 8 LAB $ 3;
ARRAY FSCONCB FSCONCB1-FSCONCB8;
ARRAY FSRRF<8) FSRRF1-FSRRF8;
ARRAY FSCONC{8} FSCONC1-FSCONC8;
J = INDEXCFSSMPL.'HS1);
IF FSALID='AQI' THEN LABID=1;
IF FSALID='CEC' THEN LABID=2;
IF FSALID='VER' THEN LABID=3;
IF FSALID='NUS' THEN LABID=4;
IF FSALID='EMS' THEN LABID=5;
IF FSALID='MGM' THEN LABID=6;
IF FSALID='CAA' THEN LABID=7;
K = 10 • J + 1;
HSSAMP = SUBSTRCFSSMPL.J.K);
DO I = 1 TO 8;
FSCONCO) = 0;
IF FSRRFtlJr' ' THEN FSCONC{I}=FSCONCB<:i} * (100-FSMOIST)/100;
END;
KEEP MSSAMP ALANALID CLEANHS FSCONC1-FSCONC8 LABID LAB;
PROC SORT DATA=FS; BY MSSAMP;
DATA MS;
SET VAXDB1.QCFILE;
LENGTH MSSAMP $8 MSLAB $ 3;
ARRAY QCCONCB{8> QCCONCB1-QCCONCB8;
ARRAY MSCONCX8} MSCONC1-MSCONC8;
IF INDEXCQCSMPL,'MS')>0 AND INDEXCQCSMPL,'EM')=0 AND
INDEX(QCSMPL/'MSD')=0;
J = INDEX(QCSMPL,'MS') + 2;
K = 10 - J + 1;
MSSAMP = SUBSTR(QCSMPL,J,K);
MSCADD = 5 * 20 / QCWTEXT;
DO I = 1 TO 8;
MSCONCCI) = QCCONCB<:i> * (100-QCMOIST)/100;
END;
KEEP QCSMPL QCALID MSSAMP MSCADD MSCONC1-MSCONC8 QCSPRCU1-OCSPRCU8
QCSPRCL1-QCSPRCL8 QCSPRL1-QCSPRL8;
PROC SORT DATA=MS; BY MSSAMP;
DATA MSD;
SET VAXDB1.QCFILE;
LENGTH MSSAMP $8 MSDLAB $ 3;
ARRAY QCCONCB<:8> QCCONCB1-QCCONCB8;
ARRAY MSDCONCCS} MSDCONC1-MSDCONC8;
IF INDEXCQCSMPL,'MSD1)>0 AND INDEXCQCSMPL,'EM1)=0;
J = INDEXCQCSMPL,'MSD1) + 3;
K = 10 - J + 1;
83
-------
MSSAMP = SUBSTR(QCSMPL,J,K);
MSDCADD = 5 * 20 / QCUTEXT;
DO I = 1 TO 8;
MSDCONCU} = QCCONCBd) * (100-QCMOIST)/100;
END;
KEEP QCSMPL QCALID MSSAMP MSDCADD MSDCONC1-MSDCONC8;
PROC SORT DATA=MSD; BY MSSAMP;
DATA MRGMSMSD ERRMS MRG2MS MRG3MS;
ARRAY MSCONCX8} MSCONC1-MSCONC8;
ARRAY MSDCONC{8> MSDCONC1-MSDCONC8;
ARRAY FSCONC{8) FSCONC1-FSCONC8;
ARRAY MSPR{8> MSPR1-MSPR8;
ARRAY MSDPR{8) MSDPR1-MSDPR8;
ARRAY MSRPD{8> MSRPD1-MSRPD8;
ARRAY QCSPRCUC8} QCSPRCU1-QCSPRCU8;
ARRAY QCSPRCL{8> QCSPRCL1-QCSPRCL8;
ARRAY QCSPRL{8> QCSPRL1-QCSPRL8;
MERGE FS(IN=INFS) MS(IN=INMS) MSD(IN=1NMSD);
BY MSSAMP;
IF INFS AND (INMS OR INMSD);
IF NOT FIRST.MSSAMP AND NOT LAST.MSSAMP THEN OUTPUT ERRMS;
ELSE DO;
INTFLAG = 1;
DO I = 1 TO 8;
MSPRU) = (MSCONC<:i}-FSCONC<:i})/MSCADD*100;
MSDPR{I> = (MSDCONC{I>-FSCONC{I»/MSDCADD*100;
LCIC = I;
LOWLIM = QCSPRCLtl}; UPLIM = QCSPRCUCI};
MS2PR = MSPRO>;
OUTPUT MRG2MS;
MS2PR = MSDPRCO;
OUTPUT MRG2MS;
MSRPDO> = ABS(MSPR<;i>-MSDPR<:i»/(MSPR{I}+MSDPR<:i»*200;
UPLIM= QCSPRCL{I>; LOWLIM=0.;
MS2RPD = MSRPDCI};
OUTPUT MRG3MS;
END;
OUTPUT MRGMSMSD;
END;
84
-------
8.6 Creating the Subset Used for Statistical Analysis
The SAS code used to create the subset of data used for
statistical analysis is as follows:
DATA F1FILE;
SET VAXDB1.FORM1;
KEEP ANALID;
LENGTH ANALID $ 20;
ANALID=F1ANALID;
IF ANALID EQ "CAA8711125-01AS" THEN DELETE;
IF ANALID EQ "MGMLC09974R03 " THEN DELETE;
IF ANALID EQ "VER41283 " THEN DELETE;
IF ANALID EQ "EMSREHS0219 " THEN DELETE;
IF ANALID EQ "EMSREHS0253 " THEN DELETE;
IF ANALID EQ "EMSHS0344 " THEN DELETE;
IF ANALID EQ "VER40438RE " THEN DELETE;
IF ANALID EQ "VER40075 " THEN DELETE;
IF ANALID EQ "MGMLC09976T01 " THEN DELETE;
IF ANALID EQ "MGMLC10005R08 " THEN DELETE;
IF ANALID EQ "EMSHS0661 " THEN DELETE;
IF ANALID EQ "EMSHS0771 " THEN DELETE;
IF ANALID EQ "MGMLC10020R8 " THEN DELETE;
IF ANALID EQ "MGMLC09974007 " THEN DELETE;
IF ANALID EQ "EMSREHS1315 " THEN DELETE;
IF ANALID EQ "CEC587799 » THEN DELETE;
IF ANALID EQ "AQI78554I2 " THEN DELETE;
IF ANALID EQ "AQI77390E2 " THEN DELETE;
IF ANALID EQ "CAA8710222-01T " THEN DELETE;
