R
  EPA-540/R
  94-095
          United States        Office of        Publication 9240.1 -13
          Environmental Protection    Solid Waste and      DR^aS^f095
          Agency          Emergency Response    PB95-963514
                                 December 1994
          Superfund
v>EPA     USEPA CONTRACT
           LABORATORY PROGRAM
           STATEMENT OF WORK
           FOR INORGANICS ANALYSIS
           MULTI-MEDIA,
           MULTI-CONCENTRATION
           ILMO 2.1

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                                                 9240.1-13
                                                 PB95-963514
                                                 EPA540/R-94/095
     USEPA CONTRACT LABORATORY PROGRAM
             STATEMENT OF WORK
                   FOR
            INORGANICS ANALYSIS
               Multi-Media
            Multi-Concentration

       .   Document Number ILM02.0

Including Revision ILM02.1 (September  1991)

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                                                                ATTACHMENT A
                              STATEMENT OF WORK

                              TABLE OF CONTENTS
EXHIBIT A:   SUMMARY OF REQUIREMENTS
EXHIBIT B:   REPORTING AND DELIVERABLES REQUIREMENTS
EXHIBIT C:   INORGANIC TARGET ANALYTE LIST
EXHIBIT D:   ANALYTICAL METHODS
EXHIBIT E:   QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS
EXHIBIT F:   CHAIN-OF-CUSTODY, DOCUMENT CONTROL AND STANDARD OPERATING
             PROCEDURES
EXHIBIT G:   GLOSSARY OF TERMS
EXHIBIT H:   DATA DICTIONARY AND FORMAT FOR DATA DELIVERABLES  IN COMPUTER-
             READABLE FORMAT
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                                  EXHIBIT A
                           SUMMARY OF REQUIREMENTS
SECTION I       GENERAL REQUIREMENTS 	




SECTION II      SPECIFIC REQUIREMENTS 	




SECTION III     TECHNICAL AND MANAGEMENT REQUIREMENTS
PAGE




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                                  SECTION  I
                            GENERAL REQUIREMENTS


The Contractor shall employ procedures specified in this Statement of Work
(SOW) in the preparation and analysis of aqueous (vater) and solid
(soil/sediment) samples for the presence and quantitation of 23 indicated
elements and cyanide.

The Contractor shall use proven instruments and techniques to identify and
measure the elements and inorganic species presented in the Target Analyte
List (Exhibit C).  The Contractor shall perform sample preparation and
analysis procedures as prescribed in Exhibit D, meeting specified sample
preservation and holding time requirements.

If dissolved metals are requested by the EPA Regional offices, the
Contractor shall follow the instructions provided on the Traffic Reports.
If there are no instructions on the Traffic Report, the Contractor shall
contact SMO for resolution.

The Contractor shall adhere to the quality assurance/quality control
protocol specified in Exhibit E for all samples analyzed under this
contract.

Following sample analysis, the Contractor shall perform data reduction and
shall report analytical activities, sample data, and quality control
documentation as designated in Exhibit B.

Exhibit F contains chain-of-custody and document control requirements which
the Contractor must follow in processing samples and specifies requirements
for written laboratory standard operating procedures.

To ensure proper understanding of language utilized in this contract,
Exhibit G contains a glossary of terms.  When a term is used in the text
without explanation, the glossary meaning shall be applicable.  Glossary
definitions do not replace or take precedence over specific information
included in the SOW text.

Exhibit H contains the Agency Standard implementation for reporting data
electronically.

The samples to be analyzed by the Contractor are from known or suspected
hazardous vaste sites and, potentially, may contain hazardous inorganic
and/or organic materials at high concentration levels.  The Contractor
should be aware of the potential hazards associated with the handling and
analyses of these samples.  It is the Contractor's responsibility to take
all necessary measures to ensure the health and safety of its employees.

In addition, the Contractor must be aware of the importance of maintaining
the integrity of the data generated under the contracts as it is used to
make major decisions regarding public health and environmental welfare.
The data nay also be used in litigation against Potentially Responsible
Parties in the enforcement of Superfund legislation.
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Prior to accepting any samples from the Agency, the Contractor shall have,
in house, the appropriate standards for aJJL target analytes listed in
Exhibit C.
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                                 SECTION II
                            SPECIFIC REQUIREMENTS


A.   FOR EACH SAMPLE, THE CONTRACTOR SHALL PERFORM THE  FOLLOWING  TASKS:

     Task I:     Receive and Prepare Hazardous Waste Samples.

     1.   The Contractor shall receive  and handle samples under the chain-
          of-custody and sample documentation procedures described in
          Exhibit F.  A sample consists of all components, perhaps more than
          one phase, contained inside appropriate receptacles.  More than
          one container may be used for a single sample; individual
          containers may contain preservatives for different analysis
          portions.   Containers may be  glass or plastic.

     2.   The Contractor shall provide  the required analytical expertise and
          instrumentation for analyses  of Target Analyte List (TAL) elements
          and cyanide equal to or lover than the detection limits specified
          in Exhibit C.   In Exhibit D.  EPA provides the Contractor with the
          specific sample preparation techniques for water and soil/sediment
          samples and the analytical procedures which must be used.  A
          schematic flow chart depicting the complete low level-medium level
          inorganics analytical scheme  is presented in  Section I  of Exhibit
          D.

     3.   The Contractor shall prepare  and analyze samples within the
          maximum holding time specified in Section II  of Exhibit D even if
          these times are less than the maximum data submission time allowed
          in this contract.

     4.   The Contractor is advised that the samples received under this
          contract are usually from known or suspected  hazardous  waste sites
          and may contain high (greater than 15%) levels of organic and
          inorganic materials of a potentially hazardous nature and of
          unknown structure and concentration, and should be handled
          throughout the analysis with  appropriate caution.  It is the
          Contractor's responsibility to take all necessary measures to
          ensure laboratory safety.

     Task II:    Analyze Samples for Identity and Quantitation of Specific
                 Inorganic Constituents.

     1.   For each sample received, the Contractor may  be required to
          perform the analyses described in the  following paragraphs 2.,  3.
          and 4.  The documentation that accompanies - the sample(s) to  the
          Contractor facility shall indicate specific analytical
          requirements for that sample  or set of samples.

     2.   Exhibit D specifies the analytical procedures that must be used.
          Exhibit D contains instructions and references for preparation of
          samples containing low-to-medium concentrations of inorganics  for
          ICP analysis; flame, graphite furnace  and  cold vapor AA analysis
          and cyanide analysis.  The identification  and quant i tat ion of

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     analytes other than cyanide  shall be accomplished using the ICF or
     AA methods specified in Exhibit D and achieves the Contract
     Required Detection Limit (CRDL) specified in Exhibit C. Cyanide
     shall be analyzed by the individual procedures specified  in
     Exhibit D.

3.   All samples must initially be  run undiluted (i.e., the final
     product of sample preparation  procedure).  When an analyte
     concentration exceeds the calibrated or  linear range, appropriate
     dilution (but not below the  CRDL) and reanalysis of the prepared
     sample is required,  as specified in Exhibit D.

4.   For the purpose of this contract, a full sample analysis  Is
     defined as the analysis for  ALL of the target constituents
     identified in Exhibit C in accordance with the methods in Exhibit
     D and performance of related QA/QC as specified in Exhibit E.
     Duplicate sample, laboratory control sample, and spike sample
     analyses shall each be considered a separate full sample  analysis.
     All other QA/QC requirements are considered an inherent part of
     this contract Statement of Work and are  included in the contract
     sample unit price.

Task III:   Perform Required Quality Assurance/Quality Control
            Procedures

1.   All specific QA/QC procedures  prescribed in Exhibit E shall be
     strictly adhered to by the Contractor.   Records documenting the
     use of the protocol shall be maintained  in accordance with the
     document control procedures  prescribed in Exhibit F, and  shall be
     reported in accordance with  Exhibit B requirements.

2.   The Contractor shall establish and use on a continuing basis QA/QC
     procedures including the daily or (as required) more frequent use
     of standard reference solutions from EPA, the National Institute
     of Standards and Technology  or secondary standards traceable
     thereto, where available at  appropriate  concentrations  (i.e.,
     standard solutions designed  to ensure that operating parameters  of
     equipment and procedures, from sample receipt through
     identification and quantitation, produce reliable data).   Exhibit
     E specifies the QA/QC procedures required.

3.   The Contractor shall establish a Quality Assurance Plan (QAP)  as
     defined in Exhibit E with the  objective  of providing  sound   :
     analytical chemical measurements.  This  program shall  incorporate
     the quality control procedures, any necessary corrective action,
     and all documentation required during data  collection as well as
     the quality assessment measures performed by management to ensure
     acceptable data production.

4.   Additional quality assurance and quality-.control shall be required
     in the form of Performance Evaluation Samples submitted by EPA for
     Contractor analysis, and in the form of verification of instrument
     parameters, as described in Exhibit E.
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     5.   Laboratory Control Sample (LCS)  -  This  standard solution is
          designed to assure that the operating parameters of the analytical
          instrumentation and analytical procedures  from sample  preparation
          through identification and quantitation produce reliable data.
          The Contractor must analyze the  LCS  concurrently with the analysis
          of the samples in the Sample Delivery Group  (see Exhibit A, Part
          I).

B.   EPA has provided to the Contractor formats for  the reporting of data
     (Exhibits B and H).  The Contractor shall be responsible for completing
     and returning analysis data sheets and submitting computer-readable
     data on diskette in the format specified in this  SOU and within the
     time specified in the Contract Performance/Delivery Schedule (see
     Exhibit B).

     1.   Use of formats other than that designated  by EPA will be deemed as
          noncompliant.   Such data are unacceptable.   Resubmission in the
          specified format at no additional  cost  to  the government will be
          required.

     2.   Computer generated forms may be  submitted  in the hardcopy data
          package(s)  provided that the forms are  in  EXACT EPA FORMAT.  This
          means that the order of data elements is the same as on each EPA
          required form, including form numbers and  titles, page numbers and
          header information,  columns and  lines.

     3.   The data reported by the Contractor  on  the hardcopy data forms and
          the associated computer-readable data submitted by the Contractor
          on diskette must contain identical information.   If during
          government inspection discrepancies  are found,  the Contractor
          shall be required to resubmit either or both sets of data, at no
          additional cost to the Government.  The resubmitted diskette
          and/or hardcopy must contain all of  the initially correct
          information previously submitted for all samples including the
          Laboratory Control Sample,  standards, and  blanks in the SDG in
          addition to the corrections replacing the  variables which were
          incomplete or incorrect according  to the requirements in the SOW.

C.   The Contractor shall provide analytical equipment and technical
     expertise for this contract as specified by the following:

     1.   Inductively coupled plasma (ICP) emission  spectrometer with the
          capability to analyze metals sequentially  or simultaneously.-  •• -
                                               *".
     2.   Atomic absorption (AA) spectrometer  equipped with graphite
          furnace, flame, and cold vapor AA  (or a specific mercury analyzer)
          analysis capabilities.

     3.   Analytical equipment/apparatus for analysis  of cyanide as
          described in Exhibit D.

D.   The minimum functional requirements necessary'to meet the terms and
     conditions of this contract are  listed in items 1-7 below.  The
     Contractor shall designate and utilize qualified key personnel to

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     perform these functions.   The EPA reserves the right to  review
     personnel qualifications  and experience.   See Section III, Technical &
     Management Requirements.

     1.    Inorganic  Laboratory Supervisor
     2.    Quality Assurance Officer
     3.    Systems Manager
     4.    Programmer Analyst
     5.    ICP Spectroscopist
     6.    ICP Operator
     7.    Atomic Absorption (AA)  Operator
     8.    Inorganic  Sample Preparation Specialist
     9.    Classical  Techniques (Cyanide)  Analyst
     10.   Inorganic  Chemist (Backup)

E.   The  Contractor  shall respond (within seven days)  to written  requests
     from data recipients for  additional information or explanations  that
     result from the Government's inspection activities unless otherwise
     specified in the  contract (see Exhibit E for details on  Government
     inspection activities).

F.   The  Contractor  is required to retain unused sample volume and used
     sample containers for a period of 60 days after data submission.   From
     time of receipt until analysis,  the Contractor shall maintain
     soil/sediment samples at  4°C (±2°C).

G.   The  Contractor shall adhere to chain-of-custody and document control
     procedures described-in Exhibit F,-  Documentation, as. described
     therein, shall be required to show that all  procedures are being
     strictly followed.  This  documentation shall be reported in  the
     Complete SDG File (see Exhibit B).

H.   Sample shipments  to the Contractor's facility will be scheduled and
     coordinated by the EPA CLP Sample Management Office (SMO), acting on
     behalf of the Administrative Project Officer.  The Contractor shall
     communicate with  SMO personnel by telephone as necessary throughout the
     process of sample scheduling, shipment, analysis and data reporting,  to
     ensure that samples are properly processed.

     If there are problems with the samples (e.g., mixed media, containers
     broken or leaking) or sample documentation/paperwork (e.g.,  Traffic
     Reports not with  shipment, or sample and Traffic Report  numbers do not
     correspond) the Contractor shall immediately contact SMO for
     resolution. The Contractor shall immediately notify SMO  regarding any
     problems and/or laboratory conditions that affect the timeliness of
     analyses and data reporting.  In particular, .the Contractor  shall
     immediately notify SMO personnel in advance regarding sample data that
     will be delivered late and shall specify the estimated delivery date.

I.   Sample analyses will be scheduled by groups of samples,  each- defined as
     a Case and identified by a unique EPA Case number assigned by SMO. A
     Case signifies a group of samples collected at one site  or geographical

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     area over a finite time period,  and will include  one  or more  field
   •  samples with associated blanks.   Samples may be shipped to the
     Contractor in a single shipment or multiple shipments over a  period of
     time, depending on the size of the Case. A Case consists of one or more
     Sample Delivery Groups (SDG).   An SDG is defined  by the following,
     whichever is most frequent:

          o  each Case of  field samples received, OR

          o  each 20 field samples within a  Case, OR

          o  each 14 calendar day period during which field samples in a
             Case are received  (seven calendar day period for 14-day data
             turnaround contracts), said period begins with the receipt of
             the first sample in the SDG.

     Samples may be  assigned to Sample Delivery Groups by  matrix (i.e., all
     soils in one SDG,  all waters in another), at the  discretion of the
     laboratory.   Such assignment must be made at the  time the samples are
     received,  and may not be made retroactively.

     Data for all samples in an  SDG must be submitted together (in one
     package) in the order specified in Exhibit B.  The SDG number is the
     EPA sample number of the first sample received in the SDG. When
     several samples are received together in the first SDG shipment,  the
     SDG number is the lowest sample number (considering both alpha and
     numeric designations) in the first group of samples received  under the
     SDG.  The SDG number is reported on all data reporting forms. The SDG
     Receipt Date is the day that the last sample in the SDG is received.

     The Contractor is responsible for identifying each SDG as samples are
     received,  through proper sample documentation (see Exhibit B) and
     communication with SMO personnel.

J.   Each sample received by the Contractor will be labeled with an EFA
     sample number,  and accompanied by a Traffic Report form bearing the
     sample number and descriptive information regarding the sample.  EPA
     field cample numbers are six digits in  length.  If the Contractor
     receives a sample number of any other length, contact SMO immediately.
     The Contractor shall complete and sign  the Traffic Report, recording
     the date of sample receipt and sample condition on receipt for each
     sample container.  The Contractor mustp  also follow the instructions
     given on the Traffic Report in choosing the OC s?TBPl?-s when such
     information is provided.

     The Contractor shall  submit signed copies of Traffic Reports for  all
     samples in a Sample Delivery Group to SMO within three calendar days
     following receipt of  the last sample in the  SDG.  Traffic Reports
     shall be submitted in SDG  sets  (i.e.,  all Traffic Reports for an  SDG
     shall be clipped together) with an SDG  Cover Sheet containing
     information regarding the  Sample Delivery Group, as  specified in
     Exhibit B.
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K.   EPA Case numbers (including SDG numbers)  and EPA sample numbers shall
     be used by the Contractor in identifying  samples received under this
     contract both verbally and in reports/correspondence.

L.   Samples will routinely be shipped directly to the Contractor through a
     delivery service.   The Contractor shall be available to receive sample
     shipments at any time the delivery service is operating, including
     Saturdays and holidays.  As necessary,  the Contractor shall be
     responsible for any handling or processing required for the receipt of
     sample shipments,  including pick-up of samples at the nearest servicing
     airport, bus station or other carrier service within the Contractor's
     geographical area.

M.   The Contractor shall accept all samples scheduled by SMO, provided that
     the total number of samples received in any calendar month  does not
     exceed the monthly limitation expressed in the contract.  Should the
     Contractor elect to accept additional samples,  the Contractor shall
     remain bound by all contract requirements for analysis of those-samples
     accepted.
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                                 SECTION III
                     TECHNICAL AND MANAGMENT  REQUIREMENTS
I.   TECHNICAL CAPABILITY

As cited in Section II the Contractor shall have the following technical
and management capabilities.  Note:  For those technical functions which
require a minimum educational degree and experience, an advanced degree in
chemistry or any scientific/engineering discipline, (e.g., Master's or
Doctorate) does not substitute for the minimum experience requirements.

Any personnel changes affecting the key personnel &s stated in Exhibit A,
Section III, Items I and II, shall require the Contractor to notify in
writing the Technical Project Officer and the Administrative Project
Officer within 14 days of the personnel change.  The Contractor shall
provide a detailed resume to the Technical Project Officer, Administrative
Project Officer, and EMSL/LV for the replacement personnel within 14 days
of the Contractor's assignment of the personnel.  The resume shall include
position description of titles, education (pertinent to this contract),
number of years of experience (pertinent to this contract) month and year
hired, previous experience and publications.

     A.   Technical  Supervisory Personnel/Key  Personnel

         1.   Inorganics Laboratory Supervisor

              a.   Responsible for all technical efforts of the Inorganics
                   Laboratory to meet all terms and conditions of the EPA
                   contract.

              b.   Qualifications

                   (1)  Education:

                        Minimum of Bachelor's degree in chemistry or any
                        scientific/engineering disc ipline.

              -^   (2)  Experience:

                        Minimum of three years of -laboratory experience,
                        including at least one year in a supervisory
                        position.

         2.   Quality Assurance Officer

              a.   Responsible for overseeing the quality assurance aspects
                   of the data and reporting  directly to  upper management
                   to meet all terms and conditions of the EPA contract.
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     b.    Qualifications:

          (1)  Education:

              Minimum of Bachelor's degree in chemistry or any
              scientific/engineering disc ipline.

          (2)  Experience:

              Minimum of three years of laboratory experience,
              including at least one year of applied experience
              with QA principles and practices in an analytical
              laboratory.

3.   Systems Manager

     a.    Responsible for the management and quality control of
          all  computing systems  (hardware, software, documentation
          and  procedures), generating, updating, and performing
          quality control reviews of automated deliverables to
          meet all terms and conditions of the EPA contract.

     b.    Qualifications:

          (1)  Education:

              Minimum of Bachelor's degree with four or more
              intermediate courses in programming, information
              management, database management systems, or systems
              requirements analysis.

          (2)  Experience:

              Minimum of three years experience in data or
              systems management or programming including one
              year experience with the software being utilized
              for data management and generation of deliverables.

4.   Programmer Analyst

     a.    Responsible for the  installation, operation and
          maintenance of software and programs,  generating,
          updating and performing quality control reviews of
          analytical databases and automated deliverables to meet
          all terms  and conditions of the EPA contract.

     b.    Qualifications:

          (1) Education:

              Minimum of Bachelor's degree with four or more
               intermediate courses  in programming,  information
              management, information systems,  or systems
              requirements analysis.

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               (2)  Experience:

                   Minimum of two years experience in systems or
                   applications programming including one year of
                   experience with the software being utilized for
                   data management and generation of deliverables.

B.   Technical Staff

     1.    ICF  Spectroscopist Qualifications

          a.   Education:

              Minimum of  Bachelor's degree in chemistry or any
              scientific/engineering discipline.

              Specialized training in ICP Spectroscopy.

          b.   Experience:

              Minimum of  two years of applied experience with ICP
              analysis of environmental samples.

     2.    ICP  Operator Qualifications

              Minimum of  Bachelor's degree in chemistry or any
              scientific/engineering discipline with one year of
              experience  in operating and maintaining  ICP
              instrumentation,  or, in lieu of the educational
              requirement,  three  additional years of experience in
              operating and maintaining ICP instrumentation.

     3.    Atomic Absorption (AA) Operator Qualifications

              Minimum of  Bachelor's degree in chemistry or any
              scientific/engineering discipline with one year of
              experience  in operating and maintaining  AA
         -~    instrumentation for graphite furnace, flame, and  cold
              vapor  AA, or,  in  lieu of the educational requirement,
               three  additional  years of experience  in  operating and
              maintaining AA instrumentation, including graphite
               furnace,  flame, and cold vapor techniques.

     4.   Inorganic Sample Preparation Specialist Qualifications

          a.    Education:

               Minimum of high school  diploma and a college level
               course in general chemistry or equivalent.

          b.    Experience:

               Minimum of 1 year of experience in sample preparation in
               an analytical laboratory.

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         c.   Experience (Required if microwave digestion is used):

              Minimum of six months experiencn in an analytical
              laboratory and six months experience in sample
              dissolution using microwave digestion techniques.

     5.   Classical Techniques  (Cyanide) Analyst Qualifications

         a.   Education:

              Minimum of Bachelor's degree in chemistry or any
              scientific/engineering discipline.

         b.   Experience:

              Minimum of 1 year of experience with classical chemistry
              laboratory procedures, in conjunction with the
              educational qualifications; or, in lieu of educational
              requirement, two years of additional equivalent
              experience.

     6.   Technical Staff Redundancy

         In order to ensure continuous operations to accomplish the
         required work as specified by the EPA contract, the bidder
         shall have a minimum  of one (1) chemist available at all
         times as a back-up technical person with the following
         qualifications.

         a.   Education:

              Minimum of Bachelor's degree in chemistry or any
              scientific/engineering discipline.

         b.   Experience:

              Minimum of one year of experience in each of the
         _   following areas —

              o    ICP operation and maintenance

              o    AA operation and maintenance

              o    Classical chemistry analytical procedures
              o    Sample preparation for inorganics analysis

C.   Facilities

     The adequacy of the facilities and equipment is of equal
     importance for the technical staff to accomplish the required work
     as specified by the EPA contract.
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1.   Sample Receipt Area
     Adequate,  contamination-free,  well-ventilated work space
     provided with chemical resistant bench top  for receipt and
     safe handling of EPA samples.

2.   Storage Area
     Sufficient refrigerator space  to maintain unused EPA sample
     volume for 60 days after data  submission.   Soil  samples must
     be stored in a refrigerator at 4°C  (±2°C).   Samples and
     standards must be stored separately ~o prevent cross-
     contaminat ion.

3.   Sample Preparation Area
     Adequate,  contamination-free,  well-ventilated work space
     provided with:

     a.    Benches with chemical  resistant tops.
     b.    Exhaust hoods.   Note:   Standard:: must be prepared in  a
          glove box  or isolated  area.
     c.    Source of  distilled or demineralized organic-free water.
     d.    Analytical balance(s)  located  away from draft  and rapid
          change in  temperature.
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D.
Instrumentation
     At a minimum,  the Contractor shall have the following instruments
     operative at the time of the Preaward Site Evaluation and
     committed for the full duration of the contract.

     1.   Primary Instrument Requirements for 200 Samples/Month
          Capacity  Requirements
Fraction
ICP Metals
GFAA Metals
Mercury
Cyanide
No. of
Instrument(s)
1
2
2
12 distillation
units + 1
photometer
Type of
Instrument
ICP Emission
Spec t r opho tome ter
Atomic Absorption
Spectropho tome ter
with Graphite
Furnace Atomizer
Mercury Cold Vapor
AA Analyzer or AA
instrument
modified for Cold
Vapor Analysis
See Cyanide
Methods , Statement
of Work Exhibit D,
Section IV, Part E
1
There are no Secondary Instrument Requirement's for 200 Samples/Month
Capacity.
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2.   300 Samples/Month Capacity Requirements
Fraction
ICP Metals
GFAA Metals
Mercury
Cyanide
No. of
Ins trument ( s )
1
3
2
18 distillation
units + 1
photometer
Type of
Instrument
ICF Emission
Spectrophotometer
Atomic Absorption
Spectrophotometer
with Sraphite
Furnace Atomizer
Mercury Cold Vapor
AA Analyzer or AA
instrument
modified for Cold
Vapor Analysis
See Cyanide
Me tho ds , S ta tement j
of Work Exhibit D,
Section IV, Fart E|
Secondary Instrument Requirements for 300 Samples/Month Capacity

     The Contractor shall have the following instruments in place
     and operational at any time as a back-up system:
     Quantity
         One
                                   Instruments
                                   GFAA

3.   Additional Instrument Requirements for greater than 300
     Samples/Month Capacity
     Quantity

         One

         One
                                   Instruments

                                   GFAA

                                   ICP Emission Spectrophotometer
4.   Instrument Specifications

     Further information on instrument specifications and  required
     ancillary equipment may be found in the Statement of Work.
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     E.   Data Management and Handling

          1.    Hardware  -  Contractor will have an I."5M or IBM-compatible
               mini-computer  or PC capable of recording required sample data
               on 5.25 inch double-sided, double-density 360 K-byte or high
               density 1.2 M-byte diskettes; or a 3.5 inch double-sided,
               double-density 720 K-byte or 1.44 M-byte diskettes in ASCII
               text  file format and in accordance with the file, record and
               field specifications listed in the SOW, Exhibit H.

               Other minimum  requirements include:

                   Hard disk of at least 20 M-bytes.

                   Asynchronous, Hayes-compatible nodem capable of.at least
                   2,400 baud transmission speed.  In addition, MNP level 5
                   compatibility or compatibility with EPA V.32/V.42bis
                   equipment is recommended.

          2.    Software  -  Software, utilized in generating, updating and
               providing quality control for analytical databases and
               automated deliverables  shall have the following additional
               capabilities:

                   Editing and updating databases.

                   Controlled.access using user ID and file password
                   protection.

          3.    The Contractor shall also be able to submit reports and data
               packages  as specified in the SOW Exhibit B.  To complete this
               task,  the Contractor shall be required to provide space,
               tables and  adequate copy machines to meet the contract
               requirements.

II.  LABORATORY MANAGEMENT CAPABILITY

     The Contractor must have an organization with well-defined
     responsibilities for each individual in  the  management system to ensure
     sufficient resources for EPA contract(s). and to maintain a successful
     operation.  To establish this capability,  the Contractor shall
     designate personnel to carry out the following responsibilities for the
     EPA contract.  Functions include, but are  not limited to, the
     following:

     A.   Technical Staff

          Responsible for all technical efforts for the EPA contract.
                                   A-16                                ILM02.0

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B.   Project Manager

     Responsible for overall aspects of EPA contract(s)  (from sample
     receipt through data delivery), and shall serve as  the primary
     contact for EPA Headquarters Administrative Project Officer and
     Regional Technical Project Officers.

C.   Sample Custodian

     Responsible for receiving the EPA samples (logging,  handling and
     storage).

D.   Quality Assurance Officer

     Responsible for overseeing the quality assurance aspects of the
     data and reporting directly to upper management.

E.   Document Control Officer

     Responsible for all aspects of data deliverables:   organization,
     packaging,  copying, and delivery.  Responsible for  ensuring that
     all documents generated are placed in the complete  SDG file for
     inventory and are delivered to the appropriate EPA  Regional
     personnel  or other receiver.
                               A-17                               ILM02.0

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                                 EXHIBIT B

                  REPORTING AND DELIVERABLES REQUIREMENTS

                                                              Page No.

SECTION I:   Contract Reports/Deliverables Distribution ....  B-2

SECTION II:   Report Descriptions and Order of Data
             Deliverables 	  B-4

SECTION III: Form Instruction Guide	B-13

SECTION IV:   Data Reporting Forms	B-39
                                                                       ILM02.0

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                                                                 Exhibit B Section I
                                        SECTION I

                       CONTRACT REPORTS/DELIVERABLES DISTRIBUTION
                            (For 35-Day Turnaround Contracts)

 The  following table  reiterates  the  Contract  reporting and deliverables requirements
 specified in the  Contract  Schedule  and specifies  the distribution that is required
 for  each deliverable.  NOTE:  Specific  recipient names and addresses are subject to
 change  during the term of  the contract.   The Administrative  Project Officer will
 notify  the Contractor  in writing  of such  changes  when they occur.
Item
*****A. Standard
Operating
Procedures
B. Sample Traffic
Reports
***C. Sample Data
Package
D. Data in Computer
Readable Format
****E. Complete SDG File
*F. Quarterly/Annual
Verification
of Instrument
Parameters
*****G. Quality
Assurance
Plan
No.
Copies
3
1
2
1
1
2
3

Delivery
Schedule
60 days after
contract award
and as required
in Exhibit E.
3 days after
receipt of last
sample in Sample
Delivery Group
(SDG)***
35 days after
receipt of last
sample in SDG
35 days after
receipt of last
sample in SDG
35 days after
receipt of last
sample in SDG**
Quarterly:
15th day of
January, April
July , October
60 days after
contract award
and as required
in Exhibit E.
(D

X
X
X

X
Ai

Distri
(2)
X



X

s dire

butior
(3)
X

X


X
:ted

i
X







Distribution:
(1)  Sample Management Office (SMO)
(2)  Region-Client
(3)  Environmental Monitoring Systems Laboratory  (EMSL/LV)
(4)  NEIC
                                        B-2A
ILM02.0

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                                                                 Exhibit B Section I
                                        SECTION I

                       CONTRACT REPORTS/DELIVERABLES DISTRIBUTION
                            (For 14-Day Turnaround Contracts)

The  following  table  reiterates the  Contract reporting and deliverables requirements
specified  in the  Contract Schedule  and specifies  the distribution that is required
for  each deliverable.  NOTE:  Specific  recipient names and addresses are  subject  to
change during  the term of the contract.  The Administrative Project Officer will
notify the Contractor  in writing  of such changes  when they occur.
Item
*****A. Standard
Operating
Procedures
B. Sample Traffic
Reports
***C. Sample Data
Package
D. Data in Computer
Readable Format
****E. Complete SDG File
~
*F. Quarterly/Annual
Verification
of Instrument
Parameters
*****G. Quality
Assurance
Plan
No.
Copies
3
1
2
1
1
2
3

Delivery
Schedule
60 days after
contract award
and as required
in Exhibit E.
3 days after
receipt of last
sample in Sample
Delivery Group
(SDG)***
14 days after
receipt of last
sample in SDG
14 days after
receipt of last
sample in SDG
14 days after
receipt of last
sample in SDG**
Quarterly:
15th day of
January, April
July, October
60 days after
contract award
and as required
in Exhibit E.
(D

X
X
X

X
A.

Distri
(2)
X



X

s dire

.butior
(3)
X

X


X
.ted
1
i
(4)
X







Distribution:
(1)  Sample Management Office  (SMO)
(2)  Region-Client
(3)  Environmental Monitoring  Systems Laboratory (EMSL/LV)
(4)  NEIC
                                        B-2B
ILM02.0

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                                                                     Exhibit  B  Section I
      *     Also required  in each Sample Data Package.

•—\   **    Concurrent delivery of these items to all recipients is required.

      ***   Sample Delivery Group (SDG) is a group of samples within a Case, received over a
            period of 14 days or less (seven days or less for 14-day data turnaround contracts)
            and not exceeding 20 samples.   Data for all samples in the SDG are due
            concurrently.  (See SOW Exhibit A,  for further description).

      ****  Complete SDG file will contain the original sample data package plus all of the
            original documents described in Exhibit B of the Statement of Work under Complete
            SDG File.

      *****See Exhibit E for description

     NOTE:   As specified in the Contract Schedule (Government Furnished Supplies and
     Materials),  unless otherwise instructed by the CLP Sample Management Office, the
     Contractor shall dispose of unused sample volume and used sample bottles/containers no
     earlier than sixty (60) days following submission of analytical data.

Distribution Addresses:

(1)  USEPA Contract Laboratory Program (CLP)
     Sample Management Office (SMO)
     P.  0.  Box 818
     Alexandria,  VA  22313
     For overnight delivery service,  use street address:
     300 ft. Lee Street
•""""•  Alexandria,  VA  22313

C2)  USEPA REGIONS:  The CLP Sample Management Office, acting on behalf of the Administrative
     Project Officer, will provide the Contractor with the list of addressees for the ten EPA
     Regions.   SMO will provide the Contractor with updated Regional address/name lists as
     necessary throughout the period of the contract and identify other client recipients on a
     case-by-case basis.

(3)  USEPA Environmental Monitoring Systems Laboratory (EMSL/LV)
     944 £. Harmon Avenue
     Las Vegas, NV  89199
     Attn:  Data Audit Staff

(4)  USEPA National Enforcement Investigations Center (NEIC)
     Attn:  CLP Audit Program
     Denver Federal Center Bldg.  53
     P.O. Box 25227
     Denver, CO  80225
                                            B-3                                ILM02.0

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                                                                   Exhibit  B  Section  II
                                     SECTION II

                 REPORT DESCRIPTIONS AND ORDER OF DATA DELIVERABLES

      The Contractor laboratory shall provide reports and other deliverables as
specified in the Contract Performance/Delivery Schedule (see Contract Schedule,
Section F).  The required content and form of each deliverable is described in this
Exhibit.

     All reports and documentation MUST BE as follows:

     o  Legible,

     o  Clearly labeled and completed in accordance with instructions  in
        this Exhibit,

     o  Arranged in increasing alphanumeric EPA sample number order

     o  Paginated sequentially according to instructions in this Exhibit,  and

     o  Single-sided.

      If submitted documentation does not conform to the above criteria, the
Contractor will  be required to resubmit such documentation with deficiency(ies)
corrected, at no additional cost to the government.

      The  Contractor must be prepared to receive the full monthly sample contract
requirement at the time of contract award.

      Whenever the Contractor is required to submit or resubmit data as a result of
an on-site laboratory evaluation or through an Administrative Project: Officer
(AFO)/Technical  Project Officer (TPO) action, or through a. Regional data reviewer's
request, the data must be clearly marked as ADDITIONAL DATA and must: be sent to all
three contractual data recipients (SMO,  EMSL/LV, and Region).   A cover letter shall
be included which describes what data is being delivered, to which EPA Case(s) the
data pertains, and who requested the data.

      Whenever the Contractor is required to submit or resubmit data as a result of
Contract Compliance Screening (CCS) review by SMO, the data must be sent to all
three contractual data recipients (SMO,  EMSL/LV and Region), and in all three
instances must be—accompanied by a color-coded COVER SHEET (Laboratory Response To
Results of Contract Compliance Screening) provided by SMO.  Diskette deliverables
need only be submitted or resubmitted to SMO.  Revised DC-1 and DC-2 forms shall be
resubmitted to SMO.

      Section IV of this Exhibit contains the required Inorganic Analysis Data
Reporting Forms  in Agency-specified formats; Section III of this Exhibit contains
instructions to the Contractor for properly completing all data reporting forms to
provide the Agency with all required data.  Data elements and field descriptors for
reporting data in computer-readable format are contained in Exhibit H.

      Descriptions of the requirements for each deliverable item cited in  the
Contract Performance/Delivery Schedule (see Contract Schedule, Section F)  are
specified in parts A-G of this Section.  Items submitted concurrently  must be
arranged in the order listed.  Additionally, the components of each item must be
arranged in the order presented herein when the item is submitted.
                                      B-4                                ILM02.0

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                                                                   Exhibit B Section II
A.   Quality Assurance Plan and Standard Operating Procedures

     See Exhibits E and F for requirements.

B.   Sample Traffic Reports

      Original Sample Traffic Report page marked "Lab Copy for Return to SMO" with
      lab receipt information and signed  with original Contractor signature, shall
      be submitted for each sample in the Sample Delivery Group.

      Traffic Reports (TRs) shall be submitted in Sample Delivery Group (SDG) sets
      (i.e., TRs for all samples in an SDG shall be clipped together),  with an SDG
      Cover Sheet attached.

      The SDG Cover Sheet shall contain the following; items:

      o Lab name
      o Contract number
      o Sample Analysis Price - full sample price from contract.
      o Case Number
      o List of EPA sample numbers of all samples in the SDG, identifying the first
        and last samples received, and their dates of receipt.

      NOTE:  When more than one sample is received in the first or last SDG shipment,
      the "first" sample received would be the sample with the lowest sample number
      (considering both alpha and numeric designations);  the "last" sample received
      would be the sample with the highest sample number (considering both alpha and
      numeric designations).

      In addition,  each Traffic Report must be clearly marked with .the SDG Number,
      the sample number of the first sample in the SDG (as described in the
      following paragraph).  This information should be entered below the Lab
      Receipt Date on the TR.

      EFA field sample numbers are six digits in length.  If the Contractor receives
      sample numbers of any other length, contact SMO immediately.  The EPA sample
      number of the first sample received in the SDG is the SDG number.  When
      several samples are received together in the first SDG shipment, the SDG
      number shall be the lowest sample number (considering both alplia and numeric
      designations) in the first group of samples received under the SDG.  (The SDG
      number is also reported on all data reporting forms.  See Section III, Form
      Instruction Guide.)

      If samples are received at the laboratory with multi-sample Traffic Reports
      (TRs), All the samples on one multi-sample TR may not necessarily be in the
      same SDG.  In this instance, the laboratory must make the appropriate number
      of photocopies of the TR, and submit one copy vith each SDG cover sheet.

C.   Sample Data PflCkflgf                          ,5  •    -

      The sample data package shall include data for analysis of all samples in one
      Sample Delivery Group (SDG), including field and analytical  samples,
      reanalyses, blanks, spikes, duplicates, and laboratory control samples.
                                      B-5               .                  ILM02.0

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                                                              Exhibit B Section II
 The sample data package must be complete before  submission,  must be
 consecutively paginated (starting with page number one and ending with the
 number of all pages in the package),  and shall include the following:

1.    Cover Page  for the Inorganic Analyses Data Package,  (COVER PAGE --
     Inorganic Analyses Data Package),  including:   laboratory name;  laboratory
     code;  contract number;  Case No.; Sample Delivery Group  (SDG)  No.;  SAS
     Number (if  appropriate);  EPA sample  numbers  in alphanumeric  order  showing
     EPA sample  numbers cross-referenced  with  lab ID numbers; comments,
     describing  in detail any problems  encountered  in processing  the samples in
     the data package;  and,  completion  of the  statement on use of ICP
     background  and interelement corrections for  the samples.

     The Cover Page shall contain the following statement, verbatim:  "I
     certify that this  data  package  is  in compliance with the terms and
     conditions  of the  contract, both technically and for completeness, for
     other than  the conditions detailed above.  Release of the data contained
     in this hardcopy data package and  in the  computer*readable data submitted
     on diskette has been authorized by the Laboratory Manager or the Manager's
     designee, as verified by the following signature."   This statement shall
     be directly followed by the signature of  the Laboratory  Manager or his
     designee with a typed line below it  containing the signers name and title,
     and the date of signature.                                       .

     In addition, on a  separate piece of  paper, the Contractor must also
     include any problems encountered;  both technical and administrative,  the
     corrective  action  taken,  and the resolution.

     The Contractor shall retain a copy of the Sample Data  Package for  365 days
     after final acceptance  of data.  After this  time,  the  Contractor may
     dispose of  the package.

2.    Sample Data

     Sample data shall  be submitted  with  the Inorganic  Analysis Data Reporting
     Forms for all samples  in the SDG,  arranged in. increasing alphanumeric EPA
     sample number order, followed by the QC analyses data,  Quarterly
     Verification of Instrument Parameters forms, raw data,  and copies  of  the
     digestion and distillation logs.

     a.   Results -- Inorganic Analysis Data Sheet  [FORM  I  -  IN]
          Tabulated analytical results  (identification  and quantitation) of  the
          specified analytes (Exhibit C). The validation and release of these
          results is authorized by a specific,  signed statement on the-Cover
          Page.   If the Laboratory Manager cannot verify  all data reported for
          each sample,  he/she oust provide a detailed description of the
          problems associated with the  sample(s)  on the Cover Page.

          Appropriate concentration  units must be specified and entered on Form
          I. The quantitative values shall be reported in  units  of nicrograms
          per liter (ug/L)  for aqueous  samples and milligrams per kilogram
          (mg/kg) for solid samples. No  other units are  acceptable.'Results
          for solid samples  must be  reported on a dry weight basis'.  Analytical
          results must  be reported  to two significant figures if  the result
          value  is less than 10;  to  three significant figures if  the value is
                                 B-6                                ILM02.0

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                                                          Exhibit B Section II
     greater than or equal to 10.   Results  for percent solids must be
     reported to one decimal place.  The preceding discussion concerning
     significant numbers applies to Forms I and X only.   For other Forms,
     follow the instructions specific to those forms as contained in this
     exhibit.

b.   Quality Control Data

     1)   Initial and Continuing Calibration Verification  [FORM II  (PART
          1)  -  IN]

     2)   CRDL  Standard for AA and ICP [FORM II (PART 2)  -  IN]

     3)   Blanks  [FORM III - IN]

     4)   ICP Interference Check Sample  [FORM  IV -  IN]

     5)   Spike Sample Recovery [FORM V  (PART  1)  -  IN]

     6)   Post  Digest Spike Sample Recovery [FORM V (PART 2)  -  IN]

     7)   Duplicates [FORM VI - IN]

     8)   Laboratory Control Sample [FORM VII  - IN]

     9)   Standard Addition Results [FORM VIII -  IN]

     10)  ICP Serial Dilutions [FORM IX  - IN]

     11)  Preparation Log [Form XIII - IN]

     12)  Analysis Run Log [Form XIV - IN]

c.   Quarterly  Verification of Instrument Parameters

     1)   Instrument Detection Limits (Quarterly) [FORM X - IN]

     2)   ICP Interelement Correction Factors  (Annually) [FORM XI (PART 1)
          •  INJ

     3)   ICP Interelement Correction Factors  (Annually) [FORM XI (PART 2)
          -  IN]

     4)   ICP Linear Ranges (Quarterly)  [FORM  XII - IN]

     (Note that copies of Quarterly Verification of Instrument Parameters
     forms for  the current quarter must be submitted with each data
     package.)

d.   Raw Data

     For each reported value, the Contractor shall include in the data
     package all raw data  used to obtain that value.  This applies to all
     required QA/QC measurements,  instrument: standardization, as well as
     all sample analysis results.   This  statement does not apply to the
     Quarterly Verification of Instrument Parameters submitted as a part
                            B-7                                 ILM02.0

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                                                     Exhibit B Section II
of each data package.  Raw data must contain all instrument readouts
used for the sample results.   Each exposure or instrumental reading
must be provided, including those readouts that may fall below the
IDL.  All AA and ICP instruments must provide a legible hard copy of
the direct real-time instrument readout (i.e., stripcharts, printer
tapes, etc.).  A photocopy of the instruments direct sequential
•readout must be included.  A hardcopy of the instrument's direct
instrument readout for cyanide must be included if the
instrumentation has the capability.

The order of raw data in the data package shall be:  ICP, Flame AA,
Furnace AA, Mercury, and Cyanide.  All raw data shall include
concentration units for ICP and absorbances or concentration units
for flame AA, furnace AA, Mercury and Cyanide.  All flame and furnace
AA data shall be grouped by element.

Raw data must be labeled with EPA sample number and appropriate
codes, shown in Table 1 following, to unequivocally identify:

1)   Calibration standards,  including source and prep date.

2)   Initial and continuing calibration blanks and preparation
     blanks.

3)   Initial and continuing calibration verification standards,
     interference check samples, ICP serial dilution samples, CRDL
     Standard for ICP and AA,  Laboratory Control Sample and post
     digestion spike.

4)   Diluted and undiluted samples (by EPA sample number) and all
     weights, dilutions and volumes used to obtain the reported
     values.  (If the volumes, weights and dilutions are consistent
     for all samples in a given SDG, a general statement outlining
     these parameters is sufficient).

5)   Duplicates.

6X_  Spikes (indicating standard solutions used, final spike
     concentrations, and volumes involved).  If spike information
     (source, concentration,  volume) is consistent for a given SDG, a
     general statement outlining these parameters is sufficient.

7)   Instrument used, any instrument adjustments, data corrections or
     other apparent anomalies on the measurement record, including
     all data voided or data not used to obtain reported values and a
     brief written explanation.

8)   All information for furnace analysis clearly and sequentially
     identified on the raw data, including EPA sample number, sample
     and analytical spike data, percent recovery, coefficient of
     variation, full MSA data, MSA correlation coefficient,  slope and
     intercepts of linear fit, final sample concentration  (standard
     addition concentration), and type of background correction used:
     BS for Smith-Heiftje, BD for Deuterium Arc, or BZ for Zeeman.
                       B-8                                 ILM02.0

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                                                                    Exhibit B  Section II
               9)  Time and date of each analysis.  Instrument run logs can be
                   submitteo it tney contain this information.  If the instrument
                   does not automatically provide tines of analysis, these must be
                   manually entered on all raw data for initial and continuing
                   calibration verification and blanks, as well as interference
                   check samples and the CRDL standard for ICP.

               10)  Integration times for AA analyses.

          e.    Digestion and Distillation Logs

               Logs shall be submitted  in the following order: digestion logs  for
               ICP, flame AA, furnace AA and mercury preparations, followed by a
               copy of the  distillation log for cyanide.  These logs must include:
               (1)  date,  (2) sample weights and volumes, (3) sufficient information
               to unequivocally identify which QC samples (i.e., laboratory control
               sample,  preparation blank) correspond ~o each batch digested, (4)
               comments describing any significant sample changes or reactions which
               occur  during preparation, and (5) indication of pH <2 or >12, as
               applicable.

          f.    Properly completed Forms DC-1 and DC-2.

     3.    A copy of the Sample Traffic  Reports submitted in Item A for all of  the
          samples in  the SDG.  The Traffic Reports shall be arranged in increasing
          EPA Sample  Number order, considering both alpha and numeric designations.
          A legible photocopy of  the  SDG cover sheet aust also be submitted.

D.   Data In Computer Readable Form

      The Contractor shall provide a computer-readable copy of the data on reporting
      Forms I-XIV for  all samples in the Sample Delivery Group, as specified  in the
      Contract Performance/Delivery Schedule.   Computer-readable data deliverables
      shall be submitted on an IBM or IBM-compatible,  5.25 inch floppy double-sided,
      double density 360 K-byte or a high density 1.2 M-byte diskette or on an IBM
      or IBM-compatible, 3.5 inch double-sided, double density 720 K-byte or  a high
      density 1.44 M-byte diskette.   The data shall be recorded in ASCII, text file
      format, and shall adhere to the file, record and field specifications listed
      in ExhibitJJ, Data Dictionary and Format for Data Deliverables in Computer-
      Readable Format.

      When submitted,  diskettes shall be packaged anc. shipped in such a manner that
      the diskette(s)  cannot be bent or folded, and vill not be exposed to-extreme
      heat or cold or  any type of electromagnetic radiation.  The diskette(s) must
      be included in the same shipment as the hardcopy data and shall, at a minimum,
      be enclosed in a disVetf«> ™*
                                      B-9                                ILM02.0

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                                                                   Exhibit B Section I!
                                      Table 1
                              Codes for Labelling Data
      Sample
      Sample not part of the SDG
      Duplicate
      Matrix Spike
      Serial Dilution
      Analytical Spike
      Post Digestion/Distillation Spike
      MSA:
        Zero Addition
        First Addition
        Second Addition
        Third Addition
      Instrument Calibration Standards:
        ICP
        Atomic Absorption and Cyanide
        Initial Calibration Verification
        Initial Calibration Blank
      Continuing Calibration Verification
      Continuing Calibration Blank
      Interference Check Samples:
        Solution A
        Solution AB
      CRDL Standard for AA
      CRDL Standard for ICP
      Laboratory Control Samples:
        Aqueous  (Water)
        Solid (Soil/Sediment)
      Preparation Blank (Water)
      Preparation Blank (Soil)
      Linear Range Analysis Standard
                    XXXXXX
                    ZZZZZZ
                   XXXXXXD
                   XXXXXXS
                   XXXXXXL
                   XXXXXXA
                   XXXXXXA

                   xxxxsxo
                   XXXXXX1
                   XXXXXX2
                   XXXXXXS

S or SO for blank standard
           SO,  S10,...etc.
                       ICV
                       ICB
                       CCV
                       CCB

                      ICSA
                     ICSAB
                       CRA
                       CRI

                      LCSW
                      LCSS
                       PBW
                       PBS
                       LRS
Notes:
1.   When an analytical spike or MSA is performed on samples other than field
     samples, the "A",  "0",  "1", "2" or "3" suffixes must be the  last  to be  added to
     the EPA Sample Number.   For instance,  an analytical spike of a  duplicate must
     be formatted "XXXXXXDA."
2.   The numeric suffix that follows the "S" suffix for the standards  indicates the
     true value of the concentration of the standard in ug/L.

3.   ICP calibration standards usually consist of several analytes at  different
     concentrations.  Therefore, no numeric suffix  can follow the ICP  calibration
     standards unless all the analytes in the standard are  prepared  at the same
     concentrations.  For instance, the blank for ICP must  be formatted "SO."
4.   Use suffixes of "0", "1", "2", "3" as appropriate for  samples  identified with
     ZZZZZZ on which MSA has been performed to indicate single  injections.
                                     B-10
                             ILM02.0

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                                                                   Exhibit B Section II
      Tabulation of analytical results for Intercomparison/PE  Sample  analyses
      include all requirements specified in items C.  and D., above.

F.   Complete SPG File fCSF")

     As specified in the Delivery Schedule,  one Complete SDG File  (CSF) including
     the original Sample Data Package shall be delivered to the Region concurrently
     with delivery of a copy  of the Sample Data Package  to SMO and EHSL/LV.  The
     contents of the CSF will be numbered according to the specifications described
     in Sections III and IV of Exhibit B.   The Document  Inventory  Sheet, Form DC-2,
     is contained in Section  IV.   The CSF will contain all original documents where
     possible.   No copies of  original documents will  be  placed in  the CSF unless the
     originals are bound in a loebook maintained by the  laboratory.  The CSF will
     contain all original documents specified in Sections III  and  IV, and Form DC-2
     of Exhibit B of the SOW.
         t

     The CSF will consist of  the following original documents  in addition to the
     documents in the Sample  Data Package:

     1.   Original Sample Data Package

     2.   A  completed and signed  Document  Inventory Sheet (Form DC-2)

     3.   All original shipping documents, including, but not limited to, the
         following documents:

         a.   EPA Chain-of-Custody Record

         b.   Airbills

         c.   EPA (SMO) Traffic Reports

         d.   Sample Tags (if present) sealed  in plastic bags.

     4.   All original receiving  documents,  including, but not limited to, the
         following documents:

         a.   Fora DC-1

         b.   Other receiving  forms or copies of receiving logbooks.

         c.   SDG Cover  Sheet

     5.   All  original laboratory records  of sample transfer,  preparation, and
         analysis,  including,  but not limited to,  the following documents:

         a.   Original preparation and analysis forms or copies of preparation and
              analysis logbook pages.

         b.   Internal sample  and sample  digestate/distillate transfer chain-of-
              custody records.
                                     B-ll                                ILM02.0

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                                                                   Elxhlbit  B  Section II
     6.   All other original  case-specific documents in the possession of the
          laboratory,  including, but not  limited to, the following  documents:

          a.    Telephone contact logs.

          b.    Copies  of personal logbook pages.

          c.    All  handwritten case-specific notes.

          d.    Any  other case-specific documents not covered by the above.

          NOTE:  All case-related documentation may be used or admitted as evidence
          in  subsequent legal proceedings.  Any other case-specific documents
          generated after  the CSF is sent to EPA, as veil as copies that  are altered
          in  any fashion,  are also  de live rabies to EPA  (original to the  Region and
          copies to SMO and EMSL/LV).

          If  the laboratory does submit case-specific documents to  EPA after
          submission of the CSF, the documents  should-be numbered-as an addendum to
          the CSF and a revised DC-2 form should be submitted; or the  documents
          should be numbered  as a new CSF and a new DC-2 form should be submitted to
          the Regions  only.

G.   Quarterly and  Annual  Verification of Instin^ent P^*riveters

     The Contractor shall  perform and report quarterly verification of instrument
     detection limits and  linear range by the methods specified in  Exhibit E  for
     each instrument used  under this contract.  For the ICP instrumentation,  the
     Contractor shall also perform  and report annual interelement correction  factors
     (including method of  determination), wavelengths used and integration times.
     Forms for Quarterly and  Annual Verification of Instrument Parameters for the
     current  quarter and year shall be submitted in each SDG data package,  using
     ?orms X, XIA,  XIB, and XII.  Submission of Quarterly/Annual Verification of
     Instrument Parameters shall  include  the raw data used to determine those values
     reported.

H.   Corrective Action Procedures

     If a Contractor fails to adhere to the requirements detailed  in this SOW, a
     Contractor may expect, but the Agency is not  limited to  the following actions:
     reduction of numbers  of  samples sent under this contract, suspension of sample
     shipment to the Contractor, data package audit, an on-site laboratory
     •valuation, remedial  performance evaluation .-sample, and/or contract sanctions,
     such as  a Cure Notice (see Exhibit E for additional details).
                                     B-12                                ILM02.0

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                                                                  Exhibit B Section III
                                     SECTION  III

                               FORM INSTRUCTION GUIDE

This section contains specific instructions for the completion of all required
Inorganic Data Reporting Forms.  This section is orgc.nized into the following Parts:

     A.   General Information and Header Information

     B.   Cover Page --  Inorganic Analyses  Data  Package  [COVER PAGE -  IN]

     C.   Inorganic Analysis Data Sheet   [FORM I  -  IN]

     D.   Initial and Continuing  Calibration  Verification  [FORM II (PART  1)  -  IN]

     E.   CRDL Standard  for AA and ICP  [FORM II  (PART 2) -  IN]

     F.   Blanks   [FORM  III - IN]

     G.   ICP  Interference  Check  Sample   [FORM IV - 1(7]

     H.   Spike Sample Recovery  [FORM V (PART 1)  - IN]

     I.   Post Digest Spike Sample Recovery  [FORM  V (PART 2)  -  IN]

     J.   Duplicates  [FORM VI -  IN]

     K.   Laboratory Control Sample  [FORM  VII -  IN]

     L.   Standard Addition Results  [FORM  VIII  - IN]

     M.   ICP  Serial Dilutions  [FORM IX -  IN]

     N.   Instrument Detection Limits (Quarterly)   [FORM X - IN]

     0.   ICP  Interelement  Correction Factors (Annually)  [FORM XI
          (PART H - IN]

     P.   ICP  Interelement  Correction Factors (Annually)  [FORM XI
          (PART 2) - IN]

     Q.   ICP  Linear Ranges (Quarterly)   [FORM XII - IN]

     R.   Preparation Log  [Form XIII -  IN]

     S.   Analysis Run Log  [Form XIV -  IN]

     T.   Sample Log-In Sheet  [Form DC-1]

     U.   Document Inventory Sheet  [Form DC-2]
                                     B-13                                ILM02.0

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                                                                  Ebchibit B Section III
A.   General Information and Header Information

     The data reporting forms presented in Section  IV  in  this  Exhibit have been
     designed in conjunction with the computer-readable data format specified in
     Exhibit H,  Data Dictionary and Format for  Data Deliverables  in Computer-
     Readable Format.  The specific length of each  variable for computer-readable'
     data transmission purposes is given in Exhibit H.  Information entered on these
     forms must  not exceed the size of the field given on the  form,  including such
     laboratory-generated items as Lab Name and Lab Sample ID.

     Note that on the hardcopy forms (see Section IV) , the space  provided for
     entries is  greater in some instances than  the  length prescribed for the
     variable as written to diskette (see Exhibit H).  Greater space is provided on
     the hardcopy forms for the sake of visual  clarity.

     Values must be reported on the hardcopy forms  according to the individual form
     instructions in this section.  Each form submitted must be filleoV-out
     completely  for all analytes before proceeding  to  the next form of the same
     type.    Do  not submit multiple forms in place  of  one form if the information on
     those forms can be submitted on one form.

     All characters which appear on the data reporting forms presented in the
     contract (Exhibit B, Section IV) must be reproduced  by the Contractor when
     submitting  data, and the format of the forms submitted must  be identical to
     that shown  in the contract.  No information may be added,  deleted, or moved
     from its specified position without prior  written approval of the EPA
     Administrative Project Officer.  The names of  the various fields and analytes
     (i.e., "Lab Code,* "Aluminum") must appear as  they do on  the forms in the
     contract, including the options specified  in the  form (i.e., "Matrix
     (soil/water):" must appear, not just "Matrix").

     All alphabetic entries made onto the forms by  the Contractor must be in
     UPPERCASE letters (i.e., "LOW", not "Low"  or "low"). If  an  entry does not fill
     the entire  blank space provided on the form, null .characters must be used to
     remove the  remaining underscores that comprise the blank  line.  (See Exhibit H
     for  additional instructions.)  However, do not remove  the underscores or
     vertical bar characters that delineate "boxes" on the forms.

     Six pieces  of information are common to the header sections  of each data
     reporting form.  These are:  Lab Name, Contract,  Lab Code, Case No., SAS No.,
     and SDG No.  This information oust be entered  on  every  form  and must match on
     all forms.

     The "Lab Name" must be the name chosen by  the  Contractor  to  identify the
     laboratory.  It may not exceed 25 characters.

     The "Contract" is the number of the EPA contract  under  which the analyses-were
     performed.

     The "Lab Code* is an alphabetic abbreviation of up  to 6 characters, assigned by
     EPA, to identify the laboratory and aid in data processing.   This lab code
     shall be assigned by EPA at the time a contract is  awarded,  and must not be
     modified by the Contractor, except at the  direction of EPA.


                                     B-14                                ILM02.0

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                                                              Exhibit B Section III
The  "Case No." is the EPA-assigned Case number (to 5 spaces) associated with
the  sample, and reported on the Traffic Report.

