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 ------- 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 ------- 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 ------- 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 ------- 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. ------- 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. ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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. ------- 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 ------- 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. 10 ------- 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. 11 ------- 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 12 ------- 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 13 ------- 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 14 ------- 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 15 ------- 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 16 ------- 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 17 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- 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 ------- |