IF ANALID EQ "CAA8710222-02SRE" THEN DELETE;
IF ANALID EQ "AQI78861I2 " THEN DELETE;
IF ANALID EQ "AQI77393E2 » THEN DELETE;
IF ANALID EQ "VER41364RE " THEN DELETE;
IF ANALID EQ "HGMLC09974002 " THEN DELETE;
PROC SORT DATA=F1FILE;
BY ANALID;
DATA FSFILE;
SET VAXDB1.FSFILE;
IF NEIGHID > 0 AND SUBSTR(SAMPTYPE,1.2) = 'HS';
ALANALID=LEFT(ALANALID);
ANALID=ALANALID;
PROC SORT DATA=FSFILE;
BY ANALID;
DATA VAXDB1.F1FSFILE;
MERGE F1FILE (IN=INF1) FSFILE (IN=INFS);
BY ANALID;
IF INF1 AND INFS;
85
-------
86
-------
APPENDIX A
Data Element Name Index
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name
FS FA 1C IA CC CA QC QA Fl BQ
ALANALID
ALLIONS
ALRECBY
AREAID
CBOTTLE
CCAADTE
CCAATME
CCADDDTE
CCADDTME
CCALID
CCANALID
CCANLST
CCCANAL
CCCDATE
CCCISA
CCCISR
CCCISS
CCCLCA
CCCLCR
CCCLCS
CCCPYRA
CCCPYRR
CCCPYRS
CCCSSA
CCCSSR
CCCSSS
CCCTIME
CCFILE
CCGENDTE
CCGENTME
CCHISR
CCHISS
CCHLCR
CCHLCS
CCHPYRR
CCHPYRS
CCHSSR
CCHSSS
CCINJVL
CCINSTID
CCISA
CCISPH
CCISR
CCISS
A01 A01
H04
F12
F01
B01
B02
B01
B02
COS B03
C04 B04
D02
A01 A01
E02
G03
G01
G07
G09
G08
G04
G06
G05
G10
G12
Gil
G13
G15
G14
G02
E03
C01 B01
C02 B02
Fll
F10
F09
F08
F13
F12
F15
F14
E04
E01
H04 C04
F05
H08 COS
H06 COG
A-l
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name
FS FA 1C IA CC CA QC QA Fl BQ
CCLCA
CCLCPH
CCLCR
CCLCS
CCPC2ID
CCPDC
CCPDF
CCPDOUT
CCPDRF
CCPYRA
CCPYRPH
CCPYRR
CCPYRS
CCQFILE
CCQION
CCQMTH
CCRECALC
CCRFA
CCRFPH
CCRIR
CCRR
CCSMPL
CCSSA
CCSSPH
CCSSR
CCSSS
CCSTATUS
CCUPDCNT
CCUPDDTE
CCUPDTME
CLEANHS
COLFORM
COLFORMR
COLLECTR
COLMLEN
COMM
CONG
CSMPL
CSPIKE
DUPLICAT
DVCCCALA
DVCCCALB
DVCCCALC
DVCCCOM
DVCCDT
HOI C01
F04
H03 C03
H02 C02
A02
105
106
107
104
H05 C05
F06
H09 C09
H07 C07
F01
F03
F02
L01
101
102
103
108
D01
H10 CIO
F07
H12 C12
Hll Cll
A03
C07 B07
C05 BOS
C06 B06
BOS
F01
F02
F15
F18
A03
A02
G01
E41
A01
B02
F19
K30
K31
K32
K35
K33
A-2
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name
FS FA 1C IA CC CA QC QA Fl BQ
DVCCTM
DVCHKA
DVCHKB
DVCHKC
DVCHKD
DVCOM
DVDELIV
DVEPAA
DVEPAB
DVEPAC
DVEPACM
DVEPAD
DVEPASMP
DVHALF
DVMISS
DVPC1A
DVPC1B
DVPC1C
DVPC1CM
DVPC1D
DVPC1DT
DVPC1E
DVPC1F
DVPC1TM
DVPC2A
DVPC2B
DVPC2C
DVPC2CM
DVPC2D
DVPC2DT
DVPC2E
DVPC2F
DVPC2TM
DVPCMDP
DVRES
DVSAMP
EXCPFLAG
EXT_DATE
E_FLAG1A
E_FLAG1B
E_FLAG1C
E_FLAG1D
E_FLAG1E
E_FLAG2A
E FLAG2B
K34
001
O02
O03
O04
006
KOI
K24
K25
K26
K29
K27
K28
K13
K02
K04
K05
K06
K14
K07
K10
K08
K09
Kll
K15
K16
K17
K23
K18
K21
K19
K20
K22
K12
K03
O05
G21
E42
E01
E02
E03
E04
EOS
E06
E07
A-3
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
E_FLAG2C EOS
E_FLAG2D E09
E_FLAG2E E10
E_FLAG3A Ell
E_FLAG3B E12
E_FLAG3D E14
E_FLAG3E E15
E_FLAG4A E16
E_FLAG4B E17
E_FLAG4C E18
E_FLAG4D E19
E_FLAG4E E20
E_FLAG5A E21
E_FLAG5B E22
E_FLAG5C E23
E_FLAG5D E24
E_FLAG5E E25
E_FLAG6A E26
E_FLAG6B E27
E_FLAG6C E28
E_FLAG6D E29
E_FLAG6E E30
E_FLAG7A E31
E_FLAG7B E32
E_FLAG7C E33
E_FLAG7D E34
E_FLAG7E E35
E_FLAG8A E36
E_FLAG8B E37
E_FLAG8C E38
E_FLAG8D E39
E_FLAG8E E40
F1AADTE Bll
F1AATME B12
F1ANALID A01
F1ANLST B09
F1CONCD B13
F1DFILE B15
F1GENDTE BOS
F1GENTME B04
F1LDVER BO5
F1MOIST B06
F1PRESCR B07
F1QFILE B14
F1SMPL B01
A-4
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
F1SULFUR BOS
F1TRACK HOI
F1TYPE B02
F1WTEXT BIO
FCOCFORM F21
FDUPID C02
FHBID C03
FLDCOM F20
FLFEDEX F23
FLPRVBLK F25
FLSRMKS F24
FSAADTE Dll
FSAATME D12
FSAD P03
FSADCL P07
FSADCU P08
FSADDDTE EOS BOS
FSADDTME E04 B04
FSAEDTE D10
FSAF P05
FSALCOND HO3