The  "SAS No." is the EPA-assigned number for analyses performed under Special
Analytical Services.  If samples are to be analyzed under SAS only, and
reported on these forms, then enter SAS No. and leave Case No. blank.  If
samples are analyzed according to this SOW (Routine Analytical Services
protocol) and have additional SAS requirements, list both Case No. and SAS No.
on all forms.  If the analyses have no SAS requirements, leave "SAS No." blank.
(NOTE:  Some samples in an SDG may have a SAS No., while others do not.)

The  "SDG No." is the Sample Delivery Group (SDG) number.  The SDG number is the
EPA  Sample Number of the first sample received in the SDG.  When several
samples are received together in the first SDG shipment,the SDG number must be
the  lowest sample number (considering both alpha and numeric designations) in
the, first group of samples received under the SDG.

The  other information common to several of the forms is the "EPA Sample No.".
This number appears either in the upper righthand corner of the form, or as the
left column of a table summarizing data from a number of samples.  When "EPA
Sample No." is entered into the triple-spaced box in the upper righthand corner
of a form, it must be centered on the middle line of the three lines that
comprise the box.

All samples, matrix spikes and duplicates must be identified with an EPA Sample
Number.  For samples, matrix spikes and duplicates, the EPA Sample Number is
the unique identifying number given in the Traffic Report that accompanied that
sample.

In order to facilitate data assessment, the sample suffixes listed in Table 1
must be used.

Other pieces of information are common to many of the Data Reporting Forms.
These include:  Matrix and Level.

For  "Matrix", enter "SOIL" for soil/sediment samples, and enter "WATER" for
water sample*.  NOTE:  The matrix must be spelled out.  Abbreviations such as
"S" or "W" must not be used.

For  "Level", enter the determination of concentration level.  Enter as "LOW" or
"MED", not "L" or "M".

Note:  All results must be transcribed to Forms II-XIV from the raw data to the
specified number of decimal places that are described in Exhibits B and H.  The
raw data result is to be rounded only when the number of figures in the raw
data result exceeds the maximum number of figures specified for that result
entry for that form.  If there are not enough figures in the raw data result to
enter in the specified space for that result, then zeros must be used for
decimal places to the specified number of reporting decimals for that result
for  a specific form.  The following examples are provided:
                                B-15                                ILM02.0

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                                                                  Exhibit B Section II!
Raw

Data Result
95
95
95
95
95
.99653
.99653
.99653
.996
.9
5
5
5
5
5
.4
.3
.2
.4
.4
Specified Format
(to
(to
(to
(to
(to
four decimal places)
three decimal places)
two decimal places)
four decimal places)
four decimal places)
Correct Entrv on
95
95
96
95
95
.9965
.997
.00
. 9960
. 9000
Form

     For rounding off numbers to the appropriate level of precision,  observe the
     following common rules.  If the figure following those  to be  retained is less
     than 5, drop it (round down).   If the figure is  greater than  5,,  drop it and
     increase the last digit to be retained by 1 (round up).  If the  figure
     following the last digit to be retained equals 5 and there  are no  digits to the
     right of the 5 or all digits to the right of the 5 equal zero, then round up if
     the digit to be retained is odd,  or round down if that  digit  is  even.   See also
     Rounding Rules entry in Glossary (Exhibit G).

     Before evaluating a number for being in control  or out  of control  of a certain
     limit, the number evaluated must be rounded using EPA rounding rules to the
     significance reported for that limit.  For instance,  the control limit for an
     ICV is plus or minus 10% of the true value.  A reported percent:  recovery value
     of 110.4 would be considered in control while a  reported value of  110.6 would
     be considered out of control.   In addition, a calculated value of  110.50 would
     be in control while a calculated value of 110.51 would  be out of control.

B.   Cover Page - Inorganic Analyses Data Package [COVER PAGE-IN]

     This form is used to list all samples analyzed within a Sample Delivery Group,
     and to provide certain analytical information and general comments.   It is also
     the document which is signed by the Laboratory Manager  to authorize and release
     all data and deliverables associated with the SDG.

     Complete the header information according to the instructions in Part A.

     For samples analyzed using this SOW, enter " ILM02.0" for SOW No.

     Enter the EPA Sample No. (including spikes and duplicates)  (to  seven spaces) of
     every sample-analyzed within the SDG.  Spikes must contain  an "S"  suffix and
     duplicates a "D* suffix.  These sample numbers must be  listed on the form in
     ascending alphanumeric order.   Thus, if MAB123 is the lowest (considering both
     alpha and numeric characters)  EPA Sample No. within the SDG,  it would be
     entered in the first EPA Sample No. field.  Samples would be listed below it,
     in ascending sequence - MAB124, MAB125, MAC111.  MAllll, MA1111I), etc.

     A maximum of twenty (20) sample numbers can be entered on this  form.  Submit
     additional Cover Pages, as appropriate, if the total number of samples,
     duplicates, and spikes in the SDG is greater than twenty (20).

     A Lab Sample ID (to ten spaces) may be entered for each EPA Sample No.  If a Lab
     Sample ID is entered, it must be entered identically (for each EPA Sample No.)
     on all associated data.
                                     B-16                                ILM02.0

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                                                                   Exhibit  B  Section  III
     Enter "YES" or "NO" in answer to each of the two questions concerning ICP
     corrections.  Each question must be explicitly answered with a "YES"  or a "NO."
     The third question must be answered with a "YES" or "NO" if the answer to the
     second question is "YES."  It should be left blank if the answer to the second
     question is "NO."

     Under "Comments," enter any statements relevant to the analyses performed under
     the SOG as a whole.

     Each Cover Page must be signed,  in original, by the Laboratory Manager or the
     Manager's designee and .dated,  to authorize the release and verify the contents
     of all data and deliverables associated with an SDG.

C.   Inorganic Analysis Data Sheet (FORM 1-IN]

     This form is used to tabulate and report sample analysis results for  target
     analytes (Exhibit C).

     Complete the header information  according  to the instructions  in Fart A and as
     follows.

     "Date Received"  is the date (formatted MM/DD/YY) of sample receipt at the
     laboratory,  as recorded on the Traffic Report,  i.e.,  the Validated Time of
     Sample Receipt (VTSR).

     "% Solids"  is the percent of solids on a weight/weight basis in the sample as
     determined by drying the sample  as specified in Exhibit D.  Report percent
     solids to one decimal  place (i.e.,  5.3%).   If the percent solids is not
     required because  the sample is fully aqueous or less than 1% solids,  then enter
     "0.0."

     Enter the appropriate  concentration units  (UG/L for water or MG/KG dry weight
     for soil).   Entering "MG/KG" means "mg/Kg  dry weight* on this  form.

     Under the column  labeled "Concentration,"  enter for each analyte either the
     value of tfte result (if the concentration  is greater than or equal to the
     Instrument Detection Limit) or the Instrument Detection Limit for the analyte
     corrected for any dilutions (if  the concentration is less than the ^Instrument
     Detection Limit).   The concentration result must be reported to two significant
     figures  if the result  is less  than 10;  to  -three sigfigures^if; the value is
     greater  than or equal  to 10.

     Under the columns  labeled "C," "Q," and "M," enter result qualifiers  as
     identified below.   If  additional qualifiers are used, their explicit
     definitions must be included on  the Cover  Page in the Comments section.

     FORM I-IN includes fields for  three types  of result qualifiers.   These
     qualifiers  must be completed as  follows:   "   ~

     o   C  (Concentration) qualifier  --  Enter "B"  if the reported value was  obtained
        from a reading that was less than the Contract Required Detection Limit
        (CRDL) but greater than or equal to the Instrument Detection Limit  (IDL).
        If the analyte was analyzed  for but not detected, a  "U" must be entered.


                                     B-17                               ILM02.0

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                                                              Exhibit B Section III
o   Q qualifier --  Specified entries and their meanings are as  follows:

    E  -    The reported value is estimated because of the presence of
            interference.  An explanatory note  oust be included under Comments
            on the Cover Page (if the problem applies to  all  samples) or on the
            specific FORM I-IN (if it is an isolated problem).

    M  -    Duplicate injection precision not met.

    N  -    Spiked sample recovery not within control limits.

    S  -    The reported value was determined by the Method of Standard
            Additions (MSA).

    V  -    Post-digestion spike for Furnace AA analysis  is out of control
            limits (85-115%), while sample absorbance is  less than 50% of spike
            absorbance.   (See Exhibit E.)

    *  -    Duplicate analysis not within control limits.

    +  -    Correlation coefficient for the MSA is less than 0.995.

     Entering "S,"  "W,"  or "+" is mutually exclusive.   No combination of these
     qualifiers can appear in the same field for an analyte.

o   M (Method)  qualifier --  Enter:

     -  "P" for ICP
        "A" for Flame AA
        "F" for Furnace  AA
        "PM" for ICP when Microwave Digestion  is  used
        "AM" for flame AA when Microwave  Digestion is used
        "FM" for Furnace AA when Microwave Digestion  is  used
     -  "CV" for Manual  Cold Vapor AA
        *AV" for Automated  Cold  Vapor AA
        "CA" for Midi-Distillation Spectrophotonetric
        "AS" for Semi-Automated  Spectrophotometrie
        "C" for Manual  Spectrophotometric
        "T" for Titrimetric
        "  " where  no data has been entered
        "NR^_if the analyte is not required to be analyzed.

A brief physical description of the sample, both before  and after  digestion,
	 _^ *.. _ «*_.» ._._B^.B J M __. ^1». A  £f »! .J A £^a* A A.1 .»*•  f^^.^.£^.m*^  K^.J  ^£^,^m+\  ^1 A^£ ^» f\^ ^^_. «i &
oust be reported in the fields for color (before and after), clarity (before
and after), texture and artifacts.  For water samples, report color .and
clarity.  For soil samples, report color, texture and artifacts.

The following descriptive terms are recommended:
                                            "t
      Color         -   red, blue, yellow, green, orange, violet, white,
                       colorless, brown, grey, black
      Clarity       -   clear, cloudy, opaque,.
      Texture       -   fine (powdery), medium {'sand), coarse  (large crystals or
                       rocks)
                                 B-18                                ILM02.0

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                                                                  Exhibit B Section III
     If artifacts are present, enter "YES" in the  artifacts field and describe the
     artifacts in the Comments field.   If artifacts  are not present,  leave this
     field blank.

     Note any significant changes that occur during  sample preparation (i.e.,
     emulsion formation) in the Comments field.  Enter any sample-specific comments
     concerning the analyte results in the Comments  field.

D.   Initial and Continuing Calibration Verification [FORM II(PART 1)-IN]

     This form is used to report analyte recoveries  from calibration  solutions.

     Complete the header information according to  the  instructions in Part A and as
     follows.

     Enter the Initial Calibration Source (12 spaces maximum)  and the Continuing
     Calibration Source (12 spaces maximum).   Enter  "EPA-LV" or "EPA-CI"  to indicate
     EPA EMSL Las Vegas or Cincinnati,  respectively, as the source of EPA standards.
     When additional EPA supplied solutions are prepared in the future, the
     Contractor must use the codes supplied with those solutions for  identification.
     If other sources were used, enter sufficient  information  in the  available 12
     spaces to identify the manufacturer and the solution used.

     Use additional FORMs II(PART 1)-IN if more calibration sources were  used.

     Under "Initial Calibration True,"  enter the value (in ug/L, to one decimal
     place) of the concentration of each analyte in  the Initial Calibration
     Verification Solution.

     Under "Initial Calibration Found," enter the  most recent  value (in-ug/L,  to two
     decimal places), of the concentration of each analyte measured in the Initial
     Calibration Verification Solution.

     Under "Initial Calibration %R," enter the value (to one decimal  place) of the
     percent recovery.computed according to the following equation:

       %R       -      Found(ICV)      x 10Q              (2.1)
                ~      True(ICV)

     Where, True(ICV) is the true concentration of the analyte in the Initial
     Calibration Verification Solution and Found(ICV)  is the found concentration of
     the analyte in the Initial Calibration Verification Solution.

     The values used in equation 2.1 for True(ICV) and Found(ICV) must be exactly
     those reported on this form.

     Under "Continuing Calibration True," enter the  value (in ug/L, to one decimal
     place) of the concentration of each analyte  in the Continuing Calibration
     Verification Solution.

     Under "Continuing Calibration Found," enter  the value (in ug/L,  to two decimal
     places) of the concentration of each analyte measured in the Continuing
     Calibration Verification Solution.


                                     B-19                                ILM02.0

-------
                                                              Exhibit B Section II]
Note that the form contains two "Continuing Calibration Found" columns.  The
column to the left must contain values for the first Continuing Calibration
Verification, and the column to the right must contain values for the second
Continuing Calibration Verification.  The column to the right should be left
blank if no second Continuing Calibration Verification was performed.

If more than one FORM II(PART 1)-IN is required to report multiple Continuing
Calibration Verifications, then the column to the left on the second form must
contain values for the third Continuing Calibration Verification, the column to
the right must contain values for the fourth Continuing Calibration
Verification, and so on.

Under "Continuing Calibration %R," enter the value (to one decimal place) of
the percent recovery computed according to the following equation:

  %R       -      Found(CCV)       x 100              (2.2)
                   True(CCV)

where, True(CCV) is the true concentration of each analyte, and Found(CCV) is
the found concentration of the analyte in the Continuing Calibration
Verification Solution.

The values used in equation 2.2 for True(CCV) and Found(CCV) must be exactly
those reported on this form.

Note that the form contains two "Continuing Calibration %R" columns.  Entries
to these columns must follow the sequence detailed above for entries to the
"Continuing Calibration Found" columns.

Under "M," enter the method used or "NR," as explained in Part C.

If more than one wavelength is used to analyze an analyte, submit additional
FORMs II(PART 1)-IN as appropriate.

The order of reporting ICVs and CCVs for each analyte must follow the temporal
order in which the standards were run starting with the first Form IIA and
moving from the left to the right continuing to the. following Form IIA's as
appropriate.  For instance, the first ICV for all analytes must be reported on
the first Form IIA.  In a run where three CCVs were analyzed, the first CCV
aust be reported in the left CCV column on the first Form IIA and the second
CCV must be reported in the right column of the sane form.  The third CCV must
be reported in the left CCV column of the second Form IIA.  On the second Form
IIA, the ICV column and the right CCV column must be left empty in this
example.  In the previous example, if a second run for an analyte was needed,
the ICV of that run must be reported on a third Form IIA and the CCVs follow in
the same fashion as explained before.  In the case where two wavelengths are
use used for an analyte, all ICV and CCV results of one wavelength from all
runs must be reported before proceeding to report the results of the second
wavelength used.
                                 B-20                                ILM02.0

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                                                                  Exhibit B Section III
E.   CRDL Standard for AA and TCP [FORM II(PART  2)-IN]

     This form is  used to report  analyte recoveries  from analyses of the CRDL
     Standards for AA (CRA)  and 2x the  CRDL Standards  for  ICP  (CRI).

     Complete  the  header  information according to  the  instructions in Part A and as
     follows.

     Enter the AA  CRDL Standard Source  (12  spaces maximum) and the ICP CRDL Standard
     Source (12 spaces maximum),  as explained in Part  D.

     Under "CRDL Standard for AA   True," enter the value (in ug/L, to one decimal
     place) of the concentration  of each analyte in  the CRDL Standard Source
     Solution  that was analyzed.

     Under "CRDL Standard for AA   Found," enter  the  value  (in  ug/L, to two decimal
     places) of the concentration of each analyte measured in  the CRDL Standard
     Solution.

     Under "CRDL Standard for AA   %R,"  enter the value (to one decimal place) of the
     percent recovery computed according to the  following  equation:

       %R   -         Found CRDL Standard  for AA    x  jQO    (2.3)
                       True  CRDL  Standard for AA

     Under "CRDL Standard for ICP  Initial  True,"  enter the value  (to one decimal
     place) of the concentration  of each analyte in  the CRDL Standard Solution that
     was  analyzed  by ICP  for analytical samples  associated with  the SDG.
     Concentration units  are ug/L.

     Under "CRDL Standard for ICP  Initial  Found," enter the value (to two decimal
     places) of the concentration of each analyte  measured in  the CRDL Standard
     Solution  analyzed at the beginning of  each  run.   Concentration units are ug/L.

     Under "CRDL Standard for ICP, Initial  %R,"  enter  the  value  (to one decimal
     place) of the percent recovery computed according to  the  following equation:

       %R   -    CRDL Standard for ICP Initial Found    x iQO       (2.4)
                    CRDL Standard for  ICP  True

     Under "CRDL Standard for ICP  Final Found," .enter the value (in ug/L,, to two
     decimal places) of the concentration of eacK analyte  measured in the CRDL
     Standard  Solution analyzed at the  end  of each run.                 .-  .

     Under "CRDL Standard for ICP  Final %R," enter  the value  (to one decimal place)
     of the percent recovery computed according  to the following equation:

         %R     -       CRDL Standard for ICP Final Found   x ^QO   (2.5) V
                          CRDL Standard for ICP True                 :     :

     All %R values reported in equations 2.3, 2.4, and 2.5 mist  be calculated using
     the exact true and found values reported on this  form.
                                     B-21                                ILM02.0

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                                                                  Exhibit B Section III
     Note that for every initial  solution reported there must be a final one.
     However,  the opposite is  not true.  If a CRDL Standard for ICP  (CRI) was
     required to be analyzed in the middle of a run  (to avoid exceeding the 8-hour
     limit),  it must be  reported  in the  "Final Found" section of this form.

     If more  CRI or CRA  analyses  were  required or analyses were performed using more
     than one wavelength per analyte,  submit additional FORMs II(PART 2)-IN as
     appropriate.

     The order of reporting CRAs  and CRIs for each analyte must follow the temporal
     order in which the  standards were run starting  with the first Form IIB and
     continuing to the following  Form  I IBs as appropriate.  The order of reporting
     CRA and  CRI is independent with respect to each other.  When multiple
     wavelengths are used for  one analyte, all the results of one wavelength must be
     reported before proceeding to the next wavelength.

F.   Blanks [FORM III-IN]

     This form is used to report  analyte concentrations found in the Initial
     Calibration Blank (ICB),  in  Continuing Calibration Blanks (CCB), and in the
     Preparation Blank (PB).

     Complete the header information according to the instructions in Part A and as
     follows.

     Enter "SOIL"  or "WATER" as appropriate as the matrix of the Preparation Blank.
     No abbreviations or other matrix  descriptors may be used.

     According to the matrix specified for the Preparation Blank, enter "UG/L"  (for
     water) or "MG/KG" (for soil) as the Preparation Blank concentration units.

     Under "Initial Calib. Blank, * enter the concentration  (in ug/L, to one decimal
     place) of each analyte in the most  recent Initial Calibration Blank.

     Under the "C" qualifier field, for  any analyte  enter "B" if th« absolute value
     of the analyte concentration is less than the CRDL but greater  than  or equal  to
     the IDL.  Enter "U" if the absolute value of the analyte in the blank is  less
     than the IDL.

     Under "Continuing Calibration Blank 1," enter the concentration (in  ug/L,  to
     one decimal place)  of each analyte  detectedvin  the first required Continuing
     Calibration Blank  (CCB) analyzed  after  the  Initial Calibration  Blank.   Enter
     any appropriate qualifier, as explained for the "Initial Calibration Blank,"  to
     the "C"  qualifier column immediately following  the "Continuing  Calibration
     Blank 1" column.

     If only  one Continuing Calibration Blank was analyzed, then leave the columns
     labeled "2" and "3" blank.  If up to three  CCBs were analyzed,  complete the
     columns  labeled "2" and "3," in accordance  with the  instructions for the
     "Continuing Calibration Blank 1"  column.  If more  than three  Continuing
     Calibration Blanks  were analyzed, then complete additional FORMs III-IN as
     appropriate.
                                     B-22                                ILM02.0

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                                                                   Exhibit B Section III
     Under "Preparation Blank," enter the concentration in ug/L (to three decimal
     places) for a water blank or in mg/Kg (to three decimal places) for a soil
     blank, of each analyte in the Preparation Blank.   Enter any appropriate
     qualifier, as explained for the "Initial Calibration Blank," to the "C"
     qualifier column immediately following the "Preparation Blank" column.

     For all blanks, enter the concentration of each analyte (positive or negative)
     measured above the IDL or below the negative value of the IDL.

     Under "M," enter the method used, as explained in Part C.

     If more than one wavelength is used to analyze an analyte,  submit additional
     FORMs III-IN as appropriate.

     The order of reporting ICBs and CCBs for each analyte oust follow the temporal
     order in which the blanks were run starting with the first Form III and moving
     from left to right and continuing to the following Form Ills as explained in
     Fart D.   When multiple wavelengths are used for the analysis of one analyte,
     all the results of one wavelength must be reported before proceeding to the
     next wavelength.

G.   ICP Interference Check Sample [FORM IV-IN]

     This form is used to report Interference Check Sample (ICS) results for each
     ICP instrument used in Sample Delivery Group analyses.

     Complete the header information according to the  instructions in Part A and as
     follows:

     For "ICP ID Number," enter an identifier that uniquely identifies a specific
     instrument within the Contractor laboratory.  No two ICP instruments within a
     laboratory may have the same ICP ID Number.

     Enter "ICS Source" (12 spaces maximum) as explained in Part D.  For EPA
     solutions, include in the source name a number identifying it (e.g., EPA-LV87).

     Under "True-Sol. A," enter the true concentration (in ug/L, to the nearest
     whole number)  of each analyte present in Solution A.

     Under "True Sol. AB," enter the true concentration (in ug/L, to the nearest
     whole number)  of each analyte present in Solution AB.

     Under "Initial Found Sol.  A," enter the concentration (in ug/L, to the nearest
     whole number)  of each analyte found in the initial analysis of Solution A as
     required in Exhibit E.

     Under "Initial Found Sol.  AB," enter the concentration (in ug/L, to one decimal
     place) of each analyte in the initial analysis of Solution AB as required in
     Exhibit E.

     Under "Initial Found %R," enter the value (ta one decimal place) of the percent
     recovery computed for true solution AB greater than zero according to the
     following equation:


                                     B-23                                ILM02.0

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                                                                  Exhibit B Section III
        %R      -        Initial Found Solution AB   x IQQ         (2.6)
                              True Solution AB

     Leave the field blank if true solution AB equals zero.

     Under "Final Found Sol.  A,"  enter the concentration (in ug/L,  to the nearest
     whole number) of each analyte found in the final analysis of Solution A as
     required in Exhibit E.

     Under "Final Found Sol.  AB," enter the concentration (in ug/L.  to one decimal
     place)  of each analyte found in the final analysis  of Solution AB as required
     in Exhibit E.

     For All Found values of  solutions A and AB,  enter the concentration (positive,
     negative, or zero) of each analyte at each wavelength used for analysis by  ICP.

     Under "Final Found %R,"  enter the .value (to  one  decimal place)  of the percent
     recovery computed according  to the following equation:

        %R      -        Final Found Solution AB     x IQQ         (2.7)
                              True Solution AB

     All %R values reported must  be calculated using  the exact true and found values
     reported on this form.

     Note  that for every initial  solution reported there must be a final one.
     However, the opposite is not true.   If an ICS was required to be analyzed in
     the middle of a run (to  avoid exceeding the  8-hour  limit), it must be reported
     in the."Final Found" section of this form.

     If more ICS analyses were required, submit additional FORMs IV-IN as
     appropriate.

     The order of reporting ICSs  for each analyte must follow the temporal order in
     which the standards were run starting with the first Form IV and continuing to
     the following. Form TVs as appropriate.  When multiple wavelengths are used for
     one analyte, all the results of one wavelength must be reported before
     proceeding to the next wavelength.

H.   Spike Sample Recovery TFORM V(PART I)-INI

     This  form is used to report results for the pre-digest spike.

     Complete the header information according to the instructions in Part A and as
     follows.

     Indicate the appropriate matrix, level and concentration units  (ug/L for water
     and mg/Kg dry weight for soil) as explained in..Farts A and C.

     For "%Solids for Sample," enter the percent solids  (as explained in Part C) for
     the original sample of the EPA Sample Number: reported on the form.   Note that
     this  number must equal the one reported on Form I for that sample.
                                     B-24                                ILM02.0

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                                                                  Exhibit B Section III
     In the "EPA Sample No."  box,  enter the EPA Sample Number  (7 places maximum) of
    ' the sample from which the spike results on this form were obtained.  The number
     must be centered in the  box.

     Under "Control Limit %R," enter "75-125" if the spike added value was greater
     than or equal to one-fourth of the sample result value.   If not, leave the
     field empty.

     Under "Spiked Sample Result (SSR)," enter the measured value  (to four decimal
     places), in appropriate  units, for each relevant analyte  in the matrix spike
     sample.  Enter any appropriate qualifier, as explained in Part C, to the "C"
     qualifier column immediately following the "Spiked  Sample Result (SSR)" column.

     Under "Sample Result (SR),* enter the measured value (to  four decimal places)
     for each required analyte in the sample (reported in the  EPA  Sample No. box) on
     which the matrix spike was performed.  Enter any appropriate  qualifier, as
     explained in Part C, to  the "C" qualifier column immediately  following the
     •Sample Result (SR)" column.

     Under "Spike Added (SA)," enter the value (to two decimal places) for the
     concentration of each analyte added to the sample.  The same  concentration
     units must be used for spiked sample results, unspiked (original sample)
     results, and spike added sample results.  If the "spike added" concentration is
     specified in the contract, the value added and reported oust  be that specific
     concentration in appropriate units, corrected for spiked  sample weight and %
     solids (soils) or spiked sample volume (waters).

     Under "%R," enter the value (to one decimal place)  of the percent recovery for
     all spiked analytes computed according to the following equation:
              %R    -      - (SSR ' — §*2 — x  100                (2.8)
                                   SA

     %R must be  reported, whether it is negative, positive or zero.

     The values  for SSR, SR,  and SA must be exactly those reported on this form.   A
     value  of zero must be  used in calculations for SSR or SR if the analyte value
     is less than^the  IDL.

     Under  "Q,"  enter  "N" if the Spike Recovery  (%R)  is out of the control limits
     (75-125) and the  Spike Added (SA) is greater than or equal to one-fourth of the
     Sample Result (SR) .

     Under  "M,"  enter  the method used (as explained in Part C) or enter "NR" if the
     analyte is  not required in the spike.

     If different samples were used for spike sample analysis of different analytes,
     additional  FORMs  V(PART 1)-IN oust be submitted for each sample as appropriate.

I.   Post Digest Spike Sample Recovery [FORM V(PART> 2)-IN]

     This form is used to report results for the post -digest spike recovery which is
     based  upon the addition of a known quantity of analyte to an aliquot of the
     digested sample.

                                     B-25                                ILM02.0

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                                                             Exhibit B Section  III
Complete the header information according to the instructions in Part A and as
follows.

In the "EPA Sample No." box, enter the EPA Sample Number (7 spaces maximum) of
the sample from which the spike results on this form were obtained.  The number •
must be centered in the box.

The "Control Limit %R" and "Q" fields must be left blank until limits are
established by EPA.  At that time, the Contractor will be informed how to
complete these fields.

Under "Spiked Sample Result (SSR)," enter the measured value (in ug/L, to two
decimal places) for each analyte in the post-digest spike sample,  Enter any
appropriate qualifier, as explained in Part C, to the "C" qualifier column
immediately following the "Spiked Sample Result (SSR)" column.

Under "Sample Result (SR)," enter the measured value (in ug/L, to £wo decimal
places) for the concentration of each analyte in the sample (reported in the
EPA Sample No. box) on which the spike was performed.  Enter any appropriate
qualifier, as explained in Part C, to the "C" qualifier column immediately
following the "Sample Result (SR)" column.

Under "Spike Added (SA)," enter the value (in ug/L, to one decimal place) for
each analyte added to the sample.  The same concentration units must be used
for spiked sample results, unspiked (original sample) results, and spike added
sample results.  If the spike added concentration is specified in the contract,
the value added and reported must be that specific concentration in appropriate
units.

Under "%R," enter the value (to one decimal place-) of the percent recovery for
all spiked analytes computed according to Equation 2.8 in Part H

%R must be reported, whether it is negative, positive or zero.

The values for SSR, SR, and SA must be exactly those reported on this form.  A
value of zero must be substituted for SSR or SR if the analyte value is less
than the IDLT

Under "M," enter the method used as explained in Part C, or enter  *NR" if  the
spike was not required.

If different samples were used for spike sample analysis of different analytes,
additional FORMS V(PART 1)-IN must be submitted.

Duplicates [FORM VI-IN]

The duplicates form is used to report results of duplicate analyses.  Duplicate
analyses are required for % solids values and all  analyte results.

Complete the header information  according to  the  instructions in Part A and as
follows.

Indicate the appropriate matrix,  level  and  concentration units (ug/L for water
and mg/Kg dry weight  for  soil) as explained in Parts A and C.

                                 B-26                                ILM02.0

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                                                              Exhibit B Section III
 For "% Solids for Sample,"  enter the percent solids  (as explained in Part C)
 for the original sample of  the EPA Sample Number reported on the form.  Note
 that this number must equal the one reported on Form I for that sample.

 For "% Solids for Duplicate,"  enter the percent solids (as explained in Part C)
 for the duplicate sample of the EPA Sample Number reported on the form.

 In the "EPA Sample No." box, enter the EPA Sample Number  (7 spaces maximum) of
 the sample from which the duplicate sample results on this form were obtained.
 The number must be centered in the box.

 Under "Control Limit,"  enter the CRDL (in appropriate units, ug/L for water or
 mg/kg dry weight basis  compared to the original sample weight and percent
 solids)  for the analyte if  the sample or duplicate values were less than 5x
 CRDL and greater than or equal to  the CRDL.  If the sample and duplicate values
 were greater than or  equal  to  5x CRDL, leave the field empty.

 Under Sample (S),  enter the original measured value  (to four decimal places)
 for the  concentration of each  analyte in the sample  (reported in the EPA Sample
 No.  box)  on which a Duplicate  analysis was performed.  Concentration units are
 those specified on the  form.   Enter any appropriate qualifier, as explained in
 Part C,  to the  "C"  qualifier column immediately following the "Sample (S)"
 column.

 Under Duplicate (D),  enter  the measured value  (to four decimal places) for
 each analyte in the Duplicate  sample.   Concentration units are those specified
 on the form.   Enter any appropriate qualifier,  as explained in Part C, to the
 "C"  qualifier column  immediately following the "Duplicate (D)* column.

 For solid samples,  the  concentration of the original sample must be computed
 using the weight and  %  solids of the original sample.  The concentration of the
 duplicate sample must be  computed using the weight of the duplicate sample, but
 the % solids  of the original sample.

Under RPD,  enter the  absolute value (to one decimal place) of the Relative
 Percent Difference  for  all  analytes detected above the IDL in either the sample
 or the duplicate, computed  according to the following equation:

                RPD -_il_LJL! x    100        (2.9)
                      (S + D)/2

The  values for  S and  D  must be exactly those reported on this form.  A value of
 zero mist be substituted for S or  D if the analyte concentration is less than
 the  IDL  in either one.   If  the analyte concentration is less than the IDL in
both S and D,  leave the RPD field  empty.

Under "Q," enter "*"  if the duplicate analysis for the analyte is out of
control.   If both sample  and duplicate values are greater than or equal to 5x
CRDL,  then the  RPD  oust be  less  than or equal to 20% to be in control.  If
 either sample or duplicate  values  are less than 5x CRDL, then the absolute
 difference between  the  two  values  must be less than the CRDL to be in control.
 If both values  are  below the CRDL,  then no control limit is applicable.

Under "H,"  enter method used as  explained in Part C.

                                 B-27                                ILM02.0

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                                                                  Exhibit B Section III
K.   Laboratory Control Sample [FORM VII-IN]

     This form is used to report results for the solid and aqueous Laboratory
     Control Samples.

     Complete the header information according to the instructions in Part A and as
     follows.

     For the Solid LCS Source (12 spaces maximum),  enter the appropriate EPA sample
     number if the EPA provided standard was used.   Substitute an appropriate number
     provided by the EPA for LCS solutions prepared in the future.  If other sources
     were used,  identify the source as  explained in Part D.  For the Aqueous LCS
     Source, enter the source name (12 spaces maximum) as explained in Part D.

     Under "Aqueous True," enter the value (in ug/L, Co one decimal place) of the
     concentration of each analyte in the Aqueous LCS Standard Source.

     Under "Aqueous Found," enter the measured concentration (in ug/L, to two
     decimal places) of each analyte found in the Aqueous LCS solution.

     Under "Aqueous %R," enter the value of the percent recovery (to one decimal
     place) computed according to the following equation:

       %R    -     Aqueous LCS Found    x 1QO                   (2.10)
                     Aqueous  LCS  True

     Under "Solid True," enter the value (in mg/Kg, to one decimal place) of the
     concentration of each analyte in the Solid LCS Source.

     Under "Solid Found," enter the measured value  (in mg/Kg, to one  decimal place)
     of each analyte found in the Solid  LCS solution.

     Under "C," enter "B" or "U" or leave empty, to describe the found value of the
     solid LCS as explained in Part C.

     Under "Limits," enter the lower limit  (in mg/Kg, to one decimal  place) in the
     left column,-and the upper limit (in mg/Kg, to one decimal place) in the right
     column, for each analyte in the Solid  LCS Source solution.

     Under "Solid %R," enter the value of the percent recovery (to one decimal
     place) computed .according to the following equation:

       %R    -      Solid LCS Found     x  100                    (2.11)
                      Solid LCS True

     The values for  true and found aqueous  and solid LCSs used in equations 2.10 and
     2.11 must be exactly those reported on this form.   If  the analyte concentration
     is less than the IDL, a value of zero  must be  substituted for the solid  LCS
     found.

     Submit additional FORMs VII-IN as appropriate, if more than one  aqueous  LCS or
     solid LCS was required.                     "
                                      B-28                               ILM02.0

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                                                                  Exhibit B Section III
L.   gtandard Addition Results  [FORM VIII-IN]

     This form is used to  report  the results of samples analyzed using the Method of
     Standard Additions (MSA) for Furnace AA analysis.

     Complete the header information according to the instructions in  Part A.

     Under "EPA Sample No.," enter the EPA Sample Numbers  (7 spaces maximum) of all
     analytical samples analyzed  using the MSA.  This includes reruns  by MSA (if the
     first MSA was out of  control) as explained in Exhibit E.

     Note that only field  samples and duplicates may be reported on this form, thus
     the  EPA Sample Number usually has no suffix or a "D."

     A maximum of 32 samples can  be entered on this form.  If additional samples
     required MSA,  submit  additional FORMs VIZI-IN.  Samples must be listed in
     alphanumeric order per analyte, -continuing to .the_next FORM; VIII-IN if
     applicable.

     Under "An,"  enter the chemical symbol (2 spaces maximum) for each analyte for
     which MSA was  required for each sample listed.  The analytes must be in
     alphabetic listing of the chemical symbols.

     Results  for  different samples for each analyte must be reported sequentially,
     with the analytes ordered according to the alphabetic listing of  their chemical
     symbols.   For  instance, results for As (arsenic) in samples MAA110, MAAlll, and
     MAA112 would be reported in  sequence, followed by the result for  Pb (lead) in
     MAA110 etc.

     Under "0 ADD ABS," enter the measured value in absorbance units (to three
     decimal  places) for the analyte before any addition is performed.

     Under "1 ADD CON," enter the final concentration in ug/L (to two  decimal
     places)  of the analyte (excluding sample contribution) after the  first addition
     to the sample  analyzed by MSA.

     Under "1 ADD,ABS," enter the measured value (in the same units and decimal
     places as "0 ADD  ABS") of the sample solution,spiked with the first addition.

     Under "2 ADD CON," enter the final concentration in ug/L (to two  decimal
     places)  of the analyte (excluding sample contribution) after the/second
     addition to  the sample analyzed by MSA.

     Under "2 ADD ABS," enter the measured value (in the same units and decimal
     places as "0 ADD  ABS") of the sample solution spiked with the second addition.

     Under "3 ADD CON,* enter the final concentration in ug/L (to.two  decimal
     places)  of the analyte (excluding sample contribution) after the  third addition
     to the sample  analyzed by MSA.              '                    '   '   \

     Under "3 ADD ABS,* enter the measured value (in the same units and decimal
     places as "0 ADD  ABS") of the sample solution spiked with the third addition.
                                     B-29                                ILM02.0

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                                                                   Exhibit B Section III
     Note that "0 ADD ABS , " "1 ADD ABS" "2 ADD ABS," and "3 ADD ABS" must have the
     same dilution factor.

     Under "Final Cone.," enter the final analyte concentration (in ug/L, to one
     decimal place) in the sample  as determined by MSA computed according to the
     following formula:

     Final Cone.   -    - (x- intercept)                          (2.12)

     Note that the final concentration of an analyte does not have to equal the
     value for that analyte which is reported on FORM I -IN for that sample.

     Under "r," enter the correlation coefficient (to four decimal places) that is
     obtained for the least squares regression line representing the following
     points (x,y):(0.0, "0 ADD ABS"), ("1 ADD CON," "1 ADD ABS"),  ("2 ADD CON," "2
     ADD ABS"), ("3 ADD CON," "3 ADD ABS").

     Note that the correlation coefficient must be calculated using the ordinary
     least squares linear regression (unweighted) according to the following
     formula:

                            N  £
                   IN I Xj.2  - (  I Xi)2]* [N  I yi2 - ( X yi)2]h


     Under "Q," enter "+" if r is less than 0.995.   If  r is greater than or equal to
     0.995,  then leave the field empty.

M.   ICP Serial Dilutions [FORM IX- IN]

     This form is used to report results for ICP serial dilution.

     Complete 'the header information according to the instructions IB Part A and as
     follows .

     In the "EPA Sample No." box, enter the EPA Sample  Number (7 places maximum) of
     the sample for which serial dilution analysis results on this form were
     obtained.  The number must be centered in the box.

     Under "Initial Sample Result (I)," enter the measured value (in ug/L, to two
     decimal places) for each ICP analyte in the undiluted sample  (for the EPA
     sample number reported on this form).  Enter any appropriate qualifier, as
     explained in Part C, to the "C* qualifier column immediately following the
     "Initial Sample Result (I)" column.

     Note that the Initial Sample Concentration for an analyte does not have to
     equal the value for that analyte reported on FORM I -IN for that sample.  It  is
     the value of the analyte concentration (uncorrected for dilution) that is
     within the linear range of the instrument.
                                     B-30                                ILM02.0

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                                                                  Exhibit B Section III
     Under "Serial Dilution Result (S)",  enter the measured concentration value  (in
     ug/L, to two decimal places) for each ICP analyte in the  diluted sample.  The
     value must be adjusted for that dilution.  Enter any appropriate qualifier,  as
     explained in Part B, to the "C" qualifier column immediately following the
     "Serial Dilution Result (S)n column.

     Note that the Serial Dilution Result (S)  is obtained by multiplying by five the
     instrument measured value (in ug/L)  of the serially diluted sample and that the
     "C" qualifier for the serial dilution must be established based on the serial
     dilution result before correcting it for  the dilution regardless of the value
     reported on the form.
     Under "% Difference," enter the absolute value (to one decimal place)  of the
     percent difference in concentration of required analytes,  between the  original
     sample and the diluted sample (adjusted for dilution) according to the
     following formula:

       % Difference   -         \ l  ' s  \   * 100                 (2.14)
                                   I

     The values for I and S used to calculate % Difference in equation 2.14 must be
     exactly those reported on this form.  A value of zero must be substituted for S
     if the analyte concentration is less than the IDL.   If the analyte
     concentration in (I) is less than the IDL, concentration  leave "% Difference"
     field empty.

     Under "Q," enter "E" if the % Difference is greater than 10% and the original
     sample concentration (reported on FORM I -IN) is greater than 50x the IDL
     reported on FORM X-IN.

     Under "M," enter the method of analysis for each analyte as explained in Part
     C.
N.   Tng^yunent: Detection Limits (Quarterly) [FORM X-IN1

     This form documents the Instrument Detection Limits for each instrument that
     the laboratory used to obtain data for the Sample Delivery Group.  Only the
     instrument and wavelengths used to generate data for the SDG must be included.

     Although the Instrument Detection Limits (IDLs) are determined quarterly (every
     three calendar months) a copy of the quarterly instrument detection limits must
     be included with each SDG data package on FORM(s) X-IN.

     Complete the header information according to the instructions in Part A and as
     follows .

     Enter the date (formatted MM/DD/YY) on which the IDL values were obtained  (or
     became effective) .
                                                 'f  c \

     Enter ICP ID Number, Flame AA ID Number, and Furnace AA ID Number  (12 spaces
     maximum each).  These ID Numbers are used to uniquely  identify each instrument
     that the laboratory uses to do CLP work.

     Enter the Mercury instrument ID number in the  Flame AA ID Number field.

                                     B-31                                ILM02.0

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                                                                  Exhibit B Section II]
     Under "Wavelength,"  enter the wavelength in nanometers (to two decimal places)
     for each analyte for which an Instrument Detection Limit (IDL) has been
     established and is  listed in the  IDL column.  If more than one wavelength  is
     used for an analyte,  use other  FORMs X-IN as appropriate to report the
     Instrument Detection Limit.

     Under "Background,"  enter the type  of background correction used to obtain
     Furnace AA data.  Enter "BS" for  Smith Hieftje, "BD" for Deuterium Arc, or "BZ"
     for Zeeman background correction.

     Contract Required Detection Limits  (in ug/L) as established.in Exhibit C,  must
     appear in the  column headed "CRDL."

     Under "IDL," enter  the Instrument Detection Limit (ug/L, to one decimal place)
     as determined  by the laboratory for each analyte analyzed by the instrument for
     which the ID Number is listed on  this form.    The IDL results must be reported
     to two significant  figures if the result value is less than 10, and to three
     significant figures  if the value  is greater than or equal-to 10.  When
     calculating IDL values, always  round up to the appropriate significant figure.
     This deviation from the EPA rounding rule is necessary to prevent the reporting
     of detected values  for results  that fall in the noise region of the calibration
     curve.

     Under "M," enter the method of  analysis used to determine the instrument
     detection limit for  each wavelength used.  Use appropriate codes as explained
     in Part C.

     Use additional FORMs X-IN if more instruments and wavelengths are used.  Note
     that the date  on this form must not exceed the analysis dates in the SDG data
     package or precede  them by more than three months.

     Use the Comments section to indicate alternative wavelengths and the conditions
     under which they are used.

0.   ICP Interelement Correction Factors (Annually)  [FORM XI(PART 1)-IN]

     This form documents for each ICP  instrument the interelement correction factors
     applied by Che Contractor laboratory to obtain data for the Sample Delivery
     Group.

     Although the correction factors are determined annually  (every  twelve calendar
     months), a copy of the results  of the annual  interelement correction factors
     oust be included with each SDG  data package on  FORM XI (PART  1)-IN.

     Complete the header information according to  instructions  in Part A and as
     follows.

     Enter the ICP ID Number (12 spaces  maximum),  which is a unique number
     designated by the laboratory to identify each ICP instrument used to produce
     data in the SDG package.  If more than one ICP instrument is used, submit
     additional FORMs XI(PART 1)-IN as appropriate.
                                     B-32                                ILM02.0

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                                                                   Exhibit B Section III
     Report the date (formatted as MM/DD/YY) on which these correction factors were
     determined for use.   This date must not exceed the ICP analysis dates in the
     SDG data package or precede them by more than twelve calendar months.

     Under "Wavelength," list the wavelength in nanometers (to two decimal places)
     used for each ICP analyte.  If more than one wavelength is used, submit
     additional FORMs XI(PART 1)-IN as appropriate.

     Under "Al," "Ca," "Fe," "Mg, enter the correction factor (negative,  positive or
     zero, to seven decimal places, 10 spaces maximum) for each ICP analyte.  If
     correction factors for another analyte are applied, use the empty column and
     list the analyte's chemical symbol in the blank two-space header field provided
     for that column.

     If corrections are not applied for an analyte,  a zero must be entered for that
     analyte to indicate that the corrections were determined to be zero.  If
     correction factors are applied for more than one additional analyte, use FORM
     XI(PART 2)-IN.

P.   ^CP Interelement Correction Factors (Annually)  [FORM  XI(PART 2)-IN]

     This form is used if correction factors for analytes other than Al,  Ca, Fe,  Mg,
     and one more analyte of the Contractor's choice,  were applied to the analytes
     analyzed by ICP.  Complete this form as for FORM XI(PART 1)-IN by listing the
     chemical symbol for additional analytes in the  heading of the empty columns  in
     the two-space fields provided.

     Columns of correction factors for additional analytes must be entered left to
     right starting on FORM XI(PART 1)-IN and proceeding to FORM XI(PART 2)-IN,
     according to the alphabetic order of their chemical symbols.  Note that
     correction factors for Al, Ca, Fe, and Mg are all required and are to  be listed
     first (as they appear on FORM XI(PART 1)-IN).

Q.   ICP Linear Ranges (Quarterly) [FORM XII-IN]

     This form documents the quarterly linear range analysis for each ICP instrument
     that the laboratory used to obtain data for the SDG.

     Complete the header information according to the instructions in Part A and as
     follows.

     Enter the ICP ID Number (12 spaces maximum) .which is a unique number
     designated by the Contractor to identify each ICP instrument used to produce
     data for the SDG.  If more than one ICP instrument is used, submit additional
     FORMs XII-IN as appropriate.

     Report the date (formatted as MM/DD/YY) on which these linear ranges were
     determined for use.  This date must not exceed the dates of analysis by ICP in
     the SDG data package and must not precede the,analysis dates by .more than three
     calendar months.

     Under "Integ.. Time (Sec.)," enter the integration time (in seconds to two
     decimal places) used for each measurement taken from the ICP instrument.


                                     B-33                                ILM02.0

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                                                                  Exhibit B Section II]
     Under "Concentration," enter the concentration (in ug/L)  that  is  the upper
     limit of the ICP instrument linear range as  determined in Exhibit E.   Any
     measurement in the  SDG data package at or below this  concentration is  within
     the linear range.   Any measurement above it  is out of the linear  range,  and
     thus, is an estimated value and  must be diluted into  the  linear range.

     Under "M," enter the method of analysis for  each analyte  as  explained  in Part
     C.

     If more instruments or analyte wavelengths are  used,  submit  additional FORMs
     XII-IN as appropriate.

R.   Preparation Log [Form XIII-IN]

     This Form is used to report the  preparation  run log.

     All field samples and all quality control preparations  (including duplicates,
     matrix spikes,  LCSs,  PBs and repreparations) associated with the  SDG must be
     reported on Form XIII.

     Submit one Form XIII per batch,  per method,  if no  more  than  thirty-two
     preparations,  including quality  control preparations, were performed.  If more
     than thirty-two preparations per batch,  per  method, were  performed, then submit
     additional copies of Form XIII as appropriate.  Submit  a  separate Form XIII for
     each batch.

     The order in which  the Preparation Logs are  submitted is  very  Important.  Form
     XIII must be organized by method,  by batch.  Later batches within a method  must
     follow earlier ones.   Each  batch must  start  on a separate Form XIII.

     Complete the header information  according to the instructions  in  Part  A,  and as
     follows:

     For "Method," enter the method of analysis (two characters maximum) for  which
     the preparations listed on  the Form were made.  Use appropriate method codes as
     specified in Fart C.

     Under "EPA Sample No. ," enter the EPA  Sample Number of each  sample in  the SDG,
     and of all other preparations such as  duplicates,  matrix  spikes,  LCSs, PBs, and
     repreparations (all formatted according to Table 1).   All EPA  Sample Numbers
     must be listed in ascending alphanumeric order, continuing to  the next Form
     XIII if applicable.

     Under "Preparation  Date," enter  the date (formatted MM/DD/YY)  on  which each
     sample was prepared for analysis by the method indicated  in  the header section
     of the Form.

     Rote that the date  never changes cm a  single Form  XIII because the form must  be
     submitted per batch.

     Under "Weight," enter the wet weight (in grams, to two decimal places) of each
     soil sample prepared for analysis by the method indicated in the  header  section
     of the Form.   If the sample matrix is  water, then  leave the  field empty.


                                     B-34                               ILM02.0

-------
                                                                  Exhibit B Section III
     Under "Volume," enter the final volume (in mL,  to ..the nearest whole  number)  of
     the preparation for each sample prepared for analysis by the method  indicated
     in the header section of the Form.  This field must have a value for each
     sample listed.

S.   Analysis Run Log [Form XIV-IN]

     This Form is used to report the sample analysis run log.

     A run is defined as the totality of analyses performed by an instrument
     throughout the  sequence initiated by, and including, the first SOW-required
     calibration standard and terminated by, and including, the continuing
     calibration verification and blank following the last SOW-required analytical
     sample.

     All field samples and all quality control analyses (including calibration
     stahdards, ICVs, CCVs, ICBs, CCBs, CRAs, CRIs,  ICSs, LRSs, LCSs, PBs,
     duplicates, serial dilutions, pre-digestionspikes, post-digestion spikes,
     analytical spikes, and each addition analyzed for the method of standard
     addition determination) associated with the SDG must be reported on  Form XIV.
     The run must be continuous and inclusive of all analyses performed on the
     particular instrument during the run.

     Submit one Form XIV per run if no more than thirty-two (32) analyses, including
     instrument calibration, were analyzed in the run.  If more than thirty-two
     analyses were performed in the run, submit additional Forms XIV as appropriate.

     The order in which the Analysis Run Logs are submitted is very important. Form
     XTV must be organized by method, by run. -Later runs within a method must
     follow earlier ones.  Each analytical XUXL must-start-on a separate Form XIV.
     Therefore, instrument calibration must be the first entry on the form for each
     new ran.  In addition, the run is considered to have ended if it is  interrupted
     for any reason, including termination for failing QC parameters.

     Complete the header information according to the instructions in Fart A, and as
     follows:

     For "Instrument ID Number," enter the instrument ID number,  (12 spaces
     maximum), which must be an identifier designated by  the laboratory to uniquely
     identify each instrument used to produce data which  are required to be reported
     in the SDG deliverable.  If more than one instrument  is used, submit additional
     Forms XIV as appropriate.                                         •

     For "Method," enter the method code  (two characters maximum) according to the
     specifications in Part C.

     For "Start Date," enter the date  (formatted MM/DD/YY) on which the analysis run
     was started.

     For "End Date," Enter the date (formatted MM/DD/YY)  on  which the analysis run
     was ended.
                                     B-35                                ILM02.0

-------
                                                              Exhibit B Section III
Under "EPA Sample No.," enter the EPA sample number of each analysis, including
all QC operations applicable to the SDG (formatted according to Table 1).  All
EPA Sample Numbers must be listed in increasing temporal (date and time) order
of analysis, continuing to the next Form XIV for the instrument run if
applicable.  .The analysis date and time of other analyses not associated with
the SDG, but analyzed by the instrument in the reported analytical run, must be
reported.  Those analyses must be identified with the EPA Sample No. of
"ZZZZZZ."

Under "D/F," enter the dilution factor (to two decimal places) by which the
final digestste or distillate needed to be diluted for each analysis to be
performed.  The dilution factor does not include the dilution inherent in the
preparation as specified by -the preparation procedures in Exhibit D.

The dilution factor is required for all entries on Form XIV.

Note that for a particular sample a dilution factor of "1" must be entered if
the digestate or distillate were analyzed without adding any further volume of
dilutant or any other solutions to the "Volume" or an aliquot of the "Volume"
listed on Form XIII for that sample.

For EPA supplied solutions such as ICVs,  ICSs, and LCSs, a dilution factor must
be entered if the supplied solution had to be diluted to a dilution different
from that specified by the instructions provided with the solution.  The
dilution factor reported in such a case must be that which would make the
reported true values on the appropriate  form for the solution equal those that
were supplied with the solution by the EPA.  For instance, ICV-2(0887) has a
true value of 104.0 ug/L at a 20 fold dilution.  If the solution is prepared at
a 40 fold dilution, a dilution factor of "2" must be entered on Form XIV and
the uncorrected instrument-reading is-compared to a true value of 52 ug/L.  In
this example, Form II will have a true value of 104.0 regardless of the
dilution used.  The found value for the ICV must be corrected for the dilution
listed on Form XIV using the following formula:

Found value on Form II  -  Instrument readout in ug/L  x  D/F

Under "Time7" enter the time, (in military format - HHHM), at which each
analysis was performed.  If an auto sampler is' used with equal .analysis time
and intervals between analyses, then only the start time of the run  (the time
of analysis of the first calibration standard) and end time of the run (the
time of analysis of the final CCV or CCB, which ever is later)' need  to be
reported.

Under "% R," enter the percent recovery (to one decimal place) for each Furnace
AA analytical spike analyzed.  If the analytical spike was performed on more
than one analyte, use additional Forms XIV as appropriate.  Leave the "% R"
field empty  if the analysis reported  is not for an analytical spike.   %R must
be recorded  even if the result is not used.

A %R value of "-9999.9" must be entered for the analytical  spike  if either the
sample or analytical results is greater than  the calibration range  of the
instrument.
                                 B-36                                ILM02.0

-------
                                                                  Exhibit B Section III
    . Under "Analytes," enter "X" in the column of the  designated analyte to indicate
     that the analyte value was used from the reported analysis  to report data in
     the SDG.  Leave the column empty for each analyte if the  analysis was not used
     to report the particular analyte.

     Entering "X" appropriately is very important.   The "X"  is used to link the
     samples with their related QC.  It also links the dilution  factor with the
     appropriate result reported on Forms I-IX.   For each analyte result reported on
     any of the Forms I-IX, there must be one, and only one, properly identified
     entry on Form XIV for which an "X" is entered in  the column for that analyte.

T.   Sample Log-In Sheet [Fora DC-1]

      This form is used to document the receipt and inspection of samples and
      containers.  One original of Form DC-1 is required for each sample shipping
      container, e.g., cooler.  If the samples in a single sample shipping container
      must be assigned to more than one Sample Delivery Group, the original Form DC-
      1 shall be placed with the deliverables for the  Sample Delivery Group of the
      lowest Arabic number and a copy of Form DC-1 must be placed with the
      deliverables for the other Sample Delivery"Group(s).  The  copies should be
      identified as "copy(ies)," and the location of the original should be noted on
      the copies.

      Sign and date the airbill (if present).  Examine the shipping container and
      record the presence/absence of custody seals and their condition (i.e.,
      intact, broken) in item 1 on Form DC-1.  Record  the custody seal numbers in
      item 2.

      Open the container, remove the enclosed sample documentation, and record the
      presence/absence, of chain-of-custody record(s),  SMO forms-(i-e-T-Traffic
      Reports, Packing Lists), and airbills or airbill stickers  in items 3-5 on Form
      DC-1.   Specify if there is an airbill present or an airbill sticker in item 5
      on Form DC-1.  Record the airbill or sticker number in item 6.

      Remove the samples from the shipping container(s), examine the samples and the
      sample tags (if present), and record the condition of the  sample bottles
      (i.e.,  intact, broken,  leaking) and presence or  absence  of sample tags in
      items 7 and"8 on Form DC-1.

      Review the sample shipping documents and complete the header information
      described in Part A.  Compare the information recorded on  all the documents
      and samples and mark the appropriate answer in item 9 on Form DC-1.

      If there are no problems observed during receipt, sign and date (include time)
      Form DC-1, the chain-of-custody record, and Traffic Report, and write the
      sample numbers on Form DC-1.  Record the appropriate sample tags and assigned
      laboratory numbers if applicable.  The log-in date should-be recorded at the
      top of Form DC-1 and the date and time of cooler receipt at the laboratory
      should be recorded in items 10 and 11.  Cross out unused columns and spaces.

      If there are problems observed during receipt, contact SMO and document the
      contact as well as resolution of the problem on a CLP Communication Log.
      Following resolution, sign and date the forms ts specified in the preceding
      paragraph and note, where appropriate, the resolution of the problem.

                                     B-37                                ILM02.0

-------
                                                                   Exhibit B Section III
      Record the fraction designation (if appropriate) and the specific area
      designation (e.g., refrigerator number) in the Sample Transfer block located
      in the bottom left corner of Form DC-1.  Sign s.nd date the sample transfer
      block.
U.   ftoyiiment Inventory Sheet (Form DC-2)

      This form is used to record the inventory of the Complete SDG File (CSF)
      documents which are sent to the Region.

      Organize all EPA- CSF documents as described in Exhibit B, Section II and
      Section III.  Assemble the documents in the order specified on Form DC-2 and
      Sections II and III, and stamp each page with the consecutive number.  (Do not
      number the DC-2 form) .  Inventory the CSF by reviewing the document numbers
      and recording page numbers ranges in the column provided on the Form DC-2.  If
      there are no documents for a specific document type, enter an "MA" in the
      empty space.

      Certain laboratory specific documents related to the CSF may not fit into a
      clearly defined category.  The laboratory should review DC* 2 to determine if
      it is most appropriate to place them under No. 29, 30, 31, or 32.  Category 32
      should be used if there is no appropriate previous category.  'These types of
      documents should be described or listed in the blanks under each appropriate
      category.
                                     B-38                                ILM02.0

-------
     SECTION IV .




DATA REPORTING FORMS
                                         ILM02.0

-------

-------
 Lab Name:

 Lab Code:

 30W No.:
               U.S.  EPA - CLP

COVER PAGE - INORGANIC ANALYSES  DATA PACKAGE


                          Contract:  	

                          SAS No.:
Case No.:
SDG No.
               EPA Sample No.
                               Lab  Sample  ID.
Were ICP interelement corrections applied?

Were ICP background corrections applied?
     If yes-were raw data generated before
     application of background corrections?

Comments:
                                                Yes/No

                                                Yes/No

                                                Yes/No
I certify that this data package is in compliance with the terms and
conditions of the contract, both technically and for completeness, for other
than the conditions detailed above.  Release of the data~contairied in this
hardcopy data package and in the computer-readable data submitted on •
diskette has been authorized by the Laboratory Manager or the Manager's
designee, as verified by the following signature.
Signature
Date:
                            Name:

                           Title:
                                COVER PAGE - IN
                                                    ILM02.0

-------
Lab Name:
Lab Code:
                               U.S. EPA - CLP
                         INORGANIC ANALYSIS  DATA  SHEET
               Contract:
                                                            EPA SAMPLE NO.
                                                           r
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):
Level (lov/med):
% Solids:
                           Lab Sample ID:
                           Date Received:
           Concentration Units  (ug/L or mg/kg dry weight):
Color Before:
Color After:
Comments:
1 1
|CAS No. | Analyte
1 1
(7429-90-5 (Aluminum
(7440-36-0 | Antimony
17440-38-2 (Arsenic
17440-39-3 | Barium
17440-41-7 (Beryllium
(7440-43-9 (Cadmium
(7440-70-2 (Calcium
(7440-47-3 (Chromium
17440-48-4 I Cobalt
17440-50-8 1 Copper
17439-89-6 I Iron
17439-92-1 ILead
(7439-95-4 (Magnesium
(7439-96-5 (Manganese
(7439-97-6 (Mercury
17440-02-0 1 Nickel
(7440-09-7 (Potassium
(7782-49-2 (Selenium
17440-22-4 I Silver
17440-23-5 (Sodium
(7440-28-0 (Thallium
(7440-62-2 (Vanadium
17440-66-6 IZinc
I I Cyanide
1 1
Concentration

























C

























Q

























                                                           M
       Clarity Before:
       Clarity After:
                 Texture:
                 Artifacts:
                                  FORM I - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                                     2A
              INITIAL AND  CONTINUING CALIBRATION VERIFICATION
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Initial Calibration Source:
Continuing Calibration Source:
                         Concentration Units: ug/L
1
1
I Analyte
1
| Aluminum_
j Antimony
1 Arsenic
| Barium
j Beryllium
I Cadmium
1 Calcium
| Chromium
1 Cobalt
I Copper
(Iron
[Lead
j Magnesium
(Manganese
| Mercury
(Nickel
j Potassium
j Selenium
1 silver
(Sodium
j Thallium
| Vanadium
1 Zinc 	
I Cyanide
Initial Calibration
True Found %R(1)













.


-






1
1 1





























	


















Continuing Calibration
True Found %R(1) Found %R(1)












































• --

—
— •















































	








	














,



1
M
























(1)   Control Limits: Mercury 80-120; Other Metals 90-110; Cyanide 85-115
                             FORM II (PART 1) - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                                     2B
                        CRDL STANDARD FOR AA AND ICP
Lab Name:

Lab Code:
Case No.:
Contract:

SAS No.:
AA CRDL Standard Source:

ICP CRDL Standard Source:
SDG No.:
                          Concentration Units: ug/L
1
1
1
I Analyte
1
| Aluminum
| Antimony
I Arsenic
1 Barium
j Beryllium
1 Cadmium
j Calcium
j Chromium
1 Cobalt
I Copper
llron
(Lead
j Magnesium
| Manganese
I Mercury
1 Nickel
j Potassium
| Selenium
1 Silver
(Sodium
(Thallium
| Vanadium
IZinc
1
CRDL S
True














, —


-






tandard f o
Found
























                              %R
True
























CRDL Star
Initial
Found





















,
;

idard 1
%R
























for ICP
Final
Found
























                                                %R
                             FORM II  (PART 2) - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                                      3
                                   BLANKS
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.
Preparation Blank Matrix  (soil/water):
Preparation Blank Concentration Units  (ug/L or mg/kg):
1
1
1
1
(Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
j Beryllium
I Cadmium
I Calcium
| Chromium
I Cobalt
I Copper
(Iron
ILead
1 Magnesium
j Manganese
(Mercury
(Nickel
j Potassium
j Selenium
1 Silver
I Sodium
j Thallium
j Vanadium
| Zinc 	
j Cyanide
1
Initial
Calib.
Blank
(ug/L) C












































""




Continuing Calibration
Blank (ug/L)
1 C 2 C 3 C





































"~





























.".

































































~



—



-




Prepa-
ration
Blank C
















r -

17.-' - -,.,-• -




















"~"









M












1












                                 FORM III - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                        ICP INTERFERENCE CHECK SAMPLE
Lab Name:
Lab Code:
ICP ID Number:
Case No.
Contract:
SAS No.:
                   ICS Source:
SDG No.
                          Concentration Units: ug/L
I
1
1
| Analyte
1
| Aluminum
| Antimony
I Arsenic
I Barium
(Beryllium
1 Cadmium
1 Calcium
| Chromium
1 Cobalt
1 Copper
(Iron
(Lead
| Magnesium
| Manganese
(Mercury
(Nickel
1 Potassium
| Selenium
(Silver
1 Sodium
(Thallium
(Vanadium
izinc
1
Tl
Sol.
A

















.






•ue
Sol.
AB
















	







Initial Founc
Sol. Sol.
A AB













































-


                                                %R
Final Found
Sol . Sol .
A AB
















































                                                %R
                                  FORM IV - IN
                                               ILM02.0

-------
Lab Name:
Lab Code:
                               U.S. EPA - CLP
                                      5A
                             SPIKE SAMPLE RECOVERY
               Contract:
                                     EPA SAMPLE NO.
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):
% Solids for Sample:
                              Level (low/med):
            Concentration Units (ug/L or mg/kg dry weight):
1
1
1
| Analyte
1
| Aluminum
| Antimony
1 Arsenic
(Barium
| Beryllium
| Cadmium
1 Calcium
j Chromium
1 Cobalt
| Copper
(Iron
ILead
| Magnesium
| Manganese
1 Mercury
1 Nickel
j Potassium
| Selenium
1 Silver
1 Sodium
| Thallium
j Vanadium
I Zinc
I Cyanide
1
Control
Limit
%R



















•tmf





Spiked Sample
Result (SSR)

























c

























Sample
Result (SR)




















**-




c

























Spike
Added (SA)























•--.. .

%R























-,,•-.

Q

























M

























Comments:
                              FORM V (PART 1) - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                                      5B
                       POST  DIGEST SPIKE SAMPLE RECOVERY
                                     EPA SAMPLE NO.
Lab Name:

Lab Code:
               Contract:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):
                              Level  (low/med):
                          Concentration Units:  ug/L
1
1
1
(Analyte
1
| Aluminum
| Antimony
j Arsenic
1 Barium
I Beryllium
| Cadmium
I Calcium
| Chromium
1 Cobalt
1 Copper
llron
ILead
| Magnesium
| Manganese
1 Mercury
1 Nickel
| Potassium
I Selenium
1 Silver
1 Sodium
| Thallium
| Vanadium
IZinc
I Cyanide
1
Control
Limit
%R



















' -





Spiked Sample
Result (SSR)



















•





c

























Sample
Result (SR)
























••>
c

























Spike
Added (SA)

























%R

























Q

























M

























Comments:
                              FORM V (PART 2) - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                                  DUPLICATES
                                                            EPA SAMPLE NO.
Lab Name:
Lab Code:
               Contract:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):
% Solids for Sample:
                              Level (low/med):
                       % Solids for Duplicate:
           Concentration Units  (ug/L or mg/kg dry weight):
1
1
| Analyte
1
| Aluminum_
|Antimony_
{Arsenic.
j Barium 	
{Beryllium
| Cadmium_
| Calcium
j Chromium
j Cobalt 	
{Copper
jlron
{Lead 	
(Magnesium
{Manganese
{Mercury
(Nickel
j Potassium
(Selenium
(Silver
(Sodium
(Thallium
| Vanadium
(Zinc
j Cyanide
1
Control
Limit


















	
































Sample (S)

























c



















































Duplicate (D)
— — -






















•**"*
'* '
C



















































RPD





















'

f ' ' 	
1


























Q

























M

























                                 FORM VI  - IN
                                              ILM02.0

-------
Lab Name:
Lab Code:
      U.S.  EPA - CLP
            7
LABORATORY CONTROL SAMPLE
	    _       Contract:
                SAS  No.:
Case No.:
SIX? No. :
Solid LCS Source:
Aqueous LCS Source:
1
1
j Analyte
1
| Aluminum
| Antimony
t Arsenic
j Barium
j Beryllium
j Cadmium
1 Calcium
| Chromium
1 Cobalt
1 Copper
llron
(Lead 	
j Magnesium
| Manganese
I Mercury
| Nickel^ 	
j Potassium
j Selenium
1 Silver
(Sodium
| Thallium
j Vanadium
| Zinc 	
1 Cyanide
1
Aqueous (ug/L)
True Found %R



























































	












Sol
True Found


















































                                                     C       Limits
                                               %R
                                  FORM VII - IN
                                          ILM02.0

-------
                               U.S. EPA - CLP
                                      8
                          STANDARD ADDITION RESULTS
Lab Name:

Lab Code:
              Case No.
                              Contract:

                              SAS No.:
                                         SD6 No.
                          Concentration Units:  ug/L
   EPA
 Sample
   No.
An
0 ADD
 ABS
 1 ADD
CON   ABS
 2 ADD
CON   ABS
 3 ADD
CON   ABS
Final
Cone.
Q
                                 FORM VIII - IN
                                                             ILH02.G

-------
Lab Name:
Lab Code:
                               U.S. EPA - CLP
                             ICP SERIAL DILUTIONS
               Contract:
                                                            EPA  SAMPLE NO.
                                                            I'
Case No.:
SAS No.
SDG No.:
Matrix (soil/water):
                              Level (low/med):
                          Concentration Units:  ug/L
1
1
(Analyte
1
(Aluminum
(Antimony
(Arsenic
(Barium
(Beryllium
| Cadmium
1 Calcium
1 Chromium
I Cobalt
1 Copper
llron
(Lead
(Magnesium
| Manganese
1 Mercury
(Nickel
j Potassium
I Selenium
1 Silver
(Sodium
(Thallium -
j Vanadium
(Zinc
t
Initial Sample
Result (I)
























c
























Serial
Dilution
Result (S)
























C
























%
Differ-
ence
























Q
























M
























                                  FORM IX - IN
                                              ILM02.0

-------
                               U.S. EPA - CLP
                                     10
                   INSTRUMENT DETECTION LIMITS (QUARTERLY)
Lab Name:
Lab Code:
Case No.:
ICP ID Number:
Flame AA ID Number:
Furnace AA ID Number:
Contract:
SAS No.:
Date:
SD6 No.
1
1
1
1 Analyte
1
| Aluminum
(Antimony
I Arsenic
I Barium
(Beryllium
I Cadmium
j Calcium
j Chromium
| Cobalt
I Copper
(Iron
(Lead
(Magnesium
(Manganese
(Mercury
Jttickel
j Potassium
| Selenium
(Silver
(Sodium
(Thallium^
(Vanadium
(Zinc
1
Wave-
length
(nm)

-






















Back-
ground
























"
CRDL
(ug/L)
200
60
10
200
5
5
5000
10
50
25
100
3
5000
15
0.2
40
5000
5
10
5000
10
50
20

IDL
(ug/L)
























M
























Comments:
                                   FORM X -  IN
                           ILM02.0

-------
                               U.S. EPA - CLP
                                     11A
               ICP INTERELEMENT CORRECTION FACTORS  (ANNUALLY)
Lab Name:

Lab Code:
Case No.
ICP ID Number:
Contract:

SAS No.:

Date:
SDG No.
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
1 Barium
| Beryllium
1 Cadmium
I Calcium
| Chromium
I Cobalt
1 Copper
llron
ILead
(Magnesium
| Manganese
(Mercury
1 Nickel
| Potassium
| Selenium
1 Silver
1 Sodium
| Thallium
| Vanadium
(Zinc
1
Wave-
length
(nm)
























Ir
Al
























iter element
Ca
























Correction
Fe






















....

Factors for
Mg
























* •
























comments:
                              FORM XI (PART 1) - IN
                                               ILM02.0

-------
                               U.S. EPA - CLP

                                     11B
               ICP INTERELEMENT CORRECTION FACTORS  (ANNUALLY)
Lab Name:

Lab Code:
Case No.
ICP ID Number:
Contract:

SAS No.:

Date:
SDG No.
1
1
1
(Analyte
1
| Aluminum
| Antimony
j Arsenic
1 Barium
j Beryllium
1 Cadmium
1 Calcium
| Chromium
1 Cobalt
| Copper
llron
[Lead
(Magnesium
| Manganese
(Mercury
1 Nickel
j Potassium
| Selenium
1 Silver
1 Sodium
(Thallium
j Vanadium
IZinc
1
Wave-
length
(nm)


















•<«•*






























Ii
























iter element
























Correction
























Factors foi
























<• •
























Comments:
                              FORM XI (PART 2)  - IN
                                              ILM02.0

-------
                               U.S. EPA  - CLP
                                      12
                        ICP LINEAR RANGES (QUARTERLY)
Lab Name:

Lab Code:
ICP ID Number:
Case No.:
Contract:

SAS No.:

Date:
SDG No.:
1
1
1
I Analyte
1
| Aluminum
| Antimony
j Arsenic
I Barium
| Beryllium
I Cadmium
I Calcium
j Chromium
| Cobalt
1 Copper
llron
ILead
(Magnesium
| Manganese
(Mercury
(Nickel
j Potassium
| Selenium
(Silver
1 Sodium
(Thallium
j Vanadium
(Zinc
I
Integ.
Time
(Sec.)
























Concentration
(ug/L)
























M
























Comments:
                                  FORM XII - IN
                                              ILM02.0

-------
                                 U.S. EPA - CLP
                                        13
                                 PREPARATION LOG
Lab Name:

Lab Code:

Method:
Case No.:
Contract:

 SAS No.:
 SDG No.
                EPA
               Sample
                No.
       Preparation
           Date
      Weight
      (gram)
Volume
 (mL)
                                  FORM XIII - IN
                                                   ILM02.G

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   U.S. EPA - CLP




          14




   ANALYSIS RUN LOG
Lab Name:
Lab Code: Case No.:
Instrument ID Number:
Start Date:
Contract :
SAS No.:
Method:
End Date:
                                  SDG No.:
EPA
Sample
No.

































D/F

















'















Tine

















-




	









% R

































Analytes |
A|
L|

































S|
B|

































A|
S|

































B|
A|

































B
E|

































C|
D|

































C|
A|

































C|
R|

































C|
0|

































C|
U|





















.











F|
E|

































PI
B|

































M|
Gl

































M|
N|

































H|
G|














.


















N
I





















ii











K|

































S|
E

































A|
G'

































N|
A|

































T|
L|

































V|
1

































Z
N|































C|
N!







,,











i
i


i





1


FORM XIV - IN
ILM02.0-

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                                  SAMPLE LOG-IN SHEET
Lao Name
Receiveo By (Pnm Name)
Page . ._ . . .. . ot 	
Log- m Date
Received By {Signature)
Case Number
Remarks
v Custody Seal(s)
2 Custody Seal Nos.
3 Chain-ot-Custody
Records
Sample Delivery Group No SAS Number
Present/Absent'
Intact/Broken
Present/ Absent*
4 Traffic Reports or Packing Present/Absent*
Lists
5 Airoill
6 Airbill No
7 Sample Tags
Sample Tag Numbers
a Sample Condition:
Airbill/Sticker
P'esenv Absent'


Present/ Absent'
listed/Not Listed
on Chain-of-Cu$tody
Intact/Broken '/Leaking
9 Does information on Yes/No*
custody records, traffic
reports, and sample tags
agree'
10 Date Received al Lab.
n. Tune Received


Sample Transfer
fraction
Area*
By
On
Fraction
Area*
By
On
EPA
Sample*


















Corresponding
Sample
Tag*


















Assigned
Lab*


















Remarks.
Condition of Sample Shipment, etc


















* Contact SMO and attacfi record ot resolution.
Received By
Date
Logbook No
Logbook Page No.
                                       FORM DC-1
ILM02.0

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                               FULL INORGANICS
                           COMPLETE SDG FILE (CSF)
                               INVENTORY SHEET

Lab Name:	City /State:

Case No. 	  SDG No. 	  SDG Nos. to Follow:

SAS No. 	  Contract No. 	  SOW No. 	

All documents delivered in the Complete SDG File must be original documents
where possible.  (Reference Exhibit B, Section II D and Section III V)
                                                 Page Nos.    (Please Check:)
                                                From    To      Lab   Region
1.   Inventory Sheet (DC-2) (Do not number)
2.   Cover Page
3.   Inorganic Analysis
     Data Sheet (Form I-IN)
4.   Initial & Continuing Calibration
     Verification  (Form IIA-IN)
5.   CRDL Standards For AA and ICP
      (Form IIB-IN)
6.   Blanks  (Form III-IN)
7.   ICP Interference Check
     Sample  (Form IV-IN)
8.   Spike Sample Recovery  (Form VA-IN)
9.   Post Digest Spike
     Sample Recovery (Form VB-IN)
10.  Duplicates  (Form VI-IN)
11.  Laboratory Control Sample
      (Form VII-IN)
12.  Standard Addition Results
     (Form VIT1-IN)
13.  ICP Serial Dilutions  (Form IX-IN)
14.  Instrument Detection Limits
     (Form X-IN)
15.  ICP Interelement Correction Factors
     (Form XIA-IN)
16.  ICP Interelement Correction Factors
     (Form XIB-IN)
17.  ICP Linear Ranges (Form XII-IN)
18.  Preparation Log  (Form XIII-IN)
19.  Analysis Run Log (Form XIV-IN)
20.  ICP Raw Data
21.  Furnace AA Raw Data
22.  Mercury Raw Data
                                  Form DC-2                           ILM02.0

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                                                 Page Nos.
23.
24.
25.
26.
27.
28.
29.
30.
31.
                                                From     To      Lab
                                                          (Please Check:)
                                                                  Region
 Cyanide Raw Data
 Preparation Logs Raw Data
 Percent Solids Determination Log
 Traffic Report
 EPA Shipping/Receiving Documents
    Airbill  (No, of Shipments 	)
    Chain-of-Custody Records
    Sample Tags
    Sample Log-In Sheet (Lab & DC1)
    SDG Cover Sheet
 Misc. Shipping/Receiving Records
 (list all individual records)
    Telephone Logs
.Internal Lab Sample Transfer Records &
 Tracking Sheets (describe or list)
 Internal Original Sample Prep & Analysis Records
 (describe or list)
    Prep Records 	           	
    Analysis Records 	         	
    Description	          	
 Other Records (describe or list)
    Telephone Communication Log
32.  Comments:
Completed by (CLP Lab):

          (Signature)

Audited by (EPA):

          (Signature)
                                  (Print Name & Title)
                                  (Print Name & Title)
(Date)
(Date)
                            Form DC-2 (continued)
                                                                  ILM02.0

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          EXHIBIT C
INORGANIC TARGET ANALYTE LIST
                                               ILM02.0

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                        INORGANIC TARGET ANALYTE LIST (TAL)
          Analyte
Contract Required
  Detection Limit (1>Z)
      (ug/L)
          Aluminum
          Antimony
          Arsenic
          Barium
          Beryllium
          Cadmium
          Calcium
          Chromium
          Cobalt
          Copper
          Iron
          Lead
          Magnesium
          Manganese
          Mercury
          Nickel
          Potassium
          Selenium
          Silver
          Sodium
          Thallium
          Vanadium
          Zinc
          Cyanide
        200
         60
         10
        200
          5
          5
       5000
         10
         50
         25
        100
          3
       5000
         15
          0.2
         40
       5000
          5
         10
       5000
         10
         50
         20
         10
(1)  Subj«et to  the  restrictions  specified in the  first page of Part G,
     Section IV  of Exhibit D (Alternate Methods  -  Catastrophic Failure) any
     analytical  method specified  in SOU Exhibit  D  may be utilised as long as
     the documented  instrument or method detection limits meet the Contract
     Required Detection Limit (CRDL) requirements.   Higher detection limits
     may only be used in the following circumstance:

              If  the  sample  concentration exceeds five times the detection
              limit of the  instrument  or method in use, the value may be
              reported even  though  the  instrument or method detection limit
              may not equal  the  Contract Required Detection Limit.  This is
              illustrated in the example below:

              For lead:

              Method  in use  - ICP
              Instrument  Detection  Limit  (IDL) - 40
              Sample  concentration  - 220
              Contract Required  Detection Limit (CRDL) - 3
                                   C-l
                           ILM02.0

-------
              The value of 220 may be reported even though the instrument
              detection limit is greater than CRDL. The instrument or
              method detection limit must be documented as described in
              Exhibits B and E.

(2)  The CRDLs  are  the  instrument detection limits  obtained in pure water
     that must  be met using the procedure in Exhibit E.  The  detection
     limits for samples may be considerably higher  depending  on  the sample
     matrix.
                                    C-2                                 ILM02.0

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                                 EXHIBIT D
                             ANALYTICAL METHODS
                                                                       No.
SECTION I   - INTRODUCTION   ......................................   D-l
  Figure 1- Inorganic Methods Flow Chart   .........................   D-3
SECTION II  - SAMPLE PRESERVATION AND HOLDING TIMES   .............   D-4
  Part A - Sample .Preservation   ............................ '. ..... .  D-4
  Part B - Holding Times   ............ -. ...........................   D-4
SECTION III - SAMPLE PREPARATION   . . . .' ............................   D-5
  Part A - Water Sample Preparation    .............................   D-5
  Part B - Soil/Sediment Sample Preparation   .....................   D-5
  Part C - Microwave Digestion Method   ...........................   D-8
  Part D - Mercury and Cyanide Preparation   .....................  D-14
SECTION IV  - SAMPLE ANALYSIS   ..................................  D-15
  Part A - Inductively Coupled Plasma-Atomic
        Emission Spectrometric Method   ..........................  D-16
  Part B - Atomic Absorption Methods, Furnace Technique   ........  D-28
  Part C - Atomic Absorption Methods, Flame Technique   ..........  D-40
  Part D - Cold Vapor Methods for Mercury Analysis   .............  D-45
  Part E - Methods for Total Cyanide Analysis   ..................  D-62
  Part F - Percent Solids Determination Procedure   ..............  D-89
  Part G - Alternate Methods (Catastrophic. ICP Failure)   ........  D-90
                                                                       ILM02.0

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                                                                     Exhibit D  Section I
                                      SECTION I

                                    INTRODUCTION


Inorganic Methods Flow Chart:  Figure I outlines the general analytical scheme the
Contractor will follow in performing analyses under this contract.

Permitted Methods:  Subject to the restrictions specified in Section IV, Part G -
Alternate Methods (Catastrophic ICP Failure), any analytical method specified in
Exhibit D may be used as long as the documented instrument or method detection
limits meet the Contract Required Detection Limits (Exhibit C). Analytical methods
with higher detection limits may be used only if the sample concentration exceeds
five times the documented detection limit of the instrument or method.

Initial Run Undiluted:  All samples must initially be run undiluted (i.e., final
product of the sample preparation procedure).  When an analyte concentration exceeds
the calibrated or linear range (as appropriate), re-analysis for that analyte(s) is
required after appropriate dilution.  The Contractor must use-the least-dilution
necessary to bring the analyte(s) within the valid analytical range (but not below
the CRDL) and report the highest valid value for each analyte as measured from the
undiluted and diluted analyses.  Unless the Contractor can submit proofthat dilution
was required to obtain valid results, both diluted and undiluted sample measurements
must be contained in the raw data.  ICP data showing a high concentration for a..
particular analyte, combined with an analyte result that is close to the middle
range of the calibration curve in the diluted sample, constitute sufficient proof
that the sample had to initially be run diluted for that analyte on a furnace AA
instrument.  All sample dilutions shall be made with deionized water appropriately
acidified to maintain constant acid strength.

Quality Assurance/Quality Control Measurements:  The Contractor is reminded and
cautioned that Exhibit D is a compendium of required and/or permitted analytical
methods to be used in the performance of analyses under this contract.  The quality
assurance/quality control procedures or measurements to be performed in association
with these methods or analyses are specified in Exhibit E.  In the event references
to quality assurance measurements in any of the methods appear to be in conflict
with or to be less stringent than the requirements of Exhibit E, the requirements of
Exhibit E will prevail.

Raw Data Requirements:  The Contractor is reminded and cautioned that the collection
and provision of raw data may or may not be referred to within the individual
methods of Exhibit D or the Quality Assurance Protocol of Exhibit E.  The Raw Data
Deliverables requirements are specified in Exhibit B, Section II.D.2.d.  Raw data
collected and provided in association with the performance of analyses under this
contract shall conform to the appropriate provisions of Exhibit B.

Glassware Cleaning:  Lab glassware to be used in metals analysis must be acid
cleaned according to EPA's manual "Methods for Chemical Analysis of Water and
Wastes* or an equivalent procedure.

Standard Stock Solutions:  Stock solutions to be used for preparing instrument or
method calibration standards may be purchased or prepared as  described  in the
individual methods of Exhibit D.  All other  solutions to be used for Quality
Assurance/Quality Control measurements shall conform to the specific requirements of
Exhibit E.
                                      D-l                                ILM02.0

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                                                                     Exhibit D Section
Aqueous Sample pH Measurement:  Before sample preparation is initiated on an aqueous
sample received in shipment, the Contractor must check the pH of the sample and note
in a preparation log if the pH is <2 for a metals sample or if the pH is >12 for a
cyanide sample.  The Contractor shall not perform any pH adjustment action if the
sample has not been properly preserved.  If the sample has not been preserved,
contact SMO before proceeding with the preparation and analysis for further
instructions.

Sample Mixing:  Unless instructed otherwise by the EPA Administrative Project
Officer or Technical Project Officer, all samples shall be mixed thoroughly prior to
aliquoting for digestion.  No specific procedure is provided herein, for	
homogenization of soil/sediment samples; however, an effort should be made to obtain
a representative aliquot.

Background Corrections:  Background corrections are required for Flame AA
measurements below 350 nm and for all Furnace AA measurements.  For ICP background
correction requirements, see Exhibit D Section IV, Part A, paragraph 2.1.

Replicate In1 ections/Exposures:  Each furnace analysis requires a minimum of two
injection (burns), except for full method of standard addition (MSA).  All ICP
measurements shall require a minimum of two replicate-, exposures.  Appropriate hard
copy raw data for each exposure/injection shall be included in the data package in
accordance with Exhibit B, Section II, Part D, paragraph 2.d.  The average of each
set of exposures/injections shall be used for standardization, sample analysis, and
reporting as specified in Exhibit D.
                                      D-2                                ILM02.0

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          Figure 1

INORGANICS METHODS FLOW CHART
    Field Sample

         j
         I
         I
    	I	
Traffic Report or SMO
 Specifies Parameters.
 I
I
Water
Matrix
Soil/Sediment
Matrix

Cyanide | |Acid Digestion)
Analysis j j for Metals |
in Water j j Analysis j
| | in Water |
1
1
1
| Metal Anal.)
| ICP/AAS |
1
" 1
\
1
1
1
1
jAcid Digestion) |% Solids | (Cyanide |
j for Metals j JDetermin-j j Analysis!
(Analysis in ( ( ation | (in Soil/|
(Soil/Sediment | | | (Sediment)
1
(Metals Anal.)
| ICP/AAS |

1
1 1
1 Data Reports I
1
1
1
1
1
1
1
1
1
1
            D-3
                               ILM02.0

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                                                                   Exhibit D Section II
                                     SECTION  II

                        SAMPLE PRESERVATION AND HOLDING TIMES
A.   SAMPLE PRESERVATION

     1.    Water Sample Preservation

          Measurement
                           Container'  '     Preservative'  '
         Metals              P.G          HN03 to pH <2

         Cyanide,  total      P,G          0.6g ascorbic acid(3)
            and amenable                   NaOH to pH >12
            to  chlorination                Cool, maintain at 4°C(±2°C)
                                           until analysis

         FOOTNOTES:

         (1)   Polyethylene (P) or glass (G).
         (2)   Sample preservation is performed by the sampler, immediately upon
               sample collection.
         (3)   Only used in the presence of residual chlorine.

     2.   Soil/Sediment Sample Preservation

         The preservation required for soil/sediment samples  is maintenance at  4°C
         (± 2°)  until  analysis.


B.   HOLDING TIMES FOR, WATER  AND SOIL/SEDIMENT SAMPLES

     Following  are the maximum sample holding times  allowable under this contract.
     To be  compliant with this contract,  the Contractor must analyze samples within
     these  times  even if these times  are  less than the  maximum data submission times
     allowed in_this contract.

                                       No.  of Days  Following
            Analvte                        Sample Receipt
                                            bv Contractor

         Mercury                           .  *  26 days
         Metals  (other than  mercury)      '   180 days
         Cyanide                                12  days
                                      D-4                                 ILM02.0

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                                                                   Exhibit  D  Section III
                                     SECTION III

                                 SAMPLE PREPARATION


A.   WATER SAMPLE PREPARATION

     1.    Acid Digestion Procedure  for Furnace Atomic Absorption Analysis

          Shake sample  and transfer 100 mL of well-mixed sample to a 250-mL beaker,
          add 1 mL of (1+1) HN03  and 2 mL 30% ^2^2 to the sample.  Cover with watch
          glass or similar cover  and heat on a steam bath or hot plate  for 2 hours
          at 95°C or until sample volume is reduced to between 25 and 50 mL, making
          certain sample does  not boil.   Cool sample and filter to remove insoluble
          material.   (NOTE: In place of filtering,  the sample, after dilution and
          mixing,  may be centrifuged or allowed to settle by gravity overnight to
          remove insoluble material.) Adjust sample volume to 100 mL with deionized
          distilled water.  The sample is now ready-for  analysis.-

          Concentrations so determined shall be reported as "total."

          If Sb is to be determined by furnace AA,  use the digestate prepared for
          ICP/flame  AA  analysis.

     2.    Acid Digestion Procedure  for ICP and Flame AA  Analyses

          Shake sample  and transfer 100 mL of well-mixed sample to a 250-mL beaker,
          add 2 mL of (1+1) HN03  and 10 mL of (1+1) HC1  to the sample.  Cover with
          watch glass or similar  cover and heat on a steam bath or hot  plate for 2
          hours at 95°C or until  sample volume is reduced to- between 25 and 50 mL,
          making certain sample does not boil. Cool sample and filter  to remove
          insoluble material.   (NOTE: In place of filtering, the sample, after
          dilution and  mixing, may  be centrifuged or allowed to settle  by gravity
          overnight to  remove  insoluble material.) Adjust sample volume to 100 mL
          with deionized distilled  water.   The sample is now ready for  analysis.

          Concentrations so determined shall be reported as "total."

B.   SOIL/SEDIMENT SAMPLE PREPARATION

     1.    Acid Digestion Procedure  for ICP, Flame AA and Furnace AA Analyses

          a.   Scope and Application

               This  method is  an  acid digestion procedure used to prepare sediments,
               sludges,  and soil  samples for analysis by flame or furnace atomic
               absorption spectroscopy (AAS) or by inductively coupled  plasma
               spectroscopy (ICP).   Samples prepared by  this method may be analyzed
               by AAS or ICP for  the following metals:
                                      D-5                                ILM02.0

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                                                         Exhibit D Section III
        Aluminum        Chromium       Potassium
        Antimony        Cobalt         Selenium
        Arsenic         Copper         Silver
        Barium          Iron           Sodium
        Beryllium       Lead           Thallium
        Cadmium         Magnesium      Vanadium
        Calcium         Manganese      Zinc
                        Nickel

b.   Summary of Method

     A representative 1 g (wet weight) sample is  digested in nitric acid
     and hydrogen peroxide.  The digestate is then refluxed with either
     nitric acid or hydrochloric acid.  Hydrochloric acid is used as the
     final reflux acid for the furnace AA analysis of Sb, the Flame AA or
     ICP analysis of Al, Sb, Ba, Be, Ca,  Cd,  Cr,  Co, Cu, Fe, Pb, Mg, Mn,
     Ni, K, Ag, Na, Tl, V and Zn.  Nitric acid is employed as the final
     reflux acid for the Furnace AA analysis  of As, Be; Cd,, Cr, Co, Cu,
     Fe, Pb, Mn, Ni, Se, Ag, Tl, V, and Zn.   A separate sample shall be
     dried for a percent solids determination (Section IV,Part F).

c.   Apparatus and Materials

     (1)  250 mL beaker or other appropriate  vessel

     (2)  Watch glasses

     (3)  Thermometer that covers range of 0° to  200°C

     (4)  Whatman No. 42 .filter_p*per.pr  equivalent

d.   Reagents

     (1)  ASTM.Type II water (ASTM D1193):  Water must be monitored.

     (2)  Concentrated nitric acid (sp. gr. 1.41)

     (3)  Concentrated hydrochloric acid (sp. gr.  1.19)

     (4)  Hydrogen Peroxide (30%)

e.   Sample Preservation and Handling

     Soil/sediment (nonaqueous) samples must  be refrigeraced at 4°C (±2°)
     from receipt until analysis.
                            D-6                                 ILM02.0

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                                                         Exhibit D Section III
f .    Procedure

     (1)   Mix the  sample  thoroughly  to achieve homogeneity.  For each
          digestion procedure,  weigh (to th« nearest O.Olg) a 1.0 to 1.5 g
          portion  of sample  and transfer to a beaker.

     (2)   Add 10 mL of  1:1 nitric acid (HNO:i) , mix the slurry, and cover
          with a  watch glass.   Heat the sample  to 95°C and reflux for 10
          minutes  without boiling.   Allow the sample to cool, add 5 mL of
          concentrated  HN03, replace the watch glass, and reflux for 30
          minutes.   Do  not allow the volume to be reduced to less than 5
          mL while maintaining  a covering of solution over the bottom of
          the beaker.

     (3)   After the second reflux step has been  completed and the sample
          has cooled, add 2 mL  of Type II water  and 3 mL of 30% hydrogen
          peroxide (H2<>2).  Return the beaker to the hot-plate for warming
          to start the  peroxide reaction.  Care, must be taken to ensure
          that losses do  not  occur  due to excessively vigorous
          effervescence.  Heat  until effervescence subsides, and cool the
          beaker .

     (4)   Continue to add 30% H^ in 1 mL aliquots with warming until the
          effervescence is minimal or until the  general sample appearance
          is  unchanged.  (NOTE:  Do not add more than a total of 10 mL
          30%
     (5a)  If the  sample  is being prepared for the furnace AA analysis  of
          Sb, the flame AA or ICP analysis of Al,  Sb, Ba,  Be, Ca, Cd;  Cr,
          Co, Cu,  Fe, Pb, Mg, Hn, -KI-, K, Ag, Na,  Tl, V,  and Zn, add 5 mL
          of 1:1 HC1 and 10 mL of Type 11 water,  return the  covered beaker
          to the hot plate, and heat for an additional 10 minutes.  After
          cooling, filter through Whatman No. 42  filter paper (or
          equivalent) and dilute  to 100 mL with Type 11 water.  NOTE:  In
          place of filtering, the sample (after dilution  and mixing) may
          be centrifuged or allowed to settle by  gravity  overnight to
     _   .remove insoluble material.  The diluted sample  has an
          approximate acid concentration of 2.5%  (v/v) HC1 and 5% (v/v)
          HN03-  Dilute the digestate 1:1 (200 mL final volume) with
          acidified water to maintain constant acid strength.  The sample
          is now ready for analysis.

     (5b)  If the  sample  is being ptepared for the furnace analysis of  As,
          Be, Cd, Cr, Co, Cu, Fe, Pb, Mn, NL, Se,  Ag, Tl,  V, and Zn,
          continue heating the acid-peroxide  digestate until the volume
          has been reduced to approximately 2 mL,  add 10  mL  of Type II
         water, and warm the mixture.  After cooling, filter through
          Whatman No. 42 filter paper (or equivalent) and dilute the
          sample to 100 mL with Type II water  (or centrifuge the sample) .
          NOTE:  In place of filtering, the sample (after dilution and
                            D-7                                ILM02.0

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                                                                  Exhibit D Section I
                   mixing) may be centrifuged or allowed to settle by gravity
                   overnight to remove insoluble material.  The diluted digestate
                   solution contains approximately 2% (v/v) HN03.  Dilute the
                   digestate 1:1 (200 mL final  volume) with acidified water to
                   maintain constant acid strength.  For  analysis, withdraw
                   aliquots of appropriate volume, and add any required reagent or
                   matrix modifier.  The sample is now ready for analysis.

          g.   Calculations

              (1)  A separate determination of percent solids must be performed
                   (Section IV, Part F).

              (2)  The concentrations determined in the digest are to be reported
                   on the basis of the dry weight of the sample.

                        Concentration (dry wt.)  (mg/kg)  -  C x V
                                                           V x S

                        Where,
                          C —  Concentration  (mg/L)
                          V -  Final volume in liters after sample
                               preparation
                          V -  Weight in  kg of wet sample
                          S -  % Solids/100

C.    TOTAL METALS  SAMPLE PREPARATION USING MICROWAVE  DIGESTION

1.     SCOPE AND  APPLICATION

      This method is  an acid digestion procedure using microwave energy to prepare
      water and soil  samples for analysis by GFAA, ICP,  or Flame AA for the
      following metals:
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium

Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc

                         *NOTE: This microwave digestion method is not appropriate
                         for the quantitative recovery of Antimony from soil  and
                         sediment samples.

-------
                                                                   Exhibit D Section III
 2.     SUMMARY OF METHOD

       a.       Water Sample Preparation
               A representative 45 mL water sairple is digested in 5 mL of
               concentrated nitric acid in a TeflonR PFA vessel for 20 minutes using
               microwave heating.  The digestate is then filtered to remove
               insoluble material.  The sample may be centrifuged or allowed to
               settle by gravity overnight to remove insoluble material.

       b.       Soil ??Bffpli*>' Preparation
               A representative 0.5 g (wet weight)  sample is digested in 10 mL of
               concentrated nitric acid in a TeflonR PFA vessel for 10 minutes using
               microwave heating.  The digestate is then filtered to remove
               insoluble material.  The sample may be centrifuged or allowed to
               settle by gravity overnight to remove insoluble material.   NOTE: This
               microwave digestion method is not appropriate for the quantitative
               recovery of Antimony from soil and sediment samples.

3.    APPARATUS AND MATERIALS

      a.       Commercial kitchen or home-use microwave  ovens shall  not be used for
               the digestion of samples under this contract.   The oven cavity must
               be corrosion resistant and-well ventilated.   All electronics must be
               protected against corrosion for safe operation.

      b.       Microwave oven with programmable power settings up to at least 600
               Watts.

      c.       The system must  use PFA TeflonR digestion vessels (120 mL  capacity)
               capable of withstanding pressures of up to 110 ±10 psi (7.5 ±0.7
               atm).   These vessels are capable of controlled pressure relief at
               pressures exceeding 110 psi.
      d.       A rotating turntable must be used to ensure homogeneous distribution
               of microwave radiation within the oven.   The speed of the  turntable
               must be a. minimum of 3 rpm.
                                                           n
      e.      -Polymeric volumetric ware in plastic (Teflon  or polyethylene) 50 mL
               or 100  mL capacity.
      f.       Whatman No.  41 filter paper (or equivalent).

      g.       Disposable polypropylene filter funnel.
      h.       Analytical balance,  300 g capacity,  and minimum ±0.01 g.

      i.       Polyethylene bottles,  125 mL,  with caps.

4.    REAGENTS

      a.       ASTM Type II water (ASTM D1193):   water must be monitored.

      b.       Sub-boiled,  concentrated nitric acid (sp. gr.  1.41).

      c.       Concentrated hydrochloric acid (sp.  gr. 1.19).
                                      D-9                                ILM02.0

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                                                                  Exhibit D Section III
5.     MICROWAVE CALIBRATION PROCEDURE

      a.       The calibration procedure is a critical step prior to the use of any
              microwave unit.  The microwave unit must be calibrated every six
              months.  The calibration data for each calibration must be available
              for review during on-site audits.   In order that absolute power
              settings may be interchanged from one microwave unit to another, the
              actual delivered power must be determined.

              Calibration of a laboratory microwave unit  depends on the type of
              electronic system used by the manufacturer.  If the un.it has a
              precise and accurate linear relationship between the output power and
              the scale used in controlling the microwave unit,  then the
              calibration can be a two-point calibration  at maximum and 40% power.
              If the unit is not accurate or precise for  some portion of the
              controlling scale, then a multiple-point calibration is necessary.
              If the unit power calibration needs a multiple point calibration,
              then the point where linearity begins must  be identified.   For
              example:  a calibration at 100,  99, 98,  97, 95, 90,  80, 70,  60,  50
              and 40% power settings can be applied and the data plotted.   The non-
              linear portion of the calibration curve can be excluded or restricted
              in use.  Each percent is equivalent to approximately 5.5-6 watts
              and becomes the smallest unit of power that can be controlled.  If 20
              - 40 watts are contained from 99-100%,  that portion of the microwave
              calibration is not controllable by 3-7 times that of the linear
              portion of the control scale and will prevent duplication of precise
              power conditions specified in that portion  of the power scale.

              The power available for heating is evaluated so that the absolute
            •  power setting (watts) may be compared from  oneL microwave to another.
              This is accomplished by measuring the temperature rise in 1 Kg of
              water exposed to microwave radiation for a  fixed period of time.  The
              water is placed in a Teflon  beaker (or a beaker that is made of some
              other material that does not adsorb microwave energy) and stirred
              before measuring the temperature.  Glass beakers adsorb microwave
              energy and may not be used.  The initi.il temperature of the water
              most be between 19 and 25 *C.  The beaker is circulated continuously
              through the field for at least two (2) minutes at full power.  The
              beaker is removed from the microwave, the water is stirred
              vigorously, and the final temperature recorded.  The final reading is
                                     D-10                                ILM02.0

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                                                                   Exhibit  u  section ill
               the maximum  temperature reading after each  energy  exposure.  These
               measurements must be accurate to ± 0.1  *C and made within 30 seconds
               of the  end of heating.  If more measurements  are needed,  do not use
               the same water until it has cooled down to  room temperature.
               Otherwise, use a fresh water sample.

               The absorbed power  is determined by  the following  formula:

                         p _ (IP  (Go") (m"> (DT)
                                    t

      Where:

      F - The apparent power absorbed by the sample in watts (joules per second),

      K - The conversion factor for thermochemical calories per second to watts
               (-4.184),

      Cp - The heat capacity,  thermal capacity,  or specific heat (cal. g~ . C'1) of
               water (-1.0),

      m — The mass of the sample in grams (g),

      DT - the final temperature minus the initial tempereture (*C), -and

      t - the time in seconds  (s)

      Using 2 minutes and 1 Kg of distilled water,  the calibration equation
      simplifies to:

      P - (DT) (34.87).

      The microwave user can now relate power in watts to the percent power setting
      of the microwave

6.    CLEANING PROCEDURE

a.    The initial cleaning of the PFA vessels:

(1)   Prior to first use - new vessels must be annealed before they are used.  A
      pretreatment/cleaning procedure must be followed.   This procedure  calls for
      heating  the vessels for 96 hours at 200*C.  The vessels must be disassembled
      during annealing and the sealing surfaces (the  top  of the  vessel  or its rim)
      must not be used to support the vessel during annealing.

(2)   Rinse in ASTM Type I water.
                                     D-ll                                ILM02.0

-------
                                                                  Exhibit  D Section  III
(3)   Immerse in 1:1 HC1 for a minimum of 3 hours after the cleaning bath has
      reached a temperature just below boiling.

(4)   Rinse in ASTM Type I water.

(5)   Immerse in 1:1 HN03 for a minimum of 3 hours after the cleaning bath has
      reached a temperature just below boiling.

(6)   The vessels are then rinsed with copious amounts of ASTM Type I water prior to
      use for any analyses under this contract.
b.    Cleaning procedure between g?"rp^ *B digestions

(1)   Wash entire vessel in hot water using laboratory- grade nonphosphate detergent.

(2)   Rinse with 1:1 nitric acid.

(3)   Rinse three times with ASTM Type I water.  If contaminants are found in the
      preparation blank, it is mandatory that steps a.(2)  through a(6) be strictly
      adhered to.

7.    DIGESTION PROCEDURE

a.    Water San|ple Digestion Procedure
                                                            TJ
(1)   A 45 mL aliquot of the sample are measured into Teflon  digestion vessels
      using volumetric glassware.

(2)   5 mL of high purity concentrated HNC>3 is added to the digestion vessels.

(3)   The caps with the pressure release valves are placed on the vessels hand tight
      and then tightened, using constant torque, to 12 ft./lbs.  The weight of each
      vessel is recorded to 0.02 g.

(4)   Place 5 sample vessels in the carousel, evenly spaced around its  periphery in
      the microwave unit.  Venting tubes connect each sample vessel with a
      collection vessel.  Each sample vessel is attached to a clean., double-ported
      vessel to "collect any sample expelled from the sample vessel in the event of
      over pressurization.  Assembly of the vessels into the carousel may be  done
      inside or outside the microwave.

(5)   This procedure is energy balanced for five 45 mL water samples  (each with 5 ml.
      of acid) to produce consistent conditipns.  When fewer than 5 samples are
      digested, the remaining vessels must be  filled with 45 mL of tap, DI or Type
      II water and 5 mL of concentrated nitric acid.

      Newer microwave ovens may be capable of  higher power  settings which may allow
                                      D-12                                ILM02.0

-------
                                                                   Exhibit D Section III
       a larger number of samples.   If the  analyst wishes  to digest more  than 5
       samples at a time,  the analyst  may use  different power  settings as long as
       they result in the same time  temperature conditions defined in the power
       programming for this method.

       The  initial temperature of the  samples  should be 24 ± 1*C.  The preparation
       blank must have 45 mL of deionized water and the same amount (5 mL) of acid
       that is added to the samples.

       The  microwave unit first-stage  program  must be set  to give 545 watts for 10
       minutes and the second-stage  program to give 344 watts  for 10 minutes.  This
       sequence brings the samples to  160 ±4°C in ten minutes  and permits a slow rise
       to 165-170 "C during the second 10 minutes.

(6)    Following the 20 minute program, the samples are left to cool in the microwave
       unit  for five  minutes,  with  the exhaust fan ON.  The samples and/or carousel
       may  then be removed from the  microwave  unit.  Before opening the vessels, let
       cool  until they are no longer hot  to the touch.

(7)    After the sample vessel has cooled,  weigh the sample vessel and compare to the
       initial weight as reported in the  preparation log.  Any sample vessel
       exhibiting a < 0.5  g loss  must have  any excess sample from the associated
       collection vessel added to the original sample vessel before proceeding with
       the  sample preparation.  Any  sample  vessel exhibiting a > 0.5 g loss. must be
       identified in the preparation log  and the sample redigested.

(9)    Sample Filtration:

       The digested samples are shaken well to mix in any  condensate within the
       digestion vessel before being opened.   The digestates are then filtered into
       50 mL glass volumetric flasks through ultra-clean filter paper and diluted to
       50 mL (if necessary).   The samples are  now ready for analysis.  The sample
       results must be corrected  by  a  factor of 1.11 in order  to report final
       concentration values based on an initial volume of  45 ml.  Concentrations so
       determined shall be reported. as  "total."
b.    Soil ??njr»H«i Digestion Procedure

(1)   Add a representative 0.5 ±0.050 grams of sample to  the TeflonR PFA vessel.

(2)   Add 10 ±0.1 mL of  concentrated nitric acid.  If a vigorous reaction occurs,
      allow the  reaction to stop before capping the vessel.

(3)   Cap the vessel,  then tighten using constant torque  to 12  ft/lbs,  according  to
      the manufacturer's direction.

(4)   Connect the sample vessel to the overflow vess€:l using Teflon^ PFA tubing.

(5)   Weigh the  vessel assembly to the nearest O.Olg.
                                     D-13                                ILM02.0

-------
                                                                  Exhibit  D  Section III
(6)   Place sample vessels in groups of 2 sample vessels or 6 sample vessels in the
      carousel, evenly spaced around its periphery in the microwave unit.  If fewer
      than the recommended number of samples are to be digested, i.e. 3 samples plus
      1 blank then the remaining vessels must be filled with 10 mL of nitric acid to
      achieve the full complement of vessels.

      Each sample vessel must be attached to a clean, double-ported vessel to
      collect any sample expelled from the sample vessel in the event of over
      pressurization.  Assembly of the vessels into the carousel may be done inside
      or outside the microwave.  Connect the overflow vessel to the center well of
      the oven.

(7)   The preparation blank must have 0.5 nL of deionized water and- the same amount
      (10 mL) of acid that is added to the samples.   The preparation blank must
      later be diluted to 50 mL in the same manner as the samples.

(8)   Irradiate the 2 sample vessel group at 344 watts for 10 minutes,  or the 6-
      sample vessel group at 574. watts for 10 minutes.

      This program brings the samples to 175"C in 5.5 minutes, and remains between
      170-180*C for the balance of the 10 minute irradiation period.   The pressure
      should peak at less than 6 atm for most samples.  The pressure may exceed
      these limits in the case of high concentrations of carbonate or organic
      compounds.   In these cases,  the pressure will  be limited by the relief
      pressure of the vessel to 7.5 ±0.7 atm.

(9)   Allow the vessels to cool for a minimum of five minutes before removing them
      from the microwave unit,  with exhaust fan ON.   Allow the vessels to cool to
      room temperature before opening.   The vessels  must be carefully vented and
      uncapped in a fume hood.

(10)  Weigh each  vessel assembly.   If the weight of acid plus the sample has
      decreased by more than 10% from the original weight, discard Che digests.
      Determine the reason for the loss.  Losses typically are attributed to use of
      digestion time longer than ten minutes, using too large of a sample, or having
      improper heating conditions.  Once the source  of the losses has been
      corrected,  prepare a new set of samples for digestion.

(11)  Sample Filtration:

      Shake the sample well to mix in any condensate within the digestion vessel
      before being opened.  Filter the digestion vessel into a 50 mL glass
      volumetric  flask through ultra-clean filter paper.  Rinse the sample digestion
      vessel, cap, connecting tube, and (if venting occurred) the overflow vessel
                                     D-14                                ILM02.0

-------
                                                                   Exhibit D Section III
      into the SO mL glass flask.  Dilute to 50 mL.  The samples are now ready for
      analysis.  Concentrations so determined shall be reported as "total."

(12)  Calculations:

      The concentrations determined in the digest are to be reported on the basis of
      the dry weight of the sample.

                        Concentration (dry wt.) (mg/Kg) -  C x V
                                                           W x S

                        Where
                          C -  Concentration  (mg/L)
                          V -  Final volume in liters after sample  ------
                               preparation
                          W -  Weight in kg of wet sample
                          S -  % Solids/100

D.   MERCURY AND CYANIDE PREPARATION

      Refer to each specific method in this Exhibit for mercury and cyanide
      preparations.
                                     D-15                                ILM02.0

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                                                                      Exhibit D ICP-AI
      PART A  -  INDUCTIVELY COUPLED  PIASMA-ATOMIC EMISSION SPECTROMETRIC METHOD'*'


                                Method  200.7 CLP-M*
          INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROMETRIC METHOD
                   FOR TRACE ELEMENT ANALYSIS  OF WATEIR AND WASTES


1.    Scope and Application                                      ......

1.1   Dissolved elements are determined in filtered a.nd acidified samples.
      Appropriate steps must be taken in all analyses  to ensure that potential
      interferences are taken into account. This is especially true when dissolved
      solids exceed 1500 mg/L.   (See 5.)

1.2   Total elements are determined after appropriate  digestion procedures are
      performed.  Since digestion techniques increase  the dissolved solids content
      of the samples, appropriate steps must be taken to correct for potential
      interference effects.  (See 5.)

1.3   Table 1 lists elements along with recommended wavelengths and typical
      estimated instrumental detection limits  using conventional pneumatic
      nebulization.  Actual working detected limits £.re sample dependent and as the
      sample matrix varies, these concentrations may also vary.  In time,  other
      elements may be added as more information becomes available and as required.

1.4   Because of the differences between various makes and models of satisfactory
      instruments, no detailed instrumental operating; instructions can be provided. ••'•
      Instead, the analyst is referred to the  instructions provided by the
      manufacturer of the particular instrument.

2.    Summary of Method

      The method describes a technique for the simultaneous or sequential
      multielement determination of trace elements in solution.  The basis of the
      method is the measurement of atomic emission by an optical spectroscopic
      technique..  Samples are nebulized and the aerosol that is produced is
      transported to the plasma torch where excitation occurs.  Characteristic
      atomic-line emission spectra are produced by a radio-frequency inductively
      coupled plasma (ICF).  The spectra are dispersed by a grating spectrometer and
      the intensities of the line are monitored by photomultiplier tubes.  The
      photocurrents from the photomultiplier tubes are processed and controlled by a
      computer system.  A background correction technique is required to compensate
      for variable background contribution to the determination of trace elements.
      Background must be measured adjacent to analyte lines on samples during
      analysis.  The position selected for the background intensity measurement, on
      either or both sides of the analytical line, will be determined by the
      complexity of the spectrum adjacent to the analyte line.  The position used
      must be free of spectral interference and reflect the same change in
      background intensity as occurs at the analyte wavelength measured.  Background
*A bibliography citing method references appears in paragraph 11 of the method.

 CLP-M modified for the Contract Laboratory Program.


                                     D-16                                ILM02.0

-------
                                                                       Exhibit  D ICP-AES
      correction  is not required in cases of line broadening where a background
      correction  measurement would actually degrade t.he analytical result.  The
      possibility of additional interferences named in 5.1 (and tests for their
      presence as described in 5.2) should also be recognized and appropriate
      corrections made.

3.    Safety

      The toxicity or carcinogenicity of each reagent: used in this method has not
      been precisely defined; however, each chemical compound should be treated as a
      potential health hazard.  The laboratory is responsible for maintaining a
      current awareness file of OSHA regulations regarding the safe handling of the
      chemicals specified in this method. - A reference file.of material handling
      data sheets should be made available to all personnel involved in the chemical
      analysis.

4.    Interferences

4.1   Several types of interference effects may contribute to inaccuracies in the
      determination of trace elements.  They can be summarized as follows:

      4.1.1   Spectral interferences can be categorized as 1) overlap of  a spectral
              line from 'another element; 2) unresolved overlap of molecular band
              spectra; 3) background contribution from continuous or recombination
              phenomena; and 4} background contribution from stray light  from the
              line emission of high concentration elements.  The first of these
              effects can be compensated by utilizing a computer correction of the
              raw data, requiring  the monitoring and measurement of the interfering
              element.  The second effect may -require selection_of an alternate
              wavelength.  The third-and-fourth effects can usually be compensated
              by  a background correction adjacent to the analyte line.  In
              addition, users of simultaneous multi-element instrumentation must
              assume the responsibility of verifying the absence of spectral
              interference from an element that could occur in a sample but for
              which there is no channel in the instrument array.

              Lisjted in Table 2 are some interference effects for  the recommended
              wavelengths given in Table 1.  The data in Table  2 are intended for
              use only as a rudimentary guide for the indication of .potential
              spectral interferences.  For this purpose, linear relations between
              concentration and intensity for the analytes and  the interferents  can
              be  assumed.  The interference information, which  was collected  at  the
              Ames Laboratory   , is expressed as analyte concentration equivalents
               (i.e., false analyte concentrations)  arising from 100 mg/L  of the
              interferent element.

              The suggested use of this  information is as follows:  Assume that
              arsenic (at 193.696  no) is to be determined in a  sample containing
              approximately 10 mg/L of of aluminum.  According  to  Table 2, 100 mg/L
              of  aluminum would yield a false signal for arsenic equivalent  to
              approximately 1.3 mg/L.  Therefore, 10 mg/L of aluminum would result
              in  a false signal for arsenic equivalent to approximately 0.13  mg/L.
  Ames Laboratory, USDOE, Iowa State University, Ames, Iowa 50011.


                                     D-17                                ILM02.0

-------
                                                                      Exhibit D ICP-AE,
               The  reader  is  cautioned  that other analytical systems may exhibit
               somewhat  different levels  of interference than those shown in Table
               2, and  that the  interference effects must be evaluated for each
               individual  system.  Only those interferents listed were investigated
               and  the blank  spaces  in  Table 2 indicare that measurable
               interferences  were not observed from the interferent concentrations
               listed  in Table  3.  Generally, interferences were discernible if they
               produced  peaks or background shifts corresponding tc 2-5% of the
               peaks generated  by the analyte concentrations also listed in Table 3.

               At present,  information  on the listed silver and potassium
               wavelengths are  not available but it has been reported that second
               order energy from the magnesium 383.231 run wavelength interferes with
               the  listed  potassium line  at 766.491 run.

      4.1.2    Physical  interferences are generally considered to be effects
               associated  with  the sample nebulization and transport processes.
               Such properties  as change  in viscosity and surface tension can cause
               significant inaccuracies especially in samples which may contain high
               dissolved solids and/or  acid concentrations.  The use of a
               peristaltic pump may lessen these interferences.  If these types of
               interferences  are operative, they must be reduced by dilution of the
               sample  and/ or utilization .of standard addition techniques.  Another
               problem which  can occur  from high dissolved solids is salt buildup at
               the  tip of  the nebulizer.  This affects aerosol flow rate causing
               instrumental drift.

               Wetting the argon prior  to nebulization, the use of a tip washer, or
               sample  dilution  have been  used to control this problem.  Also, it has
               been reported  .that better  control of the argon flow rate improves
               instrument  performance.  This is accomplished with the use of mass
               flow controllers.

      4.1.3    Chemical  interferences are characterized by molecular compound
               formation,  ionization effects and solute vaporization effects.
               Normally  these effects are not pronounced with the ICP technique,
               however,  if observed they  can be minimized by careful selection of
               operating conditions  (that is, incident power, observation position,
               and  so  forth), by buffering of the sample, by matrix matching, and by
               standard  addition procedures.  These types of interferences can be
               highly  dependent on matrix type and the specific analyte element.

4.2  Prior to reporting concentration data for  the  analyte elements,  the Contractor
     must analyze and report the  results  of the ICP Serial Dilution Analysis.   The
     ICP Serial Dilution Analysis must be performed on a sample  from each group of
     samples of a similar matrix  type (i.e., water,  soil)  and  concentration (i.e.,
     low, medium) or for each Sample Delivery Group,  whichever is more frequent.
     Samples identified as field  blanks cannot  be used for Serial Dilution Analysis.