FSALDTEL DO9
FSALDTES DOS
FSALID H02
FSANLST J02
FSCANAL LOS
FSCCREF R04
FSCDATE L01
FSCISA L07
FSCISR L09
FSCISS LOS
FSCLCA L04
FSCLCR L06
FSCLCS L05
FSCONCA N05
FSCONCB N04
FSCONCDF 104
FSCPYRA L10
FSCPYRR L12
FSCPYRS Lll
FSCSSA L13
FSCSSR L15
FSCSSS L14
FSCTIME L02
FSDBDTE D13
A-5
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
FSDIFLAB R16
FSDQ Q24
FSDUP R09
FSEXTANL 105
FSF1FLAG R02
FSFCDTE D01
FSFCTME DO2
FSFHB RIO
FSFILE J03
FSFSDTE DOS
FSGENA Q19
FSGENB Q20
FSGENC Q21
FSGENCM Q23
FSGEND Q22
FSGENDTE E01 B01
FSGENTME E02 B02
FSHISR Kll
FSHISS K10
FSHLCR K09
FSHLCS K08
FSHPYRR K13
FSHPYRS K12
FSHSSR K15
FSHSSS K14
FSICREF R03
FSIDA Q09
FSIDB Q10
FSIDC Qll
FSIDCOM Q14
FSIDD Q12
FSIDE Q13
FSIDEVF N13
FSIDEVT N12
FSINJVOL J04
FSINSTID J01
FSINTA Q05
FSINTB Q06
FSINTC Q07
FSINTCM Q08
FSIONF N07
FSIRAT N06
FSISA M04 C04
FSISADD P01
FSISPH K05
A-6
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
FSISR M08 COS
FSISS M06 C06
FSLCA M01 C01
FSLCPH K04
FSLCR M03 C03
FSLCS M02 C02
FSMAXS N09
FSMBREF R08
FSMDREF R06
FSMINS N08
FSMOIST 103
FSMSREF R05
FSORIG H07
FSPHB R13
FSPLDTE DO4
FSPLS R14
FSPMDTE DOS
FSPMTME DO6
FSPR 001
FSPRCL 004
FSPRCU 005
FSPRESCR N14
FSPRF 002
FSPROUT 006
FSPSDTE D07
FSPYRA M05 C05
FSPYRPH K06
FSPYRR M09 C09
FSPYRS MOV C07
FSQFILE KOI
FSQION K03
FSQMTH K02
FSQTA Q15
FSQTB Q16
FSQTC Q17
FSQTCOM Q18
FSRANG N10
FSRANGF Nil
FSRBREF R07
FSRD P02
FSRDC P06
FSRECALC R15
FSRERUN HO5
FSRF P04
FSRR N01
A-7
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl , BQ
FSRRC N02
FSRRF N03
FSRRSTAT HO6
FSSMPL HOI
FSSSA M10 CIO
FSSSADD 003
FSSSBF Rll
FSSSBP R12
FSSSPH K07
FSSSR M12 C12
FSSSS Mil Cll
FSSTATUS A02
FSSULFUR N15
FSSURCM Q04
FSSURRA Q01
FSSURRB Q02
FSSURRC Q03
FSTRACK R01
FSTWTEXT 101
FSUPDCNT E07 B07
FSUPDDTE EOS BOS
FSUPDTME E06 BO6
FSWTEXT 102
FTRFFORM F22
FTTEMP G22
HSID C01
ICAADTE B01
ICAATME B02
ICADDDTE CO3 BO3
ICADDTME C04 B04
ICALID DO2
ICANAL A02
ICANALID B01 A01 A01
ICANLST E09
ICCALA KOI
ICCALB K02
ICCALC K03
ICCALD K04
ICCANAL G03
ICCCCODE E06
ICCDATE G01
ICCISA G07
ICCISR G09
ICCISS G08
ICCLCA G04
A-8
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name
FS
FA 1C IA CC CA QC QA Fl BQ
ICCLCR
ICCLCS
ICCOLMMF
ICCOLMSN
ICCONC
ICCPYRA
ICCPYRR
ICCPYRS
ICCSSA
ICCSSR
ICCSSS
ICCTIME
ICDVCOM
ICFILE
ICGENDTE
ICGENTME
ICHISR
ICHISS
ICHLCR
ICHLCS
ICHPYRR
ICHPYRS
ICHSSR
ICHSSS
ICINJVL
ICINSTID
ICINSTMF
ICINSTMN
ICISA
ICISCODE
ICISPH
ICISR
ICISS
ICLCA
ICLCPH
ICLCR
ICLCS
ICMRF
ICPYRA
ICPYRPH
ICPYRR
ICPYRS
ICQFILE
ICQION
ICQMTH
G06
G05
E07
EOS
107
G10
G12
Gil
G13
G15
G14
G02
K05
E10
C01 B01
C02 B02
Fll
F10
F09
F08
F13
F12
F15
F14
Ell
E01
E02
Ł03
H04 C04
E04
F05
H08 COS
H06 C06
HOI C01
F04
H03 C03
H02 C02
101
H05 COS
F06
H09 C09
H07 C07
F01
F03
F02
A-9
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
ICRECALC L01
ICRF 106
ICRSD 102
ICRSDC 103
ICRSDF 104
ICRSDOUT 105
ICSMPL D01
ICSOLCD EOS
ICSSA H10 CIO
ICSSPH F07
ICSSR H12 C12
ICSSS Hll Cll
ICSTATUS A03
ICUPDCNT C07 B07
ICUPDDTE C05 B05
ICUPDTME CO6 BO6
IONRATI F03
LCICUSE C01
LOCDIFF Fll
MBANALID BOS
MDANALID BO4
MEDIA F06
MIXRNAME GO6
MIXTEAM GO7
MSANALID BO3
MSFLAG G13
NEIGHID F13
PC2AADTE B03
PC2AATME BO4
PCBLSEP J06
PCCONC JOS
PCIR J01
PCIRF J04
PCIRLC JO2
PCIROUT JOS
PCIRUC JO3
PCISADD JOS
PCOCFORM Gil
PCPR JO6
PCPRF J07
PCPRLC J02
PCPROUT J04
PCPRUC JO3
PCPV J07
PCPVC J09
A-10
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
PCPVF JOS