     If the analyte concentration is sufficiently high (minimally a factor of 50
     above the instrumental detection limit in  the  original sample),  the serial
     dilution (a five fold dilution) must then  agree within 10%  of the original
     determination after correction for dilution.   If the dilution analysis for one
     or more analytes is not within 10%,  a chemical or physical  interference effect


                                     D-18                                ILM02.0

-------
                                                                      Exhibit D ICP-AES
     .must be suspected,  and the data for all  affected  analytes  in the samples
     received associated with that serial dilution must be  flagged with an "E"  on
     FORM IX-IN and FORM I-IN.

5.    Apparatus

5.1   Inductively Coupled Plasma-Atomic Emission Spectrometer.

      5.1.1    Computer controlled atomic emission spectrometer with background
               correction.

      5.1.2    Radio frequency generator.

      5.1.3    Argon gas supply, welding grade or  better.

5.2   Operating conditions -- Because of the differences between various makes  and
      models of satisfactory instruments, no detailed operating instructions can be
      provided.  Instead,  the analyst should follow the instructions provided by the
      manufacturer of the particular instrument..  Sensitivity,  instrumental
      detection limit, precision,  linear dynamic range, and interference effects
      must be investigated and established for each individual  analyte line on that
      particular instrument.  All measurements must be within the instrvipent linear
      range where correction factors are valid.   It is the responsibility of the
      analyst to verify that the instrument configuration and operating conditions
      used satisfy the analytical requirements and to  maintain quality control  data
      confirming instrument performance and analytical results.

6.    Reagents and Standards

6.1   Acids used in the  preparation of standards and for sample processing must be
      ultra-high purity  grade or equivalent.   Redistilled acids are acceptable.

      6.1.1   Acetic acid, cone,   (sp gr 1.06).

      6.1.2   Hydrochloric acid,  cone,   (sp  gr  1.19).

      6.1.3    Hydrochloric acid,  (1+1):   Add 500  mL cone.  HC1  (sp gr 1.19)  to 400
               mlTdeionized,  distilled water  and dilute to  1  liter.

      6.1.4    Nitric acid, cone.   (sp gr 1.41).

      6.1.5    Nitric acid,  (1+1):  Add  500 mL cone.  HN03  (sp  gr 1^41) to 400 mL
               deionized,  distilled water and'dilute to 1 liter.

6.2   Deionized, distilled water:   Prepare by passing; distilled water  through a
      mixed bed of cation and anion exchange resins.  Use deionized. distilled water
      for the preparation of all reagents, calibration standards and as dilution
      water.  The purity of this water must be equivalent to «ASTM Type II reagent
      water of Specification D 1193.

6.3   Standard stock solutions may be purchased or  prepared  from ultra high purity
      grade chemicals or metals.  All salts must  be dried  for  1  hour at 105° unless
      otherwise specified.
                                     D-19                                ILM02.0

-------
                                                                Exhibit D ICP-AES
(CAUTION:  Many metal salts are extremely toxic  and may be fatal if swallowed.
Wash hands thoroughly after handling.) Typical stock solution preparation
procedures follow:

6.3.1    Aluminum solution, stock, 1 mL - 100 u;§ Al:  Dissolved  0.100 g of
         aluminum metal in an acid mixture of 4 mL of (1+1) HC1  and 1 mL of
         cone.  HNC>3  in a beaker.  Warm gently 70 effect solution.  When
         solution is  complete,  transfer quantitatively to a liter flask, add
         an additional 10 mL of (1+1) HC1 and dilute to 1000 mL  with
         deionized, distilled water.

6.3.2    Antimony solution stock, 1 mL - 100 ug Sb:  Dissolve 0.2669 g
         K(SbO)CAH406 in deionized distilled water, add .10 mL (1+1) HC1 and
         dilute to 1000 mL with deionized, distilled water.

6.3.3    Arsenic solution, stock, 1 mL - 100 ug As:  Dissolve 0.1320 g of
         As203 in 100 mL of deionized, distilled water containing 0.4 g NaOH.
         Acidify the  solution with 2 mL cone.  HN03 and dilute to 1,000 mL
         with deionized, distilled water.

6.3.4    Barium solution, stock, 1 mL - 100 ug Ba:  Dissolve 0.1516 g Bad2
         (dried at 250°C for 2  hrs) in 10 mL deionized,  distilled water with  1
         mL (1+1) HC1.  Add 10.0 mL .(1+1) HC1 and dilute to 1,000 mL with
         deionized, distilled water.

6.3.5    Beryllium solution, stock, 1 mL - 100 ug Be:  Do not  dry.  Dissolve
         1.966 g BeS04*4H20, in deionized, distilled water, add  10.0 mL cone.
         HN03 and dilute to 1,000 mL with deionized, distilled water.

6.3.6    Boron solution, stock, 1 mL - 100 ug B:  Do not dry.  -Dissolve 0.5716
         g anhydrous  113603  in deionized, distilled water and dilute to 1,000
         mL.  Use a reagent meeting ACS specifications, keep the bottle
         tightly stoppered  and  store in a desiccator to prevent  the entrance
         of atmospheric moisture.

6.3.7    Cadmium solution,  stock, 1 mL - 100 ug Cd:  Dissolve 0.1142 g CdO  in
         « minimum amount of  (1+1) HN03-  Heat to  increase  rate  of
         dissolution. Add  10.0 mL cone. HN03  and  dilute to 1,000 mL with
         deionized, distilled water.

6.3.8    Calcium solution,  stock, 1 mL - 100 ug  Ca:  Suspend  0.2498 g  CaC03
         dried at 180°C for 1 h before weighing  in deionized,  distilled water
         and dissolve cautiously with  a'minimum  amount  of  (1+1)  HN03-  Add
         10.0 mL cone.  HN03 and dilute to 1,000 mL with deionized, distilled
         water.

6.3.9    Chromium solution,  stock,  1 mL -  100  ug Cr:  Dissolve 0.1923  g of
         Cr03  in deionized,  distilled  water.   When solution is complete
         acidify with 10 mL cone.   HN03 and  dilute to  1,000 mL with deionized,
         distilled water.

6.3.10   Cobalt solution stock, 1 mL - 100 ug Co:   Dissolve 0.1000 g of cobalt
         metal in a minimum amount of (1+1)  HNOj.   Add 10.0 mL  (1+1)  HC1 and
         dilute to  1,000 mL with deionized,  distilled water.
                                D-20                               1LM02.0

-------
                                                                 Exhibit  D ICP-AES
6.3.11   Copper solution,  stock,  1 mL - 100  ug  Cu:   Dissolve 0.1252 g CuO  in a
         minimum amount of (1+1)  HNC^.   Add  10.0 jnL cone.  HNC>3 and dilute to
         1,000 mL with deionized,  distilled  watsr.
6.3.12   Iron solution,  stock,  1 mL - 100 ug Fe :   Dissolve 0.1430 g Fe203 in a
         warm mixture of 20 mL (1+1) HC1 and 2 mL of cone.  HN03.  Cool, add
         an  additional 5 mL of cone.  HN03 and dilute to  1,000 mL with
         deionized,  distilled water.

6.3.13   Lead solution,  stock,  1 mL - 100 ug Pb:   Dissolve 0.1599 g Pb(N03)2
         in  a minimum amount of (1+1)  HN03.   Add  10.0 mL  of cone.  HN03 and
         dilute  to  1,000 mL with deionized,  dis-illed water.

6.3.14   Magnesium  solution,  stock,  1  mL - 100 ug Mg:   Dissolve  0.1658 g HgO
         in  a minimum amount of (1+1)  HNC^.   Add  10.0 mL  cone.   HNC>3 and
         dilute  to  1,000 mL with deionized,  distilled water.

6.3.15   Manganese  solution,  stock,  1  mL - 100 ug Mn:   Dissolve  0.1000 g of
         manganese  metal in the acid mixture, 10  mL cone.  HC1 and 1 mL cone.
         HN03, and  dilute to 1,000  mL with deionized,  distilled  water.

6.3.16   Molybdenum solution, stock, 1 mL - 100 ug Mo:  Dissolve 0.2043 g
         (NH4)2MoC«4 in deionized, distilled water and dilute  to  1,000 mL.

6.3.17   Nickel  solution,  stock, 1  mL - 100 ug Ni:   Dissolve  0.1000 g of
         nickel  metal in 10 mL hot  cone.   HN03, cool and  dilute  to 1,000 mL
         with deionized,  distilled  water.

6.3.18   Potassium  solution,  stock,  1  mL - 100 ug K:  Dissolve 0.1907 g KC1,
         dried at 110°C,  in deionized,  distilled  water.   Dilute  to JU_0_QO mL.

6.3.19   Selenium solution,  stock,  1 mL - 100 ug  Se:  Do  not  dry.  Dissolve
         0.1727  g H2Se03 (actual assay 94.6%) in  deionized, distilled water
         and dilute to 1,000 mL.

6.3.20   Silica  solution,  stock,  1  mL  - 100 ug SiC^r  Do  not  dry.  Dissolve
         0.4730  g Na2Si03'9H20  in deionized,  distilled water. Add 10.0 mL
         coac.   HN03 and dilute to  1,000 mL with  deionized, distilled water.

6.3.21   Silver  solution,  stock, 1  mL - 100 ug Ag:   Dissolve  0.1575 g AgNC>3 in
         100 mL  of  deionized, distilled water and 10 mL cone. HNC>3.  Dilute
         to  1,000 mL with deionized, distilled water.

6.3.22   Sodium  solution,  stock, 1  mL -100 ug Ha:   Dissolve  0.2542 g NaCl in
         deionized,  distilled water.  Add 10.0 uL cone.   HN03 and dilute to
         1,000 mL with deionized, distilled water.

6.3.23   Thallium solution,  stock,  1 mL - 100 ug  Tl: -Dissolve 0.1303 g T1N03
         in  deionized,  distilled water.   Add
         10.0 mL cone.   ffiK>3 and dilute to 1,000  mL with  deionized, distilled
         water .
                               D-21                                ILM02.0

-------
                                                                      Exhibit D ICP-AES
      6.3.24   Vanadium solution,  stock,  1 mL - 100 u.§ V:  Dissolve 0.2297 NH4V03 in
               a minimum amount of cone.  HN03.  Heat to increase rate of
               dissolution.   Add 10.0 mL  cone.  HN03 .ind dilute to 1,000 mL with
               deionized,  distilled water.

      6.3.25   Zinc  solution,  stock, 1 mL - 100 ug Zn:  Dissolve 0.1245 g ZnO in a
               minimum amount of dilute HN03.  Add 10.0 mL cone. HNC>3 and dilute to
               1,000 mL with  deionized, distilled watur.

6.4   Mixed calibration standard solutions --  Prepare mixed  calibration standard
      solutions by combining appropriate volumes  of the stock solutions in
      volumetric flasks.  (See 7.4.1 thru 7.4.5.)  Add 2 mL of (1+1)  HN03 and 10 mL
      of (1+1) HC1 and dilute to 100 mL with deionized, distilled water.   (See  NOTE
      in 7.4.5) Prior to preparing the mixed standards, each stock solution should
      be analyzed separately to determine possible spectral  interference or the
      presence of impurities.  Care should be  taken vhen preparing the  mixed
      standards that the elements are  compatible  and stable.   Transfer  the mixed
      standard solutions to a FEP f luorocarbon or unused polyethylene bottle £ or - :...
      storage.  Fresh mixed standards  should be prepared as  needed with the
      realization that concentration can change on aging.  Calibration  standards
      must be initially verified using a quality  control sample  and  monitored weekly
      for stability (see 7.6.3).  Although not specifically  required, some typical
      calibration standard combinations follow when using  those  specific wavelengths
      listed in Table 1.

      6.4.1   Mixed standard solution I  -- Manganese, beryllium, cadmium, lead, and
               zinc.

      6.4.2   Mixed standard solution II -- Barium, copper,  iron, vanadium, and
               cobalt.

      6.4.3   Mixed standard solution III •- Molybdenum, silica, arsenic, and
              selenium.

      6.4.4   Mixed standard solution IV -- Calcium, sodium, potassium, aluminum,
              chromium  and nickel.

      6.4.5   Mixed standard solution V  -- Antimony, boron, magnesium, silver, and
               thallium.

              NOTE:   If the  addition of  silver to the  recommended acid combination
               results in an  initial precipitation add  15 mL of deionized  distilled
              water and warm the flask until.the solution clears.  Cool and dilute
               to 100  mL with deionized,  distilled water.  For this acid combination
               the silver concentration should be limited to 2 mg/L.  Silver under
               these conditions is stable in a tap water matrix for 30  days.  Higher
               concentrations of silver require additional HC1.

6.5   Two types of blanks are required for the analysis.  The calibration blank
      (3.13) is used in establishing the analytical curve while the reagent blank
      (preparation blank, 3.12) is used to correct for possible contamination
      resulting from varying amounts of the acids used in the sample processing.
                                     D-22                                ILM02.0

-------
                                                                      Exhibit D ICP-AES
      6.5.1   The calibration blank is prepared by diluting 2 mL of (1+1) HNC>3 and
              10 mL of  (1+1) HC1 to 100 mL with deionized, distilled water.
              Prepare a sufficient quantity to be used to flush the system between
              standards and samples.

      6.5.2   The reagent blank (or preparation blank - See Exhibit E) must contain
              all the reagents and in the same volumes as used in the processing of
              the samples.  The reagent blank must be carried through the complete
              procedure and contain the same acid concentration in the final
              solution as the sample solution used for analysis.

6.6   In addition the calibration standards,  an instrument check standard (3.6),  an
      interference check sample  (3.7)  and a  quality control sample  (3.8)  are  also
      required for the analyses.

      6.6.1   The instrument check standard for continuing calibration verification
              is prepared by the analyst by combining compatible elements at a
              concentration equivalent to the mid-points of their respective  —
              calibration curves.  (See 10.1.3.>

      6.6.2   The interference check sample is prepared by the analyst, or obtained
              from EPA if available (Exhibit E).

      6.6.3   The quality control sample for the initial calibration verification
              should be prepared in the same acid matrix as the calibration
              standards and in accordance with the instructions provided by the
              supplier.  EPA will either supply a quality control sample or
              information where one of equal quality can be procured.  (See
              10.1.1.)

7.    Procedure

7.1   Set up instrument with proper operating parameters established in Section 6.2.
      The instrument must be allowed to become thermally stable before beginning.
      This usually requires at least 30 min.  of operation prior to calibration.

7.2   Initiate appropriate operating configuration of computer.

7.3   Profile and calibrate instrument according to instrument manufacturer's
      recommended procedures, using mixed calibration standard solutions such as
      those described in Section 7.4.   Flush the system with the calibration blank
      (7.5.1) between each standard.  (NOTE:  For boron concentrations greater than
      500 ug/L extended flush times of 1 to 2- minutes may be required.)

7.4   Begin the sample run flushing the system with the calibration blank solution
      (7.5.1) between each sample.  (See NOTE in 8.3.)  Analyze the instrument check
      standard (7.6.1) and the calibration blank (7.5.1) each 10 analytical samples.

7.5   A minimum of two replicate exposures are required for standardization and  all
      QC and sample analyses.  The average result of the multiple exposures for  the
      standardization and all QC and sample analyses shall be used.
                                     D-23                                ILM02.0

-------
                                                                      Exhibit D ICP-AE
8.    Calculation

8.1   Reagent blanks (preparation blanks) should be treated as specified in Exhibit
      E.

8.2   If dilutions were performed, the appropriate factor must be applied to sample
      values.

8.3   Units must be clearly specified.

9.    Quality Control (Instrumental)

9.1   Quality control must be performed as specified in Exhibit E.
                                     D-24                                ILM02.0

-------
                                                                       Exhibit D  ICP-AES
               TABLE 1 - RECOMMENDED WAVELENGTHS(2) AND ESTIMATED
                         INSTRUMENTAL DETECTION LIMITS
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnes ium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silica (Si02)
Silver
Sodium
Thallium
Vanadium
Zinc
Wavelength, nm(l)
308.215
206.833
193.696
455.403
313.042
249.773
226.502
317.933
267.716
228.616
324.754
259.940
220.353
279.079
257.610
202.030
231.604
766.491
196.026
288.158
328.068
588.995
190.864
292.402
213.856
Estimated Detection
Limit, ug/L(2)
45
32
53
2
0.3
5
4
10
7
7
6
7
42
30
2
8
15
See(3)
75
58
7
29
40
8
2
(1)  The wavelengths  listed are recommended because  of their sensitivity and overall
    acceptance.   Other wavelengths may be substituted if they can provide the
    needed sensitivity and are treated with  the  same  corrective techniques for
    spectral  interference.   (See 5.1.1).  The use of alternate wavelengths must be
    reported  (in nm)  with the sample data.

(2)  The estimated instrumental detection limits  as  shown are taken from
    "Inductively Coupled Plasma-Atomic Emission  Spectroscopy-Prominent Lines," EPA-
    600/4-79-017.  They  are given as a guide for an instrumental limit.  The actual
    method detection limits are sample dependent and  nay vary-as the sample matrix
    varies.

(3)  Highly dependent on  operating conditions and plasma position.
                                     D-25                                ILM02.0

-------
                                  Exhibit  D ICP-AES






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"
D-26
ILM02.0

-------
TABLE 3.  INTERFERENT AND ANALYTE ELEMENTAL CONCENTRATIONS USED
          FOR INTERFERENCE MEASUREMENTS IN TABLE 2
Analytes
Al
As
B
Ba
Be
Ca
Cd
Co
Cr
Cu
Fe
Mg
Mn
Mo
Na
Ni
Pb
Sb
Se
Si
Tl
V
Zn
(mg/L)
10
10
10
1
1
1
10
1
1
1
1
1
1
10
10
10
10
10
10
1
10
1
10
Interferents
Al
Ca
Cr
Cu
Fe
Mg
Mn
Ni
Ti
V





-





'

(mg/L)
1000
1000
200
200
1000
1000
200
200
200
200













                             D-27                                ILM02.0

-------
           PART B - ATOMIC ABSORPTION METHODS.  FURKACE TECHNIQUE*

      Analyte/Method                                         Page No.

      Antimony - Method 204.2 CLP-M*                           D-29
      Arsenic - Method 206.2 CLP-M                             D-30
      Beryllium - Method 210.2 CLP-M                           D-31
      Cadmium - Method 213.2 CLP-M                             D-32
      Chromium - Method 218.2 CLP-M    -                        D-33
      Lead - Method 239.2 CLP-M                                D-34
      Selenium - Method 270.2 CLP-M                            D-36
      Silver - Method 272.2 CLP-M                              D-38
      Thallium - Method 279.2 CLP-M                            D-39
+From "Methods for Chemical Analysis of Water and Wastes" (EPA-600/4-79-
 020), Metals-4, as modified for use in the Contract Laboratory Program).
 CLP-M modified for the Contract Laboratory Program.

                                   D-28                                ILM02.0

-------
                                                                 Exhibit D Method 204.2
                                      ANTIMONY

             Method 204.2 CLP-M* (Atomic Absorption,  Furnace Technique)
Optimum Concentration Range:  20-300 ug/L
Approximate Detection Limit:  3 ug/L
Preparation of Standard Solution
1.   Stock solution:   Carefully weigh 2.7426 g of antimony potassium tartrate
     (analytical reagent grade) and dissolve in deionized distilled water.   Dilute
     to 1 Liter with deionized water.  1 mL - 1 mg Sb (1000 mg/L) .
2.   Prepare dilutions of the stock solution to be used as calibration standards  at
     the time of analysis.   These solutions are also  to be used for "standard
     additions".

3.   The calibration standards must be prepared using the same type of acid and at
     the same concentration as will result in the sample to be analyzed  after  sample
     preparation.
                 ters (General^
1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec <§ 800°C.
3.   Atomizing Time and Temp:   10 sec @ 2700°C.
4.   Purge Gas Atmosphere:   Argon
5.   Wavelength:  217.6 nm
6.   Other operating parameters should be set as specified by the  particular
     instrument manufacturer.
Notes

1.   The above concentration values and instrument conditions are  for a Perkin- Elmer
     HGA- 2100, based on the use of a 20 uL injection,  contin- uous flow purge. gas
     and non-pyrolytic graphite and are to be used as  guidelines only.  Smaller size
     furnace devices or those employing faster rates of atomization can be operated
     using lower atomization temperatures for shorter  time periods than the above
     recommended settings.

2.   The use of background correction is required.
3.   Nitrogen may_also be used as the purge gas.
4.   If chloride concentration presents a matrix problem or causes a loss previous
     to atomization, add an excess 5 mg of ammonium nitrate to the furnace and ash
     using a ramp accessory or with incremental steps  until the recommended ashing
     temperature is reached.
5.   For every sample analyzed, verification 'is necessary to determine that method
     of standard addition is not required (see Exhibit E) .
6.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
 CLP-M modified for the Contract Laboratory Program.
                                     D-29                                ILM02.0

-------
                                                                 Exhibit D Method 206.2
                                      ARSENIC

             Method 206.2 CLP-M* (Atomic Absorption,  Furnace Technique)

Optimum Concentration Range:   5-100 ug/L
Approximate Detection Limit:   1 ug/L

preparation of Standard Solution

1.   Stock solution:   Dissolve 1.320 g of arsenic  trioxide,  As£03  (analytical
     reagent grade) in 100 mL of deionized distilled water containing 4  g NaOH.
     Acidify the solution with 20 mL cone.  HNC>3 and dilute to 1  Liter.   1 mL - 1 mg
     As (1000 mg/1).

2.   Nickel Nitrate Solution,  5%:  Dissolve 24.780 g of ACS  reagent grade
     Ni(NC<3)2'6H20 in deionized distilled water and make  up  to 100 mL.

3.   Nickel Nitrate Solution,  1%:  Dilute 20 mL of the  5% nickel nitrate to  100 mL
     with deionized distilled water.

4.   Working Arsenic Solution:  Prepare  dilutions  of  the  stock solution  to be used
     as calibration standards at the time of analysis . Withdraw appropriate  aliquots
     of the stock solution, add 1 mL of  cone. HN03, 2 mL  of  30%  H202 and 2 mL of the
     5% nickel nitrate solution.    Dilute to 100  mL  with deionized distilled water.

Sample Preparation

1.   Add 100 uL of the 5% nickel nitrate solution  to 5  mL of the digested sample.
     The sample is now ready  for injection into the furnace.
                      (General)

1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec <§ 1100°C.
3.   Atomizing Time and Temp:   10 sec @ 2700°C.
4. .  Purge Gas Atmosphere:   Argon
5.   Wavelength:  193.7 nm
6.   Other operating parameters should be set as specified by the particular
     instrument manufacturer.

Notes
1.   The above concentration values and instrument conditions are for a Perkin- Elmer
     HGA-2100, based on the use of a 20 uL injection,  purge gas interrupt and non-
     pyrolytic graphite. Smaller size furnace. devices or those employing faster
     rates of atomization can  be operated using lower  atomization temperatures for
     shorter time periods than the above recommended settings.

2.   The use of background  correction is required. Background correction made by the
     deuterium arc method does not adequately 'compensate for high levels of certain
     interferents (ie., Al, Fe) .  If conditions occur  where significant interference
     is suspected, the lab  must switch to an alternate wavelength or take other
     appropriate actions to compensate for the interference effects.

3.   For every sample analyzed, verification is necessary to-determine that method
     of standard addition is not required (see Exhibit E) .

4.   If method of standard addition is required, follow the procedure given in
     Exhibit E) .

5.   The use of the Electrodeless Discharge Lamps (EDL) for the light source  is
     recommended.
*CLP-M modified for the Contract Laboratory Program.


                                     D-30                                ILM02.0

-------
                                                                  Exhibit D Method 210.2
                                      BERYLLIUM

             Method 210.2 CLP-M*  (Atomic Absorption, Furnace Technique)
Optimum Concentration Range:  1-30 ug/L
Approximate Detection Limit:  0.2 ug/L

Preparation of Standard Solution  '

1.   Stock solution:   Dissolve 11.6586g of beryllium sulfate, BeS04, in deionized
     distilled water containing 2 mL concentrated nitric acid and dilute to 1 Liter.
     1 mL - 1 mg Be (1000 mg/L).

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.    These solutions are also to be used for "standard
     additions".

3.   The calibration standards oust be prepared using the sane type of acid and at
     the same concentration as will result in the sample to be analyzed after sample
     preparation.       .     .         	__

Instryqrc^n,^ Parameters (General)

1.   Drying Time and Temp:  30 sec @ 125°C.
2.   Ashing Time and Temp:  30 sec (§ 1000°C.
3.   Atomizing Time and Temp:  10 sec @ 2800°C.
4.   Purge Gas Atmosphere:  Argon
5.   Wavelength:   234.9 nm
6.   The operating parameters should be set as specified by the particular
     instrument manufacturer.

Notes

1.    The above concentration values and instrument conditions are for a Perkin-
      Elmer HGA-2100,  based on the use of a 20 uL injection, con-tinuous flow purge
      gas and non-pyrolytic graphite and are to be used as guidelines only.  Smaller
      size furnace devices or those employing faster rates of atomization can be
      operated using lower atomization temperatures for shorter time periods than
      the above recommended settings.

2.    The use of background correction is required.

3.    Because of^possible chemical  interaction,  nitrogen should  not be used  as a
      purge gas.

4.    For every sample analyzed,  verification is  necessary to determine that method
      of standard addition is not required (see Exhibit E)

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
 CLP-M modified for the Contract Laboratory Prog-ram
                                     D-31                                ILM02.0

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                                                                 Exhibit D Method 213.
                                      CADMIUM

             Method 213.2 CLP-M* (Atomic Absorption,  Furnace Technique)
Optimum Concentration Range:  0.5-10 ug/L
Approximate Detection Limit:  0.1 ug/L
Preparation of Standard Solution

1.   Stock solution:   Carefully weigh 2.282g of^ cadmium sulfate,  3  CdS04*  8 H20
     (analytical reagent grade) and dissolve in deionized distilled water.  Make up
     to 1 Liter with deionized distilled water.   1 ml - 1 mg Cd  (1000 mg/L) .
2.   Ammonium Phosphate solution (40%):   Dissolve 40  grams of ammonium  phosphate,
     (NH4)2HP04 (analytical reagent grade)  in deionized distilled water and dilute
     to 100 mL.

3.   Prepare dilutions of stock cadmium  solution to be used as calibration standards
     at the time of analysis.   To each 100  mL of standard and sample alike add 2.0
     mL of the ammonium phosphate solution.   The calibration standards  must be
     prepared using the same type of acid and at the  same concentration as will
     result in the sample to be analyzed after sample preparation.
           Partgt*ers (General)
1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec @ 500°C.
3.   Atomizing Time and Temp:  10 sec <§ 1900°C.
4.   Purge Gas Atmosphere:   Argon
5.   Wavelength:  228.8 nm
6.   The operating parameters should be set as specified by the particular
     instrument manufacturer.

Notes
1.   The above concentration values and instrument conditions are for a Perkin- Elmer
     HGA-2100, based on the use of a 20 uL injection,  continuous  flow purge gas and
     non-pyrolytic graphite and are to be used as guidelines only.  Smaller size
     furnace devices or those employing faster rates of atomization can be operated
     using lower atomization temperatures for shorter time periods than the above
     recommended_settings .
2.   The use of background correction is required.
3.   Contamination from the work area is critical in cadmium analysis.  Use pipette
     tips which are free of cadmium.
4.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit E) .

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
 CLP-M modified for the Contract Laboratory Program.
                                     D-32                                ILM02.0

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                                                                 Exhibit D Method 218.2
                                      CHROMIUM

             Method 218.2 CLP-M* (Atomic Absorption,  Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limi£:  1 ug/L

Preparation of Standard Solution

1.   Stock solution:   Prepare as described under Part C methods, AA Flame -Technique.

2.   Calcium Nitrate  solution:  Dissolve 11.8 grams of calcium nitrate,
     Ca(N03)2'4H20 (analytical reagent grade) in de ionized distilled water  and
     dilute to 100 mL.   1 mL - 20 mg Ca.

3.   Prepare dilutions  of the stock chromium solution to be used as calibration
     standards at the time of analysis.   The calibration standards  must be  prepared
     using the same type of acid and at the same concentration as will result  in  the
     sample to be analyzed after sample preparation.   To each 100 mL of standard  and
     sample alike ,  add 1 mL of 30% ^02 and 1 mL of the calcium nitrate solution. :

                      (General^
1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec @ 1000°C.
3.   Atomizing Time and Temp:   10 sec @ 2700°C.
4.   Purge Gas Atmosphere:   Argon
5.   Wavelength:  357.9 nm
6.   Other operating parameters should be  set as  specified by the particular
     instrument manufacturer.

Notes

1 .   The above concentration values and instrument conditions are for a Perkin Elmer
     HGA-2100, based on the use of a 20 uL injection,  continuous flow purge gas and
     non-pyrolytic graphite and are to be  used as guidelines only.

2.   Hydrogen peroxide is added to the acidified solution to convert all chromium to
     the trivalent state.     Calcium is added to a level above 200 mg/L where its
     suppressive effect becomes constant up to 1000 ng/L.

3.   Background correction  is  required.

4.   Nitrogen should not be used as a purge gas because of possible CN band
     interference .
5.   Pipette tips have been reported to be a possible  source of contamination.

6.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit E) .

7.   If method of standard  addition is required,  follow the procedure given in
     Exhibit E.
 CLP-M modified for the Contract Laboratory Program.
                                     D-33                                ILM02.0

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                                                                  Exhibit D Method 239.2
                                        LEAD

                               •&
             Method 239.2 CLP-M  (.Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  1 ug/L

Preparation of Standard Solution

1.   Stock solution:   Carefully weigh 1.599 g of lead nitrate,  Pb(NO3) 2 -{analytical-
     reagent grade),  and dissolve in deionized distilled water.   Wheii solution is
     complete,  acidify with 10 oL redistilled HN(>3 and dilute to 1 Liter with --
     deionized distilled water. 1 mL - 1 mg Pb (lOOOng/L) .

2.   Lanthanum Nitrate solution:.  Dissolve 58.64 g of ACS reagent grade L^OS in  100
     mL cone.  HN03 and dilute to 1000 mL with deionized distilled water.  1 mL -  50
     mg La.

3.   Working Lead solution:   Prepare dilutions of stock lead solution to be used  as
     calibration standards at the time of analysis.   The calibration stan&rdsrmnstr
     be prepared using the same type of acid and at the same concentration as will
     result  in the sample to be analyzed after sample preparation.  To each 100 mL
     of diluted standard add 10 mL of the lanthanum nitrate solution.

Sample Preparation

1.   To each 100 mL of prepared sample solution add 10 mL of the lanthanum nitrate
     solution.
                      (General)

1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec @ 500°C.
3.   Atomizing Time and Temp:   10 sec <§ 2700°C.
4.   Purge Gas Atmosphere:   Argon
5    Wavelength:  283.3 nm
6.   Other operating parameters should be set as specified by the particular
     instrument manufacturer.

ftotes   .

1.   The above concentration values and instrument conditions are for a Perkin-Elmer
     HGA-2100, based on the use of a 20 uL injection,  continuous flow purge gas and
     non-pyrolytic graphite and are to be used as guidelines only.  Smaller size
     furnace devices or those employing faster rates of atomization can be operated
     using lower atomization temperatures for shorter time periods than the above
     recommended settings.
2.   The use of background correction is required.
 CLP-M modified for the Contract Laboratory Program.
                                     D-34                                ILM02.0

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                                                                 Exhibit D Method 239.2
3.   Greater sensitivity can be acheived using the 217.0 nm line,  but the  optimum
     concentration range is reduced.  The use of a lead electrodeless discharge  lamp
     at this lower wavelength has been found to be advantageous.   Also a lower
     atomization temperature (2400°C) may be preferred.
4.   To suppress sulfate interference (up to 1500 ppra) lanthanum is added  as the
     nitrate to both samples and calibration standards.  (Atomic Absorption
     Newsletter Vol. 15, No. 3, p.  71, May-June 1976).
5.   Since glassware contamination is a severe problem in lead analysis, all
     glassware should be cleaned immediately prior to use,  and once cleaned, should
     not be open to the atmosphere except when necessary.
6.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit E).
7.   If method of standard addition is required, follow the procedure given in
     Exhibit E.                                                    ,
                                     D-35                                ILM02.0

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                                                                 Exhibit D Method 270.2
                                      SELENIUM

             Method 270.2 CLP-M* (Atomic Absorption,  Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  2 ug/L

Preparation of Standard Solution

1.   Stock Selenium solution:  Dissolve 0.3453 g of selenous acid (actual  assay
     94.6% H2$e03) in deionized distilled water and make up to 200 mL.   1  mL - 1  mg
     Se (1000 mg/L).

2.   Nickel Nitrate solution, 5%:   Dissolve 24.780 g  of ACS reagent grade
                   in deionized distilled water and make up to 100 mL.
3.   Nickel Nitrate solution,  1%:   Dilute 20 mL of the 5% nickel nitrate to  100 mL
     with deionized distilled water.

4.   Working Selenium solution:   Prepare dilutions of  the stock solution to  be used
     as calibration standards at the  time of analysis.   The calibration standards
     must be prepared using the  same  type of acid and  at the same concentration as
     will result in the sample to be  analyzed after sample preparation.   Withdraw
     appropriate aliquots of the stock solution,  add 1 mL of cone.  HN03,  2 mL of 30%
     H202 and 2 mL of the 5% nickel nitrate solution.   Dilute to 100  mL with
     deionized distilled water.

Sample Preparation

1.   Add 100 uL of the 5% nickel nitrate solution to 5 mL of the digested sample.
     The sample is now ready for injection into the furnace.

Instrm"«*fl*[; Parameters

1.   Drying Time and Temp:   30 sec <§  125°C.
2 .   Charring Time and Temp :  30 sec  <§ 1200°C .
3.   Atomizing Time and Temp:   10 sec @ 2700°C.
4.   Purge Gas Atmosphere:   Argon
5.   Wavelength:  196.0 run
6.   Other operating parameters  should be set as specified by the particular
     instrument manufacturer.

Notes            —

1.   The above concentration values and instrument conditions are for a Perkin- Elmer
     HGA-2100, based on the use of a  20 uL injection,  purge gas interrupt and non-
     pyrolytic graphite and are to be used as guidelines only.  Smaller size furnace
     devices or those employing faster rates of atomization can be operated using
     lower atomization tempera-  tures for shorter time periods than the above
     recommended settings.

2.   The use of background correction is required.    Background correction made by
     the deuterium arc method does not adequately compensate for high levels of
     certain interferents (i.e., Al,  Fe) .
 CLP-M modified for the Contract Laboratory Program.
                                     D-36                                ILM02.0

-------
                                                                  Exhibit D Method 270.2
      If  conditions occur where significant interferes Is suspected, the lab must
      switch  to  an alternate wavelength or take other appropriate actions to
      compensate for  the interference effects.
 3'    /6ioAiUm analysis suffers interference from chlorides (>800 mg/L) and sulfate
      (>200 mg/L) .  For the analysis of industrial effluents and samples with
     concentrations of sulfate from 200 to 2000 mg/L. both samples and standards
     should be prepared to contain 1% nickel.

4.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit E) .

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.

6.   The use of the Electrodeless Discharge Lamp (EDL) for  the light source is
     recommended .
                                    D-37                                ILM02.0

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                                                                 Exhibit D Method 272.2
                                       SILVER

             Method 272.2 CLP-M* (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  1-25 ug/L
Approximate Detection Limit:  0.2 ug/L

Preparation of Standard Solution

1.   Stock solution:   Dissolve 1.57-5 g- of AgN03 (analytical reagent grade) in
     deionized distilled water.   Add 10 mL of concentrated HN03 and make up to 1
     Liter.  1 mL - 1 mg Ag (1000 mg/L) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are_aLso.£o-be used for "standard
     additions".

3.   The calibration standards must be prepared using the same type of acid and at
     the same concentration as will result in the  sample to be analyzed after sample
     preparation.

                      (General)
1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec @ 400°C.
3.   Atomizing Time and Temp:   10 sec @ 2700°C.
U.   Purge Gas Atmosphere:   Argon
5.   Wavelength:  328.1 nm
6.   Other operating parameters should be set as specified by the particular
     instrument manufacturer.

Notes

1.   The above concentration values and instrument- conditions are~f or- a Perkin-Elmer
     HGA-2100, based on the use of a 20 uL" injection,  continuous flow purge gas and
     non-pyrolytic graphite and are to be used as guidelines only.  Smaller size
     furnace devices or those  employing faster rates of atomization can be operated
     using lower atomization temperatures for shorter time periods than the above
     recommended settings.
2.   The use of background  correction is required.

3.   The use of halide acids should be avoided.

4.   If absorption to container walls or formation of AgCl is suspected, see Part G,
     AA methods Flame Technique.

5.   For every sample analyzed, verification is  necessary to determine that method
     of standard addition is not required (see Exhibit E) .

6.   If method of standard  addition is required, follow the procedure given in
     Exhibit E.
*CLP-M modified for the Contract Laboratory Program.
                                     D-38                                ILM02.0

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                                                                  Exhibit D Method  279.2
                                      THALLIUM

             Method 279.2 CLP-M*  (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  1 ug/L

Preparation of Standard Solution

1.   Stock solution:  Dissolve 1.303g of thallium nitrate, T1N03 (analytical reagent
     grade) in deionized distilled water.   Add 10 mL of concentrated nitric acid and
     dilute to 1 Liter with deionized distilled water.   1 mL - 1 mg Tl (1000 mg/L) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.   These solutions are also to be used for "standard
     additions".                                             ~        ~

3.   The calibration standards must be prepared using the same type of acid and at
     the same concentration as will result in the sample to be .analyzed after sample
     preparation.

           Pr*m»eters (General)
1.   Drying Time and Temp:   30 sec @ 125°C.
2.   Ashing Time and Temp:   30 sec @ 400°C.
3.   Atomizing Time and Temp:   10 sec @ 2400°C.
4.   Purge Gas Atmosphere:   Argon
5.   Wavelength:  276.8 nm
6.   Other operating parameters should be set as specified by the particular
     instrument manufacturer.
Notes

1.    The above  concentration values . andL instrument. ..conditions _are_ for  a Perkin-
      Elmer HGA-2100, based on the  use of a 20 uL  injection,  continuous  flow purge
      gas and non-pyrolytic graphite and are to be used as guidelines only.  Smaller
      size furnace  devices or  those  employing faster  rates of atomization  can be
      operated using  lower atomization  temperatures  for shorter time  periods than
      the above recommended settings.

2.    The use of background correction is required.

3.    Nitrogen may also be used as the purge gas.
4.    For every sample analyzed, verification  is  necessary to determine that method
      of standard addition is not required (see Exhibit E) .
5.    If method of standard  addition is  required, follow  the procedure  given in
      Exhibit E.
 CLP-M modified for the Contract Laboratory Program.
                                     D-39                                ILM02.0

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            PART C -  ATOMIC ABSORPTION METHODS.  FLAME TECHNIQUE'*'
      Analvte/Method                                         Page No.


      Calcium - Method 215.1 CLP-M*                            D-41

      Magnesium - Method 242.1 CLP-M                           D-42

      Potassium - Method 258.1 CLP-M                           D-43

      Sodium - Method 273.1 CLP-M                              D-44
"*"From "Interim Methods for the Sampling and Analysis of Priority Pollutants
 in Sediments and Fish Tissue", USEPA EMSL, Cincinnati, Ohio, August  1977,
 Revised October 1980, as modified for use in the  Contract Laboratory
 Program.

 CLP-M modified for the Contract Laboratory Program.


                                   D-40                                ILM02.0

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                                                                  Exhibit D Method 215.1
                                       CALCIUM

              Method 215.1 CLP-M* (Atomic Absorption, Flame Technique)

Optimum Concentration Range:  0.2-7 mg/L using a wavelength of 422.7 nm
Sensitivity:  0.08 mg/L
Detection Limit:  0.01 mg/L
Preparation of Standard Solution

1.   Stock Solution:  Suspend 1.250 g of CaC03 (analytical reagent grade),  dried at
     180°C for 1 hour before weighing, in deionized distilled water and dissolve
     cautiously with a mimimum of dilute HC1.  Dilute to 1000 mL with deionized
     distilled water.  1 mL - 0.5 mg Ca (500 mg/L).
2.   Lanthanum chloride solution:  Dissolve 29 g of La2<>3, slowly and in small
     portions, in 250 mL cone.  HC1 (Caution:  Reaction is violent) and dilute  to
     500 mL with deionized distilled water.

3.   Prepare dilutions of the stock calcium solutions to be used as calibration
     standards at the time of analysis.  To each 10 mL of calibration standard  and
     sample alike add 1.0 mL of the lanthanum chloride solution,  i.e.,  20 mL of
     standard or sample + 2 mL LaCl3 - 22 mL.
                        (General)
1.   Calcium hollow cathode lamp
2.   Wavelength:  422.7 nm
3 .   Fuel :   Acetylene
4 .   Oxidant :  Air
5.   Type of flame:  Reducing
Notes

1.   Phosphate, sulfate and aluminum interfere but are masked by the addition of
     lanthanum.  Because low calcium values result if the pH of the sample is above
     7,  both standards and samples are prepared in dilute hydrochloric acid
     solution.  Concentrations of magnesium greater than 1000 mg/L also cause low
     calcium values.  Concentrations of up to 500 mg/L each of sodium, potassium and
     nitrate cause no interference.

2.   Anionic chemical interferences can be expected if lanthanum is not used in
     samples and standards .
3.   The nitrous oxide -acetylene flame will provide two to five times greater
     sensitivity and freedom from chemical intef erences .  lonization interferences
     should be controlled by adding a large amount of alkali to the sample and
     standards.  The analysis appears to be free from chemical suppressions in the
     nitrous oxide -acetylene flame.  (Atomic Absorption Newsletter 14, 29 [1975]).
4.   The 239.9 nm line may also be used.  This line has a relative sensitivity of
     120.
*CLP-M modified for the Contract Laboratory  Program.
                                     D-41                                ILM02.0

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                                                                 Exhibit D Method 242.1
                                      MAGNESIUM

              Method 242.1 CLP-M* (Atomic Absorption, Flame Technique)

Optimum Concentration Range:  0.02-0.5 rag/L using a wavelength of 285.2 nm
Sensitivity:  0.007 mg/L
Detection Limit:  0.001 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 0.829 g of magnesium oxide,  MgO (analytical reagent
     grade) , in 10 mL of redistilled HNC-3 and dilute to 1 liter with deionized
     distilled water.   1 mL - 0.50 mg Mg (500 mg/L).

2.   Lanthanum chloride solution:   Dissolve 29 g of La2°3>  slowly and in small
     portions in 250 mL concentrated HC1 (Caution:   Reaction is violent), and dilute
     to 500 mL with deionized distilled water.

3.   Prepare dilutions of the stock magnesium solution to be used as calibration
     standards at the time of analysis.  To each 10 mL volume of .calibration. .-- .:.-.-_;
     standard and sample alike add 1.0 mL of the lanthanum  chloride solution, i.e.,
     20 mL of standard or sample + 2 mL LaCl3 - 22  mL.

Instrumental Par^ers (General)
1.   Magnesium hollow cathode lamp
2.   Wavelength:   285.2 nm
3 .   Fuel :   Acetylene
4 .   Oxidant :   Air
5.   Type of flame:   Oxidizing

Notes

1.   The interference -caused by aluminum at -concentrations -greater _than_2 mg/L_is
    . masked by addition of lanthanum.   Sodium,, potassium and calcium cause -no
     interference at concentrations less than 400 mg/L.

2.   The following line may also be used:  202.5 nm Relative Sensitivity 25.

3.   To cover the range of magnesium values normally observed in surface waters
     (0.1-20 mg/L),  it is suggested that either the 202.5 nm line be used or the
     burner head be rotated.  A 90° rotation of the burner head will produce
     approximately one -eighth the normal sensitivity.
*CLP-M modified for the Contract Laboratory Program.
                                     D-42                                ILM02.0

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                                                                 Exhibit D Method 258.1
                                     POTASSIUM

              Method 258.1 CLP-M* (Atomic Absorption,  Flame Technique)

Optimum Concentration Range:  0.1-2 mg/L using a wavelength of 766.5 nm
Sensitivity:  0.04 mg/L
Detection Limit:  0.01 mg/L
Preparation of Standard Solution

1.   Stock Solution:  Dissolve 0.1907 g of KC1 (analytical reagent  grade),  dried at
     110°C,  in deionized distilled water and make up to 1 liter.  1  mL - 0.10 mg K
     (100 mg/L).
2.   Prepare -dilutions of the stock solution to be used as calibration standards at
     the cine of analysis.  The calibration standards  should be prepared using the
     sane type of acid and at the sane concentration as will result in the  sample to
     be analyzed either directly or after processing.
             Paraet trs (General)
1.   Potassium hollow cathode lamp
2.   Wavelength:  766.5 nm
3 .   Fuel :  Acetylene
4.   Oxidant:  Air
5.   Type of flame:  Slightly oxidizing

Notes

1.   In air-acetylene or other high temperature flames (>2800°C) , potassium can
     experience partial ionization which indirectly affects absorption sensitivity.
     The presence of other alkali salts in the sample can reduce  this  ionization and
     thereby enhance analytical results.  The ionization suppressive effect of
     sodium is small if the ratio~of Na : to K is" under* 107  Any~*nhancement- due~ to
     sodium can be stabilized by adding excess sodium (1000 ug/mL)  to  both sample
     and standard solutions. If nore stringent control of ionization is required,
     the addition of cesium should be considered.   Reagent blanks oust be analyzed
     to correct for potassium impurities in the buffer zone.
2.   The 404.4 nm line nay also be used.  This line has a relative  sensitivity of
     500.        _

3.   To cover the range of potassium values normally observed in surface waters
     (0.1-20 mg/L), it is suggested that the burner head be rotated. A 90° rotation
     of the burner head provides approximately one-eighth the normal sensitivity.
 CLP-M modified for the Contract Laboratory Program.
                                     D-43                                ILM02.0

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                                                                 Exhibit D Method 273.1
                                       SODIUM

              Method 273.1 CLP-M  (Atomic Absorption,  Flame Technique)

Optimum Concentration Range:  0.03-1 mg/L using a wavelength of 589.6 nm
Sensitivity:  0.015 mg/L
Detection Limit:  0.002 ffig/L
Preparation of Standard Solutions

1.   Stock Solution:   Dissolve 2.542 g of NaCl  (analytical  reagent grade),  dried at
     140°C,  in deionized distilled water  and make  up to  1 liter.  1 mL - 1 mg Na
     (1000 mg/L).
2.   Prepare dilutions of the stock  solution to be used  as  calibration standards at
     the tine of analysis.  The calibration standards  should be prepared using the
     sane type of acid and at the same concentration as  will result in the sample to
     be analyzed either directly or  after processing.
Instrumental Par?pgtr?rs (General)

1.   Sodium hollow cathode lamp
2.   Wavelength:   589.6 nm
3.   Fuel:   Acetylene
4.   Oxidant:   Air
5.   Type of flame:   Oxidizing

Notes

1.   The 330.2 nm resonance line of  sodium, which  has  a  relative  sensitivity of 185,
     provides a convenient way to avoid the need to dilute  more concentrated
     solutions of sodium.

2. _  Low-temperature flames increase sensitivity by reducing the extent of  . _	
     ionization of this easily ionized metal.   lonization may also be controlled by
     adding potassium (1000 mg/L) to both standards and  samples.
*CLP-M modified for the Contract Laboratory Program.
                                     D-44                                ILM02.0

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           PART D - COLD VAPOR METHODS FOR MERCURY ANALYSIS
Method                                                            Page No.

Mercury Analysis in Water by Manual Cold Vapor Technique            D-46
Method 245.1 CLP-M

Mercury Analysis in Water by Automated Cold Vapor Technique         D-52
Method 245.2 CLP-M

Mercury Analysis in Soil/Sediment by Manual Cold Vapor Technique    D-58
Method 245.5 CLP-M
 CLP-M modified for the Contract Laboratory Program.
                                   D-45                                ILM02.C

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-------
                                                                  Exhibit D Method 245.1
              MERCURY ANALYSIS IN WATER BY MANUAL CPU) VAPOR TECHNIQUE

                                      MERCURY
                  Method 245.1 CLP-M*  (Manual Cold Vapor Technique)


1.    Scope and Application       (

1.1   In addition to inorganic forms of mercury, organic mercurials may also be
      present.  These organo-mercury compounds will not respond to the cold vapor
      atomic absorption technique unless they are first broken down and converted to
      mercuric ions.  Potassium permanganate oxidizes many of these compounds,  but
      recent studies have shown that a number of organic mercurials, including
      phenyl mercuric acetate and methyl mercuric chloride, are only partially
      oxidized by this reagent.  Potassium persulfate has been found to give
      approximately 100% recovery when used as the oxidant with these compounds.
      Therefore, a persulfate oxidation step following the addition of the
      permanganate has been included to insure that organo-mercury compounds, if
      present, will be oxidized to the mercuric ion before measurement.  A heat step
      is required for methyl mercuric chloride when present in or spiked to a
      natural system.

1.2   The range of the method may be varied through instrument and/or recorder
      expansion.  Using a 100 mL sample, a detection limit of 0.2 ug Hg/L can be
      achieved (See 10.2).

2.    gymjfla|*v of Method

2.1   The flameless AA procedure is a physical method based on the absorption of
      radiation at 253.7 not by mercury vapor.  Organic mercury compounds are
      oxidized and the mercury is reduced to the elemental state and aerated from
      solution in a closed system.  The mercury vapor passes through a cell
      positioned in the light path of an atomic .absorption spectrophotometer.
      Absorbance (peak height) is measured as a function of mercury concentration
      and recorded in the usual manner.

3.    Sample Handling and Preservation

3.1   Until more conclusive data are obtained, samples are preserved by
      acidification with nitric acid/ to a pH of 2 or lower immediately at the time
      of collection  (Exhibit D, Section II).

4.    Interference

4.1   Possible interference from sulfide is eliminated by the addition of potassium
      permanganate.  Concentrations as high as 20 mg/1 of sulfide as sodium  sulfide
      do not interfere with the recovery of added inorganic mercury from distilled
      water (Exhibit D, Section II).

4.2   Copper has also been reported to  interfere; however, copper concentrations as
      high as 10 mg/L had no effect on  recovery of mercury from  spiked samples.
 CLP-M modified for the Contract Laboratory Program.
                                     D-46                                ILM02.0

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                                                                 Exhibit D Method 245.1
4.3   Sea waters,  brines and industrial effluents high in chlorides require
      additional permanganate (as much as 25 mL).  During the oxidation step,
      chlorides are converted to free chlorine which will also absorb radiation of
      253 run.  Care must be taken to assure that  free chlorine is absent before the
      mercury is reduced and swept into the cell.  This may be accomplished by using
      an excess of hydroxylamine sulfate reagent  (25 mL).   Both inorganic and
      organic mercury spikes have been quantitatively recovered from the sea water
      using this technique.

5.     Apparatus

5.1   Atomic Absorption Spectrophotometer:   (See  Note  1)  Any atomic absorption unit
      having an open sample presentation area in  which to mount the absorption cell
      is suitable.  Instrument settings recommended by the particular manufacturer
      should be followed.

      NOTE 1:  Instruments designed specifically  for the  measurement of mercury
      using the cold vapor technique are commercially available and may be
      substituted for the atomic absorption Spectrophotometer^
5.2
Mercury Hollow Cathode Lamp:  Vestinghouse VL-22847,  argon filled, or
equivalent.
5.3   Recorder:  Any multi-range variable speed recorder that is compatible with the
      UV detection system is suitable.

5.4   Absorption Cell:  Standard spectrophotometer cells 10 cm long,  having quartz
      end windows may be used.  Suitable cells may be  constructed from plexiglass
      tubing, 1" O.D. X 4-1/2".  The ends are ground perpendicular to the
      longitudinal axis and quartz windows (1" diameter X 1/16" thickness) are
      cemented in place.

      The cell is strapped to a burner for support and aligned in the light beam by
      use of two 2" by 2" cards.  One inch diameter holes are cut in the middle of
      each card; the cards are then placed over each end of the cell.  The cell is
      then positioned and adjusted vertically and horizontally to find the maximum
      transmittance.

5.5   Air Pump:  Any peristaltic pump capable of delivering 1 liter of air per
      minute may be used.  A Masterflex pump with electronic speed control has been
      found to be satisfactory.

5.6   Flowmeter:  Capable of measuring an air,'flow of 1 liter per minute.

5.7   Aeration Tubing:  A straight glass frit having a coarse porosity.  Tygon
      tubing is used for passage of the mercury vapor from the sample bottle to the
      absorption cell and return.

5.8   Drying Tube:  6" X 3/4" diameter tube containing 20 g of magnesium perchlorate
      (see Note 2).  The apparatus is assembled as shown in Figure 1.

      NOTE 2:  In place of the magnesium perchlorate drying tube, a small reading
      lamp with SOW bulb may be used to prevent condensation of moisture inside the
      cell.  The lamp is positioned to shine on the absorption cell maintaining the
      air temperature in the cell about 10°C above ambient.
                                     D-47                                ILM02.0

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                                             Exhibit D Method 245.1
   Figure 1.  Apparatus for Flameless Mercury Determination
            AIR PUMP
             DESICCANT
                      ABSORPTION
           6UB8LER      CELL
SAMPLE SOLUTION
IN BOO BOTTLE
SCRUBBER
CONTAINING
A MERCURY
ABSORBING
MEDIA
                      D-48
 ILM02.0

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                                                                 Exhibit D Method 245.1
6.    Reagents

6.1   Sulfuric Acid, Cone:  Reagent grade.

      6.1.1   Sulfuric acid, 0.5 N:  Dilute 14.0 mL of cone,  sulfuric acid to 1.0
              liter.

6.2   Nitric Acid, Cone:   Reagent grade of low mercury content (see Note  3).

      NOTE 3:  If a high reagent blank is obtained,  it may be  necessary to  distill
      the nitric acid.

6.3   Stannous Sulfate:   Add 25 g stannous sulfate to 250  mL of 0.5 N  sulfuric acid.
      This mixture is a suspension and -should be stirred continuously  during use.
      (Stannous chloride may be used in place of stannous  sulfate.)

6.4   Sodium Chloride-Hyroxylamine Sulfate Solution:   Dissolve 12 g of sodium
      chloride and 12 g of hydroxylamihe sulfate in distilled  water and dilute to
      100 mL.  (Hydroxylamine hydrochloride may be used in place of hydroxylamine
      sulfate.)

6.5   Potassium Permanganate:  5% solution, w/v.  Dissolve 5 g of potassium
      permanganate in 100 mL of distilled water.

6.6   Potassium Persulfate:  5% solution, w/v.   Dissolve 5 g of potassium persulfate
      in 100 mL of distilled water.

6.7   Stock Mercury Solution:  Dissolve 0.1354 g of mercuric chloride  in  75 mL of
      distilled water.   Add 10 mL of cone,  nitric acid and adjust the  volume to
      100.0 mL.   1 mL - 1 mg_Hg.	  ._.

6.8   Working Mercury Solution:  Make successive dilutions of  the stock mercury
      solution to obtain a working standard containing 0.1 ug  per ml..   This working
      standard and the dilutions of the stock mercury solution should  be  prepared
      fresh daily.  Acidity of the working standard should be  maintained  at 0.15%
      nitric acid.  This acid should be added to the flask as  needed before the
      addition of the aliquot.

7.    Calibration

7.1   Transfer 0, 0.5,  1.0, 5.0 and 10.0 mL aliquots of the working mercury solution
      containing 0 to 1.0 ug of mercury to a series of 300 mL BOD bottles.  Add
      enough distilled water to each bottle to make a total volume  of 100 mL.   Mix
      thoroughly and add 5 mL of cone,  sulfuric acid (6.1) and 2.5 mL of cone.
      nitric acid (6.2)  to each bottle.  Add 15 mL of KMn04 (6.5)  solution to each
      bottle and allow to stand at least 15 minutes.  Add 8 mL of potassium
      persulfate (6.6) to each bottle and heat for 2 hours in a water bath
      maintained at 95°C.  Alternatively, cover the BOD bottles with foil and heat
      in an autoclave for 15 minutes at 120°C and 15 Ibs.   Cool and add 6 mL of
      sodium chloride-hydroxylamine sulfate solution (6.4) to reduce the excess
      permanganate.  When the solution has been decolorized wait 30 seconds,  add 5
      mL of the stannous sulfate solution  (6.3) and immediately attach the bottle to
      the aeration apparatus forming a closed system.  At this point the sample is
      allowed to stand quietly without manual agitation.
                                     D-49                                ILM02.0

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                                                                 Exhibit D Method 245.1
      The circulating pump, which has previously been adjusted to a rate of 1 liter
      per minute, is allowed to run continuously (see Note 4).  The absorbance will
      increase and reach maximum within 30 seconds.  As soon as the recorder pen
      levels off, approximately 1 minute, open the bypass valve and continue the
      aeration until the absorbance returns to its minimum value (see Note 5).
      Close the bypass valve, remove the stopper and frit from the BOD bottle and
      continue the aeration.  Proceed with the standards and construct a standard
      curve by plotting peak height versus micrograms of mercury.

      NOTE 4:  An open system where the mercury vapor is passed through the
      absorption cell only once may be used instead of the closed system.

      NOTE 5:  Because of the toxic- nature of mercury vapor precaution must be taken
      to avoid its inhalation.  Therefore, a bypass has been included in the system
      to either vent the mercury vapor into an exhaust hood or pass the vapor
      through some absorbing media, such as:  a)      equal volumes of 0.1 H KMn04,
      and 10% H2S04  or                       ''.'•' ~ '.'. ~ ~  ~. ~  .
      b) 0.25% iodine in a 3% a KI solution.  A specially treated charcoal that will
      adsorb mercury vapor is available.

8.    Procedure

8.1   Transfer 100 mL, or an aliquot diluted to 100 mL, containing not more than 1.0
      ug of mercury, to a 300 mL BOD bottle.  Add 5 mL of sulfuric acid (6.1) and
      2.5 mL of cone,  nitric acid  (6.2)  mixing after each additon.  Add 15 mL of
      potassium permanganate solution (6.5) to each sample bottle (see Note 6).  For
      sewage samples additional permanganate may be required.  Shake and add
      additional portions of potassium permanganate solution, if necessary, until
      the purple color persists for at least 15 minutes.  Add 8 mL of potassium
      persulfate (6.6) to each bottle and heat for 2 hours in a water bath at 95°C.

      NOTE 6:  The same amount of KMnO^ added to the samples should be present in
      standards and blanks.

      Cool and add 6 mL of sodium chloride-hydroxylamine sulfate (6.4) to reduce the
      excess permanganate (see Note 7).   Purge the head space in the BOD bottle for
      at least 1-minute and add 5 mL of Stannous Sulfate (6.3) and immediately
      attach the bottle to the aeration apparatus.  Continue as described under
      Calibration.

      NOTE 7:  Add reductant in 6 mL increments until KMn04 is completely reduced.

9.    Calculation

9.1   Determine the peak height of  the unknown from the chart and read the mercury
      value from the standard curve.

9.2   Calculate the mercury concentration in the sample by the formula:

                       ug Hg in                 1,000
          ug Hg/L  -    aliquot    x
                                        volume of aliquot in mL
                                                                         ILM02.0

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                                                                 Exhibit D Method 245.1
10.   Appendix

10.1  If additional sensitivity is required,  a 200 ml, sample with recorder expansion
      may be used provided the instrument does not produce undue noise.  Using a
      Coleman MAS-50 with a drying tube of magnesium perchlorate and a variable
      recorder, 2 mv was set to read full scale.   With these conditions,  and
      distilled water solutions of mercuric chloride at concentrations of 0.15,
      0.10, 0.05 and 0.025 ug/L the standard deviations were ±0.027, ±0.0006, ±0.01
      and ±0.004.  Percent recoveries at these levels were 107,  83,  84 and 96%,
      respectively.

10.2  Directions for the disposal of mercury-containing wastes are given in ASTM
      Standards, Part 31, "Water", p. 349, Method D3223 (1976).
                                     D-51                                IIM02.0

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                                                                  Exhibit D Method 245.2
             MERCURY ANALYSIS IN WATER BY AUTOMATED  COLD VAPOR  TECHNIQUE

                                       MERCURY
                Method 245.2 CLP-M   (Automated Cold Vapor Technique)


1.    Scope and Application

1.1   The working range is 0.2 to 20.0 ug Hg/L.

2 .    S'l'IPIP'Ty of Method

2.1   The flameless AA procedure is a physical method based on -the absorption of
      radiation at 253.7 run by mercury vapor.  The mercury is reduced to the
      elemental state and aerated from solution.  The mercury vapor passes through a
      cell positioned in the light path of an atomic absorption spectrophotometer.
      Absorbance (peak height) is measured as a function of mercury concentration
      and recorded in the usual manner.

2.2   In addition to inorganic forms of mercury, organic mercurials may also be
      present.  These organo -mercury compounds will not respond to the flameless
     v atomic absorption technique unless they are first broken down and converted to
      mercuric ions.  Potassium permanganate oxidizes many of these compounds, but
      recent studies have shown that a number of organic mercurials, including
      phenyl mercuric acetate and methyl mercuric chloride, are only partially
      oxidized by this reagent.  Potassium persulfate has been found to give
      approximately 100% recovery when used as the oxidant with these compounds.
      Therefore, an automated persulfate oxidation step following the automated
      addition of the permanganate has been included to insure that organo -mercury
      compounds, if present,  will be oxidized to the mercuric ion before --
      measurement .
3.    Sflnipl? Handling and Preservation

3.1   Until more conclusive data are obtained, samples are preserved by
      acidification with nitric acid to a pH of 2 or lower immediately at the time
      of collection (Exhibit D, Section II).

4.    Interferences (see NOTE 1)

4.1   Some sea waters and waste-waters high in chlorides have shown a positive
      interference, probably due to the formation of free chlorine.

4.2   Formation of a heavy precipitate, in some wastewaters and effluents, has been
      reported upon addition of concentrated sulfuric acid.  If this is encountered,
      the problem sample cannot be analyzed by this method.

4.3   Samples containing solids must be blended and then mixed while being sampled
      if total mercury values are to be reported.

      NOTE 1:  All of the above interferences can be overcome by use of the Manual
      Mercury method.
 CLP-M modified for the Contract Laboratory Program.
                                     D-52                                ILM02.0

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                                                                 Exhibit D Method 245.2
5.    Apparatus

5.1   Technicon Auto Analyzer or equivalent instrumentation consisting of:

      5.1.1    Sampler II with provision for sample mixing.

      5.1.2    Manifold.

      5.1.3    Proportioning Pump II or III.

      5.1.4    High temperature heating bath with two distillation coils (Technicon
               Part #116-0163) in series.

5.2   Vapor-liquid separator (Figure 1).

5.3   Absorption cell,  100 mm long,  10 mm diameter with quartz windows.

5.4   Atomic Absorption Spectrophotometer (see Note  2):   Any atomic  absorption unit
      having an open sample presentation area in which  to mount  the  absorption cell
      is suitable.   Instrument settings recommended  by  the particular manufacturer
      should be followed.

      NOTE 2:  Instruments designed specifically for the measurement of mercury
      using the cold vapor technique are commercially available  and  may be
      substituted for the  atomic absorption Spectrophotometer.

5.5   Mercury Hollow Cathode Lamp:   Vestinghouse WL-22847, argon filled,  or
      equivalent.

5.6   Recorder:  Any multi-range variable speed recorder that is compatible with the
      UV detection system  is suitable.

6.    Reagents

6.1   Sulfuric Acid,  Cone:   Reagent grade

      6.1.1    Sulfuric acid, 2 N:  Dilute 56 mL of cone,  sulfuric acid to  1 liter
               with distilled water.

      6.1.2    Sulfuric *cid, 10%:  Dilute 100 mL cone,  sulfuric  acid to  1  liter
               with distilled water.

6.2   Nitric acid, Cone:  Reagent grade of low mercury content.

      6.2.1.   Nitric Acid, 0.5% Wash  Solution:  Dilu.e  5 mL of  concentrated nitric
               acid to 1 liter with  distilled water.

6.3   Stannous Sulfate (See Note 3):  Add 50 g stanncus sulfate to 500 mL of 2 N
      sulfuric acid (6.1.1).  This mixture is a suspension and should be stirred
      continuously during use.

      NOTE 3:  Stannous chloride may be used in place of  stannous sulfate.
                                     D-53                                ILM02.0

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                                                                 Exhibit D Method 245.2
6.4   Sodium Chloride-Hydroxylamine Sulfate (See Note 4) Solution:   Dissolve 30  g of
      sodium chloride and 30 g of hydroxylamine sulfate in distilled water to 1
      liter.

      NOTE 4:  Hydroxylamine hydrochloride may be used in place of hydroxylamine
      sulfate.
                                  i,
6.5   Potassium Permanganate:  0.5% solution,  w/v.  Dissolve 5 g of potassium
      permanganate in 1 liter of distilled water.

6.6   Potassium Permanganate, 0.1 N:  Dissolve 3.16 g, of potassium permanganate  in
      distilled water and dilute to 1 liter.

6.7   Potassium Persulfate:  0.5% solution, w/v.  Dissolve 5-g-potassium persulf ate
      in 1 liter of distilled water.

6.8   Stock Mercury Solution:  Dissolve 0.1354 g of mercuric chloride in 75 mL of
      distilled water.   Add 10 mL of cone, nitric acid and adjust the volume to
      100.0 mL.  1.0 mL - 1.0 mg Hg.

6.9   Working Mercury Solution:  Make successive dilutions of the stock mercury
      solution (6.8) to obtain a working standard containing 0.1 ug per mL.  This
      working standard and the dilutions of the stock mercury solution should be
      prepared fresh daily.  Acidity of the working standard should be maintained at
      0.15% nitric acid.  This acid should be  added to the flask as needed before
      the addition of the aliquot.   From this  solution prepare standards containing
      0.2, 0.5, 1.0, 2.0, 5.0, 10.0, 15.0 and  20.0 ug Hg/L-

6.10  Air Scrubber Solution:  Mix equal volumes of 0.1 N potassium permanganate
      (6.6) and 10% sulfuric acid (6.1.2).

7.    Procedure (See Note 5)
7.1   Set up manifold as shown in Figure 2.
7.2   Feeding all the reagents through the system with acid wash solution (6.2.1)
      through the sample line, adjust heating bath to 105°C.

7.3   Turn on atomic absorption spectrophotometer, adjust instrument settings as
      recommended by the manufacturer, align absorption cell in light path for
      maximum transmittance and place heat lamp directly over absorption cell.

7.4   Arrange working mercury standards from Q.2 to 20.0 ug Hg/L in sampler and
      start sampling.  Complete loading of sample tray with unknown samples.

7.5   Prepare standard curve by plotting peak height of processed standards against
      concentration values.  Determine concentration of samples by comparing sample
      peak height with standard curve.

7.6   After the analysis is complete put all lines-except the H2S04 line inv
      distilled water to wash out system.  After flushing, wash out the H2S04 line.
      Also flush the coils in the high temperature heating bath by pumping staimous
      sulfate (6.3) through the sample lines followed by distilled water.  This will
      prevent build-up of oxides of manganese.
                                     D-54                                ILM02.0

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                                                           Exhibit  D Method 245.2
NOTE 5:  Because of the toxic nature of mercury vapor, precaution must be
taken to avoid its inhalation.  Venting the mercury vapor into an exhaust hood
or passing the vapor through some absorbing media such as:  a) equal volumes
of 0.1 N KMn04(6.6) and 10% H2S04 (6.1.2), or b)      0.25% iodine in a 3% KI
solution, is recommended.  A specially treated charcoal that will absorb
mercury vapor is also available.
                               D-55                                 ILM02.0

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                                                  Exhibit D Method 245.1
AIR  AND

SOLUTION
IN

                              7/25 T
                O.4 cm ID
0.7 cm 10
                                             AIR
                                             OUT
                           14 cm
                                                 SOLUTION
                                                  OUT
          Figure 1.  Vapor liquid separator

                       D-56
                                                       ILM02.0

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                                          Exhibit D Method 245.
Figure 2.  Mercury Manifold AA-1
              D-57
ILM02.0

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                                                                 Exhibit D Method 245.5
          MERCURY ANALYSIS IN SOIL/SEDIMENT BY MANUAL COLD VAPOR TECHNIQUE

                               MERCURY (in Sediments)
                 Method 245.5 CLP-M   (Manual Cold Vapor Technique)

1.    Scope and Application      v

1.1   This procedure measures total mercury (organic and inorganic) in soils,
      sediments, bottom deposits and sludge type materials

1.2   The range of the method is 0.2 to 5 ug/g.   The range may be extended above or
      below the normal range by increasing or decreasing sample size or through
      instrument and recorder control
2 .     ?VTPfHfl^y °^ Method

2.1   A weighed portion of the sample is acid digested for 2 minutes at 95°C,
      followed by oxidation with potassium permanganate and potassium persulfate.
      Mercury in the digested sample is then measured by the conventional cold vapor
      technique

2.2   An alternate digestion involving the use of an autoclave is described in (8.2)

3 .     ??nrc*le Handling and Preservation

3.1   Because of the extreme sensitivity of the analytical procedure and the
      omnipresence of mercury, care must be taken to avoid extraneous contamination.
      Sampling devices and sample containers should be ascertained to be free of
      mercury; the sample should not be exposed to any condition in the laboratory
      that may result in contact or air -borne -aercury contamination-

3.2   Refrigerate solid samples at 4°C (±2°) upon receipt until analysis (see
      Exhibit D, Section II).

3.3   The sample should be analyzed without drying.  A separate percent solids
      determination is required, (Part F) .

4.     Interferences

4.1   The same types of interferences that may occur in water samples are also
      possible with sediments, i.e., sulfides, high copper, high chlorides, etc.

4.2   Samples containing high concentrations of oxidizable organic materials, as
      evidenced by high chemical oxygen demand values , may not be completely
      oxidized by this procedure.  When this occurs, the recovery of organic mercury
      will be low.  The problem can be eliminated by reducing the weight of the
      original sample or by increasing the amount of potassium persulfate (and
      consequently stannous chloride) used in the digestion.
 CLP-M modified for the Contract Laboratory Program.
                                     D-58                                ILM02.0

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                                                                 Exhibit D Method 245.5
5.    Apparatus

5.1   Atomic Absorption Spectrophotometer (see Note 1):   Any atomic  absorption unit
      having an open sample presentation area in which to mount  the  absorption cell
      is suitable.   Instrument settings recommended by the particular  manufacturer
      should be followed

      NOTE 1:  Instruments designed specifically for the measurement of mercury
      using the cold vapor technique are commercially available  and  may be
      substituted for the atomic absorption Spectrophotometer

5.2   Mercury Hollow Cathode Lamp:   Westinghouse WL-22847, argon filled, or
      equivalent

5.3   Recorder:  Any multi-range variable speed recorder that is compatible with the
      UV detection system is suitable.
5.4   Absorption Cell:   Standard Spectrophotometer cells 10 cm long,  having quartz
      end windows may be used.   Suitable cells many be constructed from pexiglass
      tubing,  1" O.D.  X 4-1/2".  The ends are ground perpendicular to the
      longitudinal axis and quartz windows (1" diameter X 1/16" thickness) are
      cemented in place.  Gas inlet and outlet ports (also of plexiglass but 1/4"
      O.D.) are attached approximately 1/2" from each end.  The cell  is strapped to
      a burner for support and aligned in the light beam to give-the  maximum
      transmittance.  Two 2" X 2" cards with one inch diameter holes  may be placed
      over each end of  the cell to assist in positioning the cell for maximum
      transmittance.

5.5   Air Pump:  Any peristaltic pump capable of delivering 1 liter of air per
      minute may be used.  A Masterflex pump with electronic speed control has been
      found to be satisfatory.   (Regulated compressed air can be used in an open
      one-pass systern.)

5.6   Flowmeter:  Capable of measuring an air flow of 1 liter per minute

5.7   Aeration Tuning:   Tygon tubing is used for passage of the mercury vapor from
      the sample bottle to the absorption cell and return.  Straight glass tubing
      terminating in a  coarse porous frit is used for sparging air into the sample

5.8   Drying Tube:  6"  X 3/4" diameter tube containing 20 g of magnesium perchlorate
      (see Note 2).

      NOTE 2:      In place of the magnesium perchlorate drying tube,  a small reading
      lamp with 60V bulb may be used to prevent condensation of moisture inside the
      cell.  The lamp is positioned to shine on the absorption cell maintaining the
      air temperature in the cell about 10°C above ambient.

6.    Reagents

6.1   Sulfuric acid, cone.:  Reagent grade of low mercury content

6.2   Nitric acid, cone.:  Reagent grade of low mercury content
                                                                         ^» »*/»rt

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                                                                  Exhibit D Method 245.5
6.3   Stannous Sulfate:  Add  25 g stannous sulfate to 250 mL of 0.5 N sulfuric acid
      (6.2).  This mixture  is a suspension and should be stirred continuously during
      use

6.4   Sodium Chloride-Hydroxylamine Sulfate (See Note 3) Solution:  Dissolve 12 g of
      sodium chloride and 12  g of hydroxylamine sulfate in distilled water and
      dilute to 100 mL

      NOTE 3:     A 10% solution of stannous chloride may be substituted for (6.3)
      and hydroxylamine hydrochloride may be used in place of hydroxylamine sulfate
      in (6.4)

6.5   Potassium Permanganate:  5% solution, w/v.  Dissolve 5 g-of potassium
      permanganate in 100 mL of distilled water

6.6   Potassium Persulfate:   5% solution, w/v.  Dissolve 5 g of potassium persulfate
      in 100 mL of distilled water

6.7   Stock Mercury Solution:  Dissolve 0.1354 g of mercuric chloride in 75 mL of
      distilled water.   Add mL of cone,  nitric acid and adjust the volume to 100.0
      mL.  1.0 - 1.0 mg Hg

6.8   Working Mercury Solution:   Make successive dilutions of the stock mercury
      solution (6.7) to obtain a working standard containing 0.1 ug/mL.  This
      working standard and the dilution of the stock mercury solutions should be
      prepared fresh daily.   Acidity of the working standard should be maintained at
      0.15% nitric acid.  This acid should be added to the flask as needed before
      the addition of the aliquot

7.    Calibration

7.1   Transfer 0,  0.5,  1.0,  5.0 and 10 mL aliquots of the working mercury solutions
      (6.8) containing 0 to 1.0 ug of mercury to a series of 300 mL BOD bottles.
      Add enough distilled water to each bottle to make a total volume of 10 mL.
      Add 5 mL of cone.   H2S(>4 (6.1) and 2.5 mL of cone.  HNOs (6.2) and heat 2
      minutes in a water bath at 95°C.  Allow the sample to cool and add 50 mL
      distilled Hater,  15 mL of KMnC<4 solution (6.5) and 8 mL of potassium
      persulfate solution (6.6) to each bottle and return to the water bath for 30
      minutes.  Cool and add 6 mL of sodium chloride-hydroxylamine sulfate solution
      (6.4) to reduce the excess permanganate.  Add 50 mL of distilled water.
      Treating each bottle individually, add 5 mL of stannous sulfate solution (6.3)
      and immediately attach the bottle to the aeration apparatus.  At this point
      the sample is allowed to stand quietly without manual agitation.  The
      circulating pump,  which has previously been .adjusted to a rate of 1 liter per
      minute, is allowed to run continuously.  The absorbance, as exhibited either
      on the spectrophotometer or the recorder, will increase and reach maximum
      within 30 seconds.  As soon as the recorder pen levels off, approximately 1
      minute, open the bypass valve and continue the aeration -until the absorbance
      returns to its minimum value (see Note 4).  Close the bypass valve, remove the
      fritted tubing from the BOD bottle and continue the aeration.  Proceed with
      the standards and construct a standard curve by plotting peak height versus
      micrograms of mercury
                                     D-60                                ILM02.0

-------
                                                                 Exhibit D Method 245.!
      NOTE 4:     Because of the toxic nature of mercury vapor,  precaution must be
      taken to avoid its inhalation.  Therefore, a b>-pass has been included in the
      system to either vent the mercury vapor into an exhaust hood or pass the vapor
      through some absorbing sedis., such as:   a) equal volumes of 0.1 N KMn04 and
      10% H2S04, or b) 0.25% iodine in a 3% KI solution.  A specially treated
      charcoal that will absorb mercury vapor is also available.

8.    Procedure

8.1   Weigh a representative 0.2 g portion of wet sample and place in the bottom of
      a BOD bottle.  Add 5 mL of sulfuric acid (6.1)  and 2.5 mL of concentrated
      nitric acid (6.2) mixing after each addition.  Heat two minutes in a water
      bath at 95°C.  Cool, add 50 mL distilled water,  15 mL potassium permanganate
      solution (6.5) and 8 mL of potassium persulfate solution (6.6)  to each sample
      bottle.  Mix thoroughly and place in the water  bath for 30 minutes at 95°C.
      Cool and add 6 mL of sodium chloride-hydroxylamine sulfate (6.4) to reduce the
      excess permanganate.  Add 55 mL of distilled water.   Treating each bottle
      individually, purge the head space of the sample bottle for at  least one
      minute and add 5 mL of stannous sulfate (6.3) and immediately attach the
      bottle to the aeration apparatus.   Continue as  described under  (7.1)

8.2   An alternate digestion procedure employing an autoclave may also be used.  In
      this method 5 mL of cone.   ^804 and 2  mL of cone.  HN03 are added to the 0.2
      g of sample.  5 mL of saturated KMn04 solution  and 8 mL of potassium
      persulfate solution are added and the bottle is covered with a  piece of
      aluminum foil.   The sample is autoclaved at 121°C and 15 Ibs.  for 15 minutes.
      Cool, make up to a volume of 100 mL with distilled water and add 6 mL of
      sodium chloride-hydroxylamine sulfate solution  (6.4) to reduce  the excess
      permanganate.  Purge the head space of the sample bottle for at least one
      minute and continue as described under (7.1)

9.    Calculations

9.1   Measure the peak height of the unknown from the chart and read  the mercury
      value from the standard curve

9.2   Calculate the mercury concentration in the sample by the formula:

                    ug Hg in the aliquot
          «g Hg/g - wt of the aliquot in gms
                    (based upon dry wt of the sample)

9.3   Report mercury concentrations as described for aqueous mercury  samples
      converted to units of mg/kg.  The sample result or the detection  limit for
      each sample must be corrected for sample weight and % solids before reporting.
                                     D-61                                ILM02.0

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                    PART E -  METHODS  FOR CYANIDE ANALYSIS
Method                                                            Page No.

Method for Total Cyanide Analysis in Water
Method 335.2 CLP-M                                                 D-63

Method for Total Cyanide Analysis in Soil/Sediment
Method 335.2 CLP-M                                                 D-71

Method for Total Cyanide Analysis by Midi Distillation
Method 335.2 CLP-M                                                 D-82
 CLP-M Modified for  the Contract Laboratory Program.
                                   D-62                                ILM02.0

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-------
                                                                 Exhibit D Method 335.2
                     METHOD FOR TOTAL CYANIDE ANALYSIS IN WATER

                              CYANIDE,  TOTAL (in Water)

                                stric;  Manual Spectr<
                                 Spectrophotometrie)
Method 335.2 CLP-M  (Titrimetric; Manual Spectrophotometric;  Semi-Automated
1.    Scope and Application

1.1   This method is applicable to the determination of cyanide in drinking, surface
      and saline waters, domestic and industrial wastes.

1.2   The titration procedure using silver nitrate with p-
      dimethylaminobenzalrhodanine indicator is used for measuring concentrations of
      cyanide exceeding 1 mg/L (0.25 mg/250 mL of absorbing liquid).  (Option A,
      8.2).

1.3   The manual colorometric procedure is used for concentrations below:.l mg/L of ._
      cyanide and is sensitive to about 0.01 mg/L.  (Option B, 8.3).

1.4   The working range of the semi-automated Spectrophotometric method is 0.020 to
      0.200 mg/L.  Higher level samples must be diluted to fall within the working
      range.  (Option C, 8.4).

2.    Stiimnarv of Method

2.1   The cyanide as (HRN) hydrocyanic acid (HCN) is released from cyanide complexes
      by means of a reflux-distillation operation and absorbed in a scrubber
      containing sodium hydroxide solution.  The cyanide ion in the absorbing
      solution is then determined by volumetric titration or colorioetrically.   	

2.2   In the colorimetric measurement the cyanide is converted to cyanogen chloride,
      CNC1, by reaction with chloramine-T at a pH less than 8 without hydrolyzing to
      the cyanate.  After the reaction is complete, color is formed on the addition
      of pyridine-pyrazolone or pyridinebarbituric acid reagent.  The absorbance is
      read at 620 nm when using pyridine-pyrazolone or 578 nm for pyridine-
      barbituric acid.  To obtain colors of comparable intensity, it is essential to
      have the vane salt content in both the sample and the standards.
2.3   The titimetric measurement uses a standard solution of silver nitrate to
      titrate cyanide in the presence of a silver sensitive indicator.

3.    Definitions

      Cyanide is defined as cyanide ion and complex cyanides converted to
      hydrocyanic acid (HCN) by reaction in a reflux system of a mineral acid in the
      presence of magnesium ion.

4.    Sample Handling and Preservation

4.1   All bottles must be thoroughly cleansed and rinsed to remove soluble material
      from containers.
 CLP-M Modified for the Contract Laboratory Program.
                                     D-63                                ILM02.0

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                                                                 Exhibit D Method 335.
4.2   Oxidizing agents such as chlorine decompose most of the cyanides.   Test  a  drop
      of the sample with potassium iodide-starch test paper (Kl-starch paper); a
      blue color indicates the need for treatment.   Add ascorbic acid, a few
      crystals at a time, until a drop of sample produces no color on the indicator
      paper.  Then add an additional 0.6 g of ascorbic acid for each liter of  sample
      volume.

4.3   Samples are preserved with 2 mL of 10 N sodium hydroxide per liter of sample
      (pH> 12) at the time of collection (Exhibit D,  Section II).

4.4   Samples must be stored at 4°C(±2°C) and must be analyzed within the holding
      time specified in Exhibit D, Section II.

5.    Interferences

5.1   Interferences are eliminated or reduced by using the distillation  procedure
      described in Procedure 8.1.

5.2   Sulfides adversely affect the colorimetric and titration procedures.  If a
      drop of the distillate on lead acetate test paper indicates the presence of
      sulfides, treat 25 mL more of the sample than that required for the cyanide
      determination with powdered cadmium carbonate.   Yellow cadmium sulfide
    •  precipitates if the sample contains sulfide.   Repeat this operation until  a
      drop of the treated sample solution does not darken the lead acetate test
      paper.  Filter the solution through a dry filter paper into a dry  beaker,  and
      from the filtrate measure the sample to be used for analysis.   Avoid a large
      excess of cadmium carbonate and a long contact time in order to minimize a
      loss by complexation or occlusion of cyanide on the precipitated material.
      Sulfides should be removed prior to preservation with sodium hydroxide as
      described in 4.3.

5.3   The presence of surfactants may cause the sample to foam during refluxing.  If
      this occurs, the addition of an agent such as Dow Corning 544 antifoam agent
      will prevent the foam from collecting in the condenser.  Fatty acids will
      distill and form soaps under alkaline titration conditions, making the end
      point almost impossible to detect.  When this occurs, one of the
      spectrophotometric methods should be used.

6.    Apparatus

6.1   Reflux distillation apparatus such as shown in Figure 1 or Figure 2.  The
      boiling flask should be of 1 liter size with inlet tube and provision for
      condenser.  The gas absorber may be a Fisher -Mill igan scrubber.

6.2   Microburet, 5.0 mL (for titration)

6.3   Spectrophotometer suitable for measurements at 578 nm or 620 nm with a  1.0 cm
      cell or larger  (for manual spectrophotometric method).

6.4   Technicon AA II System or  equivalent instrumentation,  (for automated
      spectrophotometric method)  including:

      6.4.1    Sampler

      6.4.2    Pump III
                                     D-64                                ILM02.0

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                                                                 Exhibit D Method 335.2
      6.4.3    Cyanide Manifold  (Figure 3)

      6.4.4    SCIC  Colorimeter  with 15 mm flowcells and 570 nm filters

      6.4.5    Recorder

      6.4.6    Data  System  (optional)

      6.4.7    Glass or plastic  tubes for the sampler

7.    Reagents

7.1   Distillation and Preparation Reagents

      7.1.1    Sodium hydroxide  solution, 1.25N:  Dissolve 50 g of NaOH in distilled
               water, and dilute to 1 liter with distilled water.

      7.1.2    Cadmium carbonate:  powdered

      7.1.3    Ascorbic acid:  crystals

      7.1.4    Sulfuric acid:  concentrated

      7.1.5    Magnesium chloride solution:  Weight 510 g of MgC^'ei^O into a 1000
               mL flask, dissolved and dilute to 1 lizer with distilled water.

7.2   Stock Standards and Titration Reagents

      7.2.1    Stock cyanide solution:  Dissolve 2.51 g of KCN and 2 g KOH in 1
               liter of distilled water.  Standardize with 0.0192 N AgN03.

      7.2.2    Standard cyanide  solution, intermediate:  Dilute 50.0 mL of stock (1
              mL -  1 mg CN) to  1000 mL with distilled water.

      7.2.3    Standard cyanide  solution:  Prepare fresh daily by diluting 100.0 mL
               of intermediate cyanide solution to 1000 mL with distilled water and
               store in a glass  stoppered bottle.  1 mL- 5.0 ug CN (5.0 mg/L).

      7.2.4    Standard silver nitrate solution, 0.0192 N:  Prepare by crushing
               approximately 5 g AgN(>3 crystals and drying to constant weight at
               40bC.  Weight out 3.2647 g of dried AgN<>3, dissolve in distilled
               water, and dilute to 1000 mL (1 mL - 1 mg CN).
                                             ft
      7.2.5    Rhodanine indicator:  Dissolve 20 mg of p-dimethy1-
               aminobenzalrhodanine in 100 mL of acetone.

      7.2.6    Sodium hydroxide  solution, 0.25 N:  Dissolve 10 g or NaOH in
               distilled water and dilute to 1 liter.

7.3 Manual  Spectrophotometric Reagents

      7.3.1    Sodium dihydrogenphosphate,  1 M:  Dissolve 138 g of NaH2P04*H20 in  a
               liter of distilled water.  Refrigerate this solution.
                                     D-65                                ILM02.0

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                                                                 Exhibit D Method 335.2
      7,3,2   Chloramine-T solution:  Dissolve 1.0 g of white, water soluble
              chloramine-T in 100 mL of distilled water and refrigerate until ready
              to use.  Prepare fresh weekly.

      7.3.3   Color Reagent-One of the following may be used:

              7.3.3.1    Pyridine -barbituric acid reagent:   Place 15 g of
                         barbituric acid in a 250 mL volumetric flask and add just
                         enough distilled water to wash the sides of the flask and
                         wet the barbituric acid.  Add 75 mL of pyridine and mix.
                         Add 15 mL of HC1 (sp gr 1.19), mix,  and cool to room
                         temperature.  Dilute to 250 mL with distilled water and
                         mix.  This reagent is stable for approximately six months
                         if stored in a cool, dark place.

              7.3.3.2    Pyridine -pyrazolone solution: 7. 3. 3. 2.1 3 -Methyl -1-phenyl -
                         2-pyrazolin-5-one reagent, saturated solution:  Add 0.25  g
                         of 3-methyl-l-phenyl-2-pyra2olin-5-one to 50 mL of
                         distilled water, heat to 60°C with stirring.  Cool to room
                         temperature .

                         7.3.3.2.1     3-Methyl-lphenyl-2-pyrazolin-5-one reagent,
                                      saturated solution:  Add 0.25 g of 3 -methyl - 1-
                                      phenyl-2-pyrazelin-5-one to 50 mL of distilled
                                      water,  heat to 60°C with stirring.  Cool to
                                      room temperature.

                         7.3.3.2.2     3,3'Dimethyl-l,l'-diphenyl [4,4'-bi-2
                                      pyrazolin]-5,5'dione  (bispyrazolone) : . . .
                                      Dissolve 0.01 g of bispyrazolone in 10 mL of
                                      pyridine .

                         7.3.3.2.3     Pour solution (7.3.3.2.1) through nonac id-
                                      washed filter paper.   Collect the filtrate.
                                      Through the same filter paper pour solution
                __                    (7.3.3.2.2) collecting the filtrate in the
                                      same container as filtrate from (7.3.3.2.1).
                                      Mix until the filtrates are homogeneous.  The
                                      mixed reagent develops a pink color but this
                                      does not affect the color production with
                                      cyanide if used within 24 hours of
                                      preparation.

7.4   Semi -Automated Spec trophotome trie Reagents

      7.4.1   Chloramine-T solution:  Dissolve 0.40  g  of chloramine-T in distilled
              water and dilute to 100 mL.  Prepare fresh daily.
      7.4.2   Phosphate buffer:  Dissolve 138 g of Na^PCV^O in distilled water
              and dilute to 1 liter.  Add 0.5 mL of Brij-35  (available from
              Technicon).  Store at 4°C(±2°C) .

      7.4.3   Pyridine -barbituric acid solution:  Transfer 15 g  of barbituric  acid
              into a 1 liter volumetric flask.  Add about 100 mL of  distilled  water
              and swirl the flask.  Add 74 mL of pyridine and mix.   Add  15 mL  of
                                     D-66                                ILM02.0

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                                                                  Exhibit  D Method 335.2
               concentrated HC1  and mix.   Dilute  to  about  900 mL with distilled
               water and mix until  the  barbituric acid is  dissolved.  Dilute to 1
               liter with distilled water.   Store at 4°C(±2°C).

      7.4.4    Sampler wash:   Dissolve  10  g of NaOH  in distilled water and dilute to
               1 liter.

8.    Procedure

8.1   Distillation

      8.1.1    Place 500 mL of sample in the 1 liter boiling flask.  Add 50 mL, of
               sodium hydroxide  (7.1.1) to the absorbing tube and dilute if
               necessary with distilled water to  obtain an adequate depth of-liquid
               in the absorber.   Connect the boiling flask, _condenser, absorber and
               trap  in the train.

          8.1.2   Start a slow stream  of air  entering  the boiling flask by. adjusting
                  the vacuum source.  Adjust  the vacuum so that approximately one
                  bubble of air per second enters the boiling flask through the air
                  inlet tube.

                  NOTE:  The bubble rate will not remain constant after the reagents
                  have been added and while heat is being applied to the flask.  It
                  will be necessary to readjust the sir rate occasionally to prevent
                  the solution in the boiling flask from backing up into the air
                  inlet tube.

      8.1.3    Slowly add 25 mL  concentrated sulfuric acid (7.1.4) through the  air
               inlet tube.   Rinse the tube with distilled, water. and_allow the
               airflow to mix the flask contents  for-3-minutes.- Pour- 20 mL  of
               magnesium chloride solution (7.1.5) ir~o the air inlet and wash  down
               with  a stream of  water.

      8.1.4    Heat  the  solution to boiling,  taking  care to prevent  the solution
               from  backing up into and overflowing  from the air inlet tube.  Reflux
               for one hour.  Turn  off  heat and continue the airflow for at  least 15
               minutes.  After cooling  the boiling flask,  disconnect absorber and
               close off the vacuum source.

      8.1.5    Drain the solution from  the absorber  into a 250 mL volumetric flask
               and bring up to volume with distilled water washings  from the
               absorber  tube.

8.2   Titrimetric Determination  (Option A)

      8.2.1    If the sample contains more than 1 mg of CN, transfer the distillate,
               or a  suitable aliquot diluted to 250  mL, to a 500 mL  Erlenmeyer
               flask.  Add 10-12 drops  of  the benzalrhodanine indicator.

      8.2.2    Titrate with standard silver nitrate  to the first change  in color
               from  yellow to brownish-pink.  Titrate a distilled water blank using
               the same  amount of sodium hydroxide and indicator as  in the sample.
                                     D-67                                ILM02.0

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                                                                 Exhibit D Method 335.2
      8.2.3   The analyst should familiarize himself with the end point of the
              titration and the amount of indicator :o be used before actually
              titrating the samples.  A 5 or 10 mL mLcroburet may be conveniently
              used to obtain a more precise titration.

8.3   Manual Spectrophotometric Determination  (Optior.  B)

      8.3.1   Withdraw 50 mL or less of the solution from the flask and transfer to
              a 100 mL volumetric flask.   If less than 50 mL is taken, dilute to 50
              mL with 0.25 N sodium hydroxide  solution (7.2.6).  Add 15.0 mL of
              sodium phosphate solution (7.3.1) and mix.   The dilution factor must
              be reported on Form XIV.

              8.3.1.1    Pyridine -barbituric acid method:   Add 2 mL of chloramine-T
                         (7.3.2) and mix.   After 1 to  2 minutes, add 5 mL of
                         pyridine -barbituric acid solution (7.3.3.1) and mix.
                         Dilute to mark with .distilled water and mix again.  Allow
                         8 minutes for color development  then read absorbance at
                         578 nm in a 1 cm cell within 15  minutes.

              8.3.1.2    Pyridine -pyrazolone method:  Add 0.5 mL of chloramine-T
                         (7.3.2) and mix.   After 1 to  2 minutes, add 5 mL of
                         pyridine -pyrazolone solution (7.3.3.2) and mix.  Dilute to
                         mark with distilled water and mix again.  After 40
                         minutes, read absorbance at 620  nm in a 1 cm cell.  NOTE:
                         More than 0.5 mL of chloramine-T will prevent the color
                         from developing with  pyridine -pyrazolone.

      8.3.2   Prepare a minimum of 3 standards and a blank by pipetting suitable
              volumes of standard. solution into 250 raL volumetric  flasks.  NOTE:
              One calibration  standard must be at the Contract  Required Detection
              Limit  (CRDL) .  To each standard, add 50 mL of 1.25 N sodium hydroxide
              and dilute to 250 mL with distilled wa~er.  Standards must bracket
              the concentration of the samples.  If dilution is required,  use  the
              blank  solution.

              As "Hh  example , standard solutions could be prepared  as:  follows :

                        mL of Standard Solution      Cone, ug CN
                            (1.0 - 5 u  CW           er 250 mL
                                  0                     Blank
                                  1.0        '.             5
                                  2.0                     10
                                  5.0                     25
                                 10.0                     50
                                 15.0                     75
                                 20.0                    100

               8.3.2.1    It is not  imperative that all standards be distilled in
                          the same manner as the samples.  At least one standard
                          (mid-range) must be distilled and compared to similar
                          values  on  the  curve to ensure that the distillation
                          technique  is reliable.   If  the  distilled  standard does not
                                      D-68                                ILM02.0

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                                                                  Exhibit D Method 335.2
                          agree within +15% of the unclistilled standards,  the
                          operator should  find and correct the cause of  the apparent
                          error before proceeding.

               8.3.2.2    Prepare a standard  curve by plotting absorbance  of
                          standard vs.  cyanide  concentrations (per 250  mL) .

8.4   Semi-Automated  Spectrophotometrie Determination (Option~C)

      8.4.1    Set up  the manifold as shown in Figure  3.   Pump the reagents through
               the system until a steady baseline is obtained.

      8.4.2    Calibration standards:  Prepare a blank and at  least three
               calibration standards over  the range  of the analysis.  One
               calibration standard must be  at the CRDL.   For  a  working  range  of 0-
               200 ug/L,  the following standards may be used:

                          mL Standard Solution        Concentration
                         (7.2.3)  diluted to 1 liter       ug CN/L

                                       0                     0
                                     4.0                    20
                                   10.0                    50
                                   20.0                   100
                                   30.0                   150
                                   40.0                   200

               Add 10  g of NaOH to each standard.  Store  at 4°C(±2°C)

      8.4.3    Place calibration standards, blanks,  and control  standards  in the
               sampler tray,  followed by distilled samples, distilled duplicates,
               distilled  standards, distilled spikes-,  and distilled blanks.

      8.4.4    When a  steady reagent baseline is obtained arid before starting  the
               sampler, adjust  the baseline using the  appropriate knob on  the
               colorimeter.   Aspirate a calibration  standard and adjust  the STD CAL
               dial on the colorimeter until  the desired  signal  is obtained.   Record
               the STD CAL value.  Re-establish  the  baseline and proceed to analyze
               calibration standards, blanks,  control  standards, distilled samples,
               and distilled QC audits.

9.    Calculations

9.1   Using the titrinetrie procedure, calculate concentration  of CN as follows:

                         (A,-B"> 1.000  mL/L     	250 m^	
          CN, mg/L -     mL orig. sample  x  mL of aliquot titrated
                                     D-69                                ILM02.0

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                                                                  Exhibit  D Method  335.2
          WHERE:   A - volume of AgNC>3 for titration of sample
                     (1 mL - 1 mg Ag)

                  B - volume of AgNC>3 for titration of blank
                     (1 mL - 1 mg Ag)

          AND:    250 mL - distillate volume (See 8.1.5)
                  1000 mL - conversion mL to L
                  mL original sample (See 8.1.1)
                  mL of aliquot titrated  (See 8.2.1)

9.2   If the semi-automated method is used,  measure the peak heights of the
      calibration standards (visually or using a date, system) and calculate a linear
      regression equation.   Apply the equation to the samples and QC audits to
      determine the cyanide concentration in the distillates.   To determine the
      concentration of cyanide in the original sample. MULTIPLY THE RESULTS BY ONE-
      HALF (since the original volume was 500 mL and the distillate volume was 250
      mL).   Also, correct for, and report on Form XIV, any dilutions which were made
      before or after distillation.              :..--.-_-_ -.-_--...    _

      The minimum concentration that can be  reported from the calibration curve is
      20 ug/L that corresponds to 10 ug/L in a sample that has been distilled.

9.3   If the colorimetric procedure is used, calculate the cyanide, in ug/L, in the
      original sample as follows:

                      A X 1.000 mL/L    x   50 mL
          CN, ug/L        B                 C

         WHERE:   A - ug CN read from standard curve (per 250 mL)
                  B - mL of original-sample  for_distillation_(See 8,.1.1)
                  C - mL taken for colorimetrie analysis- (See-8;3^1)

         AND:    50 mL - volume of original sample aliquot (See 8.3.1)
                  1000 mL/L - conversion mL  to L

         The minimum value that can be substituted for A is 5 ug per 250 mL.  That
         yields  a concentration of 10 ug/L  in the distilled sample,.
                                     D-70                                ILM02.0

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                                                                 Exhibit D Method 335.2
                 METHOD FOR TOTAL CYANIDE ANALYSIS IX SOIL/SEDIMENT
                           CYANIDE, TOTAL  (in Sediments)

                           •P-M* (Titrimetric; Manual Spec
                         Semi-Automated Spectrophotometrie)
Method 335.2 CLP-M* (Titrimetric;  Manual Spectrophotometric;
1.    Scope and Application

1.1   This method is applicable to the determination of cyanide in sediments and
      other solids.

1.2   The detection limit is dependent upon the weight of sample taken for analysis.

2 .    gtiflflpflTv of Method
2.1   The cyanide as hydrocyanic acid (HCN) is released from cyanide complexes by
      means of a reflux-distillation operation and absorbed in a scrubber containing
      sodium hydroxide solution.  The cyanide ion in the absorbing solution is then
      determined by volumetric titration or colorimetrically.

2.2   In the colorimetric measurement the cyanide is converted to cyanogen chloride ,
      CNC1, by reaction with chloramine-T at a pH less than 8 without hydrolyzing to
      the cyanate.  After the reaction is complete, color is formed on the addition
      of pyridine-pyrazolone or pyridine -barbituric acid reagent.  The absorbance is
      read at 620 nm when using pyridine-pyrazolone for 578 nm for pyridine -
      barbituric acid.  To obtain colors of comparable intensity, it is essential to
      have the same salt content in both the sample &nd the standards.

2.3   The titrimetric measurement uses a -standard solution -of -silver nitrate to   —
      titrate cyanide in -the -presence of a silver sensitive indicator;   -------

3.    Definitions

3.1 -  Cyanide is defined as cyanide ion and complex cyanides converted to
      hydrocyanic acid (HCN) by reaction in a reflux system of a mineral acid in the
      presence of magnesium ion.

4.    Sample Handling and Preservation

4.1   Samples must be stored at 4°C(±2°C) and must be analyzed within the holding
      time specified in Exhibit D, Section II.

4.2   Samples are not dried prior to analysis/  A separate percent solids
      determination must be made in accordance with the procedure in Part F.

5.    Interferences

5.1   Interferences are eliminated or reduced by using the distillation procedure
      described in Procedure 8.1.

5.2   Sulfides adversely affect the colorimetric and titration procedures.

 CLP-M  Modified for the Contract Laboratory Program.
                                     D-71                                ILM02.0

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                                                                 Exhibit D Method 335.2
5.3   The presence of surfactants may cause the sample to foam during refluxing.   If
      this occurs, the addition of an agent such as EOW Corning 544 antifoam agent
      will prevent the foam from collecting in the cc-ndenser.   Fatty acids will
      distill and form soaps under the alkaline titrs.tion conditions;, making the  end
      point almost impossible to detect.   When this occurs,  one of the
      spectrophotometric methods -should be used.

6.     Apparatus

6.1   Reflux distillation apparatus such as shown in Figure  1  or Figure 2.  The
      boiling flask should be of 1 liter size with inlet tube  and provision for
      condenser.  The gas absorber may be a Fisher-Milligan  scrubber.

6.2   Microburet, 5.0 mL (for titration)

6.3   Spectrophotometer suitable for measurements at 578 nm  or 620 run with a 1.0  cm
      cell or larger.

6.4   Technicon AA II System or equivalent instrumentation (for automated
      spectrophotometric method) including:

      6.4.1   Sampler

      6.4.2   Pump  III

      6.4.3   Cyanide Manifold  (Figure 3)

      6.4.4   SCIC  Colorimeter  with  15 mm  flowcells  and 570 nm filters

      6.4.5   Recorder

      6.4.6   Data  System  (optional)

      6.4.7   Glass or  plastic  tubes for the sampler

7.     Reagents

7.1   Distillation and Preparation Reagents

      7.1.1   Sodium hydroxide  solution, 1.25N:   Dissolve 50  g of NaOH in distilled
              water, and dilute to 1 liter with distilled water.

      7.1.2   Cadmium carbonate:   powdered

      7.1.3   Ascorbic  acid:   crystals

      7.1.4   Sulfuric  acid:   concentrated

      7.1.5   Magnesium chloride solution:  Weigh 510 g of  MgC12.6H20 into a 1000
              mL flask, dissolve and dilute to 1 liter with distilled water.

7.2   Stock Standards and  Titration  Reagents

      7.2.1    Stock cyanide solution:  Dissolve 2.51 g of KCN and 2 g KOH in 1
               liter of distilled water.   Standardize with 0.0192 N
                                     D-72                                ILM02.0

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                                                                  Exhibit  D Method 335.2
      7.2.2    Standard cyanide  solution,  intermediate:  Dilute 50.0 nL of stock (1
               mL -  1  ng CN)  to  1000  mL with  distilled water  (1 n»L - 50.0 ug) .

      7.2.3    Standard cyanide  solution:   Prepare  fresh daily by diluting 100.0 mL
               of intermediate cyanide  solution  to  1000 mL with distilled water and
               store in a glass  stoppered  bottle.   1 raL - 5.0 ug CN (5.0 mg/L).
                                   ».
      7.2.4    Standard silver nitrate  solution, 0.01'J2 N:  Prepare by crushing
               approximately  5 g AgNC>3  crystals  and d:rying to constant weight at
               40°C.  Weigh out  3.2647  g of dried AgN03, dissolve in distilled
               water, and dilute to 1000 mL (1 mL - 1 mg CN).

      7.2.5    Rhodanine  indicator:  Dissolve 20 mg of p-dimethy1-amino-
               benzalrhodanine in 100 mL acetone.

7.3   Manual Spectrophotometric  Reagents

      7.3.1    Sodium dihydrogenphosphate,  1 M:  Dissolve 138 g of NaH2P04'H20 in 1
               liter of distilled water.   Refrigerate this solution.

      7.3.2    Chloramine-T solution:   Dissolve  1.0 g of white, water soluble
               Chloramine-T in 100 mL of distilled water and refrigerate until ready
               to use.  Prepare  fresh weekly.
      7.3.3   Color reagent - One of the following may be used:
              7.3.3.1    Pyridine-barbituric acid reagent:  Place 15 g of
                         barbituric acid in a 250 mL volumetric flask and add just
                         enough distilled water to wash the sides of the flask and
                         wet the barbituric acid.  Add 75 mL of pyridine and mix.
                         Add 15 mL of HC1 (sp gr 1.19), mix, and cool to room
                         temperature.  Dilute to 250 mL with distilled water and
                         mix.  This reagent is stable for approximately six months
                         if stored in a cool, dark place.

              7.3.3.2    Pyridine-pyrazolone solution:

                -«.       7.3.3.2.1    3-Methyl-l-phenyl-2-pyrazolin-5-one reagent,
                                      saturated solution:  Add 0.25 g of 3-methyl-1-
                                      phenyl-2-pyrazolin-5-one to 50 mL of distilled
                                      water, heat to 60°C with stirring.  Cool to
                                      room temperature.

                         7.3.3.2.2    3,3 'Dime'thyl-1,1' -diphenyl- [4,4' -bi-2-
                                      pyrazolin]-5,5'dione (bispyrazolone):
                                      Dissolve 0.01 g of bispyrazolone in 10 mL of
                                      pyridine.

                         7.3.3.2.3    Pour solution (7.3.3.2.1) through non-acid-
                                      washed filter ?aper.  Collect tihe filtrate.
                                      Through the same filter paper pour solution
                                      (7.3.3.2.2) collecting the filtrate in the
                                      same container as filtrate from (7.3.3.2.1).
                                      Mix until the filtrates are homogeneous.  The
                                      mixed reagent develops a pink color but this
                                     D-73                                ILM02.0

-------
                                                                 Exhibit D Method 335.2
                                      does not affect the color production with
                                      cyanide if used within 24 hours of
                                      preparation.

7.4   Semi-Automated Spectrophotometric Reagents

      7.4.1    Chloramine-T solution:  Dissolve 0.40 g of chloramine-T in distilled
               water and dilute  to 100 mL.  Prepare fresh daily.

      7.4.2    Phosphate Buffer:  Dissolve 138 g of Nal^PtV^O in distilled water
               and dilute to 1 liter.  Add 0.5 mL of Brij-35 (available from
               Technicon).   Store at 4°C.

      7.4.3    Pyridine-barbituric acid solution:  Transfer 15 g of barbituric acid
               into  a 1  liter volumetric flask.  Add about 100 mL of distilled water
               and swirl the flask.  Add 74 mL of pyridine and mix.  Add 15 mL of
               cone.  HC1 mix until the barbituric acid is dissolved.  Dilute to 1
               liter with distilled water.  Store at 4°C.

      7.4.4    Sampler Wash:  Dissolve 10 g of NaOH in distilled water and dilute to
               1 liter.

8.    Procedure

8.1   Distillation

      8.1.1    Accurately weigh  a representative 1-5 g portion of wet sample and
               transfer  it  to a  boiling flask.  Add 500 mL of distilled water.
               Shake or  stir the sample so that it is dispersed.

      8.1.2    Add 50 mL of sodium hydroxide  (7.1.1) ~o the absorbing tube and —
               dilute if necessary with distilled water to obtain an adequate depth
               of liquid In the  absorber.  Connect the boiling flask,, condenser,
               absorber,  and trap in the train.

      8.1.3    Start a slow stream of air entering the boiling flask by adjusting
               the vacuum source.  Adjust the vacuum so that approximately one
               bubble of air per second enters the boiling flask through the air
               inlet tube.

                  NOTE:   The bubble rate will not remain constant after the reagents
                  have been added and while heat is being applied to the flask.  It
                  will be necessary to readjust the air rate occasionally to prevent
                  the solution in the boiling flask from backing up into the air
                  inlet tube.

      8.1.4    Slowly add 25 mL  of cone, sulfuric acid (7.1.4) through the air  inlet
               tube.  Rinse the  tube with distilled water and allow the airflow to
               •ix the flask contents for 3 minutes.  Pour 20 mL of magnesium
               chloride  solution (7.1.5) into the air inlet and wash down with  a
               stream of water.
                                     D-74                                ILM02.0

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                                                                 Exhibit D Method 335.2
      8.1.5   Heat the solution to boiling, taking c.ire to prevent the solution
              from backing up and overflowing into the air inlet tube.  Reflux for
              one hour.  Turn off heat and continue -he airflow for at least 15
              minutes.  After cooling the boiling fLisk, disconnect absorber and
              close off the vacuum source.

      8.1.6   Drain the solution from the absorber into a 250 mL volumetric flask
              and bring up to volume with distilled water washings from the
              absorber tube.

8.2   Titrimetric Determination (Option A)

      8.2.1   If the sample contains more than 1 mg of CN, transfer the distillate,
              or a suitable aliquot diluted to 250 ml, to a 500 mL Erlenmeyer
              flask.  Add 10-12 drops of the benzalrhodanine indicator.

      8.2.2   Titrate with standard silver nitrate to the first change in color
              from yellow to brownish-pink.  Titrate a distilled water 4>lank using
              the same amount of sodium hydroxide and indicator as in the sample.

      8.2.3   The analyst should familiarize himself with the end point of the
              titration and the amount of indicator to be used before actually
              titrating the samples.  A 5 or 10 mL microburet may be conveniently
              used to obtain a more precise titration.

8.3   Manual Spectrophotometric Determination (Option B)

      8.3.1   Withdraw 50 mL or less of the solution from the flask and transfer to
              a 100 mL volumetric flask.   If less than 50 mL is taken, dilute to 50
              mL with 0.25 N sodium hydroxide solution (7.2.6).  Add 15.0 mL of
              sodium phosphate solution (7.3.2) and mix.

              8.3.1.1    Pyridine-barbituric acid method:  Add 2 mL of Chloramine-T
                         (7.3.2) and mix.   After 1 to 2 minutes, add 5 mL of
                         pyridine-barbituric acid solution (7.3.3.1) and mix.
                         Dilute to mark with distilled water and mix again.  Allow
               —        8 minutes for color developnent then read absorbance at
                         578 nm in a 1 cm cell within 15 minutes.

              8.3.1.2    Pyridine-pyrazolone method:  Add 0.5 mL of chloramine-T
                         (7.3.2) and mix.  After 1 to 2 minutes add 5 mL of
                         pyridine-pyrazolone solution (7.3.3.2) and mix.  Dilute to
                         mark with distilled-Water and mix again.  After 40 minutes
                         read absorbance at 620 nm in a 1 cm cell.

                         NOTE:  More than 0.5 mL of chloramine-T will prevent the
                         color from developing with pyridine-pyrazolone.

      8.3.2   Prepare a minimum of three  standards and a blank by pipetting
              suitable volumes of standard solution into  250 mL volumetric flasks.

          NOTE:   One calibration standard, must be made at the CRDL.  To each
          standard add 50 mL of 1.25 N sodium hydroxide and dilute to 250 mL with
          distilled water.   Standards must bracket the concentrations of the sample.
          If dilution is required,  use the blank solution.
                                     D-75                                ILM02.0

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                                                                 Exhibit D Method 335.S
          As an example,  standard solutions could be prepared as follows:

                        mL of Standard Solution       Cone, ug CN
                            (1.0 - 5 ue CIO            per  250 mL

                                  0                      Blank
                                  1.0                      5
                                  2.0                      10
                                  5.0                      25
                                 10.0                      50
                                 15.0                      75
                                 20.0                     100

              8.3.2.1    It is not imperative .that, all  standards be distilled, in . _
                         the same manner as  the  samples.   At  least one standard
                         (mid-range) must be distilled  and compared to .similar
                         values on the curve to  insure that- the. dtstillation -.-..-  ^.-_ .
                         technique is reliable.   If the distilled standard does not
                         agree within +15% of the undistilled standards the
                         operator should find and correct the  cause of the apparent
                         error before proceeding.

              8.3.2.2    Prepare a standard curve by plotting absorbance of
                         standard vs. cyanide concentrations  (per 250 mL)

8.4   Semi-Automated Spectrophotometrie Determination (Option  C)

      8.4.1   Set up the manifold as shown in Figure 3.  Pump the reagents through
              the system until a steady baseline is obtained,	  	

      8.4.2   Calibration standards:  Prepare a blank and at least three
              calibration standards over the range of the analysis.  One
              calibration standard must be at the CRDL.  For a working range of  0-
              200 ug/L, the following standards may be used:

                          mL Standard Solution           Concentration
                       (7.2.3) diluted to 1  liter          ug CN/L	

                                   0                            0
                                   4.0                         20
                                   10.0                        50
                                   20.0      ,                 100
                                   30.0      '                 150
                                   40.0                       200

                  Add 10 g of NaOH to each standard.  Store at 4°C(±2°C).

          8.4.3   Place calibration standards,  blanks,  and control standards in  the
                  sampler tray, followed by distilled samples, distilled duplicates,
                  distilled standards, distilled spikes, and distilled blanks.

      8.4.4   When  a steady reagent baseline is obtained and before starting the
               sampler, adjust the baseline using  the appropriate knob on the
               colorimeter.   Aspirate a calibration standard and adjust the STD CAL
               dial  on  the colorimeter until  the desired signal  is obtained.   Record
                                     D-76                                ILM02.0

-------
                                                                 Exhibit D Method 335.2
              the STD CAL value.  Reestablish the baseline and proceed to analyze
              calibration standards, blanks, control standards, distilled samples,
              and distilled QC audits.

9.    Calculations

9.1   A separate determination of percent solids must be performed (see  Part  F).

9.2   The concentration  of  cyanide in the sample is determined as  follows.

          9.2.1    (Titration)

                               (A -  B) x  	250 mL       x iQOO gAg
                  _,    _                mL aliquot titrated     . 	  	
                  CN, fflgAg -	
                                           c x  %solids
                                                 100

                 WHERE:  A  - mL of AgNC>3  for titration of sample
                              (1 mL  - 1 mg Ag)
                        B  - mL of AgN03  for titration of blank
                              (1 mL  - 1 mg Ag)
                        C  - wet weight of original sample in g
                              (See 8.1.1)

                 AND:  250 mL  - volume of distillate (See 8.1.6)
                      1000 g/kg — conversion factor g to kg
                      mL aliquot titrated (See 8.2.1)
                  % solids (see Part F)

      9.2.2    (Manual  Spectrophotometrie)

                                             50 mL
                           CN,  mgAg -     x   B
                                         C x  % solids
                                                100

                 WHERE:  A -  ug CN read from standard curve  (per 250 mL)
                         B -  mL of distillate taken  for  colorimetric
                               determination  (8.3.1)
                         C -  wet weight of  original  sample in g
                               (See 8.1.1)
                                            '*
                 The minimum value that can be substituted for A is 5  ug/250 mL.
                 That yields a concentration  of 10 ug/L in the distilled sample.

                 AND:    50 mL - volume of standard  taken  for  colorimetric
                                 determination  (See  8.3.1)
                         % solids (see Part F)
                                     D-77                                ILM02.0

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                                                        Exhibit D Method 335.2
9.2.3   (Semi-Automated Spectrophotometrie)

        If the semi-automated method is used, measure the peak heights of
        the calibration standards (visually or using a data system) and
        calculate a linear regression equation.  Apply the equation to the
        samples and QC audits to determine the cyanide concentration in
        the distillates.             -

                                A x .25
                  CN, mgAg  -  C x * solids
                                       100

        WHERE:  A  -  ug/L determined from standard curve
                C  -  wet weight of origin&l sample in g
                      (See 8.1.1)

        AND:    .25  -  conversion factor for distillate final
                        volume (See 8.1.6)
                % solids (see Part F)

        The minimum value that can be substituted for A is 5 ug/250 mL.
                           D-78                                 I1M02.0

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                                             Exhibit D Method 335.2
COOLING WATER
INLET
      HEATER -
SCREW CLAMP
       I
 -_   ft
                                       TO LOW VACUUM
                                          SOURCE
                                   - ABSORBER
                             DISTILLING FLASK
                   O
Figure 1.  Cyanide distillation apparatus

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                                             Exhibit D Method  335.
AtllHN CONDENSER


AIR INLET TUBE
— CONNECTING TUBING
ONE LITER
BOILING FLASK
                                              SUCTION
                         CAS ABSORBER
 Figure 2.   Cyanide distillation apparatus

-------
                                          Exhibit D Method 335.2
Figure 3.  Cyanide Manifold

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                                                                 Exhibit D Method 335.2
               METHOD FOR TOTAL CYANIDE ANALYSIS BY KIDI DISTILLATION

                          CYANIDE, TOTAL (water and soils)

               Method 335.2 CLP-M (Semi-automated Spcctrophotometric)

1.     Scope and Application

1.1   Cyanide determined by this method is defined as cyanide ion and complex
      cyanides converted to hydrocyanic acid by reaction in a reflux system with
      mineral acid in the presence of magnesium ion.