PCSNR J10
PCSNRC J12
PCSNRF Jll
PCTCON J01
PCVOLMCS JO9
PHBID C06
PLFEDEX G18
PLJARNBR G14
PLPOSHI G16
PLPRVBLK G20
PLRECBY G04
PLSHMETH G17
PLSID C07
PLSPACE G15
PLSRMKS G19
PREPCOM GO8
PREPCOMM GO3
PREPCOND G02
PREPLAB G01
PTRFFORM G12
QCAADTE BOS
QCAATME B04
QCAD L03
QCADCL ' L07
QCADCU LOS
QCADDDTE COS BOS
QCADDTME C04 B04
QCAEDTE B02
QCAF LOS
QCALDTE B01
QCALID D02
QCANALID B07 A01 A01
QCANLST F02
QCCANAL HO3
QCCDATE HOI
QCCISA H07
QCCISR H09
QCCISS H08
QCCLCA H04
QCCLCR HO6
QCCLCS H05
QCCONCA J05
QCCONCB J04
QCCONCDF E04
A-ll
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
QCCONF M04
QCCPYRA H10
QCCPYRR H12
QCCPYRS Hll
QCCSSA H13
QCCSSR H15
QCCSSS H14
QCCTIME H02
QCDBDTE BOS
QCDQ 042
QCF1FLAG P01
QCFILE F03
QCGENA 035
QCGENB O36
QCGENC 037
QCGENCM O39
QCGEND 038
QCGENDTE C01 B01
QCGENTME CO2 BO2
QCHISR Gil
QCHISS G10
QCHLCR G09
QCHLCS GO8
QCHPYRR G13
QCHPYRS G12
QCHSSR G15
QCHSSS G14
QCIDA O21
QCIDB O22
QCIDC 023
QCIDCOM 026
QCIDD 024
QCIDE O25
QCIDEVF J13
QCIDEVT J12
QCINJVOL F04
QCINSTID F01
QCINTA 015
QCINTB O16
QCINTC O17
QCINTCM 018
QCIONF J07
QCIRAT J06
QCISA 104 C04
QCISADD L01
A-12
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element
Name FS FA 1C IA CC CA QC QA Fl BQ
QCISPH G05
QCISR 108 COS
QCISS 106 C06
QCLCA 101 C01
QCLCPH G04
QCLCR 103 C03
QCLCS 102 C02
QCMAXCON MO3
QCMAXS J09
QCMINS JOS
QCMOIST E03
QCORIG DOS
QCPR KOI
QCPRCL K04
QCPRCU K05
QCPRESCR J14
QCPRF K02
QCPROUT K06
QCPYRA 105 COS
QCPYRPH GO6
QCPYRR 109 C09
QCPYRS 107 C07
QCQFILE G01
QCQION G03
QCQMTH GO2
QCQTA O29
QCQTB 030
QCQTC O31
QCQTCOM 032
QCRANG J10
QCRANGF Jll
QCRD L02
QCRDC L06
QCRECALC P02
QCRERUN DO3
QCRF L04
QCRR J01
QCRRC J02
QCRRF JO3
QCRRSTAT DO4
QCSADDED N01
QCSICON M01
QCSMPL D01
QCSPDD N07
QCSPR N06
A-13
-------
DATA ELEMENT NAME INDEX
Data Element ID = column heading.cell contents (e.g. BQ.B01)
Data
Element " ,
Name FS FA 1C IA CC CA QC QA Fl , BQ
QCSPRCL N04
QCSPRCU NO3
QCSPRL N05
QCSRECV N02
QCSSA 110 CIO
QCSSADD K03
QCSSPH G07
QCSSR 112 C12
QCSSS 111 Cll
QCSTATUS A02
QCSULFUR J15
QCSURCM O12
QCSURRA O09
QCSURRB 010
QCSURRC Oil
QCTICON M02
QCTWTEXT E01
QCTYPE DO 6
QCUPDCNT C07 B07
QCUPDDTE COS BOS
QCUPDTME C06 B06
QCWTEXT E02
RBANALID BO6
RRT F04
SAMPTYPE F03
SCANRNG F02
SITENBR F04
SOILCOMP F16
SPFORM COS
SPLIT G10
SSBIDF C04
SSBIDP COS
STREET F05
S_FLAG D01
S_FLAG5 DOS
TEAMNBR F14
TRAKCOM GO9
TRTEMP G23
TUBENBR F17
XACTUAL F09
XCOORD F07
YACTUAL F10
YCOORD F08
A-14
-------
APPENDIX B
Names of Equivalent Data Elements Contained in Multiple Files
-------
LOVE CANAL HABITABILITY STUDY
NAMES OF "LIKE" DATA ELEMENTS CONTAINED IN MULTIPLE FILES
FIELD DESCRIPTION
FS
OC
F1
1C
CC
Keys
Analysis Lab Sample Id
Project Field Sample Id (HS #)
Chronology
Analysis Lab Login Date
Analysis Lab Analysis Date
Analysis Lab Analysis Time
Data Xfer Tracking
Labdata Gen Date
Labdata Gen Time
DB Add Date
DB Add Time
DB Most Recent Update Date
DB Most Recent Update Time
DB Update Count
Analysis Lab Sample Login Data
Project Sample Id
Analytic Laboratory Id
Analysis Lab Sample Extraction Data
Target Height to Extract
Weight Extracted (gm)
Percent Moisture
Concentration Dilution Factor
ALANALID QCANALID F1ANALID I CANAL ID CCANALID
HSID QCSMPL F1SMPL ICSAMPL CCSMPL
FSALDTES QCALDTE
FSAADTE QCAADTE F1AADTE ICAADTE CCAADTE
FSAATME QCAATME F1AATME ICAATME CCAATME
FSGENDTE QCGENDTE F1GENDTE ICGENDTE CCGENDTE
FSGENTME QCGENTME F1GENTME ICGENTME CCGENTME