1.2   This method covers the determination of cyanide by midi distillation with a
      semi-automated colorimetrie analysis of the distillate.

1.3   The detection limit for the semi-automated colc-rimetric method is
      approximately 10 ug/L.

2.     Svinnflf7 of Method

2.1   The cyanide as hydrocyanic acid (HCN) is released from cyanide complexes by
      means of a midi reflux-distillation operation &nd absorbed in a scrubber
      containing sodium hydroxide solution.  The cyanide ion in the absorbing
      solution is then determined colorimetrically.

2.2   In the colorimetric measurement, the cyanide is converted to cyanogen
      chloride, CNC1, by reaction with chloramine-T s.t pH less than 8 without
      hydrolysis to the cyanate.  After the reaction is complete, color is formed on
      the addition of pyridinebarbituric acid reagent.  The absorbance is read at
      580 nm.  To obtain colors of comparable intensity, it is essential to have the
      same salt content in both the samples and the standards.

3.     Sample Handling and Preservation

3.1   All bottles must be thoughly cleansed and rinsed to remove soluble materials
      from containers.

3.2   Oxidizing agents such as chlorine decompose most cyanides.  Test a drop of the
      sample with potassium iodide-starch test paper (KI-Starch paper); a blue color
      indicates the need for treatment.  Add ascorbic acid, a few crystals at a
      time, until a drop of sample produces no color on the indicator paper.  Then
      add additional 0.6 g of ascorbic acid for each liter of sample volume.

3.3   Samples are preserved with 2 mL of 10 H sodium hydroxide per liter of sample
      (pH > 12) at the time of collection.

3.4   Samples must be stored at 4°C (±2°C) and must be analyzed within the holding
      time specified in Exhibit D, Section II.

4.     Interferences

4.1   Interferences are eliminated or reduced by using the distillation procedure.
                                     D-82                                ILM02.0

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                                                                 Exhibit D Method 335.2
4.2   Sulfides adversely affect the colorimetric procedures.  If a drop of
      distillate on lead acetate test paper indicates the presence of sulfides,
      treat the sample with powdered cadmium carbonate.  Yellow cadmium sulfide
      precipitates if the sample contains sulfide.  Repeat this operation until  a
      drop of the treated sample solution does not darken the lead acetate test
      paper.  Filter the solution through a dry filter paper into a dry beaker,  and
      from the filtrate, measure the sample to be used for analysis.  Avoid a large
      excess of cadmium carbonate and long contact time in order to minimize loss by
      complexation or occlusion of cyanide on the precipitated material.

4.3   The presence of surfactants may cause the sample to foam during refluxing.  If
      this occurs, the addition of an agent such as Dow Corning 544 ant if earning
      agent will prevent the foam from collecting in the condenser.

5.    Apparatus

5.1   Midi reflux distillation apparatus as shown in figure 1.

5.2   Heating block - Capable of maintaining 125°C ±5°C.

5.3   Auto analyzer system with accessories:

      5.3.1   Sampler

      5.3.2   Pump

      5.3.3   Cyanide  cartridge

      5.3.4   Colorimeter with 50 mm flowcells  and -530 nm filter  - . - ......

      5.3.5   Chart recorder or data system.

5.4   Assorted volumetric  glassware, pipets, and micropipets.

6.    Reagents

6.1   Distillation and Preparation Reagents

      6.1.1   Sodium hydroxide absorbing solution, and sample wash solution, 0.25
              N.  Dissolve 10.0 g NaOH in ASTM Type II water and dilute to one
              liter.

      6.1.2   Magnesium chloride solution, 51% (w/v) .  Dissolve 510 g of MgCl2-6H20
              in ASTM  Type II water and dilute to one liter.

      6.1.3   Sulfuric acid, 50% (v/v).  Carefully add a portion of concentrated
                     to an equal portion of ASTM Type II water.
      6.1.4    Sodium hydroxide solution, 1.25 N.  Dissolve 50 g of NaOH in ASTM
               Type II water and dilute to one liter.

-------
                                                                 Exhibit D Method 335.2
6.2   Standards
      6.2.1   Stock cyanide solution, 1000 mg/L CN.   Dissolve 2.51 5 of KCN and 2.0
              g KOH in ASTM Type II water and dilute one liter.   Standardize with
              0.0192 N AgNC>3.

      6.2.2   Intermediate cyanide standard solution, 10 mg/L CN.  Dilute 1,0 mL of
              stock cyanide solution (6.2.1) plus 20 mL of 1.25  N NaOH solution
              (6.1.4) to 100 mL with ASTM Type II wazer.  Prepare this solution at
              time of analysis.

      6.2.3   Rhodamine indicator.   Dissolve 20 mg of p-dimethylamino-benzal-
              rhodamine in 100 mL acetone.

      6.2.4   Silver nitrate solution,  0.0192 N.  Prepare by crushing approximately
              5 g AgN03 crystals and drying to a constant weight at 104 C.  Weigh
              out 3.2647 g of dried AgNOs and dissolve in ASTM Type II water.
              Dilute to one liter ( 1 mL corresponds to 1 mg CN) .
      6.2.5    Potassium chromate indicator solution.   Dissolve 50 g K£CR04 in
              sufficient ASTM Type II water.   Add silver nitrate solution until a
              definite red precipitate is formed.  Let stand for at least 12 hours,
              filter, and dilute to one liter with ASTM Type II water.

      6.2.6    Primary standard sodium chloride, 0.0141 N.  Dissolve 824.1 mg NaCl
              (NBS-dried 20 minutes at 104°C) in ASTM Type II water and dilute to
              one liter.

      6.2.7    Sodium hydroxide solution, 0.1 N.  Dissolve 4 g of NaOH in ASTM Type
              II water and dilute to one liter.

6.3   Semi-Automated Spectrophotometric Reagents

      6:3.1   Phosphate buffer solution, 1 M.  Dissolve 138 g of NaH2PC>4-H20 in
              ASTM Type II water and dilute to one liter.  Add 0.5 mL of Brij-35
              (available from Technicon) . Store at 4°C .

      6.3.2    Chloramine-T solution, 0.4% (w/v) .  Dissolve 0.4 g of chloramine-T  in
              ASTM Type II water and dilute to 100 raL.  Prepare fresh at time of
              analysis.

      6.3.3    Color Reagent Solution,  Pyridine barbituric acid color  reagent
              solution.  Prepare this  solution in the hood.  Transfer 15 g of
              barbituric acid into a one liter Erlenraeyer flask.  Add about 100 mL
              of ASTM Type II water and swirl the flask to mix.  Add  75 mL of
              pyridine and 15 mL concentrated HCL and mix until all the barbituric
              acid is dissolved.  Dilute to one  liter with ASTM Type  II water and
              store at 4°C.

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                                                                 Exhibit D Method 335.2
7.    Procedure

7.1   Distillation

      7.1.1   The procedure described here utilizes .1 midi distillation apparatus
              and requires a sample aliquot of SO mL.s or less for aqueous samples
              and one gram for solid materials.  NOTE:  All samples must ini tally
              be run undiluted (i.e., aqueous samples must first be run with a 50
              mL aliquot and solid samples using a one gram sample).  When the
              cyanide concentration exceeds the highest calibration standard,
              appropriate dilution (but not below the CRDL) and reanalysis of the
              sample is required.  The dilution factor must be reported on Form
              XIV.

      7.1.2   For aqueous samples:  Pipet 50 mL of sample, or an aliquot diluted to
              50 mL, into the distillation flask along with 2 or 3 boiling chips.

      7.1.3   For solid samples:   Weigh 1.0 g of sample (to the nearest 0.01 g)
              into the distillation flask and dilute to 50 mL with ASTM Type II
              water.  Add 2 or 3 boiling chips.

      7.1.4   Add 50 mL of 0.25 N NaOH (6.1.1) to the gas absorbing impinger.

      7.1.5   Connect the boiling flask, condenser,  and absorber in the train as
              shown in figure 2.   The excess cyanide trap contains 0.5 N NaOH.

      7.1.6   Turn on the vacuum and adjust the gang (Whitney) values to give a
              flow of three bubbles per second from -he impingers in each reaction
              vessel .
      7.1.7    After five minutes of vacuum flow, inject 5 mL of 50% (v/v)
              (6.1.3) through the top air inlet tube of the distillation head into
              the reaction vessel.  Allow to mix for 5 minutes.  (NOTE:  The acid
              volume must be sufficient to bring the sample/solution pH to below
              2.0.)

      7.1.8    Add 2 mL of magnesium chloride solution (6.1.2) through the top air
              inlet tube of the distillation head in~o the reaction flask.
              Excessive foaming from samples containing surfactants may be quelled
              by the addition of another 2 mL of magnesium chloride solution.

      7.1.9    Turn on the heating block and set for 123-125°C.  Heat the solution
              to boiling, taking care to prevent solution backup by periodic
              adjustment of the vacuum flow.
      7.1.10   After one and » fcslf hours of refluxing, turn off the heat and
              continue the vacuum for an additional 15 minutes.  The- flasks should
              be cool at this tine .

      7.1.11   After cooling, close off the vacuum at the gang valve and remove the
              absorber.  Seal the receiving solutions and store them at 4°C until
              analyzed.  The solutions must be analyzed for cyanide within the 12
              day holding time specified in Section II.
                                     D-85                                 ILM02.0

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                                                                 Exhibit D Method 335.;
7.2   Semi-Automated Spectrophotometric  Determination

      7.2.1   Operating conditions:  Because of the difference between various
              makes and models of satisfactory instruments, no detailed operating
              instructions can be provided.  The analyst should follow  the
              instructions provided by the manufacturer of the particular
              instrument.  It is the responsibility of the analyst to verify that
              the instrument configuration and operating conditions used satisfy
              the analytical requirements and to maintain quality control data
              confirming instrument performance and analytical results.

              The following general procedure applies to most semi-automated
              colorimeters.  Set up the manifold and complete system per
              manufacturer's instructions.  Allow the colorimeter and recorder warm
              up for at least 30 minutes prior to use.  Establish a steady reagent
              baseline feeding ASTM Type II water through the sample line and
              appropriate reagents (6.3) through reagent lines.  Adjust the
              baseline using the appropriate control on the colorimeter.

      7.2.2   Prepare a minimum of 3 standards and a blank by pipetting suitable
              volumes of standard solution into 50 mL volumetric flasks.  NOTE:
              One calibration standard must be.at the Contract Required Detection
              Limit (CRDL).

              As an example, standard solutions could be prepared as follows:

                  Total ug CN
               standard solution         BlL 19 Bg/L CN       mj. 0.05 N NaOH

                     0.00                   0.000                 20
                     0.10                   0.010                 20
                     0.25                   0.025                 20
                     0.50                   0.050                 20
                     1.00                   0.100                 20
                     2.00                   0.200                 20
                     5.00                   0.500                 20

              7.2.2.1    Dilute standards to 50 mL using ASTM Type II water.  It is
                         not imperative that all standards be distilled in the same
                         Banner as the samples.  At least one standard (mid-range)
                         must be distilled and compared to similar values on the
                         curve for each SDG to ensure the distillation technique is
                         reliable.  If the distilled standard does not agree within
                         ±15% of the undistilled standards, the operator oust find
                         and correct the cause of the error before proceeding.

      7.2.3   Aspirate the highest calibration standard and adjust the colorimeter
              until the desired  (maximum)  signal-range is obtained.

      7.2.4   Place calibration  standards, blanks, control standards  in the  sampler
              tray, followed by  distilled samples, distilled duplicates, distilled
              standards, distilled spikes, and distilled blanks.

      7.2.5   Switch sample line from the ASTM Type  II water to sampler, set the
              appropriate  sampling rate and begin the analysis.
                                     D-86                                ILM02.0

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                                                                 Exhibit D Method 335.2
8.    Calculations

8.1   Calculations for Semi-automated Colorimetrie Determination

      8.1.1   Prepare a. standard curve by plotting absorbance (peak heights,
              determined visually or using a data system) of standards, (y) versus
              cyanide concentration values (total ug CN/L) (x).   Perform a linear
              regression analysis.

      8.1.2   Multiply all distilled values by the standardization value to correct
              for the stock cyanide solution not being exactly 1000 mg/L (See
              6.2.1).

      8.1.3   Using the regression analysis equation, calculate sample receiving
              solution concentrations from the calibration curve.

      8.1.4   Calculate the cyanide of aqueous samples in ug/L of original sample,
              as follows:

                                          A x D x F
                           CN, ug/L   -       B


                where:     A - ug/L CN of sample froa regression analysis

                           B - Liter  of original sample for distillation  (0.050  L)
                                (See 7.1.2)

                           D  - any  dilution  factor necessary to  bracket  sample
                                 value within standard values

                           F - sample receiving solution volume (0.050 L)

              The minimum value that can be substituted for A is 10 ug/L.

      8.1.5   Calculate the cyanide of solid samples in mg/kg of original sample,
              as follows:

              8.1.5.1    A separate determination of percent solids must be
                ~~        performed (See Part F).

              8.1.5.2    The concentration of cyanide in the sample is determined
                         as follows:

                                          A x D x F
                           CN, ng/kg   -    B x E

                         where:   A - ug/L  CN of  sample from regression analysis
                                        curve
                                  B -  wet weight  of original  sample  in g  (See
                                        7.1.3)
                                     D-87                                ILM02.0

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                                        Exhibit D Method 335.2
          D -  any  dilution  factor necessary  to  bracket
                sample value  within standard values
          E -  % solids (See Part F)/100.
          F -  sample receiving solution volume (0.050 L)
The minimum value that can be substituted for A is 10 ug/L
            D-88                                ILM02.0

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                                                                        Exhibit D Part F
                   PART F - PERCENT SOLIDS  DETERMINAT[ON PROCEDURE

1.   Immediately following the weighing of the sample to be processed for analysis
     (see Section III, Part B- Soil/Sediment Sample Preparation),  add 5-10 g of
     sample to a tared weighing dish.  Weigh and record the weight to the nearest
     0.01 g.

2.   Place weighing dish plus sample, with the cover tipped to allow for moisture
     escape, in a drying oven maintained at 103-105°C.  Sample handling and drying
     should be conducted in a. well-ventilated area.

3.   Dry the sample overnight (12-24 hours) but no longer  than 24  hours.   If dried
     less than 12 hours, it must be documented that constant weight was attained.*
     Remove Che sample from the oven and cool in a dessicator with the weighing dish
     cover in place before weighing.  Weigh and record weight to nearest 0.01 g.   Do
     not analyze the dried sample.

4.   Duplicate percent solids determinations are required  at the same frequency as
     are other analytical determinations.  Duplicate results are to be recorded on
     FORM VI-IN.

5.   For the duplicate percent solids determination, designate one sample aliquot as
     the "original" sample and the other aliquot as the "duplicate" sample.
     Calculate dry weight using the results of the "original" sample aliquot.

6.   Calculate percent solids by the formula below.  The value thus obtained will be
     reported on the appropriate FORM I-IN and, where applicable,  FORM VI-IN .  This
     value will be used for calculating analytical concentration on a dry weight
     basis.

                   % Solids  -   Sample Dry Weight x  100
                                    Sample Wet Weight
*For the purpose of paragraph 3, drying tine is defined as the elapsed time in the
 oven; thus raw data must record time  in  and out  of the oven to  document  the  12
 hour drying time minimum.  In  the  event  it is necessary  to  demonstrate the
 attainment of constant weight, data oust be recorded for a  minimum of two
 repetitive weigh/dry/dessicate/weigh  cycles with a ninimum  of 1 hour drying  time
 in each cycle.  Constant weight would be defined as a loss  in weight of  no greater
 than 0.01 g between the start  weight  and final weight of the last  cycle.


                                     D-89                                ILM02.0

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           PART G - ALTERNATE METHODS  (CATASTROPHIC  ICP  FAILURE1
      Analvte                                                Page No.

      Aluminum - Method 202.2 CLP-M*,  Furnace AA             D-92
      Barium • Method 208.2 CLP-M,  Furnace AA                D-93
      Cobalt - Method 219.2 CLP-M,  Furnace AA                D-94
      Copper - Method 220.2 CLP-M,  Furnace AA                D-95
      Iron - Method 236.2 CLP-M,  Furnace AA                  D-96
      Manganese - Method 243.2 CLP-M,  Furnace AA             D-97
      Nickel - Method 249.2 CLP-M,  Furnace AA                D-98
      Vanadium - Method 286.2 CLP-M,  Furnace AA              D-99
      Zinc - Method 289.2 CLP-M,  Furnace AA                  D-100
      Aluminum - Method 202.1 CLP-M,  Flame AA                D-102
      Antimony - Method 204.1 CLP-M,  Flame AA                D-104
      Barium - Method 208.1 CLP-M,  Flame AA                  D-105
      Beryllium - Method 210.1 CLP-M_,  Flame AA      ...... D-J.0.6
      Cadmium - Method 213.1 CLP-M, Flame AA                 D-107
      Chromium - Method 218.1 CLP-M,  Flame AA                D-108
      Cobalt - Method 219.1 CLP-M,  Flame AA                  D-109
      Copper - Method 220.1 CLP-M,  Flame AA                  D-110
      Iron - Method 236.1 CLP-M,  Flane AA                    D-lll
      Lead - Method 239.1 CLP-M,  Flame AA                    D-112
      Manganese - Method 243.1 CLP-M,  Flame AA               D-113
      Nickel - Method 249.1 CLP-M,  Flame AA                  D-114
      Silver - Method 272.1 CLP-M,  Flame AA                  D-11S
      Thallium - Method 279.1 CLP-M,  Flame AA                D-117
      Vanadium • Method 286.1 CLP-M,  Flame AA                D-118
      Zinc - Method 289.1 CLP-M,  Flame AA                    D-119
"'"Furnace AA Methods are from "Methods for Chemical Analysis of Water and
 Wastes". (EPA-600/4-79-02), March 1979, as modified for use in the
 Contract Laboratory Program (CLP).  Flame AA (Flame Technique) Methods are
 from "Interim Methods  for  the Sampling and Analysis of Priority Pollutants
 in Sediments and Fish  Tissue," USEPA Environmental Monitoring and Support
 Laboratory, Cincinnati. Ohio, August 1977, Revised October 1980. as
 modified for use in the CLP.

*CLP-M  Modified for the Contract Laboratory Program.
                                   D-90                                ILM02.0

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                                                                        Exhibit D Part G
                       CONDITIONS FOR USE OF ALTERNATE METHODS


The methods contained in Part G may be used only if £.11 of the following conditions
are met:

     1)   Catastrophic failure of ICP occurs,

     2)   Administrative Project Officer authorization  for use  of alternate methods
          is  granted,  and

     3)   The IDLs  for the  instrumentation have been determined,  as per Exhibit E,
          within the  current  calendar quarter.
                                     D-91                                ILM02.0

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                                                                 Exhibit D Method 202.2
                                     ALUMINUM*

             Method 202.2  CLP-M**  (Atomic Absorption, Furnace Technique)


Optimum Concentration Range:  20-200 ug/L
Approximate Detection Limit:  3 ug/L

Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame  Technique  (Method  202.1
     CLP-M).

2.   Prepare  dilutions of  the stock solution to be used as calibration  standards at
     the time of analysis.   These  solutions are also to be used for  "standard
     additions".

3.   The calibration standards must be  prepared using the  same  type  of  acid  and at
     the same concentration as will result in the sample to be  analyzed after  sample
     preparation.

           Paranieters (General)

                                            :0,
      1.  Drying Time and Temp:   30  sec @  125°C.
      2.  Ashing Time and Temp:   30  sec @  1300°C.
      3.  Atomizing Time and Temp:   10 sec @ 2700°C.
      4.  Purge  Gas Atmosphere:   Argon
      5.  Wavelength:  309.3 nm
      6.  Other  operating -parameter* should- be  set  as specif ied by the particular
         instrument manufacturer.

Notes

1.   The  above concentration values  and  instrument  conditions are for a  Perkin-Elmer
     HGA-2100, based on the use  of a 20  uL injection, continuous  flow purge gas  and
     non-pyrolytrc graphite and  are  to be  used as guidelines  only.

2.   Background  correction  is  required.

3.   It has been reported that chloride  ion and that nitrogen used as a  purge gas
     suppress the aluminum  signal.  Therefore  the use of halide acids and nitrogen
     as a purge  gas  should  be  avoided.

4.   For  every sample  analyzed,  verification is necessary to  determine that method
     of standard addition  is not required (Exhibit  E).

5.   If method of standard  addition is  required, follow the procedure given in
     Exhibit E.
*This method may only be used under specified conditions.

**CLP-M  Modified for the Contract Laboratory Program.
                                     D-92                                ILM02.0

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                                                                 Exhibit D Method 208.2
                                       BARIUM*

             Method 208.2  CLP-M** (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  10-200 ug/L
Approximate Detection Limit:  2 ug/L

Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame Technique  (Method 208.1
     CLP-M) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are also to be used for  "standard
     additions" .

3.   The calibration standards must be prepared using the same  type  of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.

           Pyryeters (General)

                                             °
      1.  Drying Time and Temp:   30 sec @ 125.
      2.  Ashing Time and Temp:   30 sec @ 1200°C.
      3.  Atomizing Time and Temp:   10 sec @ 2800°C.
      4.  Purge Gas Atmosphere:   Argon
      5.  Wavelength:   553.6 nm
      6.  Other operating parameters should be set as  specified by the  particular
          instrument manufacturer..  ______ _ ......... ____________ .'. _.
Notes

1.   The above concentration values and instrument conditions are for a Perkin- Elmer
     HGA-2100, based on the use of a 20 uL injection,  continuous  flow purge gas and
     pyrolytic graphite and are to be used as guidelines  only.

2.   The use of Kalide acid should be avoided.

3.   Because of possible chemical interaction, nitrogen should not be used as a
     purge gas.

4.   For every sample analyzed, verification £s necessary to determine  that method
     of standard addition is not required (see Exhibit E).

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-93                                ILM02.0

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                                                                 Exhibit D Method 219.2
                                      COBALT*
             Method 219.2  CLP-M**  (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  1 ug/L

Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame Technique  (Method 219.1
     CLP-M).

2.   Prepare dilutions of the stock solution to. be  used as calibration standards at
     the time of analysis.  These solutions are also to be used for  "standard
     additions".

3.   The calibration standards must be prepared using the same  type  of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.

Instrument Parameters (General)

      1.  Drying Time and Temp:   30 sec  @  125°C.
      2.  Ashing Time and Temp:   30 sec  @  900°C.
      3.  Atomizing Time and Temp:   10 sec @ 2700°C.
      4.  Purge Gas Atmosphere:   Argon
      5.  Wavelength:  240.7 nm
      6.  Other operating parameters should be set  as specified by the particular
          instrument manufacturer.
Notes

1.   The above concentration values and instrument  conditions are for a Perkin-Elmer
     HGA-2100, based on the use of a 20 uL injection, continuous flow purge gas and
     non-pyrolytic graphite and are to be  used as guidelines only.  Smaller size
     furnace devices or those employing faster rates of atomization c            furnace
     using lower -*tomization temperatures  for shorter time periods than the above
     recommended settings.

2.   The use of background correction is required.

3.   Nitrogen may also be used as the purge gas but with reported low sensitivity.

4.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit E).

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

-------
                                                                  Exhibit D Method 220.2
                                      COPPER*
             Method 220.2 CLP-M** (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  1 ug/L

Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame Technique (Method 220.1
     CLP-M).

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are also to be used for "standard
     additions".

3.   The calibration standards must be prepared using the same  type of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.

Instrument Parameters (General)

      1.  Drying  Time and Temp:   30 sec @  125°C.
      2.  Ashing  Time and Temp:   30 sec @  900°C.
      3.  Atomizing Time  and Temp:   10 sec @ 2700°C.
      4.  Purge Gas Atmosphere:   Argon
      5.  Wavelength:  324.7 nm
      6.  Other operating parameters should be  set as specified by the particular
          instrument manufacturer.

Notes

1.   The above concentration values and instrument conditions are for a Perkin-Elmer
     HGA-2100, based on the use cf a 20  uL injection, continuous flow purge gas and
     non-pyrolytic graphite and are to be  used as guidelines only.  Smaller size
     furnace devices or those employing  faster rates of atomization can be operated
     using lower atomization temperatures  for shorter time periods than the above
     recommended settings.

2.   Background correction is required.

3.   Nitrogen may also be used as the purge gas.

4.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see' Exhibit E).

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
*This method nay only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-95                                ILM02.0

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                                                                  Exhibit D Method 236.2
                                        IRON*
             Method 236.2  CLP-M**  (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  1 ug/L

Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame Technique (Method 236.1
     CLP-M).                                   -'

2.   Prepare dilutions of the stock solution to be  used as calibration standards at
     the time of analysis.  These solutions are also to be used for "standard
     additions".

3.   The calibration standards must be prepared using the same  type of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.

Ii\strtin>gnt Paran|et:ers (General)

      1.  Drying Time and  Temp:   30 sec @  125°C.
      2.  Ashing Time and  Temp:   30 sec @  1000°C.
      3.  Atomizing Time and Temp:   10 sec  @ 2700°C.
      4.  Purge Gas Atmosphere:  Argon
      5.  Wavelength:  248.3 nm
      6.  Other operating  parameters should be set  as specified by the particular
          instrument manufacturer.
Notes

1.   The above concentration values and instrument  conditions  are for a Perkin-Elmer
     HGA-2100, based on the use of a 20 uL injection, continuous flow purge gas and
     non-pyrolytic graphite and are to be used as guidelines only.  Smaller size
     furnace devices or those employing faster rates of atomization can be operated
     using lower  atomization temperatures for shorter time periods than the above
     recommended settings.

2.   The use of background correction is required.

3.   Nitrogen may also be used as the purge gas.

4.   For every sample analyzed, verification j,s necessary to determine that method
     of standard addition is not required (see Exhibit E).

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-96                                ILM02.0

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                                                                 Exhibit D Method 243.2
                                     MANGANESE*

             Method 243.2  CLP-M**  (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  1-30 ug/L
Approximate Detection Limit:  0.2 ug/L
                                  V
Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame Technique (Method 243.1
     CLP-M) .

2.   Prepare  dilutions of  the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are also to be used for "standard
     additions*.

3.   The calibration standards must be prepared using the same  type of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.
                      (General)

      1.  Drying Time  and Temp:   30 sec @  125°C.
      2.  Ashing Time  and Temp:   30 sec @  1000°C.
      3.  Atomizing Time and Temp:  10 sec @  2700°C.
      4.  Purge  Gas Atmosphere:   Argon
      5.  Wavelength:  279.5 nm
      6.  Other  operating parameters should be  set as  specified by  the particular
         instrument manufacturer.

Notes
1.   The  above concentration values  and instrument  conditions are for a Perkin- Elmer
     HGA-2100, based on  the use of a 20 uL injection,  continuous  flow purge gas  and
     non-pyrolytic graphite and are  to  be  used as guidelines only.   Smaller size
     furnace devices or  those  employing faster rates of atomization can be operated
     using  lower atomization  temperatures  for shorter time periods than the above
     recommended settings.

2.   The  use of ^background correction is required.

3.   Nitrogen may also be  used as the purge gas.

4.   For  every sample  analyzed, verification is necessary to determine that method
     of standard addition is  not required (see Exhibit E) .

5.   If method of standard addition is  required, follow the procedure given in
     Exhibit E.
*This method nay only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-97                                ILM02.0

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                                                                 Exhibit D Method 249.2
                                       NICKEL*
             Method 249.2 CLP-M** (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:  5-100 ug/L
Approximate Detection Limit:  1 ug/L

Preparation of Standard  Solution

1.   Stock solution:  Prepare as described under AA Flame Technique (Method 249.1
     CLP-M) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are also to be used for "standard
     additions".

3.   The calibration standards must be prepared using the same  type of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.
Instrument Parameters (General)

      1.  Drying Time and Temp:   30  sec @  12S°C.
      2.  Ashing Time and Temp:   30  sec @  900°C.
      3.  Atomizing Time  and Temp:   10 sec @ 2700°C.
      4.  Purge  Gas Atmosphere:   Argon
      5.  Wavelength: 232.0 nm
      6.  Other  operating parameters should be  set as specified by  the particular
          instrument manufacturer.

Notes

1.   The above concentration values  and instrument conditions are for a  Perkin- Elmer
     HGA-2100, based on the use of a 20 uL injection, continuous  flow purge gas  and
     non-pyrolytic graphite and are to be used as guidelines only.   Smaller size
     furnace devices or those employing faster rates of atomization can  be operated
     using lower atomization temperatures for shorter time periods than  the above
     recommended -settings .

2.   The use of background correction is required.

3.   Nitrogen may also be used as the purge gas.

4.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit  E) .

5.   If method of standard addition is required,  follow the procedure given in
     Exhibit E.
*This method may only be used ur"ter specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-98                                ILM02.0

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                                                                  Exhibit D Method 286.2
                                      VANADIUM*

             Method 286.2 CLP-M** (Atomic Absorption,  Furnace Technique)

Optimum Concentration Range:  10-200 ug/L
Approximate Detection Limit:  4 ug/L

Preparation of Standard  Solution

1.   Stock solution:  Prepare as described under AA Flame Technique (Method 286 ..1
     CLP-M) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are also to be used for "standard
     additions . *

3.   The calibration standards must be prepared using the same  type of acid and at
     the same concentration as will result in the sample to be  analyzed after sample
     preparation.
     ,      Pflrf meters (General)

      1.  Drying Time and Temp:   30 sec @ 125°C.
      2.  Ashing Time and Temp:   30 sec @ 1400°C.
      3.  Atomizing Time and Temp:   15 sec @ 2800°C.
      4.  Purge Gas Atmosphere:   Argon
      5.  Wavelength:   318.4 nm
      6.  Other operating parameters should be set as  specified by the particular
          instrument manufacturer.

flotgs

1.   The above concentration values and instrument conditions are for a Perkin- Elmer
     HGA-2100, based on the use of a 20 uL injection,  continuous flow purge gas and
     pyrolytic graphite and are to be used as guidelines only.  Smaller size furnace.
     devices or those employing faster rates of atomization can be operated using
     lower atomization temperatures for shorter time periods than the above
     recommended ^settings .

2.   The use of background correction is required.

3.   Because of possible chemical interaction, nitrogen should not be used as the
     purge gas.

4.   For every sample analyzed, verification is necessary to determine that method
     of standard addition is not required (see Exhibit E) .

5.   If method of standard addition is required, follow the procedure given in
     Exhibit E.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-99                                ILM02.0

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                                                                 Exhibit D Method 239
                                       ZINC*
Method 289.2 CLP-M** (Atomic Absorption,  Furnace Technique)

Optimum Concentration Range:  0.2-4 u§/L
Approximate Detection Limit:  0.05 ug/L

Preparation of Standard Solution

1.   Stock solution:  Prepare as described under AA Flame Technique (Method 289.1
     CLP-M) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  These solutions are also to be used for "standard
     additions".

3.   The calibration standards must be prepared using the same type of acid and at
     the same concentration as will result in-tiie sample - tir 1xei analyzed after sample
     preparation.

           Parameters (General)
      1.  Drying Time and Temp:   ?0 sec @ 125°C.
      2.  Ashing Time and Temp:   30 sec <§ 400°C.
      3.  Atomizing Time and Temp:   10 sec @ 2500°C.
      4.  Purge Gas Atmosphere:   Argon
      5.  Wavelength:  213.9 nm
      6.  Other operating parameters should be set as specified by the particular
          instrument manufacturer.

Notes
1.   The above concentration values and instrument conditions are for a Perkin- Elmer
     HGA-2100, based on the use of a 20 uL injection, continuous flow purge gas and
     non-pyrolytic graphite and are to be used as guidelines only.  Smaller size
     furnace devices or those employing faster rates of atomization can be operated
     using lower atomization temperatures for shorter time periods then the above
     recommended-settings .

2.   The use of background correction is required.

3.   Nitrogen may also be used as the purge gas.

4.   The analysis of zinc by the graphite furnace is extremely sensitive and very
     subject to contamination from the work area, reagents, and pipette tips.  Since
     all these factors affect the precision and accuracy, zinc should be analyzed by
     the direct aspiration procedure whenever possible.
*This method may only be used under specified  conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-100                                ILM02.0

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                                                                 Exhibit D Method 289.2
5.   For every sample analyzed,  verification is necessary to determine that method
     of standard addition is not required (see Exhibit E).

6.   If method of standard addition is required, follow the procedure given in
     Exhibit E.

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                                                                 Exhibit D Method 202.1
                                     ALUMINUM*

             Method 202.1  CLP-M** (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  5-50 mg/L using a wavelength of 309.3 ran
Sensitivity:  1 mg/L
Approximate Detection Limit:  0.1 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 1,000  g of aluminum  metal analytical  reagent
     grade).  Add 15 mL of cone.  HC1 and 5  mL cone.  W0$ to  the metal,  cover  the
     beaker and warm gently.  When solution  is complete, transfer quantitatively  to
     a. liter volumetric flask and make  up to volume with deionized  distilled water.
     1 mL - 1 mg Al (1000 mg/L) •

2.   Potassium Chloride Solution:   Dissolve  95 g potassium chloride (KC1) in
     deionized distilled water and make up to 1 liter.

3.   Prepare dilutions of the stock solution to be used as calibration standards  at
     the time of analysis.   The calibration  standards must be  prepared using the
     same type of acid and at the same concentration  as will  result in the  sample to
     be analyzed after sample preparation.   To each 100 mL of standard and sample
     alike add 2.0 mL potassium chloride solution.

           Paran|eters (General)
      1.  Aluminum hollow cathode lamp
      2.  Wavelength:   309.3 ran
      3 .  Fuel :   Acetylene
      4.  Oxidant:  Nitrous oxide
      5.  Type of flame:  Fuel rich
Interferences

1.   Aluminum is partially ionized in the nitrous oxide-acetylene flame.  This
     problem may be controlled by the addition of an alkali metal (potassium, 1000
     ug/mL) to both sample and standard solutions.
*This method may  only be used under  specified conditions.

**CLP-M Modified  for  the Contract  Laboratory Program.
                                     D-102                               ILM02.0

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                                                                 Exhibit D Method 202.1
Notes

 1.  The following may also be used:

       308.2 nm Relative Sensitivity 1
       396.2 nm Relative Sensitivity 2
       394.4 nm Relative Sensitivity 2.5

 2.  For concentrations of aluminum below 0.3 mg/L, use of
     Furnace Technique (Method 202.2 CLP-M) is recommended.

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                                                                 Exhibit D Method 204.1
                                     ANTIMONY*

              Method 204.1 CLP-M**  (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  1-40 mg/L using a wavelength of 217.6 tun
Sensitivity:  0.5 mg/L
Approximate Detection Limit:  0.2 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 2.7426 g of antimony potassium tartrate
     (analytical reagent grade) and dissolve in deionized distilled water.  Dilute
     to 1 liter with deionized distilled water.   1 ml -  1 mg Sb  (1000 mg/L) •

2.   Prepare dilutions of the stock solution to be used  as calibration  standards  at
     the time of- analysis.  The calibration standards must be. prepared  using  the.
     sane type of acid and at the same concentration as  will result in  the  sample to
     be analyzed after sample preparation.

                        (General)
      1.  Antimony hollow cathode lamp
      2.  Wavelength:   217.6 ran
      3 .  Fuel :   Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:   Fuel lean

Interferences    ___

1.   In the presence of lead (1000 mg/L), a special interference may occur at the
     217.6 nm resonance line.  In this case the 231.1 nm antimony line should be
     used.

2.   Increasing acid concentrations decrease antimony absorption.  To avoid this
     effect, the_acid concentration in the samples and in the standards must be
     matched.

Notes

1.   For concentrations of antimony below 0.35 mg/L,  use of the Furnace Technique
     (Method 204.2 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-104                               ILM02.0

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                                                                  Exhibit D Method 208.1
                                       BARIUM*
              Method 208.1  CLP-M** (Atomic Absorption,  Flame Technique)

Optimum Concentration Range:  1-20 mg/L using a wavelength of 553.6 nm
Sensitivity:  0.4 mg/L
Approximate Detection Limit:  0.1 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 1.7787 g of barium chloride (BaCl2'2H20,  analytical
     reagent grade) in deionized distilled water and dilute to liter.   1 mL - 1 mg
     Ba (1000 mg/L)•

2.   Potassium chloride solution:  Dissolve 95  g potassium chloride,  KC1, in
     deionized distilled water and make up to 1 liter.

3.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.   To each 100"mL of standard and sample alike add 2.0 mL
     potassium chloride solution.  The calibration standards must be prepared using
     the same type of acid and at the same concentration as will result in the
     sample to be analyzed after sample preparation.

Instrumental Pay^^ia^ers (General)

      1.  Barium hollow cathode lamp
      2.  Wavelength:  553.6 nm
      3.  Fuel:   Acetylene
      4.  Oxidant:  Nitrous oxide
      5.  Type of flame:   Fuel rich

Interferences

1.   The use of a nitrous oxide-acetylene flame virtually eliminates chemical
     interference; however, barium is easily ionized in this flame and potassium
     must be added  (1000 mg/L) to standards and samples alike to control this
     effect.

2.   If the nitrous oxide flame is not available and acetylene-air is used,
     phosphate,  silicon and aluminum will severely depress the barium absorbance.
     This may be overcome by the addition of 2000 mg/L lanthanum.

Notes

1.   For concentrations of barium, below 0.2 mg/L, use of the Furnace Technique
     (Method 208.2 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-105                               ILM02.0

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                                                                  Exhibit  D Method 210.1
                                     BERYLLIUM*

              Method 210.1 CLP-M** (Atomic  Absorption,  Flame Technique)


Optimum Concentration Range:  0.052 mg/L using a wavelength of 234.9 nm
Sensitivity:  0.025 mg/L
Approximate Detection Limit:  0.005 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 11.6586  g of beryllium sulfate, BeSO^, in deionized
     distilled water containing 2 mL cone,  nitric acid and dilute to 1 liter.  1 mL
     - 1 mg Be (1000 mg/L).

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  The calibration standards should be prepared using the
     sane type of acid and at the same  concentration as will result in the sample to
     be analyzed after sample preparation.

Instrumental Parameters (General)

      1.  Beryllium hollow cathode lamp
      2.  Wavelength:   234.9 nm
      3.  Fuel:   Acetylene
      4.  Oxidant:   Nitrous oxide
      5.  Type of flame:   Fuel rich

Interferences

1.   Sodium and silicon at concentrations in excess of 1000 mg/L have been found to
     severely depress the beryllium absorbance.

2.   Bicarbonate ion is reported to interfere;  however, its effect is eliminated
     when samples are acidified to a pH of  1.5.

3.   Aluminum at concentrations of 500  ug/L is reported to depress the sensitivity
     of beryllium [Spectrochim Acta 22, 1325 (1966)].

Notes

1.   For concentrations of beryllium below 0.02 mg/L, use of the Furnace Technique
     (Method 210.2 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-106                               ILM02.0

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                                                                  Exhibit D Method 213.1
                                      CADMIUM*

              Method 213.1 CLP-M** (Atomic  Absorption,  Flame Technique)


Optimum Concentration Range:  0.052 mg/L using a wavelength of 228.8 nm
Sensitivity:  0.025 mg/L
Approximate Detection Limit:  0.005 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 2.282 g of cadmium sulfate (3CdS04*8H20,
     analytical reagent grade) and dissolve in deionized distilled water.  Make up
     to 1 liter with dionized distilled water.  1 mL - 1 mg Cd (1000 mg/L).

2.   Prepare dilutions of the stock solution to be used as calibration standards  at
     the time of analysis.  The calibration standards must be  prepared using the
     same type of acid and at the same concentration as will result in -the sample to
     be analyzed after sample preparation.

             Paran>eters (General)
      1.  Cadmium hollow cathode lamp
      2.  Wavelength:   228.8 nm
      3 .  Fuel :   Acetylene
      A.  Oxidant:  Air
      5.  Type of flame:  Oxidizing

Notes

1.   For concentrations of cadmium below 20 ug/L, use of the Furnace Technique,
     Method 213.2 CLP-M is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-107                               ILM02.0

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                                                                 Exhibit D Method 218.
                                      CHROMIUM*

              Method 218.1 CLP-M**  (Atomic Absorption, Flame Technique)

Optimum Concentration Range:  0.5-10 mg/L using a wavelength of 357.9 nm
Sensitivity:  0.25 mg/L
Approximate Detection Limit:  0.05 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 1.923 g of chromium trioxide (CrO^- reagent grade)  in
     deionized distilled water.   When solution is complete,  acidify with redistilled
     HN03 and dilute to 1 liter with deionized distilled water.   1  iaL - 1 mg Cr
     (1000 mg/L).
2.   Prepare dilutions of the stock solution to be used  as  calibration standards at
     the time of analysis.  The calibration standards must  be prepared using the
     same type of acid and at the same concentration as  will result In the sample  to
     be analyzed after sample preparation.   -             ...
         t Parameters (General)
      1.  Chromium hollow cathode  lamp
      2.  Wavelength:   357.9 nm
      3 .  Fuel :   Acetylene
      4.  Oxidant:   Nitrous oxide
      5.  Type of flame:   Fuel rich

Notes
1.   The following wavelengths may also be used:

          359.3 nm Relative Sensitivity 1.4
          425.4 nm Relative Sensitivity 2
          427.5 nm Relative Sensitivity 3
          428.9 nm Relative Sensitivity 4
2.   The fuel rich air-acetylene flame provides greater sensitivity but is subject
     to chemical and matrix interference from iron,  nickel,  and other metals.   If
     the analysis is performed in a lean flame the interference can be lessened but
     the sensitivity will also be reduced.
3.   The suppression of both Cr (III) and Cr (VI) absorption by most interfering
     ions in fuel rich air-acetylene flames is reportedly controlled by the addition
     of 1% ammonium bifluoride in 0.2% sodium sulfate [Talanta 20, 631 (1973)].  A
     1% oxine solution is also reported to be useful .
4.   For concentrations of chromium between 50 and 200 ug/L where the air-acetylene
     flame cannot be used or for concentrations below 50 ug/L, use of the Furnace
     Technique (Method 218.2 CLP-M) is recommended.
*This method may  only be used under specified conditions.

**CLP-M Modified  for the Contract Laboratory  Program.
                                     D-108                               ILM02.0

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                                                                 Exhibit D Method 219.1
                                       COBALT*

              Method 219.1** CLP-M (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  0.5-5 mg/L using a wavelength of 240.7 nm
Sensitivity:  0.2 mg/L
Approximate Detection Limit:  0.05 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 4.307 g of cobaltous chloride  (CoC12.   6H20
     analytical reagent grade), in deionized distilled water.   Add 10 mL of
     concentrated nitric acid and dilute to 1 liter with deionized distilled water.
     1 mL - 1 mg Co (1000 mg/L) .

2.   Prepare dilutions of the stock cobalt solution to be used as calibration
     standards at the time of analysis.  The calibration  standards must be prepared
     using the same type of acid and at the same concentration as will result in the
     sample to be analyzed after sample preparation.

           Parameters (General)
      1.  Cobalt hollow cathode lamp
      2.  Wavelength:   240.7 nm
      3.  Fuel:   Acetylene
      4 .  Oxidant :   Air
      5.  Type of flame:   Oxidizing
Notes

1.   For concentrations of cobalt below 100 ug/L use of the Furnace Technique
     (Method 219.2 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-109                               ILM02.0

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                                                                  Exhibit D Method  220.1
                                       COPPER*

              Method 220.1 CLP-M** (Atomic Absorption,  Flame  Technique)


Optimum Concentration Range:  0.2-5 mg/L using a wavelength of 324.7 nm
Sensitivity:  0.1 mg/L
Approximate Detection Limit:  0.02 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 100 g  of electrolyte copper (analytical
     reagent grade).  Dissolve in 5 mL redistilled HN(>3 and make up to 1 liter with
     deionized distilled water.   Final concentration is 1 mg  Cu per mL (1000 mg/L).

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  The calibration  standards must be prepared using the
     same type of acid and at the same concentration as will  result 'in the"sample to
     be analyzed after sample preparation.

             Parflmeters (General)
      1.  Copper hollow cathode  lamp
      2.  Wavelength:   324.7  nm
      3.  Fuel:   Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:  Oxidizing

Notes

1.   For concentrations of copper below 50 ug/L use of the Furnace Technique (Method
     220.2 CLP-M) is recommended.

2.   Numerous absorption lines are available for the determination of copper.  By
     selecting a suitable absorption wavelength, copper samples may be analyzed over
     a very wide range of concentrations.  The following lines may be used:

          327.4 nm Relative Sensitivity 2
          216.5 nm Relative Sensitivity 7
          222.5 nm Relative Sensitivity 20
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-110                               ILM02.0

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                                                                 Exhibit D Method 236.1
                                        IRON*

              Method 236.1 CLP-M** (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  0.3-5 mg/L using a wavelength of 248.3 nm
Sensitivity:  0.12 mg/L
Approximate Detection Limit:  0.03 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 1.000 g of pure iron wire (analytical reagent
     grade) and dissolve in 5 mL redistilled HN03, warming if necessary.   When
     solution is complete, make up to 1 liter with deionized distilled water.   1 mL
     - 1 mg Fe (1000 mg/L) .

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  The calibration standards *ust be prepared- using the
     same type of acid and at the same concentration as will result in the sample  to
     be analyzed after sample preparation.

             Par""«*ers (General)
      1.  Iron hollow cathode lamp
      2.  Wavelength:  248.3 nm
      3 .  Fuel :   Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:   Oxidizing
Notes

1.   The following wavelengths may also be used:
     248.8 nm Relative Sensitivity 2
     271.9 nm Relative Sensitivity 4
     302.1 nm Relative Sensitivity 5
     252.7 nm Relative Sensitivity 6
     372.0 nm Relative Sensitivity 10

2.   For concentrations of iron below 0.05 mg/L use of the Furnace Technique (Method
     236.2 CLP-M) is recommended.
*This method may only be used under specified conditions,

**CLP-M Modified for the Contract Laboratory  Program.
                                     D-lll                       .        ILM02.0

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                                                                 Exhibit D Method 239.1
                                       LEAD*

             Method 239.1  CLP-M**  (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  1-20 mg/L using a wavelength of 283.3 nm
Sensitivity:  0.5 mg/L
Approximate Detection Limit:  0.1 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 1.599  g of lead nitrate,  Pb(N03>2  (analytical
     reagent grade), and dissolve deionized  distilled water.  When  solution is
     complete acidify with 10 mL redistilled HN03 and dilute  to 1 liter  with
     deionized distilled water.  1 mL - 1 mg Pb (1000 mg/L) •

2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the tine of analysis.   The calibration  standards must be prepared using the
     same type of acid and at the same concentration as will  result in the sample to
     be analyzed after sample preparation.

Instr^^^ental ParnT^eters (General)

      1.  Lead hollow cathode lamp
      2.  Wavelength:  283.3 nm
      3.  Fuel:  Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:   Oxidizing
Notes

1.   The analysis of this metal is exceptionally sensitive to turbulence and
     absorption bands in the flame.  Therefore, some care should be taken to
     position the light beam in the most stable, center portion of the flame.  To do
     this, first adjust the burner to maximize the absorbance reading with a lead
     standard.  TKen, aspirate a water blank and make minute adjustments in the
     burner alignment to minimize the signal.

2.   The concentrations of lead below 200 ug/L use of the Furnace Technique  (Method
     239.2 CLP-M) is recommended.

3.   The following wavelengths may also be used:

         217.0 nm Relative  Sensitivity 0.4
         261.4 nm Relative  Sensitivity 10
*This method may only be used under  specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-112                               ILM02.0

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                                                                 Exhibit D Method 243.1
                                     MANGANESE*

              Method 243.1  CLP-M** (Atomic Absorption, Flame Technique)

                                  t,

Optimum Concentration Range:  0.1-3 mg/L using a wavelength of 279.5 nm
Sensitivity:  0.05 mg/L
Approximate Detection Limit:  0.01 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 1.000 g of manganese metal (analytical  reagent
     grade), and dissolve in 10 mL redistilled W80$.   When solution is complete,
     dilute to 1 liter with 1% (v/v) HC1.   1 mL - 1 mg Mn (1000 mg/L) •
2.   Prepare dilutions of the stock solution to be used as calibration standards  at
     the time of analysis.  The calibration standards must be prepared using the
     same type of acid and at the same concentration as will result in the sample to
     be analyzed after sample preparation.
                        (General)
      1.  Manganese hollow cathode lamp
      2.  Wavelength:   279.5 nm
      3 .  Fuel :   Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:   Oxidizing

Notes

1.   For concentrations of manganese below 25 ug/L,  use of the Furnace Technique
     (Method 243.2 CLP-M) is recommended.

2.   The following line may also be used:   403.1 nm Relative Sensitivity 10.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

-------
                                                                  Exhibit  D Method 249.1
                                      NICKEL*

              Method 249.1  CLP-M**  (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  0.3-5 mg/L using a wavelength of 232.0 nm
Sensitivity:  0.15 mg/L
Approximate Detection Limit:  0.04 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 4.953 g of nickel nitrate,  Ni(N(>3)2'6H20 (analytical
     reagent grade) in deionizing distilled water.   Add 10 mL of cone,  nitric acid
     and dilute to 1 liter deionized distilled water.   1 mL - 1 mg Ni (1000 mg/L).

2.   Prepare dilutions of the stock solution to be  used as calibration standards at
     the tine of analysis.   The calibration standards  should be prepared using the
     same type of acid and at the same concentration as will result in the sample to
     be analyzed after sample preparation.

Instr\BP?Tiyal Parameters (General)

      1.  Nickel hollow cathode lamp
      2.  Wavelength:   232.0 nm
      3.  Fuel:   Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:   Oxidizing
Interferences

1.   The 352.4 nm wavelength is less susceptible to spectral interference and may be
     used.  The calibration curve is more linear at this wavelength; however, there
     is some loss of sensitivity.

Notes            	

1.   For concentrations of nickel below 100 ug/L, use  of the Furnace Technique
     (Method 249.2 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

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                                                                 Exhibit D Method 272.1
                                       SILVER*

              Method 272.1 CLP-M** (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  0.1-4 mg/L using a wavelength of 328.1 nm
Sensitivity:  0.06 mg/L
Approximate Detection Limit:  0.01 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 1.575 g of AgNOs,  (analytical reagent grade)  in
     deionized distilled water,  add 10 mL cone.  HN(>3 and make up to 1 liter.   1 mL -
     1 mg Ag (1000 mg/L) .

2.   Prepare dilutions of the stock solution to be used as calibration standards  at
     the time of analysis.  The calibration standards must be prepared using the
     same type of acid and at the same concentration as will result in the sample to
     be analyzed after sample preparation.

3.   Iodine Solution, 1 N:  Dissolve 20 grams of potassium iodide,  KI (analytical
     reagent grade) in 50 mL of deionized distilled water, add 12.7 grams of iodine,
     12, (analytical reagent grade) and dilute to 100 mL.  Store in a brown bottle.

4.   Cyanogen Iodide (CNI) Solution:  To 50 mL of deionized distilled water add 4.0
     mL cone.  Nl^OH, 6.5 grams KCN, and 5.0 mL of 1.0 N 12 solution.  Mix and
     dilute to 100 mL with deionized distilled water.  Fresh solution should be
     prepared every two weeks. (1)

             Prameters (General)
      1.  Silver hollow cathode lamp
      2.  Wavelength:   328.1 nm
      3.  Fuel:   Acetylene
      4 .  Oxidant :   Air
      5.  Type of Aflame:  Oxidizing

Notes

1.   For concentrations of silver below 30 ug/L, use of the Furnace Technique
     (Method 272.2 CLP-M) is recommended.

2.   Silver nitrate standards are light sensitive.  Dilutions of the stock should be
     discarded after use as concentrations below 10 mg/L are not stable over long
     periods of time.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-115                               ILM02.0

-------
                                                                 Exhibit D Method 272.1
3.   If absorption to container walls or the formation of AgCl is suspected,  make
     the sample basic using cone.  Nl^OH and add 1 mL of (CNI)  solution per 100 mL of
     sample.   Mix the sample and allow to stand for 1 hour before proceeding with
     the analysis.(1)

4.   The 338.2 nm wavelength may also be used.   This has a relative sensitivity of
     2.
                                     D-116                               ILM02.0

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                                                                  Exhibit D Method 279.1
                                      THALLIUM*

              Method 279.1 CLP-M** (Atomic Absorption,  Flame  Technique)


Optimum Concentration Range:   1-20 mg/L using  a wavelength of 276. 8 run
Sensitivity:  0.5 mg/L            ^
Approximate Detection Limit:   0.1 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Disscl-." l.:C2 5 of thallium nitrate, T1N03 (analytical
     reagent grade) in deionized distilled water.   Add 10 mL of cone,  nitric acid
     and dilute to 1 liter with deionized distilled water.  1 mL - 1 mg Tl (1000
2.   Prepare dilutions of the stock solution to be used as calibration standards at
     the time of analysis.  The calibration standards must be prepared using nitric
     acid and at the same concentration as will result in the sample to be analyzed
     after sample preparation.
                        (General)
      1.  Thallium hollow cathode lamp
      2.  Wavelength:   276.8 nm
      3 .  Fuel :  Acetylene
      4 .  Oxidant :   Air
      5.  Type of  flame:   Oxidizing

      Notes

     For concentrations of thallium below 0.2 mg/L,  use of the Furnace Technique
     (Method 279.2 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-117                               ILM02.0

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                                                                  Exhibit  D Method 286.1
                                      VANADIUM*

              Method 286.1 CLP-M** (Atomic Absorption, Flame Technique)


Optimum Concentration Range:  2-100 mg/L using a wavelength of 318.4 nm
Sensitivity:  0.8 mg/L
Approximate Detection Limit:  0.2 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Dissolve 1.7854 g of vanadium pentoxide,  ^2Q5 (analytical
     reagent grade) in 10 mL of cone, nitric acid and dilute to 1 liter with
     deionized distilled water.   1 mL - 1 ng V (1000 mg/L).

2.   Aluminum nitrate solution:   Dissolve 139 g aluminum nitrate, Al(N03)3'9H20,  in
     150 mL of deionized distilled water; heat to effect solution.  Allow to cool
     and make up to 200 mL.

3.   Prepare dilutions of the stock vandium solution to  be used as calibration
     standards at the time of analysis.   The calibration standards must be prepared
     using the same type of acid and at the same concentration as will result in the
     sample to be analyzed after sample preparation.   To each 100 mL of standard and
     sample alike, add 2 mL of the aluminum nitrate solution.

                        (General)
      1.  Vanadium hollow cathode lamp
      2.  Wavelength:   318.4 nm
      3 .  Fuel :   Acetylene
      4.  Oxidant:   Nitrous  Oxide
      5.  Type of flame:   Fuel  rich

Interferences

1.   It has been reported that  high concentrations of aluminum and titanium increase
     the sensitivity of vanadium.  This interference can be controlled by adding
     excess aluminum (1000 ppm) to both samples and standards.  [Talanta 15, 871
     (1968)].

Notes

1.   For concentrations of vanadium below 0.5 mg/L, use of the Furnace Technique
     (Method 282.6 CLP-M) is recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.
                                     D-118                               ILM02.0

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                                                                  Exhibit D Method 289.1
                                        ZINC*

              Method 289.1 CLP-M** (Atomic Absorption,  Flame Technique)


Optimum Concentration Range:  0.05-1 mg/L using a wavelength of 213.9 -nm-
Sensitivity:  0.02 mg/L
Approximate Detection Limit:  0.005 mg/L

Preparation of Standard Solution

1.   Stock Solution:  Carefully weigh 1.00 g of zinc metal (analytical reagent
     grade) and dissolve cautiously in 10 mL HN03-   When solution is complete make
     up to 1 liter with deionized distilled water.   1 mL - 1 mg Zn (1000 mg/L) •

2.   Prepare dilutions of the stock solution to be  used as calibration standards  at
     the tine of analysis.  The calibration standards must be  prepared using the
     same type of acid and at the same concentration as will result in -the sample to
     be analyzed after sample preparation.

             Pargnreters (General)
      1.  Zinc hollow cathode lamp
      2.  Wavelength:   213.9 nm
      3 .  Fuel :  Acetylene
      4.  Oxidant:   Air
      5.  Type of flame:   Oxidizing

Notes

1.   High levels of silicon may interfere.

2.   The air-acetylene flame absorbs about 25% of the energy at the 213.9 nm line.

3.   The sensitivity may be increased by the use of low -temperature flames.

4.   Some container cap liners can be a source of zinc contamination.  To circumvent
     or avoid this problem, the use of the polypropylene caps is recommended.

5.   For concentrations of zinc below 0.01 mg/L, use of the Furnace Technique
     (Method 289.2 CLP-M) is recommended.
*This method may only be used under  specified conditions.

**CLP-M Modified for  the Contract Laboratory Program.
                                     D-119                               ILM02.0

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                              EXHIBIT  E
           QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS
SECTION I




SECTION II




SECTION III




SECTION IV




SECTION V




SECTION VI




SECTION VIT




SECTION VIII




SECTION IX




SECTION X




SECTION XI
GENERAL QA/QC PRACTICES




SPECIFIC QA/QC PROCEDURES




QUALITY ASSURANCE PLAN




STANDARD OPERATING PROCEDURES




REQUIRED QA/QC OPERATIONS




CONTRACT COMPLIANCE SCREENING




ANALYTICAL STANDARDS REQUIREMENTS




DATA PACKAGE AUDITS




PERFORMANCE EVALUATION SAMPLES




ON-SITE LABORATORY EVALUATIONS




DATA MANAGEMENT
Page No.




  E-l




  E-2




  E-4




  E-8




  E-13




  E-29




  E-30



  E-35




  E-37



  E-40




  E-43
                                                                  ILM02.0

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                                  SECTION I

                           GENERAL QA/QC PRACTICES


Standard laboratory practices for laboratory cleanliness as applied to
glassware and apparatus must be adhered to.  Laboratory practices with
regard to reagents, solvents, and gases must also be adhered to.  For
additional guidelines regarding these general laboratory procedures, see
Sections 4 and 5 of the Handbook for Analytical Quality Control in Water
and Wastewater Laboratories EPA-600/4-79-019, USEPA Environmental
Monitoring and Support Laboratory, Cincinnati, Ohio, September 1982.
                                    E"1                                 ILM02.0

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                                 SECTION II

                          SPECIFIC QA/QC PROCEDURES


The quality assurance/quality control (QA/QC) procedures defined herein
must be used by the Contractor when performing the methods specified in
Exhibit 0.  When additional QA/QC procedures are specified in the methods
in Exhibit D, the Contractor must also follow these procedures.  NOTE:  The
cost of performing^*!! QA/QC procedures specified in this Statement of Work
is included in the price of performing the bid lot,  except for duplicate,
spike, and laboratory control sample analyses, which shall be considered
separate sample analyses.

The purpose of this document is to provide a uniform set of procedures for
the analysis of inorganic constituents of samples, documentation of methods
and their performance, and verification of the sample data generated.  The
program will also assist laboratory personnel in recalling and defending
their actions under cross examination if required to present court
testimony in enforcement case litigation.

The primary function of the QA/QC program is the definition of procedures
for the evaluation and documentation of sampling and analytical
methodologies and the reduction and reporting of d&ta.   The objective is to
provide a uniform basis for sample collection and handling, instrument and
methods maintenance,  performance evaluation, and analytical data gathering
and reporting.  Although it is impossible to address all analytical
situations in one document, the approach taken here is to define minimum
requirements for all major steps relevant to any inorganic analysis.  In
many instances where methodologies are available, specific quality control
procedures are incorporated into the method documentation (Exhibit D).
Ideally, samples involved in enforcement actions are analyzed only after
the methods have met the minimum performance and documentation requirements
described in this document.

The Contractor is required to participate in the Laboratory Audit and
Intercomparisoa Study Program run by EPA EMSL-Las Vegas.  The Contractor
can expect to analyze at least two samples per calendar quarter during the
contract period.

The Contractor must perform and report to SMO and EMSL as specified in
Exhibit B quarterly verification of instrument detection limits (IDL) by
the method specified in Exhibit E, by type and model for each instrument
used on this contract.  All the IDLs must meet the CRDLs specified in
Exhibit C.  For ICP methods, the Contractor must also report, as specified
in Exhibit B, linearity range verification, all interelement correction
factors, wavelengths used, and integration times.

In this Exhibit, as well as other places within this Statement of Work, the
term "analytical sample" is used in discussing the required frequency or
placement of certain QA/QC measurements.  The term "analytical sample* is
defined in the glossary, Exhibit G.  As the term is used, analytical sample
includes all field samples, including Performance Evaluation samples,
received from an external source, but it also includes all required QA/QC
samples (matrix spikes, analytical/post-digestion spikes, duplicates,

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serial dilutions, LCS, ICS, CRDL standards, preparation blanks and linear
range analyses) except those directly related to instrument calibration or
calibration verification (calibration standards, ICV/ICB, CCV/CCB).   A
"frequency of 10%" means once every 10 analytical samples.  Note:
Calibration verification samples (ICV/CCV) and calibration verification
blanks (ICB/CCB) are not counted as analytical samples when determining 10%
frequency.

In order for the QA/QC information to reflect the status of the samples
analyzed, all samples and their QA/QC analysis must: be analyzed under the
same operating and procedural conditions.

If any QC measurement fails to meet contract criteria, the analytical
measurement may not be repeated  prior to taking the appropriate corrective
action as specified in Exhibit E.

The Contractor must report all QC data in the exact: format specified in
Exhibits B and H.

Sensitivity, instrumental detection limits (IDL's), precision, linear
dynamic range and interference effects must be established for each analyte
on a particular instrument.  All reported measurements must be within the
instrumental linear ranges.  The analyst must maintain quality control data
confirming instrument performance and analytical results.

In addition, the Contractor shall establish a quality assurance program
with the objective of providing sound analytical chemical measurements.
This program shall incorporate the quality control procedures, any
necessary corrective action, and all documentation required during data
collection as well as the quality assessment measures performed by
management to ensure acceptable data production.

As evidence of such a program, the Contractor shall prepare a written
Quality Assurance Plan (QAF) (see Section III) which describes the
procedures that are implemented to achieve the following:

      Maintain-4ata integrity, validity, and useability.

      Ensure that analytical measurement systems are maintained in an
      acceptable state of stability and reproducibility.

      Detect problems through data assessment and establishes corrective
      action procedures which keep the analytical process reliable.

      Document all aspects of the measurement process in order to provide
      data which are technically sound and legally defensible.
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                                 SECTION  III

                           QUALITY ASSURANCE PLAN

The QAP must present, in specific terms,  the policies, organization,
objectives, functional guidelines, and specific QA and QC activities
designed to achieve the data quality requirements in this contract.  Where
applicable, SOPs pertaining to each element shall be included or referenced
as part of the QAP.  The QAP must be available during on-site laboratory
evaluation and upon written request by the APO.  The elements of the  QAP
are listed in the following outline.

A.   Organization and Personnel

     1.   QA Policy and Objectives

     2.   QA Management

          a.   Organization

          b.   Assignment of QC and  QA Responsibilities

          c.   Reporting Relationships

          d.   QA Document Control Procedures

          e.   QA Program Assessment Procedures

     3.   Personnel

          a.   Resumes

          b.   Education and Experience Pertinent  to this  Contract

          c.   Training Progress

B.   Facilities and Equipment

     1.   Instrumentation and Backup Alternatives

     2.   Maintenance Activities  and Schedules

C.   Document Control

     1.   Laboratory Notebook Policy

     2.   Samples Tracking/Custody Procedures

     3.   Logbook Maintenance and Archiving Procedures

     4.   SDG File Organization,  Preparation and Review Procedures
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     5.    Procedures for Preparation,  Approval, Review, Revision, and
          Distribution of SOPs

     6.    Process for Revision of Technical  or Documentation Procedures

D.   Analytical Methodblogy

     1.    Calibration Procedures and Frequency.

     2.    Sample Preparation Procedures

     3.    Sample Analysis Procedures

     4.    Standards Preparation Procedures

     5.'   Decision Processes,  Procedures, and Responsibility for Initiation
          of Corrective Action

E.   Data Generation

     1.    Data Collection Procedures

     2.    Data Reduction Procedures

     3.    Data Validation Procedures

     4.    Data Reporting and Authorization Procedures

F.   Quality Assurance

     1.    Data Quality Assurance

     2.    Systems/Internal Audits

     3.    Performance/External Audits

     4.    Corrective Action Procedures

     5.    Quality Assurance Reporting Procedures

     6.    Responsibility Designation

G.   Quality Control

     1.    Solvent. Reagent and Adsorbent Check Analysis

     2.    Reference Material Analysis

     3.   Internal Quality Control Checks

     4.   Corrective Action and Determination of QC Limit Procedures

     5.   Responsibility Designation



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Updating and  Submission of the GAP:

Within  60 Days of contract award:

During  the contract solicitation process, the Contractor was required to
submit  their  QAP to EMSL/LV and NEIC.  Within sixty (60) days after
contract award, the Contractor shall send a revised QAP, fully compliant
with the requirements of this contract, to the Technical Project Officer,
EMSL/LV and NEIC.  The revised QAP will become the official QAP under the
contract.  The revised QAP must include:

1)   Changes resulting from A)  The Contractor's internal review of their
     organization,  personnel, facility, equipment,  policy and procedures and
     B)   The Contractor's implementation of the requirements of the
     contract; and,

2)   Changes resulting from the Agency's review of  the laboratory evaluation
     sample data,  bidder supplied documentation,  and recommendations made
     during the pre-award On-Site laboratory evaluation

Subsequent submissions:

During  the term of contract,  the Contractor shall &mend the QAP when the
following circumstances occur:

1)   The Agency modifies the  contract,

2)   The Agency notifies the  Contractor of deficiencies in the QAP document

3)   The Agency notifies the Contractor of deficiencies resulting from the
     Agency's review of the Contractor's performance,

4)   The Contractor identifies deficiencies resulting from their internal
     review of their QAP document,

5)   The Contractor's organization, personnel, facility, equipment, policy
     or procedures change,

6)   The Contractor identifies deficiencies resulting from the internal
     review of their organization, personnel, facility, equipment, policy or
     procedures changes.

The Contractor shall amend the QAP within 30 days of when the  circumstances
listed  above  result in a discrepancy between what was previously  described
in the  QAP and what is presently occurring at the Contractor's facility.

When the QAP  is amended, all  changes in the QAP must be  clearly marked
(e.g.,  a bar  in the margin indicating where the change  is found in the
document, or  highlighting the change by underlining the  change, bold
printing the  change, or using a different print font).   The amended section
pages must have the date on which  the  changes were  implemented.   The
Contractor shall incorporate  all amendments  to  the  current  QAP document.
The Contractor shall archive  all  amendments  to  the  QAP document for future
reference by  the Agency.
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The Contractor shall send a copy of the current QAP document within 14 days
of a request by the Technical Project Officer or Acininistrative Project
Officers to the designated recipients.

Corrective Action:

If a Contractor fails to adhere to the requirements listed in this section,
a Contractor may expect, but the Agency is not limited to the following
actions:  reduction of numbers of samples sent under this contract,
suspension of sample shipment to the Contractor, d£.ta package audit, an On-
Site laboratory evaluation, remedial performance evaluation sample, and/or
contract sanctions, such as a Cure Notice.
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                                 SECTION IV
                        STANDARD OPERATING  PROCEDURES


In order to obtain reliable results, adherence to prescribed analytical
methodology is imperative. In any operation that i£ performed on a
repetitive basis, reproducibility is best accomplished through the use of
Standard Operating Procedures (SOPs).  As defined by the EPA, an SOP is a
written document which provides directions for the step-by-step execution
of an operation, analysis, or action which is commonly accepted as the
method for performing certain routine or repetitive tasks.

SOPs prepared by the Contractor must be functional: i.e., clear,
comprehensive, up-to-date, and sufficiently detailed to permit duplication
of results by qualified analysts.  All SOPs, as presented to the Agency,
must reflect activities as they are currently performed in the laboratory.
In addition, all SOPs must be:

o   Consistent with current EPA  regulations,  guidelines,  and the CLP
    contract's requirements.
o   Consistent with instruments  manufacturers's  specific  instruction
    manuals.
o   Available to  the EPA during  an On-Site  Laboratory  Evaluation.   A
    complete set  of SOPs shall be bound together and available for
    inspection at such evaluations.   During On-Site Laboratory evaluations,
    laboratory personnel may be  asked to demonstrate the  application of the
    SOPs.

o   Capable of providing for the development of documentation that is
    sufficiently  complete to record the performance of all tasks required by
    the protocol.
o   Capable of demonstrating the validity of data reported by the Contractor
    and explain—the cause of missing or inconsistent results.
o   Capable of describing the corrective measures and  feedback mechanism
    utilized when analytical results do not meet protocol requirements.
o   Reviewed regularly and updated as necessary when contract, facility, or
    Contractor procedural modifications are made.
o   Archived for  future reference in usability or evidentiary situations.
o   Available at  specific work stations as appropriate
o   Subject to a document control procedure which precludes the use of
    outdated or inappropriate SOPs.


SOP FORMAT:

The format for SOPs may vary  depending upon the kind  of  activity for which
they are prepared, however, at  a minimum,  the following  sections must be
included:

o   Title Page

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o   Scope and Application
o   Definitions
o   Procedures
o   QC Limits
o   Corrective Action Procedures,  Including Procedures for Secondary Review
    of Information Being Generated
o   Documentation Description and Example  Forms
o   Miscellaneous Notes and Precautions
o   References

SOPS REQUIRED:
The following SOPs are required by the Agency:
1.    Evidentiary SOP
      Evidentiary SOPs for required chain-of-custody and document control
      are discussed in Exhibit F
2.    Sample Receipt and Storage
      a.    Sample receipt and identification logbooks
      b.    Refrigerator temperature logbooks
      c.    Security precautions
3.    Sample preparation
4.    Glassware cleaning
5.    Calibration (Balances, etc.)
      a.    Procedures
      b.    Frequency requirements
      c.    Preventative maintenance schedule and procedures
      d.    Acceptance criteria and corrective actions
      e.    Logbook maintenance authorization
6.    Analytical procedures  (for each analytical system)
      a.    Instrument performance specifications
      b.    Instrument operating procedures
      c.    Data acquisition system operation
      d.    Procedures when  automatic quantitation algorithms are
      overridden
      e.    QC required parameters
      f.    Analytical run/injection logbooks
      g.     Instrument error and editing  flag descriptions  and  resulting
             corrective actions
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7.    Maintenance activities (for each analytical system)
      a.    Preventative maintenance schedule and procedures
      b.    Corrective maintenance determinants anci procedures
      c.    Maintenance authorization
8.    Analytical standards
      a.    Standard coding/identification and inventory system
      b.    Standards preparation logbook(s)
      c.    Standard preparation procedures
      d.    Procedures for equivalency/traceability analyses and
            documentation
      e.    Purity logbook (primary standards and solvents)
      f.    Storage, replacement, and labelling requirements
      g.    QC and corrective action measures
9.    Data reduction procedures
      a.    Data processing systems operation
      b.    Outlier identification methods
      c.    Identification of data requiring corrective action
      d.    Procedures for format and/or forms for each operation
10.   Documentation policy/procedures
      a.    Laboratory/analyst's notebook policy, including review policy
      b.    Complete SDG File contents
      c.    Complete SDG File organization and assembly procedures,
            including review policy
      d.    Document inventory procedures, including review policy
11.   Data validation/self inspection procedures
      a.    Dot* flow and chain-of -command for date, review
      b.    Procedures for measuring precision and accuracy
      c.    Evaluation parameters for identifying systematic errors
      d.    Procedures to assure that hardcopy and diskette deliverables
            are complete and compliant with the recuirements in SOW
            Exhibits B and H.
      e.    Procedures to assure that hardcopy deliverables are in
            agreement with their comparable diskette deliverables.
      f.    Demonstration of internal QA inspection procedure (demonstrated
            by supervisory sign-off on personal notebooks, internal
            laboratory evaluation samples, etc.).
      g.    Frequency and type of internal audits (eg.,  random, quarterly,
            spot checks, perceived trouble areas).
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      h.    Demonstration of problem identification-corrective actions and
            resumption of analytical processing.   Sequence resulting from
            internal audit (i.e., QA feedback).

      i.    Documentation of audit reports,  (internal and external),
            response, corrective action,  etc.

12.   Data management and handling

      a.    Procedures for controlling and estimating data entry errors.

      b.    Procedures for reviewing changes to data and deliverables and
            ensuring traceability of updates.

      c.    Lifecycle management procedures  for testing,  modifying and
            implementing changes to existing computing systems including
            hardware, software, and documentation or installing new
            systems.

      d.    Database security, backup and archival procedures including
            recovery from system failures.

      e.    System maintenance procedures and response time.

      f.    Individuals(s) responsible for system operation, maintenance,
            data integrity and security.

      g.    Specifications for staff training procedures.


SOPS DELIVERY REQUIREMENTS:

Updating and submission of SOPs:

Within 60 days of contract award:

During the contract solicitation process, the Contractor was required to
submit their SOPs to EMSL/LV and NEIC.  Within sixty (60) days after
contract award, the Contractor shall send a complete revised set of SOPs,
fully compliant with the requirements of this contract, to the Technical
Project Officer, EMSL/LV and NEIC.  The revised SOPs will become the
official SOPs under the contract.  The revised SOPs must include:

1)   Changes resulting from A)  the Contractor's  internal review of their
     procedures and B)  the Contractor's implementation of the requirements
     of the contract;

2)   Changes resulting from the Agency's review of the laboratory evaluation
     sample data,  bidder supplied documentation,  and recommendations made
     during the pre-award On-Site laboratory evaluation.

Subsequent Submissions:

During the term of contract, the Contractor shall aaend the SOPs when the
following circumstances occur:

1)   The Agency modifies the contract,

2)   The Agency notifies the Contractor of deficiencies in their SOPs
     documentation

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 3)   The Agency notifies the Contractor of deficiencies resulting from the
     Agency's review of the Contractor's performance,

 4)   The Contractor's procedures change,

 5)   The Contractor identifies deficiencies resulting from the internal
     review of their SOPs documentation, or

 6)   The Contractor identifies deficiencies resulting form the internal
     review of their procedures.

 The SOPs must be amended or new SOPs must be written within 30 days of when
 the circumstances listed- above result in a discrepancy between what was
 previously described in the SOPs and what is presently occurring at the
 Contractor's facility.  All changes in the SOPs must be clearly marked
 (e.g., a bar in the margin indicating where the chexige is in the document,
 or highlighting the change by underlining the change, bold printing the
 change, or using a different print font).  The amended/new SOPs must have
 the date on which the changes were implemented.

When the SOPs are amended or new SOPs are written, the Contractor shall
 document in a letter the reasons for the changes, end submit the amended
 SOPs or new SOPs to the Technical Project Officer, EMSL/LV (quality
 assurance/technical SOPs) and NEIC (evidentiary SOPs).  The Contractor
 shall send the letter and the amended sections of the SOPs or new SOPs
within 14 days of the change.  An alternate delivery schedule for the
 submittal of the letter and amended/new SOPs may be proposed by the
 Contractor, but it is the sole decision of the Agency, represented either
by the Technical Project Officer or Administrative Project Officer, to
 approve or disapprove the alternate delivery schedule.  If an alternate
 delivery schedule is proposed, the Contractor shall describe in a letter to
 the Technical Project Officer, Administrative Project Officer, and the
 Contracting Officer why he/she is unable to meet the delivery schedule
 listed in this section.  The Technical Project Officer/Administrative
 Project Officer will not grant an extension for greater than 30 days for
 •nending/writlng new SOPs.  The Technical Project Officer/Administrative
 Project OfficeT 3£iii n££ grant an extension for greater than 14 days for
 submission of the letter documenting the reasons for the changes and for
 submitting amended/new SOPs.  The Contractor shall proceed and not assume
 that an extension will be granted until so notified by the TPO and/or APO.

 The Contractor shall send a complete set of current. SOPs within 14 days of
 a request by the Technical Project Officer or Administrative Project
 Officer to the recipients he/she designates.

 Corrective action:

 If a Contractor fails to adhere to the  requirements  listed in this section,
 a Contractor may expect, but the Agency is not limited to the following
 action:  reduction of number of samples sent under  this  contract,
 suspension of sample shipment to the Contractor,  dz.ta. package audit, On-
 Site laboratory evaluation, remedial performance evaluation  sample, and/or
 contract sanction, such as a Cure Notice.
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                                  SECTION V

                          REQUIRED QA/QC OPERATIONS

This section outlines the minimum QA/QC operations necessary to satisfy the
analytical requirements of the contract.  The following QA/QC operations
must be performed as described in this Exhibit:

     1.   Instrument Calibration
     2.   Initial Calibration Verification (ICV)  and Continuing Calibration
          Verification (CCV)
     3.   CRDL Standards  for  AA (CRA)  and  ICP (CRI)
     4.   Initial Calibration Blank (ICB) ,  Continuing Calibration Blank
          (CCB),  and Preparation Blank (PB)  Analyses
     5.   ICP Interference Check Sample (ICS) Analyses
     6.   Spike Sample Analysis (S)
     7.   Duplicate  Sample Analysis (D)
     8.   Laboratory Control  Sample (LCS) Analysis
     9.   ICP Serial Dilution Analysis (L)
     10.   Instrument Detection Limit (IDL)  Determination
     11.   Interelement Corrections for ICP  (ICP)
     12.   Linear  Range Analysis (LRA)

     13.   Furnace AA QC Analyses
1 •    InstirmnftTit CflH.brflti.on

     Guidelines for instrumental calibration are given in EPA 600/4-79-020
     and/or Exhibit D.  Instruments must be calibrated daily or once every 24
     hours and each time the instrument is set up .   The instrument
     standardization date and time must be included in the raw data.
              •Mr

     For atomic absorption systems, calibration standards are prepared by
     diluting the stock metal solutions at the time of analysis.  Date and
     time of preparation and analysis must be given in the raw data.

     Calibration standards must be prepared fresh daily or each time an
     analysis La to be made and discarded after use.  For atomic absorption
     systems, prepare a blank and at least three calibration standards in
     graduated amounts in the appropriate range.  One atomic absorption
     calibration standard must be at the CRDL.  The calibration standards
     must be prepared using the same type of acid or combination of acids
     and at the same concentration as will result in the samples following
     sample preparation.

     Beginning with the blank, aspirate or inject the standards and record
     the readings. If the AA instrument configuration prevents the required
     4 -point calibration, calibrate according to instrument manufacturer's
     recommendations, and analyze the remaining required standards
     immediately after calibration.  Results for these standards must be

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     within 5% of the true value.   Each standards concentration and the
     calculations to show that the  5%  criterion has been met, must be given
     in the raw data.  If the values do not  fall within this range,
     recalibration is necessary.

     The 5% criteria does not apply to the atomic absorption calibration
     standard at the CRDL.

     Calibration standards for AA procedures must be  prepared as described
     in Exhibit D.

     Baseline correction is acceptable as long as it is performed after
     every sample or after the continuing calibration verification and blank
     check; resloping is acceptable as long  as it is immediately preceded
     and immediately followed by compliant CCV and CCB.  For cyanide and
     mercury, follow the calibration procedures outlined in  Exhibit D.  One
     cyanide calibration standard must be at the CRDL.  For ICP systems,
     calibrate the instrument according to instrument manufacturer's
     recommended procedures.  At least two standards must be used for ICF
     calibration.  One of the standards must be a blank.

2.   Initial Calibration Verification  (ICV)  and Continuing Calibration
     Verification (CC\n

     a.    Initial Calibration Verification (ICV)

          Immediately after each of the -ICP,  AA and cyanide systems have
          been calibrated,  the accuracy  of the initial calibration shall be
          verified and documented for  every  analyte by the analysis of EPA
          Initial Calibration Verification Solution(s) at each wavelength
          used for analysis.   When measurements exceed the control limits of
          Table 1-Initial and Continuing Calibration Verification Control
          Limits for Inorganic Analyses  (in  Exhibit E), the analysis must be
          terminated, the problem corrected, the instrument recalibrated,
          and the calibration reverified.

          If the Initial Calibration Verification Solution(s) are not
          available from EPA,  or where a certified solution of an analyte is
          not available from any source, analyses shall be conducted on an
          independent standard at a concentration other than that used for
          instrument calibration, but  within the calibration range.  An
          independent standard is defined as a standard composed of the
          analytes from a different source than those used in the standards
          for the instrument calibration.

          For ICP, the Initial Calibration Verification Solution(s) must be
          run at each wavelength used  for analysis.  For CN, the initial
          calibration verification  standard must be distilled.  The  Initial
          Calibration Verification  for CN serves as a Laboratory Control
          Sample; thus it must be distilled  with the batch of samples
          analyzed in association with that  ICV.  This means that an  ICV
          must be distilled with each  batch  of  samples analyzed and that the
          samples distilled with an ICV must be analyzed with that
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     particular ICV.   The values for the  initial and subsequent
     continuing calibration verification  shall be recorded on FORM II-
     IN for ICP, AA,  and cyanide analyses,  as indicated.

b.   Continuing Calibration Verification  (CCV)

     To ensure calibration accuracy during each analysis run, one of
     the following standards is to be used for continuing calibration
     verification and must be be analyzed and reported  for every
     wavelength used for the analysis of  each analyte,  at a frequency
     of 10% or every 2 hours during an analysis run, whichever is more
     frequent.  The standard must also be analyzed  and  reported for
     every wavelength used for analysis at the beginning of the run and
     after the last analytical sample.  The analyte concentrations in
     the continuing calibration standard  must be one of the following
     solutions at or near the mid-range levels of the calibration
     curve:

          1.  EPA Solutions
          2.  NIST Standards
          3.  A Contractor-prepared standard solution
         TABLE  1.  INITIAL AND CONTINUING CALIBRATION VERIFICATION
                   CONTROL LIMITS FOR  INORGANIC ANALYSES
     Analytical Method
Inorganic
 Species
% of True Value (EPA Set")
Low Limit     High Limit
     ICP/AA

     Cold Vapor AA

     Other
Metals
Mercury
Cyanide
    90
    80
    85
110
120
115
     The same continuing calibration standard oust be used throughout
     the analysis runs for a Case of samples received.

     Each CCV analyzed must reflect the conditions of analysis of all
     associated analytical samples (the preceding 10 analytical samples
     or the preceding analytical samples up to the previous CCV).  The
     duration of analysis, rinses and other related operations that may
     affect the CCV measured result may not be applied to the CCV to a
     greater extent than the extent applied to the associated
     analytical samples.  For instance, the difference in time between
     a CCV analysis and the blank immediately following it as well as
     the difference in time between the CCV and the analytical sample
     immediately preceding it may not exceed the lowest difference in
     time between any two consecutive analytical samples associated
     with the CCV.
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          If the deviation of the continuing calibration verification is
          greater than the control limits  specified in Table  1-Ini.tial and
          Continuing Calibration Verification Control  Limits  for  Inorganic
          Analyses,  the analysis must be stopped,  the  problem corrected, the
          instrument must be recalibrated,  the calibration verified  and the
          reanalysis of preceding 10 analytical samples or all analytical
          samples analyzed since the last  compliant calibration verification
          must be performed for the analytes affected.   Information
          regarding the continuing verification of calibration shall be
          recorded on FORM II-IN for ICP,  AA and cyanide as indicated.

3.   CRDL Standards for ICP (CRI) and AA  (CRA)

     To verify linearity near the CRDL for ICP analysis, the  Contractor must
     analyze an ICP standard (CRI) at two  times the CRDL or two times the
     IDL, whichever is greater, at the beginning and end of each  sample
     analysis run, or a minimum of twice per 8 hour working shift, whichever
     is more frequent, but not before Initial Calibration Verification.
     This standard must be run by ICP for  every wavelength used for
     analysis, except those for Al, Ba, Ca,  Fe, Mg, Na and K.

     To verify linearity near the CRDL for AA analysis, the Contractor must
     analyze an AA standard (CRA) at the CRDL or the IDL, whichever  is
     greater, at the beginning of each sample analysis run, but not  before
     the Initial Calibration Verification.

     Specific acceptance criteria for the  two standards will  be set  by EPA
     in the future.   In the interim, the Contractor must analyze  and report
     these Standards on FORM II(PART 2)-IN.

4.   Initial Calibration Blank (ICB). Continuing Calibration  Blank (CCB).
     and Preparation Blank (PB) Analyses

     a.   Initial Calibration Blank (ICB)  and Continuing Calibration Blank
          (CCB)  Analyses

          A calibration blank must be analyzed at  each wavelength used for
          analysis immediately after every initial and continuing
          calibration verification, at a frequency of  10% or  every 2 hours
          during the run,  whichever is more frequent.   The blank  must be
          analyzed at the beginning of the run and after the  last
          analytical sample.  Note:  A CCB must be run. after  the  last CCV
          that was run after the last analytical sample of the run.   The
          results for the calibration blanks shall be  recorded on FORM III-
          IN for ICP, AA and cyanide analyses, as  indicated.   If  the
          magnitude (absolute value) of the calibration blank result exceeds
          the IDL, the result must be so reported  in ug/L on  FORM III-IN,
          otherwise report as IDL-U.  If the absolute  value blank result
          exceeds the CRDL (Exhibit C), terminate  analysis, correct  the
          problem, recalibrate, verify the calibration and reanalyze the
          preceding 10 analytical samples  or all analytical samples  analyzed
          since the last compliant calibration blank.
                                   E-16                                ILM02.0

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     b.   Preparation Blank (PB) Analysis

          At least one preparation blank (or reagent blank),  consisting of
          deionized distilled water processed through each sample
          preparation and analysis procedure (See Exhibit D,  Section III),
          must be prepared and analyzed with every Sample Delivery Group,  or
          with each batch  of samples digested,  whichever is  more  frequent.

          The first batch of samples in an SDG is to be  assigned to
          preparation blank one,  the second batch of samples  to preparation
          blank two, etc.  (see FORM II1-IN).  Each data  package must contain
          the results of all the preparation blank analyses associated  with
          the samples in that SDG.

          This blank is  to be reported for each  SDG and  used  in all analyses
          to ascertain whether sample concentrations reflect  contamination
          in the following manner:

          1)   If the  absolute value  of  the  concentration of  the blank  is
               less  than or equal to  the Contract Required Detection Limit
               (Exhibit  C),  no correction  of sample  results is performed.

          2)   If any  analyte concentration  in the blank is above the CRDL,
               the lowest concentration  of that  analyte  in the associated
               samples must  be lOx  the blank concentration.   Otherwise, all
               samples associated with the blank with the analyte's
               concentration less than lOx the blank concentration  and  above
               the CRDL, must be redigested  and  reanalyzed for that analyte
               (except for an identified aqueous soil field blank).  The

               sample concentration is not to be corrected for the  blank
               value.

          3)   If the  concentration of the blank is  below the negative  CRDL,
               then  all  samples reported below lOx  CRDL  associated  with the
               blank must be redigested  and  reanalyzed.

          The"values for the preparation blank must be recorded in ug/L for
          aqueous samples  and in mg/Kg for solid samples on FORM III-IN for
          ICP,  AA, and cyanide  analyses.

5.   ICP Interference Check, Sample fICS) Analysis

     To verify interelement and background correction factors,  the
     Contractor must analyze and report the results for the ICP Interference
     Check Samples at the beginning and end of each analysis  run or a
     minimum of twice per 8 hour working shift,  whichever is  more  frequent,
     but not before Initial Calibration Verification.  The ICP Interference
     Check Samples must  be obtained from EPA (EMSL/LV) if available and
     analyzed according  to the instructions supplied with the ICS.
   group of samples prepared at the same time.


                                   E-17                                ILM02.0

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The Interference Check Samples consist of two solutions: Solution A and
Solution AB.  Solution A consists of the interferents, and Solution AB
consists of the analytes nixed with the interferents.  An ICS analysis
consists of analyzing both solutions consecutively (starting with
Solution A) for all wavelengths used for each analyte reported by ICP.

Results for the ICP analyses of Solution AB during the analytical runs
must fall within the control limit of +20% of the true value for the
analytes included in the Interference Check Samples.  If not, terminate
the analysis, correct the problem, recalibrate the instrument, and
reanalyze the analytical samples analyzed since the last good ICS.  If
true values for analytes contained in the ICS and analyzed by ICP are
not supplied with the ICS, the mean must be determined by initially
analyzing the ICS at least five times repetitively for the particular
analytes. This mean determination must be made during an analytical run
where the results for the previously supplied EPA ICS met all contract
specifications.  Additionally, the result of this initial mean
determination is to be used as the true value for the lifetime of that
solution (i.e., until the solution is exhausted).

If the ICP Interference Check Sample is not available from EPA,
independent ICP Check Samples must be prepared with interferent and
analyte concentrations at the levels specified in Table 2-Interferent
and Analyte Elemental Concentrations Used for ICP Interference Check
Sample.  The mean value and standard deviation must be established by
initially analyzing the Check Samples at least five times repetitively
for each parameter on FORM IV-IN.  Results must fall within the control
limit of +20% of the established mean value.  The mean and standard
deviation must be reported in the raw data.  Results from the
Interference Check Sample analyses must be recorded on FORM IV-IN for
all ICP parameters.
TABLE 2.  INTERFERENT AND ANALYTE ELEMENTAL CONCENTRATIONS USED FOR ICP
                       INTERFERENCE CHECK SAMPLE


   Analytes          (mg/L)               Interferents       (mg/L)
Ag
Ba
Be
Cd
Co
Cr
Cu
Mn
Ni
Pb
V
Zn
1.0
0.5
0.5
1.0
0.5
0.5
0.5
0.5
1.0
1.0
0.5
1.0
Al
Ca
Fe
Mg







500
500
200
500







                               E-18                                ILM02.0

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6.   Spike ??Tl? Analysis (S)

     The spike sample analysis is designed to provide  information  about  the
     effect of the sample matrix on the digestion and  measurement
     methodology.  The spike is added before the digestion (i.e.,  prior  to
     the addition of other reagents)  and prior to any  distillation steps
     (i.e., CN-).  At least one spike sample analysis  must be  performed  on
     each group of samples of a similar matrix type  (i.e., water,  soil)  and
     concentration (i.e., low, medium) or for each Sample  Delivery Group.

     If the spike analysis is performed on the same  sample that is chosen
     for the duplicate sample analysis,  spike calculations must be performed
     using the results of the sample  designated as the "original sample"
     (see section 7,  Duplicate Sample Analysis).   The  average  of the
     duplicate results cannot be used for the purpose  of determining percent
     recovery.  Samples identified as field blanks cannot  be used  for spiked
     sample analysis.   EPA may require that a specific sample  be used for
     the spike sample  analysis.

     The analyte spike oust be added  in the amount given in Table  3-Spiking
     Levels for Spike  Sample Analysis, for each element analyzed.   Note: -
     See Table 3 footnotes for concentration levels  and applications.  If
     two analytical methods are used  to obtain the reported values for the
     same element within a Sample Delivery Group (i.e. ICP,  GFAA), spike
     samples must be run by each method used.

     If the spike recovery is not at  or within the limits  of 75-125%,  the
     data of all samples received associated with that spike sample and
     determined by the same analytical method must be  flagged  with the
     letter "N" on FORMs I-IN and V-IN.   An exception  to this  rule is
     granted in situations where the  sample concentration  exceeds  the spike
     concentration by  a factor of four or more.  In  such an event, the data
     shall be reported unflagged even if the percent recovery  does not meet
     the 75-125% recovery criteria.

     For flame AA, ICP, and CN analyses, when the pre-digestion/pre-
     distillation spike recovery falls outside the control limits  and the
     sample result does not exceed 4x the spike added, a post-
     digest ioil/post- distillation spike must be performed for those elements
     that do not meet the specified criteria (exception: Ag).   Spike the
     vmspiked aliquot of the sample at 2x the indigenous level or 2x CRDL,
     whichever is greater.  Results of the post-digestion/post-distillation
     spike must be reported on FORM V(PART 2)-IN. Note:  No post digest
     spike is required for Hg.

     In the instance where there is more than one spike sample per matrix
     and concentration per method per SDG, if one spike sample recovery is
     not within contract criteria, flag all the samples of the same matrix,
     level, and method in the SDG.  Individual component percent  recoveries
     (%R) are calculated as follows:
2
 EPA may require additional spike sample analysis, upon Administrative
 Project Officer request,  for which the Contractor will be paid.


                                    E-19                                ILM02.0

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                    %Recovery  -
(SSR-StO  x 100
   SA
 Where,    SSR  -   Spiked Sample Result
           SR  -   Sample Result
           SA  -   Spike Added

When sample concentration is less than the instrument detection limit,
use SR - 0 only for purposes of calculating % Recovery.  The spike
sample results, sample results and % Recovery (positive or negative)
must be reported on FORM V-IN for ICP, AA and cyanide analyses, as
indicated.

The units for reporting spike sample results will be identical to those
used for reporting sample results in FORM I-IN 
(mgAg)

20
8


1





4


1


2


10


ioo<3)
 No spike required.  NOTE:  Elements without  spike  levels  and not
designated with an asterisk, must be spiked at  appropriate levels.

1Spiking level reported is  for both water and soil/sediment matrices.
n
 The  levels  shown indicate  concentrations in  the final digestate of the
spiked sample  (100 mL  for mercury and  200 mL  for all other metals)  when
the wet weight of 1  gram (for ICP,  Furnace, and Flame AA), or 0.2 grams
                               E-20
                                 ILM02.0

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     (for mercury) of sample is taken for analysis.  Adjustment must be made
     to maintain these spiking levels when the weight  of sample taken
     deviates by more than 10% of these values.  Appropriate  adjustment must
     be made for microwave digestion procedure where 0.5 grams of sample  or
     50.0 mL (45.0 mL of sample plus 5.0 mL of acid) of aqueous sample are
     required for analysis.
      The level shown indicates the amount of cyanide  that must be added  to
     the original (undistilled) sample.  For instance,  100 ug must be added
     per each Liter of aqueous sample.   If the sample  volume  is 500 mL, then
     50 ug of cyanide must be added.   If the volume is 50 mL, then 5 ug of
     cyanide must be added.
     For soil samples, 25 ug of cyanide must be added  per each gran of solid
     sample taken for analysis.  The spiking level is  dependent on the
     weight of the sample taken and the final distillate volume.   If one
     gram of sample is taken for analysis,  and the final distillate volume
     is 250 mL, then the distillate must contain cyanide at a concentration
     of 100 ug/L-  If five grams of sample are taken,  then the distillate
     must contain cyanide at a concentration of 500 ug/L.   Assuming a sample
     of one gram, the manual and semi-automated colorimetric  methods call
     for a cyanide concentration of 25  ug per the 500  mL mixture  of the
     sample,  reagents, and water before distillation.   The final  distillate,
     in this  case, contains cyanide at  a concentration of 100 ug/L.  For  the
     aidi-distillation method,  a cyanide concentration of 25  ug must be
     added into the 50 mL mixture of sample,  reagents,  and water  before
     distillation.  This yields a cyanide concentration of 500 ug/L in the
     final distillate of 50 mL.
7.    Duplicate Sample Analysis (D)

     One duplicate sample must be analyzed from each  group  of samples  of a
     similar matrix type (i.e., water,  soil)  and concentration (i.e.,  low,
     medium) or for each Sample Delivery Group.   Duplicates  cannot be
     averaged for reporting on FORM I-IN.

     Duplicate sample analyses are  required for percent  solids.  Samples
     identified as field blanks cannot  be used for  duplicate  sample
     analysis..,.  EPA may require that a  specific sample be used for duplicate
     sample analysis.  If two analytical methods are  used to  obtain the
     reported values for the same element for a Sample Delivery Group  (i.e.,
     IGF,  GFAA),  duplicate samples  must be run by each method used.

     The relative percent differences  (RPD) for each  component are
     calculated as follows:

                       RPD  -  IS -  PI  x 100
                              (S+D)/2

      Where, RPD  -  Relative Percent Difference
               S  -  First Sample Value (original)
               D  -  Second Sample Value (duplicate)
3EPA may require additional duplicate sample analyses, upon Administrative
 Project Officer request, for which the Contractor will be paid.


                                   E-21                                ILM02.0

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     The results of the duplicate sample analyses must be reported on FORM
     VI -IN in ug/L for aqueous samples and mg/Kg dry weight basis for solid
     original and duplicate samples.  A control limit  of 20%  for RPD shall
     be used for original and duplicate sample values  greater than or equal
     to 5x CRDL (Exhibit C) .  A control limit of (±)  the CRDL  must be used if
     either the sample or duplicate value is less than 5x CRDL, and the
     absolute value of the control limit (CRDL) must be entered in the
     "Control Limit" column on FORM VI -IN.

     If one result is above the 5x CRDL level and the  other is below, use
     the + CRDL criteria.  If both sample values are less than the IDL,  the
     RPD is not calculated on FORM VI -IN.  For solid sample or duplicate
     results < 5x CRDL, enter the absolute value of  the CRDL, corrected  for
     sample weight and percent solids, in the "Control Limit" column.  If
     the duplicate sample results are outside the control limits, flag all
     the data for samples received associated with that duplicate sample
     with an "*" on FORMs I -IN and VI -IN.  In the instance where there is
     more than one duplicate  sample per SDG, if one  duplicate result is  not
     within contract criteria, flag all samples of the same matrix,
     concentration, and method in the SDG.   The percent difference data  will
     be used by EPA to evaluate the long-term precision of the methods for
     each parameter.  Specific control limits for each element will be added
     to FORM VI -IN at a later date based on these precision results.
8 .    Laboratory Control SfllUPH? (LCS^ Analysis

     Aqueous and solid Laboratory Control Samples (LCS)  must be analyzed for
     each analyte using the same sample preparations,  analytical methods and
     QA/QC procedures employed for the EPA samples received.  The aqueous
     LCS solution must be obtained from EPA (if unavailable, the Initial
     Calibration Verification Solutions may be used) .   One aqueous LCS must
     be prepared and analyzed for every group of aqueous samples in a Sample
     Delivery Group, or for each batch of aqueous samples digested,
     whichever is more frequent.   An aqueous LCS is not required for mercury
     and cyanide analysis.

     The EPA-provided solid LCS must be prepared and analyzed using each of
     the procedures applied to the solid samples received (exception:
     percent solids determination not required) .  If the EPA solid LCS is
     unavailable, other EPA Quality Assurance Check samples or other
     certified materials may be used.  One solid LCS must be prepared and
     analyzed for every group of solid samples in a Sample Delivery Group,
     or for each batch of samples digested, whichever is more frequent.

     All LCS results and percent recovery (%R) will be reported on FORM VII-
     IN.  If the percent recovery for the aqueous LCS falls outside the
     control limits of 80-120% (exception: Ag and Sb) , the analyses oust be
     terminated, the problem corrected, and the samples associated with that
     LCS redigested and reanalyzed.

     If the results for the solid LCS fall outside the control limits
     established by EPA, the analyses must be terminated, the problem
     corrected, and the samples associated with that LCS redigested  and
     reanalyzed.
                                   E-22                                ILM02.0

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9.   TCP Serial Dilution Analysis (L)

     Prior to reporting concentration data for the analyte elements,  the
     Contractor oust analyze and report the results of the ICP Serial
     Dilution Analysis.  The ICP Serial Dilution Analysis must be performed
     on a sample from each group of samples of a similar matrix type  (i.e.,
     water, soil) and concentration (i.e., low, medium) or for each Sample
     Delivery Group, whichever is more frequent.  Samples identified as
     field blanks cannot be used for Serial Dilution Analysis.

     If the analyte concentration is sufficiently high (minimally a factor
     of 50 above the instrumental detection limit in the original sample),
     the serial dilution (a five fold dilution) must then agree within 10%
     of the original determination after correction for dilution.  If the
     dilution analysis for wue wr more analytes is not at or within 10%, a
     chemical or physical interference effect must be suspected,  and  the
     data for all affected analytes in the samples received associated with
     that serial dilution must be flagged with an "E" on FORM IX- IN and FORM
     I-IN.

     The percent differences for each component are calculated as follows:
            t Difference -    '*  "  S|    x 100
     where,  I - Initial Sample Result
             S - Serial Dilution Result (Instrument Reading x 5)

     In the instance where there is more than one serial dilution per SDG,
     if one serial dilution result is not within contract criteria, flag all
     the samples of the same matrix and concentration in the Sample Delivery
     Group.  Serial dilution results and "E" fla-*s must be reported on FORM
     IX-IN.

10.  IngttTBMUt Petection Limit (IDL) Determination

     Before any field samples are analyzed under this contract,  the
     instrument detection limits (in ug/L) must be determined for each
     instrument used, within 30 days of the start of contract analyses and
     at least quarterly (every 3 calendar months), and must meet the levels
     specified in Exhibit C.

     The Instrument Detection Limits (in ug/L)  shall be determined by
     multiplying by 3, the average of the standard deviations obtained on
     three nonconsecutive days from the analysis of a standard solution
     (each analyte in reagent water) at a concentration 3x-5x the instrument
     manufacturer's suggested IDL, with seven consecutive measurements per
     day.  Each measurement must be performed as though it were a separate
     analytical sample (i.e., each measurement must be followed by a rinse
     and/or any other procedure normally performed between the analysis of
     separate samples).  IDL's must be determined and reported for each
     wavelength used in the analysis of the samples.
                                    E-23                                ILM02.0

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     The quarterly determined IDL for an instrument must  always be used as
     the IDL for that instrument during that quarter.   If the  instrument is
     adjusted in anyway that may affect the IDL,  the IDL  for that instrument
     must be redetermined and the results submitted for use as the
     established IDL for that instrument for the  remainder of  the quarter.

     IDLs must be reported for each instrument used on  FORM X-IN submitted
     with each data package.   If multiple AA instruments  are used for  the
     analysis of an element within a Sample Delivery Group, the highest IDL
     for the AAs must be used for reporting concentration values for that
     Sample Delivery Group.   The same reporting procedure must be used for
     multiple ICFs.

11.  Interelement Corrections for ICP

     Before any field samples are analyzed under  this contract, the ICP
     interelement correction factors must be determined prior  to the start
     of contract analyses and at least annually thereafter.  Correction
     factors for spectral interference due to Al, Ca, Fe,  and  Mg must  be
     determined for all ICP instruments at all wavelengths used for each
     analyte reported by ICP.   Correction factors for spectral interference
     due to analytes other than Al,  Ca,  Fe,  and Mg must be reported if they
     were applied.

     If the instrument was adjusted in anyway that may  affect  the ICP
     interelement correction factors, the factors must  be redetermined and
     the results submitted for use.   Results from interelement correction
     factors determination must be reported on FORM XI(PART 1)-IN and  FORM
     XI(PART 2)-IN for all ICP parameters.

12.  Linear Range Analysis (LRA)

     For all ICP analyses, a linear range verification  check standard  must
     be analyzed and reported quarterly (every 3  calendar months) for  each
     element on FORM XII-IN.   The standard must be analyzed during a routine
     analytical run performed under this contract.  The analytically
     determined^ concentration of this standard must be  within  5% of the true
     value.  This concentration is the upper limit of the ICP  linear range
     beyond which results cannot be reported under this contract without
     dilution of the analytical sample.

13.  Furnace Atomic Absorption (AA> OC Analyses

     Because of the nature of the Furnace AA technique, the special
     procedures summarized in Figure 1-Furnace AA Analysis Scheme  ("MSA
     Tree*) will be required for quantitation.   (These  procedures do not
     replace those in Exhibit D of this SOW, but  supplement the guidance
     provided therein.)

     a.   All furnace analyses must fall within the calibration range.  In
          addition,  all analyses,  except during full methods of standard
          addition (MSA), will require duplicate  injections.   The absorbance
          or concentration of each injection must be reported  in the raw
          data as well as the average absorbance  or concentration values and
          the relative standard deviation (RSD) or coefficient of variation

                                   E-24                                ILM02.0

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         (CV).  Average concentration values are used for reporting
         purposes.  The Contractor must be consistent per method and SDG in
         choosing absorbance or concentration to evaluate which route is to
         be followed in the MSA Tree.  The Contractor must also indicate
         which of the two is being used if both absorbance and
         concentration are reported in the raw data.   For MSA analysis,  the
         absorbance of each injection must be included in the raw data.   A
         maximum of 10 full sample analyses to a maximum 20 injections may
         be performed between each consecutive calibration verifications
         and blanks.  For concentrations greater than CRDL,  the duplicate
         injection readings must agree within 20% RSD or CV,  or the
         analytical sample oust be rerun once (i.e.,  two additional burns).
         If the readings are still out,  flag the value reported on FORM  I-
         IN with an "M".  The "M" flag is required for the analytical spike
         as well as the sample.  If the analytical spike for a sample
         requires an "M" flag,  the flag must be reported on FORM I- IN for
         that sample.

    b.   All furnace analyses for each analytical sample,  including those
         requiring an "M" flag, will require at least an analytical spike
         to determine if the MSA will be required for quantitation.  The
         analytical spike  will be required to be at  a concentration (in
         the sample) 2x CRDL (except for lead which must be at 20 ug/L).
         This requirement for an analytical spike will include the LCS and
         the preparation blank.  (The LCS must be quantitated from the
         calibration curve and corrective action,  if  needed,  taken
         accordingly.   MSA is not to be performed on  the LCS or preparation
         blank, regardless of spike recovery results.)  If the preparation
         blank analytical spike recovery is out of control (85-115%), the
         spiking solution must be verified by respiking and rerunning the
         preparation blank once.  If the preparation  blank analytical spike
         recovery is still out of control, correct the problem and
         reanalyze all analytical samples associated  with that blank. An
         analytical spike is not required on the pre-digestion spike
         sample.

         The analytical spike of a sample must be run immediately after
         thalTsample.   The percent recovery (%R) of the spike, calculated
         by the same formula as Spike Sample Analyses (see item 6, this
         section), will then determine how the sample will be quantitated,
         as follows:

         1)  If the spike recovery is less than 40%,  the sample must be
             diluted and rerun with another spike.   Dilute the sample by a
             factor of 5 to 10 and rerun.   This step must only be
             performed once.   If after the dilution  the spike recovery  is
             still <40%,  report data and flag with an "E" to indicate
             interference problems.
Analytical Spikes are post-digestion spikes to be prepared prior to
analysis by adding a known quantity of the wialyte to an aliquot of  the
digested sample.  The unspiked sample aliquot must be compensated  for any
volume change  in the spike samples by addition of deionized water  to the
unspiked sample aliquot.  The volume of the spiking solution added must
not exceed 10% of the analytical sample volume; this requirement also
applies to MSA spikes.


                                  E-25                                ILM02.0

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         2)   If the spike recovery is greater than or equal  to 40% and  the
              sample absorbance or concentration is less  than 50% of  the
              "spike" ,  report the sample results to the  IDL.  If the spike
              recovery is less than 85% or greater than 115%,  flag the
              result with a "W".

         3)   If the sample absorbance or concentration is  greater than  or
              equal to 50% of the spike and the spike recovery is at  or
              between 85% and 115%, the sample must be quantitated directly
              from the calibration curve and reported down  to the IDL.

         4)   If the sample absorbance or concentration is  greater than  or
              equal to 50% of the spike and the spike recovery is less than
              85% or greater than 115%, the sample must be  quantitated by
              MSA.

    c.   The following procedures will be incorporated into MSA  analyses.

         1)   Data from MSA calculations must be within the linear range as
              determined by the calibration curve generated at the
              beginning of the analytical run.

         2)   The sample and three spikes must be analyzed  consecutively
              for MSA quantitation (the "initial" spike run data is
              specifically excluded from use in the MSA quantitation).
              Only single injections are required for MSA quantitation.

              Each full MSA counts as two analytical samples  towards
              determining 10% QC frequency (i.e., five full MSAs can be
              performed between calibration verifications).

         3)   For analytical runs containing only USAs, single injections
              can be used for QC samples during that run.  For instruments
              that operate in an MSA mode only, MSA can be  used to
              determine QC samples during that run.

         4)   Spikes must be prepared such that:
             ~a)  Spike  1 is approximately 50% of the sample  concentration.

              b)  Spike  2 is approximately 100% of the sample
                  concentration.
              c)  Spike  3 is approximately 150% of the sample
                  concentration.

         5)   The data for each MSA analysis  must be  clearly  identified in
              the raw data documentation (using added concentration  as  the
              x-variable  and absorbance  as  the  y-variable) along with the
              slope, x-intercept,  y-intercept and correlation coefficient
              (r) for the least squares  fit of  the data.   The results must
              be  reported on FORM VIII-IN.  Reported values  obtained by MSA
5"Spike" is defined as [absorbance or concentration of spike sample] minus
 [absorbance or concentration of the sample].
                                   E-26                                ILM02.0

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     must be flagged on the data sheet (FORM I-IN) with the letter
     "S" if the correlation coefficient is greater than or equal
     to 0.995.

6)   If the correlation coefficient (r) for a particular analysis
     is less than 0.995,  the MSA analysis  must be repeated once.
     If the correlation coefficient is still less than 0.995,
     report the results on FORM I-IN from  the run with the best
     "r" and flag the result with a "+" on FORM VIII-IN and FORM
                        E'27                                ILM02.0

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                                           Figure 1.
                      Furnace Atomic Absorption Analysis Scheme
    Prepare and Analyze
   Sample and One Spike
        (2 X CRDL)
   (Double Injections Required)
          i
      Analyses Within
     Calibration Range
          I
YES
     Recovery of Spike
      Less Than 40%
             NO
   Sample Absorbance or
  Concentration Less Than
 50% of Spike Absorbance or
      Concentration
             NO
      Spike Recovery
     Less Than 85% or
    Greater Than 115%
            YES
                                              NO
                                    If YES. Repeat Only ONCE
                                           If Still YES
                                                        NO
              YES
Spike Recovery Less Than
85% or Greater than 115%
                                                        YES
                                 NO
                                                           Dilute Sample and Spike
                                                                         Flag Data with an "E*
                                                                       Report Results Down to IDL
                                                          Report Results Down to IDL.
                                                               Flag wilha "W
                                  QuanliUite from Calibration
                                   Curve and Report Down to
                                             IDL
 Quantitate by MSA with 3
Spikes at 50. 100 & 150% of
   Sample Concentration
 (Only Single Injections Required)
          I
Correlation Coefficient Less
       Than 0.995
          I
                If YES. Repeat Only ONCE
NO
                           If Still YES
    Flag Data with "S"
                                      Flag Data with a >"
                                            E-28
                                                                       ILM02.0

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                                 SECTION VI
                        CONTRACT COMPLIANCE  SCREENING
Contract Compliance Screening (CCS) is one aspect of the Government's
contractual right of inspection of analytical data. CCS examines the
Contractor's adherence to the contract requirements based on the sample
data package delivered to the Agency.

CCS is performed by the Sample Management Office (SMO) under the direction
of the EPA.  To assure a uniform review, a set of standardized procedures
have been developed to evaluate the sample data package submitted by a
Contractor against the technical and completeness requirements of the
contract.

CCS results are mailed to the Contractor and all other data recipients.
The Contractor has a period of time to correct deficiencies.  The
Contractor must send all corrections to the Regional Client, EMSL/LV, and
SMO.

CCS results are used in conjunction with other information to measure
overall Contractor performance and to take appropriate actions to correct
deficiencies in performance.

The Agency may generate a CCS trend report which summarizes CCS results
over a given period of time.  The Agency may send the CCS trend report or
discuss the CCS trend report during an On-Site laboratory evaluation.  In a
detailed letter to the Technical Project Officer and Administrative Project
Officer, the Contractor shall address the deficiencies and the subsequent
corrective action implemented by the Contractor to correct the deficiencies
within 14 days of receipt of the report or the On-Site laboratory
evaluation.  An alternate delivery schedule may be proposed by the
Contractor, but it is the sole decision of the Agency, represented by  the
Technical Project Officer or Administrative Project Officer to approve or
disprove the alternate delivery schedule.  If an alternate delivery
schedule is proposed, the Contractor shall describe in a letter to the
Technical Project Officer, Administrative Project Officer, and Contracting
Officer why he/she is unable to meet the delivery schedule listed in this
section.  The Technical Project Officer will not grant an extension  for
greater than 14 days for the Contractor's response to the CCS trend  report.

If new SOPs are required to be written or SOPs are required to be amended
because of the deficiencies and the subsequent corrective action
implemented by the Contractor, the Contractor shall write/amend and  submit
the SOPs per the requirements listed in Exhibit E, Section  IV.

If the Contractor fails to adhere to the requirements listed  in this
section, the Contractor nay expect, but the Agency is not limited to the
following actions: reduction of number  of samples  sent under  the contract,
suspension of sample shipment to the Contractor, d&ta package audit, an  On-
Site laboratory evaluation, a remedial performance evaluation sample,
and/or contract sanctions, such as a Cure Notice.
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                                 SECTION VII

                      ANALYTICAL STANDARD REQUIREMENTS

The U.S. Environmental Protection Agency may be unable to supply analytical
reference standards either for direct analytical measurements or for the
purpose of traceability."  In these cases,  all contract laboratories will be
required to prepare from materials or purchase from private chemical supply
houses those standards necessary to successfully and accurately perform the
analyses required in this protocol.

A.   Preparation of Chemical Standards from the Neat High Purity Bulk
     Material

     If the laboratory cannot obtain analytical reference data from the
     USEPA,  the laboratory may prepare their own chemical standards.
     Laboratories should obtain the highest purity  possible when purchasing
     chemical standards;  standards purchased at less than 97% purity must be
     documented as to  why a higher purity  could not be obtained.

     1.   If required  by the manufacturer,  the  chemical standards must  be
         kept refrigerated when not being used in  the preparation  of
         standard solutions.   Proper  storage of chemicals  is essential in
         order to safeguard them from decomposition..

     2.   The purity of a  compound can sometimes be  misrepresented  by a
         chemical supply  house.   Since knowledge of purity is needed to
         calculate the concentration  of solute in  a solution standard, it
         is the contract  laboratory's responsibility to  have analytical
         documentation ascertaining that  the purity of each compound is
         correctly stated.   Purity confirmation, when performed, should use
         appropriate  techniques.   Use of  two or more independant methods is
         recommended.  The correction factor for impurity when weighing
         neat materials  in the preparation of  solution standards is:

         Equation 1

                                        weight of  cure compound
         weigEt of impure compound -    (percent  purity/100)

         where "weight of pure compound*  is that required to prepare a
         specific volume of a solution standard of a specified
         concentration.

     3.   Mis-identification of compounds  occasionally occurs and it is
         possible that a mislabeled compound may be received from  a
         chemical supply house.  It is the contract laboratory's
         responsibility to have analytical documentation ascertaining  that
         all compounds used in the preparation of  solution standards be
         correctly identified.

     4.   Log notebooks are to be kept for all weighing and dilutions.   All
         subsequent dilutions from the primary standard and the
         calculations for determining their concentrations are to be
         recorded and verified by a second person.  All solution standards

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          are  to be refrigerated,  if required, when not in use.  All
          solution standards are to be clearly labeled as to the identity of
          the  analyte or  analytes, concentration, date prepared, solvent,
          and  initials  of the preparer.