FSADDDTE QCADDDTE ICADDDTE CCADDDTE
FSADDTME QCADDTME ICADDTME CCADDTME
FSUPDDTE QCUPDDTE ICUPDDTE CCUPDDTE
FSUPDTME OCUPDTME ICUPDTME CCUPDTHE
FSUPDCNT QCUPDCNT ICUPDCNT CCUPDCNT
FSSMPL QCSMPL ICSMPL CCSMPL
FSALID QCALID ICALID CCALID
FSTUTEXT QCTUTEXT
FSWTEXT QCWTEXT F1WTEXT
FSMOIST QCMOIST F1MOIST
FSCONCDF QCCONCDF F1CONCDF
B-l
-------
LOVE CANAL HABITABILITY STUDY
NAMES OF "LIKE" DATA ELEMENTS CONTAINED IN MULTIPLE FILES
FIELD DESCRIPTION
GC/MS Shift Results File Name
Quantitat ion Method Flag
LCIC Quant it ion Ion Selection
FS
QC
F1
FSQFILE
FSQMTH
FSQION
OCQFILE
QCQMTH
QCQION
1C
ICQMTH
ICQION
CC
Analysis Lab Injection Data
GC/MS Instrument Id
GC/MS Analyst
GC/MS Datafile Id
Injection Volume
Analysis Lab Interpretation Data
FSINSTID OCINSTID ICINSTID CCINSTID
FSANLST OCANLST F1ANLST ICANLST CCANLST
FSFILE QCF1LE F1DFILE ICFILE CCFILE
FSINJVOL OCINJVOL ICINJVL CCINJVL
ICQFILE CCQFILE
CCQMTH
CCQION
Peak Height Data
Peak Height, by 8 LCICs, By 3 Ions
Peak Height, by 5 Int. Stds.
(Primary Ion)
Peak Height, Pyrene-D10
(Secondary Ion)
Peak Height, by 3 Surrogates
(Primary Ion)
Scan for Peak Height
by 8 LCICs, by 3 Ions
Retention Time for Peak Height
by 8 LCICs, by 3 Ions
Scan for Peak Height,
by 5 Internal Standards
Retention Time for Peak Height,
by 5 Internal Standards
Scan for Peak Height for
Pyrene-D10
Retention Time for Peak Height,
for Pyrene-010
FSLCPH
FSISPH
FSPYRS
FSSSPH
FSHLCS
FSHLCR
FSH1SS
FSHISR
FSHPYRS
FSHPYRR
QCLCPH
QCISPH
QCPYRS
QCSSPH
QCHLCS
QCHLCR
QCHIS
QCHISR
QCHPYRS
QCHPYRR
ICLCPH
ICISPH
ICPYRS
ICSSPH
ICHLCS
ICHLCR
ICHISS
ICHISR
ICHPYRS
ICHPYRR
CCLCPH
CCISPH
CCPYRS
CCSSPH
CCHLCS
CCHLCR
CCHISS
CCHISR
CCHPYRS
CCHPYRR
B-2
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LOVE CANAL HABITABILITY STUDY
NAMES OF "LIKE" DATA ELEMENTS CONTAINED IN MULTIPLE FILES
FIELD DESCRIPTION
FS
QC
F1
1C
CC
Scan for Peak Height,
by 3 Surrogates
Retention Time for Peak Height,
by 3 Surrogates
FSHSSS
FSHSSR
QCHSSS
OCHSSR
ICHSSS
ICHSSR
CCHSSS
CCHSSR
Correction Flags
Analysis Lab Analysis Date
Analysis Lab Analysis Time
Analyst
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs,
by 3 Ions
Area, by 5 Int. Stds.,
(Primary Ion)
Scan, by 5 Int. Stds.,
(Primary Ion)
Retention Time, by 5 Int. Stds.,
(Primary Ion)
Area, Pyrene-D10
(Secondary Ion)
Scan, Pyrene-D10
(Secondary Ion)
Retention Time, Pyrene-D10
(Secondary Ion)
Area, By 3 Surrogates
(Primary Ion)
Scan, By 3 Surrogates
(Primary Ion)
Retention Time, By 3 Surrogates
(Primary Ion)
FSCDATE
FSCTIME
FSCANAL
FSCLCA
FSCLCS
FSCLCR
QCCDATE
QCCTIME
QCCANAL
QCCLCA
QCCLCS
QCCLCR
ICCDATE
ICCTIME
ICCANAL
ICCLCA
ICCLCS
ICCLCR
CCCDATE
CCCTIHE
CCCANAL
CCCLCA
CCCLCS
CCCLCR
FSCISA
FSCISS
FSCISR
FSCPYRA
FSCPYRS
FSCPYRR
FSCSSA
FSCSSS
FSCSSR
QCCISA
QCCISS
QCCISR
QCCPYRA
QCCPYRS
QCCPYRR
QCCSSA
QCCSSS
OCCSSR
ICCISA
ICCISS
ICCISR
ICCPYRA
ICCPYRS
ICCPYRR
ICCSSA
ICCSSS
ICCSSR
CCCISA
CCCISS
CCCISR
CCCPYRA
CCCPYRS
CCCPYRR
CCCSSA
CCCSSS
CCCSSR
B-3
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LOVE CANAL HABITABILITY STUDY
NAMES OF "LIKE" DATA ELEMENTS CONTAINED IN MULTIPLE FILES
QC
F1
1C
CC
Analysis Raw Data (After Corrections, if any)
Area, by 8 LCICs, by 3 Ions
Scan, by 8 LCICs, by 3 Ions
Retention Time, by 8 LCICs,
by 3 Ions
Area, by 5 Int. Stds. (Primary Ion)
Area, Pyrene-D10 (Secondary Ion)
Scan, by 5 Int. Stds. (Primary Ion)
Scan, Pyrene-D10 (Secondary Ion)
Retention time, by 5 Int. Stds.
(Primary Ion)
Retention time, Pyrene-DIO
(Secondary Ion)
Area, by 3 Surrogates (Primary Ion)
Scan, by 3 Surrogates (Primary Ion)
Retention Time, by 3 Surrogates
FSLCA
FSLCS
FSLCR
FSISA
FSPYRA
FSISS
FSPYRS
FSISR
FSPYRR
FSSSA
FSSSS
FSSSR
QCLCA
QCLCS
QCLCR
OCISA
QCPYRA
QCISS
QCPYRS
QCISR
QCPYRR
QCSSA
QCSSS
QCSSR
ICLCA
ICLCS
ICLCR
ICISA
ICPYRA
ICISS
ICPYRS
ICISR
ICPYRR
ICSSA
ICSSS
ICSSR
CCLCA
CCLCS
CCLCR
CCISA
CCPYRA
CCISS
CCPYRS
CCISR
CCPYRR
CCSSA
CCSSS
CCSSR
(Primary Ion)
LABDATA Computations for Field and QC Samples
Relative Retention Time, FSRR OCRR
by 8 LCICs (Quant itat ion Ion)
Relative Retention Time Criteria, FSRRC OCRRC
by 8 LCICs
Flag for Rel. Ret. Time Out of FSRRF QCRRF
Criteria, by 8 LCICs
Pre-criteria Concentration, FSCONCB QCCONCB
by 8 LCICs
Criteria Concentration, by 8 LCICs FSCONCA QCCONCA
Ion Ratio, by 8 LCICs FSIRAT QCIRAT
RRT
CONC
B-4
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LOVE CANAL HABITABILITY STUDY
NAMES OF "LIKE" DATA ELEMENTS CONTAINED IN MULTIPLE FILES
FIELD DESCRIPTION
Flag for All Ions Being Present,
by 8 LCICs
Minimum Scan Number of 3 Ions,
by 8 LCICs
Maximum Scan Number of 3 Ions,
by 8 LCICs
Scan Range (Max-Min), by 8 LCICs
Flag for Scan range >2,
by 8 LCICs
Ion Ratio % Dev. from Theoretical
Values, by 8 LCICs
Flag for Ion ratio % Dev. Out of
Criteria, by 8 LCICs
FS
FSIONF
FSMINS
FSMAXS
FSRANG
FSRANGF
FSIDEVT
FSIDEVF
QC F1
OCIONF ALLIONS
QCMINS
QCMAXS
QCRANG
QCRANGF SCANRNG
QC1DEVT
QCIDEVF
Flag for Analysis Pre-screen
Flag for Sulphur Cleanup Performed
LABDATA Computations for Surrogate Standards
% Recovery by 3 Surrogates
Flag for % Rec. Out of Criteria
Amount of Surrogate added(ng)
% Recovery Criteria lower limit
% Recovery Criteria upper limit
Number of % Rec. Out of Criteria
FSPRESCR
FSSULFUR
FSPR
FSPRF
FSSSADD
FSPRCL
FSPRCU
FSPROUT
OCPRESCR
QCSULFUR
QCPR
QCPRF
QCSSADD
QCPRCL
QCPRCU
QCPROUT
LABDATA Computations for Internal Standards
Internal Standard Quantity Added
(in nanograms) FSISADD QCISADD
Ret. Time Difference From CC Val FSRD QCRD
Area Difference % From CC Val FSAD QCAD
Flag for Ret. Time Out of Criteria FSRF QCRF
1C
CC
IONRATI
B-5
-------
LOVE CANAL HABITABILITY STUDY
NAMES OF "LIKE" DATA ELEMENTS CONTAINED IN MULTIPLE FILES
FIELD DESCRIPTION
Flag for Area Out of Criteria
Retention Time Difference Criteria
Area % Diff. Crit. lower limit
Area % Diff. Crit. upper limit
FS
FSAF
FSRDC
FSADCL
FSADCU
QC
QCAF
QCRDC
QCADCL
QCADCU
F1
1C
CC
B-6
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APPENDIX C
Formulas for Computed Data Elements
-------
FORMULAS
This appendix contains the formulas used by LabData and the
Integrated Data Base for chemistry computations. This
presentation is oriented toward the computations from a data
processing perspective. The equations are presented in the form
used for the data base calculations. The equations may not
appear to be equivalent to those in the SOW but are in fact the
same. For a fuller treatment from a chemistry perspective, refer
to the Love Canal Habitability Study—Soil Sample Laboratory
Analysis Quality Assurance Project Plan.
Terminology
The objective of the chemistry method was to measure
concentrations of the eight Love Canal Indicator Chemicals
(LCICs). These eight compounds are always numbered as follows:
1 = 1,2-Dichlorobenzene DCB
2 = 1,2,4-Trichlorobenzene TCB
3 = 1,2,3,4-Tetrachlorobenzene TeCB
4 = 2-Chloronaphthalene CNP
5 = Alpha-BHC A-BHC
6 = Delta-BHC D-BHC
7 = Beta-BHC B-BHC
8 = Gamma-BHC G-BHC
All concentrations are in parts per billion (ppb).
In addition to the LCICs, concentrations (and percent recovery)
for three surrogate standard (S.S.) compounds are computed. The
three surrogates are always numbered as follows:
1 = 1,4-Dibromobenzene DBB
2 = 2,4,6-Tribromobiphenyl TBBP
3 = 1,2,4,5-Tetrabromobenzene QBE
Associated with each LCIC and surrogate is an internal standard.
For each injection into the GC/MS/SIM, the internal standards
have a known concentration so that variations in injection volume
and instrument response are compensated. There are five internal
standards, and they are always numbered as follows:
1 = D4-l,4-Dichlorobenzene IS1
2 = D8-Naphthalene IS2
3 = DIO-Acenaphthene IS3
4 = DIO-Phenanthrene IS4
5 = DIO-Pyrene IS5
C-l
-------
The associations of the LCICs and surrogates to the internal
standards (I.S.) are given below:
Compound Associated I.S. Number
LCIC #1 1
LCIC #2 2
LCIC #3 3
LCIC #4 3
LCIC #5 4
LCIC #6 4
LCIC #7 4
LCIC #8 4
S.S. #1 2
S.S. #2 4
S.S. #3 5
The basic units of direct measurement in the GC/MS/SIM itself are
area, peak height, retention time, and scan number. Area and
peak height are strictly relative units within the instrument.
Retention time is measured in seconds, and scan numbers are half-
second intervals of retention time. The predominant, and
preferred, method for computing concentrations uses the area
measurement. Peak height is used in instances of excessive
interference.
For each LCIC, three ions are measured so that there are
potentially three areas, retention times, and scan numbers for
each of the eight LCICs. These three ions are classified as
primary, secondary, and tertiary. One ion is measured for each
I.S. and S.S., except a secondary ion is also measured for D10-
Pyrene. The three ions are classified as primary, secondary, and
tertiary in relation to their relative abundance. With some
exceptions, the LCIC concentrations are computed using the
primary ion.
There are some basic relationships among GC/MS/SIM analyses that
are critical to the computations. The GC/MS/SIM instrument is
first calibrated using a five-point initial calibration (I.e.).
Each 12-hour analytical run ("shift") begins with a continuing
calibration/performance check (CC/PC1) that directly relates to
the I.e. Each analysis in the 12-hour shift relates directly to
the CC/PC1. At the end of a 12-hour shift there is a second
performance check (PC2) that relates directly to the CC/PC1. The
QAPP allows either one calibration per 12-hour shift or two
calibrations per 16-hour shift.
Calibration Computations
There are two types of calibrations used: an initial calibration
(I.C.) performed at five different concentrations and a
c-2
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continuing calibration/performance check performed at the second
lowest I.e. concentration.. The five I.e. concentrations are:
0.05
0.10
0.50
1.0
2.0
The primary numbers computed during the calibrations are relative
response factors (RRFs). RRFs are computed for each LCIC and
surrogate. They establish the relative responses of the LCICs
and surrogates to the internal standards.
The RRFs are computed as follows:
RRF = AREA / ISAREA / ICCONC,
where:
(1)
RRF = relative response factor,
AREA = LCIC or S.S. primary ion area,
ISAREA = the associated I.S. area, and
ICCONC = the appropriate calibration
concentration = (ICCONC is the
concentration of LCIC or S.S.
divided by concentration of I.S.)
RRFs are computed for the primary ions of LCICs and S.S.'s for
each of the five initial calibration runs. Over the five I.e.
runs, a mean RRF and percent relative standard deviation is
computed for each LCIC and S.S. The mean RRF is computed as:
RRFBAR = ( > RRFi) / 5
(2)
where:
RRFBAR = mean relative response factor for an
LCIC or S.S.,
i = I.e. number 1 to 5, and
RRFi = the RRF for the LCIC or S.S. for the
;tl
I.e. point
c-3
-------
SD
n
- RRFBAR)
.1=1
1/2
/ (n-1)
where:
RRFBAR = mean relative response factor for an
LCIC or S.S.,
i = I.e. number 1 to 5, and
RRFi = the RRF for the LCIC or S.S. for the
itn i.e. point
(3)
The %RSD is computed as:
%RSD = SD / RRFBAR * 100, (4)
where:
%RSD = the percent relative standard
deviation for the LCIC or S.S.,
RRFBAR = mean RRF, and
SD = standard deviation of the 5 RRFs for
the LCIC or S.S.
Stringent QA/QC criteria are set for the %RSD values because it
measures the linearity of the instrument response. The RRFBAR
values are compared to the RRFs computed in the CC/PC1 as
follows:
%D
(CCRRF - RRFBAR) / RRFBAR
* 100,
(5)
where:
%D
= CC/PC1 percent deviation for an LCIC
or S.S.,
CCRRF = CC/PC1 RRF for the LCIC or S.S., and
RRFBAR = mean RRF from the I.e.
QA/QC criteria are set for the %D to determine if the GC/MS/SIM
is still in calibration. The CCRRF is computed using equation
(1) and an ICCONC value of 0.10.
C-4
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The continuing calibration relative retention times (CCRR) are
computed for each ion of each LCIC. For Finnigan GC/MS
instruments,
CCRR = SCAN / ISSCAN, (6)
where:
CCRR = relative retention time for a given
LCIC and ion,
SCAN = the scan value of the given LCIC and ion, and
ISSCAN = the scan value of the appropriate I.S.
For Hewlett Packard GC/MS instruments,
CCRR = RT / ISRT, (7)
where:
RT = retention time (seconds) of the given
LCIC and ion, and
ISRT = retention time (seconds) of the
appropriate I.S.
The CCRR formulas are different for the two manufacturers because
of differences in quantitation report formats.
The CCRR values are used in the relative retention time LCIC
identification criteria that is discussed later. Also, the I.S.
areas and scan value for the CC/PC1 are used in I.S. QA/QC
criteria for the subsequent analyses.
Performance Check Computations
The CC/PC1 and PC2 analyses are used to check instrument
sensitivity. The measures of instrument sensitivity are ion
ratios, specific chromatographic signal-to-noise ratios, and
chromatographic signal separation measures.
The performance check ion ratios (PCIR) are computed for CC/PC1
and PC2 for each LCIC and for DIO-Pyrene (I.S. #5). Except for
LCIC #3 (1,2,3,4-Tetrachlorobenzene), the PCIR is computed as
secondary ion area divided by primary ion area. For LCIC #3,
PCIR is computed as primary ion divided by secondary ion.
The chromatographic values cannot be computed from other data.
C-5
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Concentration Computations
LCIC dry weight concentrations are computed as:
CONC = AREA / ISAREA / CCRRF / WTEXT / MSTRFACT
* ISADDED * CDFACTOR, (8)
where:
CONC = LCIC concentration in ng/gm,
AREA = LCIC quantitation primary ion area,
ISAREA = associated I.S. area,
CCRRF = continuing calibration relative
response factor for the quantitation
primary ion,
WTEXT = weight extracted in grams,
MSTRFACT = adjustment for percent moisture,
ISADDED = internal standard amount added, in
nanograms, and
CDFACTOR = concentration/dilution factor
(usually l.O).
MSTRFACT is computed as:
MSTRFACT = (100 - PCTMSTR) / 100, (9)
where:
PCTMSTR = sample percent moisture.
In almost all cases, the primary ion is used for quantitation.
The Form I concentrations are either values computed using
equation (6) or "ND" (non-detect) if one or more of the LCIC
identification criteria are not met. The four identification
criteria are:
1. All three ions are present.
2. The primary, secondary, and tertiary ions of each LCIC
must maximize within + two scans of each other. (The
range of scan numbers for the three ions is less than or
equal to 2.)
3. The secondary to primary ion ratios are within 20% of
the theoretical value.
4. The quantitation ion is within 0.005 relative retention
time (RRT) units of the same ion in the CC/PC1 run.
Method/Holding Blanks
The Method/Holding blanks have Form I concentrations computed and
also have concentrations computed for all three ions without any
identification criteria applied. These concentrations for all
C-6
-------
three ions are reported on Form IV and indicate interference in
any ion of any LCIC.
Matrix Spike/Matrix Spike Duplicates
The complete matrix spike/matrix spike duplicate (MS/MSD)
analysis consists of three extractions from the same sample:
the sample with no LCICs added (the "native sample"),
the sample with approximately 5 ng/gm of LCICs added (the
"matrix spike"), and
a second extraction of the sample with approximately 5
ng/gm (the "matrix spike duplicate") of LCICs added.
Form I concentrations are reported for all three extractions. In
addition, computations involving all three extractions are
performed. These are matrix spike percent recovery (MSPR) and
matrix spike relative percent deviation (MSRPD). A major
difference between the Form I and the Form III concentrations is
that Form I concentrations are reported as dry weights and
Form III concentrations are reported as wet weights. Wet weight
concentrations are computed using equation (8) with the MSTRFACT
term removed. The identification criteria are different from
those used to report results on Form I. The MS and MSD
calculations reported on Form III are made using only the
relative retention time for the native sample. The MS and MSD
percent recoveries are computed by:
MSPR = (MSCONC - FSCONC) / MSAMTADD * 100, (10)
where:
MSPR = MS or MSD percent recovery,
MSCONC = MS or MSD wet weight concentration (result),
FSCONC = native sample wet weight concentration (result)
with only the RRT identification criteria
applied, and
MSAMTADD = concentration of LCICs added to the MS or MSD
at extraction.
C-7
-------
The MSAMTADD is nominally 5 ng/gm, but it needs to be adjusted
for the actual weight extracted. This adjustment is done by:
MSAMTADD = MSAMT * CRITWEXT / MSWTEXT, (11)
where:
MSAMTADD = concentration of LCICs added to the MS or MSD,
in ng/gm,
MSAMT = nominal concentration added (5 ng/gm in this
study),
CRITWEXT = method criteria weight to extract (20 gm), and
MSWTEXT = actual weight extracted in the MS or MSD.
The MS/MSD relative percent deviation (MSRPD) is computed by:
MSRPD = (MSPR - MSDPR) / (MSPR + MSDPR) * 200, (12)
where:
MSRPD = the MS/MSD relative percent deviation,
MSPR = matrix spike percent recovery, and
MSDPR = matrix spike duplicate percent recovery.
c-8
-------
Surrogate Percent Recovery
The surrogate percent recovery is computed by:
SSPR
= AREA / ISAREA / CCRRF / SSADDED
* ISADDED * CDFACTOR * 100
where:
SSPR
AREA
ISAREA
CCRRF
SSADDED
ISADDED
CDFACTOR
(13)
surrogate percent recovery,
surrogate primary ion area,
internal standard primary ion area,
relative response factor from the CC/PC1,
amount of surrogate added, in ng,
amount of internal standard added, in ng, and
concentration/dilution factor (usually 1.0).
Peak Heights
The LCIC chemistry methodology permits the chemists to use peak
heights of the GC/MS response curves instead of area if there is
chemical or matrix interference that makes the areas unreliable
measures. All of the computation formulas can be used by
substituting peak height values for areas. This is possible
because the areas and peak heights are unitless, relative
measures.
Peak height concentration computations require relative response
factors computed using peak heights in the CC/PC1. For any
sample, the concentrations require peak heights for the
particular LCIC quantitation ion and the applicable internal
standard.
C-9
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C-10
-------
APPENDIX D
Box Plot - A Graphic Representation of Analytical Results
-------
Box Plot - A Graphic Representation of Analytical Results
Box plots were used to visually compare data across laboratories
or other stratifiers of interest. Although these graphic
representations are not a substitute for formal statistical
analysis, they should be generally consistent with the
statistical analysis and accordingly provide a qualitative cross-
check of the results of the statistical comparisons.
An example of a box plot is shown in Figure D-l. This box plot
shows one page (one surrogate) of surrogate recoveries. The
vertical axis is the percent recovery. The horizontal axis is
the analytical laboratory. The box includes the middle 50
percent of the data. The line in the box marks the median, or
50th percentile; 25 percent of the data are included in the part
of the box above the median line, and 25 percent are in the part
below the median line.
The upper "whisker" (vertical line above the box) extends to the
largest non-extreme value (the interpretation of "extreme" is
based on a relationship with the normal [Gaussian] distribution).
The extreme values are plotted with asterisks and the more
extreme with circles. Those extreme values that lie off the
scale are printed at the top of the figure.
SURROGATE RECOVERIES
i RECOVERY BY LAB WI1H CONTROL LIUIIS
SURR-TeBB
mi M
INll.tl
140
130
120
110
* 100
R
C 90
0
V (0
I 70
CO
so
40
30
3 4
LABORATORY
Figure D-l
Example of a Box Plot
D-l
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