B.   Purchase  of chemical standards already in solution

     1.    Solutions of  analytical  reference standards can be purchased by
          Contractors provided  they meet the following criteria:

          Laboratories  must maintain documentation of the purity
          confirmation  of the material to verify the integrity of the
          standard solutions they  purchase.

     2.    The  Contractor  must purchase standards for which the quality is
          demonstrated  statistically and analytically by a method of the
          supplier's choice.  One  way this  can be demonstrated is to prepare
          and  analyze three solutions; a high standard, a low standard, and
          a standard at the target concentration (see parts a and b below).
          The  supplier  must then demonstrate that the analytical results for
          the  high standard and low standard are consistent with the
          difference in theoretical concentrations.  This is done by the
          Student's t-test in part *d".  If this is achieved, the supplier
          must then demonstrate that the concentration of the target
          standard lies midway between the  concentrations of the low and
          high standards.  This is done by  the Student's t-test in part e.
          Thus the standard is  certified to be within 10 percent of the
          target concentration.

          If the procedure above is used, the supplier must document that
          the  following have been  achieved:

          a.   Two solutions of identical concentration must be prepared
              independently from neat materials.  An aliquot of the first
              solution must be diluted to  the intended concentration (the
              •target  standard").  One aliquot is Taken from the second
              solution and diluted to a concentration ten percent greater
              than the target  standard.  This is called the "high
              standard".  One  further aliquot is taken from the second
              solution and diluted to a concentration 10 percent less than
              the target standard.  This is called the "low standard*.

          b.   Six replicate analyses of each standard (a total of 18
              analyses)  must be performed  in the following sequence: low
              standard,  target, high standard, low standard, target
              standard,  high standard, ...

          c.   The mean and variance of the six results for each solution
              must be  calculated.

          Equation 2
              MEAN  -  (Y! + Y2 + Y3 + Y4  + Y5 + Y6  )/6
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Equation 3
     VARIANCE  -  (YxZ -I- Y22 + Y3Z + Y4Z + Y5Z + Y6Z -
     (6*MEAN)2)/5

     The values YI , Y2, Y3, .... represent the results  of the six
     analyses of each standard.  The means of the low,  target,  and
     high standards are designated MI, M2, and M3, respectively.
     The variances of the low, target, and high standards are
     designated Vj, V2, and V3, respectively.  Additionally,  a
     pooled variance, Vp, is calculated.

Equation 4
     vp -  (Vi/(0.81) + V2 + V3 /(1.21))/3

     If the square root of Vp is less than one percent  of M2, then
     M£  /10.000 is to be used as the value of Vp in all
     subsequent calculations.

d.   The- test statistic must be calculated:

     Equation 5
     TEST STATISTIC  -  |(M3 /I.I) - &i /0.9)|/(Vp /3)°'5

     If the test statistic exceeds 2.13 then the supplier has
     failed to demonstrate a twenty percent difference  between the
     high and low standards.  In such a case, the standards are
     not acceptable.

e.   The test statistic must be calculated:

     Equation 6
     TEST STATISTIC  -  |M2 - (MX /I.8) - 
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      In any event, the laboratory is responsible  for  the quality  of  the
      standards employed for analyses under this contract.

C.   Requesting Standards From the EPA Standards Repository

     Solutions of analytical reference materials can be ordered from  the
     U.S. EPA Chemical Standards Repository,  depending on availability.  The
     Contractor can place an order for standards only  after demonstrating
     that these standards are not available from commercial vendors either
     in solution or as a neat material.

D.   Documentation of the Verification and Preparation of Chemical Standards

     It is the responsibility of each laboratory to maintain the necessary
     documentation to show that the chemical standards they have used in the
     performance of CLP analysis conform to the requirements previously
     listed.   Weighing logbooks, calculations, raw data, etc., whether
     produced by the laboratory or purchased from  chemical supply  houses,
     must be  maintained by the laboratory and may  be subject to review
     during On-Site inspection visits.  In those cases where the
     documentation is supportive of the analytical results of data packages
     sent to  EPA, such documentation is to be kept on  file by the
     laboratories for a period of one year.

     Upon request by the Technical Project Officer or  Administrative  Project
     Officer, the Contractor shall submit their most recent previous  year's
     documentation (12 months) for the verification and preparation of
     chemical standards within 14 days of the receipt  of request to the
     recipients he/she designates.

     The Agency may generate a report discussing deficiencies in the
     Contractor's documentation for the verification and preparation  of
     chemical standards or may discuss the deficiencies during an  On-Site
     laboratory evaluation.  In a detailed letter  to the Technical Project
     Officer, Administrative Project Officer, and  EMSL-LV, the Contractor
     shall address the deficiencies and the subsequent corrective  action
     implemented by the Contractor to correct the  deficiencies within 14
     days of receipt of the report or the On-Site  laboratory evaluation.   An
     alternate delivery schedule may be proposed by the Contractor, but it
     is the sole decision of the Agency, represented either  by  the Technical
     Project Officer or Administrative Project  Officer, to approve or
     disapprove the alternate delivery schedule.   If an alternate  delivery
     schedule is proposed, the Contractor shall describe  in  a letter to the
     Technical Project Officer, Administrative  Project Officer, and the
     Contracting Officer why he/she is unable to meet  the delivery schedule
     listed in this section.  The Technical Project Officer/Administrative
     Project Officer yill pot grant an extension  for greater than 14 days
     for the Contractor's response letter to the  standards  documentation
     report.   The Contractor shall proceed and not assume that an extension
     will be granted until so notified by the TPO and/or APO.
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If new SOPs are required to be written or SOPs are required to be
amended because of the deficiencies and the subsequent corrective
action implemented by the Contractor, the Contractor shall write/amend
and submit the SOPs per the requirements listed in Exhibit E, Section
IV.

If the Contractor fails to adhere to the requirements listed in Section
VII, a Contractor may expect, but the Agency is not limited to the
following actions:  reduction of number of samples sent under the
contract, suspension of sample shipment to Contractor, data package
audit, an On-Site laboratory evaluation, a remedial laboratory
evaluation sample, and/or contract sanctions, such as a Cure Notice.
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                                SECTION VIII

                             DATA PACKAGE AUDITS

Data package audits arc performed by the Agency for program overview and
specific Regional concerns.  Standardized procedures have been established
to assure uniformity of the auditing process.  Date, packages are
periodically selected from recently received cases.  They are evaluated for
the technical quality of hardcopy raw data, quality assurance, and the
adherence to contractual requirements.  This function provides external
monitoring of program QC requirements.

Data package audits are used to assess the technical quality of the data
and evaluate overall laboratory performance.  Audits provide the Agency
with an in-depth inspection and evaluation of the Case data package with
regard Co achieving QA/QC acceptability.  A thorough review of the raw data
is completed including:  all instrument readouts used for the sample
results, chromatograms and other documentation for deviations from the
contractual requirements, a check for transcription and calculation errors,
a review of the qualifications of the laboratory personnel involved with
the Case, and a review of all current SOPs on file.

Responding to the data package audit report!

After completion of the data package audit, the Agency may send a copy of
the data package audit report to the Contractor or may discuss the data
package audit report on an On-Site laboratory evaluation.  In a detailed
letter to the Technical Project Officer, Administrative Project Officer,
and EMSL/LV, the Contractor shall discuss the corrective actions
implemented to resolve the deficiencies listed in the data package audit
report within 14 days of receipt of the report.  An alternate delivery
schedule may be proposed by the Contractor, but it is the sole decision of
the Agency, represented either by the Technical Project Officer or
Administrative Project Officer, to approve or disapprove the alternate.
delivery schedule.  If an alternate delivery schedule is proposed, the
Contractor shall describe in a letter to the Technical Project Officer,
Administrative^Project Officer, and the Contracting Officer, why he/she is
unable to meet the delivery schedule listed in this section.  The Technical
Project Officer/Administrative Project Officer will not grant an extension
for greater than 14 days for the Contractor's response letter to the data
package report.  The Contractor shall proceed and not assume that an
extension will be granted until so notified by the TPO and/or APO.

If new SOPs are required to be written or SOPs are required to be amended
because of the deficiencies and the subsequent corrective action
implemented by the Contractor, the Contractor shall write/amend and submit
the SOPs per the requirements listed in Exhibit E, Section IV.
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Corrective Actions

If the Contractor fails to adhere to the requirements listed in this
section, the Contractor may expect, but the Agency is not limited to the
following actions:  reduction in the numbers of samples sent under the
contract, suspension of sample shipment to the Contractor, an On-Site
laboratory evaluation, data package audit, remedial performance evaluation
sample, and/or contract sanctions, such as a Cure Notice.
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                                 SECTION IX

                       PERFORMANCE EVALUATION SAMPLES
Although intralaboratory OC nay demonstrate Contractor and method
performance that can be tracked over time, an external performance
evaluation program is an essential feature of a QA program.  As a means of
measuring Contractor and method performance, Contractors participate in
interlaboratory comparison studies conducted by the EPA.  Results from the
analysis of these performance evaluation samples (PES) will be used by the
EPA to verify the Contractor's continuing ability to produce acceptable
analytical data. The results are also used to assess the precision and
accuracy of the analytical methods for specific an&lytes.

Sample sets nay be provided to participating Contractors as frequently as
on an SDG-by-SDG basis as a recognizable QC sample of known composition; as
a recognizable QC sample of unknown composition; or not recognizable as a
QC material.  The laboratory evaluation samples may be sent either by the
Regional client or the National Program Office, and may be used for
contract action.

Contractors are required to analyze the samples and return the data package
and all raw data within the contract required turnaround time.

In addition to PES preparation and analysis, the Contractor will be
responsible for correctly identifying and quantifying the analytes included
in the PES.  The Agency will notify the Contractor of unacceptable
performance.

Contractors are required to analyze the samples and return the data package
and all raw data within the contract required turns-round time.

A Contractor's results on the laboratory evaluation samples will determine
the Contractor's performance as follows:

1.   Acceptable. No Response Required (Score greater than or equal to 90
     percent):"""
     Data Beets most or all of the scoring criteria.  No response is
     required.

     Acceptable. Response Explaining Deflc^eneWlea^ Required (Score greater
     than or equal to 75 percent but less than 90 percent):

     Deficiencies exist in the Contractor's performance.

     Within 14 days of receipt of notification from EPA, the Contractor
     shall describe the deficiency(ies) and the action(s) taken to correct
     the deficiency(ies) in a letter to the Administrative Project Officer,
     the Technical Project Officer and EMSL/LV.

     An alternate delivery schedule may be proposed by the Contractor, but
     it is the sole decision of the Agency, represented either by the
     Technical Project Officer or Administrative Project Officer, to approve

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     or disapprove the alternate delivery schedule.   If an alternate
     delivery schedule  is proposed,  the Contractor  shall  describe  in a
     letter to the Technical Project Officer,  Administrative  Project
     Officer, and the Contracting Officer why  he/she is unable  to meet the
     delivery schedule listed in this section.   The  Technical Project
     Officer /Administrative Project Officer will not grant an  extension for
     greater than 14 days for the Contractor's response letter  to the
     laboratory evaluation sample report.  The Contractor  shall proceed  and
     not assume that an extension will be granted until so notified by the
     TPO and/or APO.

     If new SOPs are required to be written or SOPs  are required to be
     amended because of the deficiencies and the subsequent corrective
     action implemented by the Contractor,  the Contractor  shall write/amend
     and submit the SOPs per the requirements  listed in Exhibit E,  Section
     IV.

3.    Unacceptable Performance. Response Explaining Deficiencvfiesl  Required
     (Score less than 75 percent):

     Deficiencies exist in the Contractor's performance to the  extent that
     the  National Program Office has  determined that the Contractor has  not
     demonstrated the capability to meet the contract requirements.

     Within 14 days of receipt of notification from  EPA, the  Contractor
     shall describe the deficiency(ies) and the action(s)  taken to  correct
     the  deficiency(ies) in a letter  to the Administrative Project  Officer,
     the  Technical Project Officer and EMSL/LV.

     An alternate delivery schedule may be proposed  by the Contractor, but
     it is the sole decision of the Agency, represented either  by the
     Technical Project Officer or Administrative Project Officer, to approve
     or disapprove the alternate delivery schedule.   If an alternate
     delivery schedule  is proposed,  the Contractor  shall  describe  in a
     letter to the Technical Project  Officer,  Administrative  Project
     Officer,  and the Contracting Officer why  he/she is unable  to meet the
     delivery schedule listed in this section.   The  Technical Project
     Officer /Administrative Project Officer will not grant an  extension for
     greater than 14 days for the Contractor's response letter  to the
     performance evaluation sample report.

     If new SOPs are required to be written or SOPs  are required to be
     amended because of the deficiencies and the subsequent corrective
     action implemented by the Contractor, the Contractor  shall write/amend
     and submit the SOPs per the requirements  listed in Exhibit E,  Section
     IV.

     The Contractor shall be notified by the Technical Project Officer or
     Administrative Project Officer concerning the remedy for their
     unacceptable performance.  A Contractor may expect, but the Agency is
     not limited to, the following actions: reduction of the number of
     samples sent under the contract, suspension of sample shipment to  the
     Contractor, an On-Site laboratory evaluation,  data package audit,
     remedial performance evaluation sample, and/or a contract  sanction,
     such as a Cure Notice.

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Note:  A Contractor's prompt response demonstrating that corrective
actions have been taken to ensure the Contractor's capability to meet
contract requirements may facilitate continuation of full sample
delivery.

If the Contractor fails to adhere to the requirements listed in this
section, a Contractor may expect, but the Agency is not limited to the
following actions:  reduction in the number of samples sent under the
contract, suspension of sample shipment to the Contractor, an On-Site
laboratory evaluation, data package audit, a remedial laboratory
evaluation sample and/or contract sanctions, such as a Cure Notice.
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                                  SECTION X

                       ON-SITE LABORATORY EVALUATIONS


At a frequency dictated by a contract laboratory's performance, the
Administrative Project Officer, Technical Project Officer or their
authorized representative will conduct an On-Site laboratory evaluation.
On-site laboratory evaluations are carried out to monitor the Contractor's
ability to meet selected terms and conditions specified in the contract.
The evaluation process incorporates two separate categories:  Quality
Assurance Evaluation, and an Evidentiary Audit.

A.   Quality Assurance On-Site Evaluation

      Quality assurance evaluators inspect the Contractor's facilities to
      verify the adequacy and maintenance of instrumentation, the
      continuity of personnel meeting experience or education requirements,
      and the acceptable performance of analytical and QC procedures.  The
      Contractor should expect that items to be monitored will include, but
      not be limited to the following:

     o  Size and appearance of the facility

     o  Quantity, age, availability,  scheduled maintenance  and performance
        of  instrumentation

     o  Availability, appropriateness, and utilization of the  QAP and SOPs

     o  Staff qualifications,  experience,  and  personnel  training programs

     o  Reagents, standards, and  sample  storage  facilities

     o  Standard preparation logbooks and raw  data

     o  Bench sheets and analytical logbook maintenance  and review

     o  Review of the Contractor's sample analysis/data  package
        inspection/data management procedures

     Prior to an On-Site evaluation,  various documentation pertaining to
     performance of the specific Contractor is integrated in a profile
     package for discussion during the evaluation.  Items that nay be
     included are  previous On-Site reports, performance evaluation sample
     scores,  Regional review of data,  Regional QA materials, data audit
     reports, results of CCS,  and data trend reports.

B.   Evidentiary Audit

     Evidence auditors conduct an On-Site laboratory evaluation to determine
     if laboratory policies and procedures are in place to satisfy evidence
     handling requirements as stated in Exhibit F.  The evidence audit is
     comprised  of the following three activities:

     1.   Procedural Audit

          The procedural audit consists of review and examination of actual
          standard operating procedures and accompanying documentation for
          the following laboratory operations:  sample receiving, sample

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          storage,  sample identification,  sample  security, sample  tracking
          (from receipt to completion of analysis)  and analytical  project
          file organization and assembly.

     2.   Written SOPs Audit

          The written SOPs audit consists  of review and  examination of  the
          written SOPs to determine  if they are accurate and complete for
          the following laboratory operations:  sample receiving,  sample
          storage,  sample identification,  sample  security, sample  tracking
          (from receipt to completion of analysis)  and analytical  project
          file organization and assembly.

     3.   Analytical  Project File Evidence Audit

          The analytical project file evidence audit consists of review and
          examination of the analytical project file documentation.  The
         ' auditors  review the files  to determine:

          o   The accuracy of the document inventory

          o   The completeness of the file
          o   The adequacy and accuracy of the docunent numbering system

          o   Traceability of sample activity
          o   Identification of activity recorded on the documents

          o   Error correction methods
C.   Discussion of the On-Site Team's Findings

     The quality assurance and evidentiary auditors discuss  their findings
     with the Administrative Project Officer/Technical  Project Officer  prior
     to debriefing the Contractor.   During the debriefing, the auditors
     present their findings and recommendations for corrective actions
     necessary to the Contractor personnel.

D.   Corrective Action Reports For Follow-Through to Quality Assurance  and
     Evidentiary Audit Reports

     On-site laboratory eval"ation:

     Following an On-Site laboratory evaluation,  quality assurance and/or
     evidentiary audit reports which discuss deficiencies found during the
     On-Site evaluation may be sent to the Contractor.   In a detailed
     letter, the Contractor shall discuss the corrective actions implemented
     to resolve the deficiencies discussed during the On-Site evaluation and
     discussed in the report(s) to the Technical Project Officer,,
     Administrative Project Officer, and EMSL/LV (response to quality
     assurance/technical report) and NEIC (response to the evidentiary
     report), within 14 days of receipt of the report.   An alternate
     delivery schedule nay be proposed by the Contractor, but it  is the sole
     decision of the Agency, represented either by  the Technical Project
     Officer or Administrative Project Officer, to  approve or disapprove the
     alternate delivery-schedule.  If an alternate  delivery schedule is
     proposed, the Contractor shall describe in a letter to the Technical

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Project Officer, Administrative Project Officer, and the Contracting
Officer why he/she is unable to meet the delivery schedule listed in
this section.  The Technical Project Officer/Administrative Project
Officer will not grant an extension for greater than 14 days for the
Contractor's response letter to the quality assurance and evidentiary
audit report.  The Contractor shall proceed and not assume that an
extension will be granted until so notified by the TPO and/or APO.

If new SOPs are required to be written or SOPs are required to be
amended because of the deficiencies and the subsequent corrective
action implemented by the Contractor, the Contractor shall write/amend
and submit the SOPs per the requirements listed in Exhibit E, Section
IV.

Corrective actions

If the Contractor fails to adhere to the requirements listed in this
section, the Contractor may expect, but the Agency is not limited to
the following actions:  reduction in the number of samples sent under
the contract, suspension of sample shipment to the Contractor, an On-
Site laboratory evaluation, data package audit, a remedial performance
evaluation sample, and/or contract sanctions,  such as a Cure Notice.
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                                 SECTION XI

                               DATA MANAGEMENT

Data management procedures are defined as procedures specifying the
acquisition or entry, update, correction, deletion, storage and security of
computer readable data and files.  These procedures should be in written
form and contain a clear definition for all databases and files used to
generate or resubmit deliverables.  Key areas of concern include:  system
organization (including personnel and security), documentation operations,
traceability and quality control.

Data manually entered from hard-copy must be quality controlled and the
error rates estimated.  Systems should prevent entry of incorrect or out-
of-range data and alert data entry personnel of errors.  In addition, data
entry error rates must be estimated and recorded on a monthly basis by
reentering a statistical sample of the data entered and calculating
discrepancy rates by data element.

The record of changes in the form of corrections and updates to data
originally generated, submitted, and/or resubmittecl must be documented to
allow traceablilty of updates.  Documentation must include the following
for each change:

o   Justification or  rationale for the  change.

o   Initials  of the person making the change or changes.   Data changes  must
    be  implemented and reviewed by a person or group independant  of the
    source  generating the deliverable.

o   Change  documentation must be retained according to  the schedule of  the
    original  deliverable.

o   Resubmitted diskettes or other deliverables must be reinspected as  a
    part of the laboratories'  internal  inspection process prior to
    resubmission.  The entire deliverable,  not just the changes,  must be
    inspected.

o   The Laboratory Manager must approve changes to originally submitted
    deliverables.

o   Documentation of  data changes may be requested by laboratory auditors.

Lifecycle management procedures must be applied to computer software
systems developed by the laboratory to be used to generate and edit
contract deliverables.  Such systems must be thoroughly tested and
documented prior to utilization.

o   A software test and acceptance plan including test requirements, test
    results and acceptance criteria must be developed,  followed,  and
    available in written form.

o   System changes oust not be made directly to production systems
    generating deliverables.  Changes  must be made first to a development
    system and tested prior to implementation.

o   Each version of  the production system will be given an identification
    number, date of  installation, date of last operation and archived.
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o   System and operations documentation must be developed and maintained for
    each system.   Documentation must include a users manual and an
    operations and maintenance manual.

Individual(s) responsible for the following functions must be identified:


o   System operation and maintenance including documentation and training.

o   Database integrity,  including data  entry,  data  updating and quality
    control.

o   Data and system security,  backup and archiving.
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             EXHIBIT F
CHAIN-OF-CUSTODT, DOCUMENT CONTROL.
 AND STANDARD OPERATING PROCEDURES
               F-l                               ILM02.0

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1.    SAMPLE CHAIN-OF-CUSTODY

      A sample is physical evidence collected from a facility or from the
      environment.  Controlling evidence is an essential part of the
      hazardous waste investigation effort.  To accomplish this, Contractors
      are required to develop and implement the following sample
      identification, chain-of-custody, sample receiving, and sample tracking
      procedures.

1.1   Sample Identification

      To assure traceability of the samples while in possession of the
      Contractor,  the Contractor shall have a specified method for
      maintaining identification of samples throughout the laboratory.

      Each sample and sample preparation container shall be labeled with the
      EPA number or a unique laboratory identifier.  If a unique laboratory
      identifier is used, it shall be cross-referenced to the EPA number.

1.2   Chain-of-Custody Procedures

      Because of the nature of the data being collected, the custody of EPA
      samples must be traceable from the time the samples are collected until
      they are introduced as evidence in legal proceedings.  The Contractor
      shall have procedures ensuring that EPA sample custody is maintained
      and documented.  A sample is under custody if:

          o   It is in your possession, or
          o   It is in your view after being in your possession, or

          o   It was in your possession and you locked it up, or
          o   It is in a designated secure area.  (Secure areas shall be
             accessible only to authorized personnel.)
1.3   Saaple^Receiving Procedures

      1.3.1   The Contractor shall designate  a sample custodian responsible
              for receiving all samples.

      1.3.2   The Contractor shall designate  a representative  to receive
              samples in the event that  the sample custodian is not
              available.

      1.3.3   The condition of the shipping containers  and sample bottles
              shall be  inspected upon receipt by the sample custodian or
              his/her representative.

      1.3.4   The condition of the custody seals (intact/not intact)  shall be
              inspected upon receipt by  the sample custodian or his/her
              representative.

      1.3.5   The sample custodian or his/her representative shall  check  for
              the presence or absence of the  following  documents  accompanying
              the sample shipment:


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              o   Airbills or airbill stickers
              o   Custody seals
              o   EPA custody records
              o   EPA traffic reports or SAS packing lists
              o   Sample tags
      1.3.6   The sample custodian or his/her representative shall sign and
              date all forms (e.g., custody records, traffic reports or
              packing lists, and airbills) accompanying the samples at the
              time of sample receipt.
    <  1.3.7   The Contractor shall contact the Sample Management Office (SMO)
              to resolve discrepancies and problems such as absent documents,
              conflicting information, broken custody seals, and
              unsatisfactory sample condition (e.g., leaking sample bottle).
      1.3.8   The Contractor shall record the resolution of discrepancies and
              problems on Telephone Contact Logs.
      1.3.9   The following information shall be recorded on Form DC-1 (See
              Exhibit B) by the sample custodian or his/her .representative as
              samples are received and inspected:
              o   Condition of the shipping container
              o   Presence or absence and condition of custody seals on
                  shipping and/or sample containers
              o   Custody seal numbers,  when present
              o   Condition of the sample bottles
              o   Presence or absence of airbills or airbill stickers
            	o   Airbill or airbill sticker numbers
              o   Presence or absence of EPA custody records
              o   Presence or absence of EPA traffic reports or SAS packing
                  lists
              o   Presence or absence of sample tags
              o   Sample tag identification numbers cross-referenced to the
                  EPA sample numbers
              o   Verification of agreement or non-agreement of information
                  recorded on shipping documents and sample containers
              o   Problems or discrepancies
1.4   Sample Tracking Procedures
      The Contractor shall maintain records documenting all phases of sample
      handling from receipt to final analysis.
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2.    DOCUMENT CONTROL PROCEDURES

      The goal of the laboratory document control program is to assure that
      all documents for a specified Sample Delivery Group (SDG) will be
      accounted for when the project is completed.  Accountable documents
      used by contract laboratories shall include, but not be limited to,
      logbooks, chain-of-custody records, sample work sheets, bench sheets,
      and other documents relating to the sample or sample analyses.  The
      following document control procedures have been established to assure
      that all laboratory records are assembled and stored for delivery to
      EPA or are available upon request from EPA prior to the delivery
      schedule.

2.1   Preprinted Laboratory Forms and Logbooks

      2.1.1   All documents produced by the Contractor which are directly
              related to the preparation and analysis of EPA samples shall
              become Che property of the EPA and shall be placed in the
              complete sample delivery group file (CSF).  All observations
              and results recorded by the laboratory but not on preprinted
              laboratory forms shall be entered into permanent laboratory
              logbooks.  When all data from a SDG is compiled, all  original
              laboratory forms and copies of all SDG-related logbook entries
              shall be included in the documentation package.

      2.1.2   The Contractor shall identify the activity recorded on all
              laboratory documents which are directly related to the
              preparation and analysis of EPA samples.

      2.1.3   Pre-printed laboratory forms shall contain the name of the
              laboratory and be dated (month/day/year) and signed by the
              person responsible for performing the activity at the time an
              activity is performed.

      2.1.4 -^Logbook entries shall be dated (month/day/year) and signed by
              the person responsible for performing the activity at the  time
              an activity is performed.

      2.1.5   Logbook entries shall be in chronological order.  Entries  in
              logbooks, with the exception of instrument run logs and
              extraction logs, shall include only one SDG per page.

      2.1.6   Pages in both bound and unbound logbooks shall be sequentially
              numbered.

      2.1.7   Instrument run logs shall be maintained so as  to enable  a
              reconstruction of the run sequence of individual instruments.

              Because the laboratory must provide copies  of  the instrument
              run logs to EPA, the laboratory may exercise the option  of
              using only laboratory or EPA sample identification numbers in
              the logs for sample ID rather than government  agency or
              commercial client names to preserve the  confidentiality of
              commercial clients.


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      2.1.8    Corrections to supporting documents  and raw data  shall be made
               by drawing a single line  through  the error and entering  the
               correct information.  Corrections  and additions to supporting
               documents and raw data shall be dated and  initialed.  No
               information shall be  obliterated  or  rendered unreadable.

               All notations shall be recorded in ink.

               Unused portions  of documents shall be "z'd"  out.

2.2   Consistency of Documentation

      The Contractor shall assign a document control officer responsible for
      the organization and assembly of the CSF.

      All copies of laboratory documents shall be complete and legible.

      Original documents which include information relating to more than one
      SDG shall be filed in the CSF of the lowest SDG number.  The copy(s)
      shall be placed in the other CSF(s) and the Contractor shall record the
      following information on the copy(s) in red ink:

      "COPY

      ORIGINAL IS FILED IN CSF 	"
      The Contractor shall sign and date this addition to the copy(s).

      Before releasing analytical results,  the document control officer shall
      assemble and cross-check the information on samples tags, custody
      records, lab bench sheets, personal and instrument logs, and other
      relevant deliverables to ensure that data pertaining to each particular
      sample or sample delivery group is consistent throughout the CSF.

2.3   Document-Numbering and Inventory Procedure

      In order to provide document accountability of the completed analysis
      records, each item in the CSF shall be inventoried and assigned a
      serialized number as described in Exhibit B).

      All documents relevant to each sample delivery group, including logbook
      pages, bench sheets, mass spectra, chromatograms, screening records,
      re-preparation records, re-analysis records, records of failed or
      attempted analysis, custody records,  library research results, etc.
      shall be inventoried.

      The Document Control Officer (DCO) shall be responsible for ensuring
      that all documents generated are placed in the CSF for inventory and
      are delivered to the appropriate EPA region or other receiver as
      designated by EPA.  The DCO shall place the sample tags in plastic bags
      in the file.
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2.4   Storage of EPA Files

      The Contractor shall maintain EPA laboratory documents in a secure
      location.

2.5   Shipment of Deliverables

      The Contractor shall document shipment of deliverables packages to the
      recipients.  These shipments require custody seals on the containers
      placed such that they cannot be opened without damaging or breaking the
      seal.  The Contractor shall document what was sent, to whom,  the date,
      and the method (carrier) used.

      A copy of the transmittal letter for the CSF shall be sent to the
      NEIC/CEAT and the SMO.

3.    SPECIFICATIONS FOR WRITTEN STANDARDOPERATIC PROCEDURES

      The Contractor shall have written standard operating procedures (SOPs)
      for receipt of samples, maintenance of custody,  sample identification,
      sample storage,  sample tracking,  and assembly of completed data.

      An SOP is defined as a written narrative stepwise description of
      laboratory operating procedures including examples of laboratory
      documents.  The SOPs shall accurately describe the actual procedures
      used in the laboratory, and copies of the written SOPs shall be
      available to the appropriate laboratory personnel.  These procedures
      are necessary to ensure that analytical data produced under this
      contract are acceptable for use in EPA enforcement case preparation and
      litigation.  The Contractor's SOPs shall provide mechanisms and
      documentation to meet each of the following specifications and shall  be
      used by EPA as the basis for laboratory evidence audits.

3.1   The Contractor shall have written SOPs describing the sample
      custodian's duties and responsibilities.
           *Mb»
3.2   The Contractor shall have written SOPs for receiving and logging in of
      the samples.  The procedures shall include but not be limited to
      documenting the following information:

      3.2.1   Presence or absence of EPA chain-of-custody forms

      3.2.2   Presence or absence of airbills  or airbill stickers

      3.2.3   Presence or absence of traffic  reports  or SAS packing lists

      3.2.4   Presence or absence of custody  seals on shipping and/or sample
              containers and their  condition

      3.2.5   Custody seal  numbers, when present

      3.2.6   Airbill or airbill sticker numbers

      3.2.7   Presence or absence of sample tags


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      3.2.8   Sample tag ID numbers

      3.2.9   Condicion of Che shipping container

      3.2.10  Condition of the sample bottles

      3.2.11  Verification of agreement or non-agreement of information on
              receiving documents and sample containers

      3.2.12  Resolution of problems or discrepancies with the SMO

      3.2.13  An explanation of any terms used by the laboratory to describe
              sample condition upon receipt (e.g., good, fine, OK)

3.3   The Contractor shall have written SOFs  for maintaining identification
      of EPA samples throughout the laboratory.

      If the Contractor assigns unique  laboratory  identifiers,  written SOPs
      shall include a description of the method used to assign the unique
      laboratory identifier and shall include a description of the document
      used to cross-reference the unique laboratory identifier to the EPA
      sample number.

      If the Contractor uses prefixes or suffixes  in addition  to sample
      identification numbers, the written  SOPs shall include their
      definitions.

3.4   The Contractor shall have written SOPs  describing all storage areas  for
      samples in the laboratory.  The SOPs shall include a list of authorized
      personnel who have access or keys to secure  storage areas.

3.5   The Contractor shall have written SOPs  describing the method by which
      the laboratory maintains samples  under  custody.

3.6   The Contractor shall have written SOPs  describing the method by which
      the laboratory maintains the security of any areas identified as
      secure.

3.7   The Contractor shall have written SOPs  for tracking the  work performed
      on any particular samples.  The tracking SOP shall include:

          o  A description of the documents used to record sample receipt,
             sample storage, sample transfers, sample preparations, and
             sample analyses.

          o  A description of the documents used to record calibration and
             QA/QC laboratory work.

          o  Examples  of document formats and laboratory documents used in
             the sample receipt, sample storage, sample transfer, and sample
             analyses.
          o  A narrative step-wise  description of  how  documents are used  to
             track samples.
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 3.8   The  Contractor  shall have written SOPs for organization and assembly of
      all  documents relating to each SDG.  Documents shall be filed on a
      sample  delivery group-specific basis.  The procedures shall ensure that
      all  documents including logbook pages, sample tracking records,
      chrcoatographic charts,  computer printouts, raw data summaries,
      correspondence,  and any other written documents having reference to the
      SDG  are compiled in one location for submission to EPA.  The written
      SOPs shall  include:

          o   A  description of the numbering and inventory method.

          o   A  description of the method used by the laboratory to verify
              consistency  and completeness of the CSF.
          o   Procedures for the shipment of deliverables packages using
              custody  seals.
4.    HANDLING OF CONFIDENTIAL INFORMATION

      A Contractor conducting work under this contract may receive EPA-
      designated confidential information from the agency.   Confidential
      information must be handled separately from other documentation
      developed under this contract.  To accomplish this,  the following
      procedures for the handling of confidential information have been
      established.

4.1   All confidential documents shall be under the supervision of a
      designated Document Control Officer (DCO).

4.2   Confidential Information

      Any samples or information received with a request of confidentiality
      shall be handled as "confidential."  A separate locked file shall be
      maintained to store this information and shall be segregated from other
      nonconfidential information.  Data generated from confidential samples
      shall be treated as confidential.  Upon receipt of confidential
      information, the DCO will log these documents into a Confidential
      Inventory Log.  The information will then be available to authorized
      personnel but only after it has been signed out to that person by the
      DCO.  The documents shall be returned to the locked file at the
      conclusion of each working day.  Confidential information may not be
      reproduced except upon approval by the: EPA Administrative or Technical
      Project Officer.  The  DCO will enter all copies into the document
      control system described above.  In addition, this information may not
      be disposed of except  upon approval by the EPA Administrative or
      Technical Project Officer.  The DCO shall remove and retain the cover
      page of any confidential information disposed of for one year and shall
      keep a record on  the disposition in the Confidential Inventory Log.
                                    F-8                               ILM02.0

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    EXHIBIT G
GLOSSARY OF TERMS
                                         ILM02.0

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                              GLOSSARY OF TERMS
ABSORBANCE  -  a measure of  the decrease in incident light passing through a
sample  into the detector.  It is defined mathematically as:

              A  —  I(solvent)   ^  log  lo
                     I(solution)         I

               Where, I -  radiation intensity

ALIQUOT • a measured  portion of a field sample taken for analysis.

ANALYSIS DATE/TIME •  the date and military time (24-hour clock) of the
introduction  of the sample, standard, or blank into the analysis system.

ANALYTE - the element or ion an analysis seeks to determine; the element of
interest.

ANALYTICAL  SAMPLE - Any solution or media introduced into an instrument on
which an analysis is  performed excluding instrument calibration, initial
calibration verification,  initial calibration blank, continuing calibration
verification  and continuing calibration blank.  Note the following are all
defined as  analytical samples:  undiluted and diluted samples (EPA and non-
EPA), predigestion spike samples, duplicate samples, serial dilution
samples, analytical spike samples,  post-digestion spike samples,
interference  check samples (ICS), CRDL standard for AA (CRA), CRDL standard
for ICP (CRI), laboratory control sample (LCS), preparation blank (PB) and
linear range  analysis sample (LRS).

ANALYTICAL  SPIKE - The furnace post-digestion spike.  The addition of a
known amount  of standard after digestion.

AUTOZERO - zeroing the instrument at the proper wavelength.  It is
equivalent to running a standard blank with the absorbance set at zero.

AVERAGE INTENSITY - The average of two different injections (exposures).

BACKGROUND CORRECTION - a technique to compensate for variable background
contribution  to the instrument signal in the determination of trace
elements.

BATCH - a group of samples prepared at the same time in the same location
using the same method.

CALIBRATION - the establishment of an analytical curve based on the
absorbance,  emission intensity,  or other measured characteristic of known
standards.  The calibration standards must be prepared using the same type
of acid or concentration of acids as used in the s&mple preparation.

CALIBRATION BLANK - a volume of acidified deionized/distilled water.

CALIBRATION STANDARDS - a series of known standard solutions used by the
analyst for calibration of the instrument (i.e., preparation of the
analytical  curve).

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CASE  - a finite, usually predetermined number of samples collected over a
given time period from a particular site.  Case numbers are assigned by the
Sample Management Office.  A Case consists of one or more Sample Delivery
Groups.

COEFFICIENT OF VARIATION (CV) - the standard deviation as a percent of the
arithmetic mean.

CONCENTRATION LEVEL (low or medium) - for inorganics analysis,  low or
medium level is defined by the appropriate designation checked by the
sampler on the Traffic Report.

CONTINUING CALIBRATION - analytical standard run every 10 analytical
samples or every 2 hours, whichever is more frequent,  to verify the
calibration of the analytical system.

CONTRACT REQUIRED DETECTION LIMIT (CRDL) - minimum level of detection
acceptable under the contract Statement of Work.

CONTROL LIMITS - a range within which specified measurement results must.
fall to be compliant.   Control limits may be mandatory, requiring
corrective action if exceeded, or advisory, requiring that noncompliant
data be flagged.

CORRELATION COEFFICIENT - a number (r) which indicates the degree of depen-
dence between two variables (concentration - absorbance).  The more
dependent they are the closer the value to one.  Determined on the basis of
the least squares line.

DAY - unless otherwise specified, day shall mean calendar day.

DIGESTION LOG - an official record of the sample preparation (digestion).

DISSOLVED METALS - analyte elements which have not been digested prior to
analysis and which will pass through a 0.45 urn filter.

DRY WEIGHT - the weight of a sample based on percent solids.  The weight
after drying in an oven.

DUPLICATE - a second aliquot of a sample that is treated the same as the
original sample in order to determine the precision of the method.

FIELD BLANK - any sample submitted from the field identified as a blank.

FIELD SAMPLE - a portion of material received to be analyzed that is
contained in single or multiple containers and  identified by a unique EPA
Sample Number.

FLAME ATOMIC ABSORPTION (AA)  - atomic absorption which utilizes flame for
excitation.

GRAPHITE FURNACE ATOMIC ABSORPTION (GFAA)  - atomic absorption which
utilizes a graphite cell for excitation.


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HOLDING TIME - the elapsed time expressed in days from the date of receipt
of the sample by the Contractor until the date of its analysis.

      Holding time - (sample analysis date  - sample receipt date)

INDEPENDENT STANDARD • a Contractor-prepared standard solution that is
composed of analytes from a different source than those used in the
standards for the initial calibration.

INDUCTIVELY COUPLED PLASMA (ICP) - a technique for the simultaneous or
sequential multi-element determination of elements in solution.  The basis
of the method is the measurement of atomic emission by an optical
spectroscopic technique.  Characteristic atomic line emission spectra are
produced by excitation of the sample in a radio frequency inductively
coupled plasma.

IN-HOUSE - at the Contractor's facility.

INJECTION - introduction of the analytical sample into the instrument
excitation system for the purpose of measuring absorbance, emission or
concentration of an analyte.  May also be referred to as exposure.

INSTRUMENT CALIBRATION - analysis of analytical standards for a series of
different specified concentrations; used to define the quantitative
response, linearity, and dynamic range of the instrument to target
analytes.

INSTRUMENT DETECTION LIMIT (IDL) - determined by multiplying by three the
standard deviation obtained for the analysis of a standard solution (each
analyte in reagent water) at a concentration of 3x-5x IDL on three
nonconsecutive days with seven consecutive measurements per day.

INSTRUMENT CHECK SAMPLE - A solution containing both interfering and
analyte elements of known concentration that can be used to verify
background and interelement correction factors.
             .*»•
INSTRUMENT CHECK STANDARD - a multi-element standard of known
concentrations prepared by the analyst to monitor &nd verify instrument
performance on a daily basis.

INTERFERENTS - substances which affect the analysis for the element of
interest.

INTERNAL STANDARDS - in-house compounds added at a known concentration.

LABORATORY - synonymous with Contractor as used herein.

LABORATORY CONTROL SAMPLE (LCS) - a control sample of known composition.
Aqueous and solid laboratory control samples are analyzed using the  same
sample preparation, reagents, and analytical methods employed  for the EPA
samples received.
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LABORATORY RECEIPT DATE - the date on which a sample is received at the
Contractor's facility, as recorded on the shipper': delivery receipt and
sample Traffic Report.  Also referred to as VTSR (validated time of sample
receipt).

LINEAR RANGE, LINEAR DYNAMIC RANGE - the concentration range over which the
ICP analytical curve remains linear.

MATRIX - the predominant material of which the sample to be analyzed is
composed.  For the purpose of this SOW, a sample matrix is either water or
soil/sediment.  Matrix is not synonymous with phase (liquid or solid).

MATRIX MODIFIER - salts used in AA to lessen the effects of chemical
interferents, viscosity, and surface tension.

MATRIX SPIKE • aliquot of a sample (water or soil) fortified (spiked) with
known quantities of specific compounds and subjected to the entire
analytical procedure in order to indicate the appropriateness of the method
for the matrix by measuring recovery.

METHOD OF STANDARD ADDITIONS (MSA) - the addition of 3 increments of a
standard solution (spikes) to sample aliquots of the same size.
Measurements are made on the original and after each addition.  The slope,
x-intercept and y-intercept are determined by least-square analysis.  The
analyte concentration is determined by the absolute value of the x-
intercept.  Ideally, the spike volume is low relative to the sample volume
(approximately 10% of the volume).  Standard addition may counteract matrix
effects; it will not counteract spectral effects.  Also referred to as
Standard Addition.

PERCENT SOLIDS - the proportion of solid in a soil sample determined by
drying an aliquot of the sample.

PERFORMANCE EVALUATION (PE) SAMPLE - a sample of known composition provided
by EPA for Contractor analysis.  Used by EPA to evaluate Contractor
performance.

PREPARATION BLANK (reagent blank, method blank) - &n analytical control
that contains distilled, deionized water and reagents, which is carried
through the entire analytical procedure (digested &nd analyzed).  An
aqueous method blank is treated with the same reagents as a sample with a
water matrix; A solid method blank is treated with the same reagents as a
soil sample.

PROTOCOL - a compilation of the procedures to be followed with respect to
•ample receipt and handling, analytical methods, d&ta reporting and
deliverables, and document control.  Used synonymously with Statement of
Work (SOW).

QUALITY CONTROL SAMPLE - a solution obtained from  en outside  source having
known concentration values to be used to verify  the calibration standards.
                                    G-4                                ILM02.0

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REAGENT BLANK - a volume of delonized, distilled wa.ter containing the same
acid matrix as the calibration standards carried through the entire
analytical scheme.

ROUNDING RULES - If the figure following those to be retained is less than
5, the figure is dropped, and the retained figures are kept unchanged.  As
an example, 11.443 is rounded off to 11.44.

If the figure following those to be retained is greater than 5, the figure
is dropped, and the last retained figure is raised by 1.  As an example,
11.446 is rounded off to 11.45.

If the figure following Chose to be retained is 5,  and if there are no
figures other than zeros beyond the five,  the figure 5 is dropped, and the
last-place figure retained is increased by one if it is an odd number or it
is kept unchanged if an even number.  As an example., 11.435 is rounded off
to 11.44, while 11.425 is rounded off to 11.42.

If a series of multiple operations is to be performed (add, subtract,
divide, multiply), all figures are carried through the calculations.  Then
the final answer is rounded to the proper number of significant figures.

See forms instructions (Exhibit B) for exceptions.

RUN - a continuous analytical sequence consisting of prepared samples and
all associated quality assurance measurements as required by the contract
Statement of Work.

SAMPLE DELIVERY GROUP (SDG) - a unit within a sample Case that is used to
identify a group of samples for delivery.   An SDG is a group of 20 or fewer
samples within a Case, received over a period of up to 14 calendar days.
Data from all samples in an SDG are due concurrently.  A Sample Delivery
Group is defined by one of the following,  whichever occurs first:

       o   Case;  or
       o   Each 20 samples within a Case;  or
       o   Eaclfc 14- day calendar period during which samples in a Case are
           received,  beginning with receipt of the first sample in the Case
           or SDG.

Samples may be assigned to Sample Delivery Groups by matrix (i.e., all
soils in one SDG, all waters in another), at the discretion of the
laboratory.

SAMPLE NUMBER (EPA SAMPLE NUMBER) - a unique identification number
designated by EPA for each sample.  The EPA Sample Number appears on the
sample Traffic Report which documents information on that sample.

SENSITIVITY - the slope of the analytical curve, i.e., functional
relationship between emission intensity and concentration.

SERIAL DILUTION • the dilution of a sample by a factor of five.  When
corrected by the dilution factor, the diluted sample must agree with the
original undiluted sample within specified limits.  Serial dilution  may
reflect the influence of interferents.


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SOIL - synonymous with soil/sediment or sediment as used herein.

STOCK SOLUTION - a standard solution which can be diluted to derive other
standards.

SUSPENDED - those elements which are retained by a 0.45 urn membrane filter.

TOTAL METALS - analyte elements which have been digested prior to analysis.

TRAFFIC REPORT (TR) - an EPA sample identification form filled out by the
sampler, which accompanies the sample during shipment to the laboratory and
which is used for documenting sample condition and receipt by the
laboratory.

VET WEIGHT - the weight of a sample aliquot including moisture (undried).

10% FREQUENCY - a frequency specification during an analytical sequence
allowing for no more than 10 analytical samples between required
calibration verification measurements, as specified by the contract:
Statement of Work.
                                    G-6                                 ILM02.0

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                EXHIBIT H
   DATA DICTIONARY AND FORMAT FOR DATA
DELIVERABLES IN COMPUTER-READABLE FORMAT
                                                     ILM02.1

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                    AGENCY STANDARD IMPLEMENTATION FOR INORGANICS ILM02.1
       1.    Format Characteristics

       1.1   This constitutes an implementation of the EPA Agency Standard for
             Electronic Data Transmission based upon analytical results and ancillary
             information required by the contract.  All data generated by a single
             analysis are grouped together, and the groups are aggregated to produce
             files that report data from an SDG.  Because this implementation is only
             a subset of the Agency Standard,  some fields have been replaced by
             delimiters as place holders for non-CLP data elements.

       1.2   This implementation includes detailed specifications for the required
             format of each record.  The position in the record where each field is to
             be contained relevant to other fields is specified,  as  well as the
             maximum length of the field.  Each field's required contents are
             specified as literal (contained in quotes),  which must  appear exactly as
             shown (without quotes),  or as a variable for which format and/or
             descriptions are listed in the format/contents column.   Options and
             examples are listed for most fields.   For fields where  more than three
             options are available, a list and description of options are supplied
             following the record descriptions.  Fields are separated from each other
             by the delimiter "|" (ASCII 124).  Fields that do not contain data should
             be zero length with the delimiter as place holder.

       1.3   Numeric fields may contain numeric digits, a decimal place, and a leading
             minus sign.  A positive sign is assumed if no negative  sign is entered in
             a numeric field and must not be entered into any numeric field.

             Requirements for significant figures and number of decimal places are
             specified in Exhibit B,   The numeric field lengths are  specified such
             that all possible numeric values  can be written to the  file.  The size of
             the numeric field indicates the maximum number of digits, decimal, and
             negative sj-gn. if appropriate, that can appear in the field at the same
             time.  Therefore, the number reported may need to be rounded (using EPA
             Rounding Rules) to fit into the field.   The rounding must maintain the
             greatest significance possible providing the field length limitation.  In
             addition, the rounded number that appears on the form,  and therefore the
             field in the diskette file, must be used in any calculation that may
             result in other numbers reported on the same form or other forms in the
             SDG.   Field lengths should only be as long as necessary to contain the
             data; packing with blanks is not allowed.

       2.    Record Types

       2.1   The Agency Standard consists of variable length ASCII records.  Maximum
             field length specifications match the reporting requirements in Exhibit
             B.  The last two bytes of each record must contain "carriage return" and
             "line feed", respectively.

       2.2   There are four groups of record types in the reporting format, as shown
             below.  Detailed record formats follow.
9/91                                             H-l                         ILM02.1

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       Type           Type ID                Contents

       Run Header         10         Information pertinent to a group of
                                    samples processed in a continuous sequence;
                                    usually several per SDG

       Sample Header      20         Sample identifying,  qualifying, and linking
                                    information

       Results Record     30         Analyte results and qualifications

       Comments Record    90         Free form comments

       2.3   All record types given are mandatory.  Type 10, representing the
             analytical run,  contains the instrument and run IDs which act as an
             identifying  label for  the run.   All 10, 20, 30, and 90 series records
             following that record pertain to the same  analytical run.   Type 20,
             representing the sample, contains the EPA  Sample ID which acts as an
             identifying  label for  the sample.  The QC  code indicates whether the data
             is from an environmental sample, calibration,  or QC sample.   All 20, 30,
             and 90 series records  following that record pertain to the same sample.
             Type 30, representing an individual analyte,  contains an identifier to
             identify the analyte.  All 30 series records following that record
             pertain to the same analyte.

       3.    Production Runs

             A production run represents a "group" or "batch" of samples that are
             processed in a continuous sequence under relatively stable conditions.
             Specifically:

             Calibration  - All samples in a run use the same initial calibration data.

             Method  -  Constant.

             Instrument conditions  - Constant throughout a run.   Results obtained on
             different instruments cannot be combined in one run.

             Thus,  each separate group of analyses on each instrument will consist of
             a separate production run,  and must be reported in a separate file.

       Example of the Sequence of Record Types in a Production Run

       10  Contains  run header  information.   Occurs  once per run.

       16  Contains  additional  run header  information.   Occurs once per run.

       20  Acts  as a header for the following instrument parameter information.
           Occurs once per run  with EPA  Sample Number equal  to "IDL".   Analysis  year,
           analysis  month, analysis day  equal the year,  month and day the IDLs were
           computed.  Analyte count equals the number of the type 30 records  that
           follow.

             30 Contains  only  the Analyte CAS Number,  IDL Label  and IDL.   Occurs once
                for each  analyte used in  the run.


9/91                                              H-2                         ILM02.1

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             30
             30

             30

       20 Acts as  a header  for Che following instrument parameter information.
          Occurs once  per run with EPA Sample Number equal to "LRV".  Analysis  year,
          analysis month, analysis day equal to the year, month and day  the  linear
          ranges were  computed.  Analyte count equals the number of type  30,  32 and
          34 groups that follow.
       20
       21

       22
             30 Contains only the Analyte CAS Number.
                used  in the run.
                                             Occurs once for each analyte
             32 Contains integration time information for the preceding analyte on
                the type 30 record.

             34 Contains the CRDL and Linear Range information for the preceding
                analyte on the type 30 record.  There are as many consecutive  type  34
                records as there are different wavelengths used for the analyte
                identified on preceding type 30.

             30

             32
             34

       20 Acts as a header for the following instrument parameter information.
          Occurs once per run with EPA Sample Number equal to "ICF".  Analysis year,
          analysis month, analysis day equal the year, month and day the  interelement
          correction factors were computed.  Analyte count equals the number of the
          type 30 and 35 groups that follow.
             30 Contains only the Analyte CAS Number.
                used in the run.
                                             Occurs once for each analyte
             35
             30
             35
      Contains the background and interelement correction information for
      the preceding analyte on the type 30 record.  There are as many
      consecutive type 35 records as there are interelement correction
      factors for the analyte identified on preceding type 30.
Contains header information for sample and QC data.
Contains additional information for analytical and instrument QC samples.
Will always be preceded by a type 20 record.

Contains additional information for analytical samples.  Will usually
follow type 21 record.

   30  Contains the sample level concentration, true or added value  and QC
      value for each analyte.  Occurs once for each analytical  result for
      the EPA Sample Number of the previous type 20 record.

   31  Reports any instrumental data necessary to obtain the result  reported
      on the previous type 30 record.  Will always be preceded  by a type  30
      record.  Occurs once per type 30 record.
   30  Values for the next analyte wavelength being measured.
9/91
                                       H-3
ILM02.1

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             31  Values for the next analyte wavelength being measured.
             30

             31  .
           Type 30-31 record sequence continues as many times as the value of the
           ANALYTE  COUNT on the previous type 20 record.
       20  Next Sample Header record - The following applies to the next sample data.

       21

       22
             30

             31
             30

             31    etc.
       20

       21

       22
             30

             31

                   etc.
       4.     Record Sequence

       4.1   A Run  Header (type 10) record must be present as the first record in the
             file.   Further occurrences of the type 10 record in the file are not
             allowed.

             A type 16 record must immediately follow the type 10 record.  Further
             occurrences of the type 16 record in the file are not allowed.

             The first three type 20 records are headers for the calculated run-wide
             instrument parameters.  The first type 20 record is a header for the
             quarterly determined instrument detection limit values (IDL) and must
             immediately follow the type 16 record.  The second type 20 record is a
             header for the linear range values (LRV) and must immediately follow the
             last type 30 record that pertains to the instrument detection limit
             values,   The third type 20 record is a header for the annually determined
             ICP interelement correction factors (ICF) and must immediately follow the
             last type 34 record that pertains to the linear range values.  These are
             the only occurrences of the type 20 records that do not correspond to
             actual analyses in the run.  Therefore, the only fields that are not
             blank  in these occurrences of the type 20 record are the RECORD TYPE
             ("20");  EPA SAMPLE NUMBER ("IDL", "LRV" and "ICF"); Analysis Year/Year
             Computed, Analysis Month/Month Computed, Analysis Day/Day Computed ("YY",
             "MM",  "DD"); and ANALYTE COUNT.
9/91                                             H-4                         ILM02.1

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             A minimum of one type 30 record must immediately follow the first type 20
             record, and the total number of type 30 records must be equivalent to the
             ANALYTE COUNT on this type 20 record.  A minimum of one group of type 30,
             32 and 34 records must immediately follow the second type 20 record.  The
             information in each group must pertain to one and only one arialyte.  The
             number of groups must be equivalent to the Analyte Count on the second
             type 20 record.  A minimum of one group of type 30 and 35 records must
             immediately follow the third type 20 record.   The information in each
             group must pertain to one and only one analyte.   The number of groups
             must be equivalent to the analyte count on the third type 20 record.
             This last group must immediately be followed by the first type 20 record
             that corresponds to an actual analysis of an instrument calibration
             standard.  After the appearance of this,  the fourth type 20 record in the
             file, further occurrences of the type 32,  34 and 35 records in that file
             are not allowed.

       4.2   Each environmental sample,  calibration, or quality control sajnple is
             represented by a group composed of a type 20, 21, and 22 records, which
             holds sample level identifying information,  followed by a minimum of one
             group composed of type 30 and 31 records  for each analyte's wavelength.

             The type 20 record holds a count for the  number of analyte wavelengths
             being used to determine results.  The ANALYTE COUNTER must have a value
             equivalent to the number of type 30 groups associated with each type 20
             record.

             Except for the first three type 20 records,  all type 20 records should
             occur in the order of sample analysis.

       4.3   Type 90 comment records may be defined to occupy any position except
             before the type 10 (header) record.  Comments pertaining to the whole run
             such as ones on Cover Page must appear before the first type 20 record.
             Comments pertaining to a particular sample such as ones on Form I must
             appear after the type 20 record for that  sample, but before the first
             type 30 record associated with that sample.   Comments pertaining to a
             particular analyte or wavelength must appear after the type 30 record of
             that wavelength, but before the type 30 record of the following
             wavelength.
9/91                                             H-5                         ILM02.1

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5.
File/Record Integrity
      All record types must contain the following check fields to ensure file
      and record integrity:
Record
Position

First Field
       Field
       Length
Contents

Record type or identifier
Remarks

"10" or as appropriate
Last Field
              4
              2
                  Record sequence  number
                  within file
                  Record checksum
                  Contains CR and  LF
                              00000-99999,  repeated as
                              necessary
                              Four hexadecimal digits
   The checksum is defined to be the sum of the ASCII representation of the data
on the record up to the Record Sequence Number plus the checksum of the previous
record.  The sum is taken modulo 65536 (21 ) and represented as four (4)
hexadecimal digits.

6.     Dates and Times

      Date or time-of-day information consists of successive groups of two      |
      decimal digits, each separated by delimiters.  Dates are given in the
      order YY MM DD, and times as HH MM.  All hours must be given as 00 to 23  |
      using a 24 hour clock and must be local time.

7.     Multiple Volume Data

      There is no requirement under this format that all the data from an
      entire SDG fit onto a single diskette.  However, each single production
      run must fit onto a single diskette if possible.  If that is not
      possible, then it is necessary that all files start with a type 10
      record, and that the multiple type 10 records for each file of the same
      production run be identical.  Information for a single sample may not be
      split between files.

8.     Deliverable

8.1   The file or files must be submitted on a 5-1/4 inch floppy diskette,
      which may be either a double-sided, double-density, 360 K-byte or a high
      capacity 1.2 M-byte, or 3.5 inch double-sided, double-density 720 K-byte
      or 1.44 M-byte, diskette.  The diskette must be formatted and recorded
      using the MS-DOS Operating System.  The diskette or diskettes must
      contain all information relevant to one and only one SDG, and must
      accompany the hardcopy package for the SDG submitted to the Sample
      Management Office (see Exhibit B).  Information on the diskette or
      diskettes must correspond exactly with information submitted in the
      hardcopy data package and on the hardcopy data package forms.  Blank or
      unused records should not be included on the diskettes.
                                          H-6
                                                                ILM02.1

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       8.2   Each diskette must be identified with an external label containing  (in
             this order) the following information:

                      Disk Density
                      File Name(s)
                      Laboratory Name (optional)
                      Laboratory Code
                      Case Number (where applicable)
                      SAS Number (where applicable)

             The format for the File Name(s) must be XXXXXX.I01 to XXXXXX.199

                     where XXXXXX is the SDG identifier,  I designates  inorganics,  and
                     01 through 99 the file number.

             Dimensions of the label must be in the range 4-3/4" to 5" long by 1 1/4"
             to 1 1/2"  wide for 5 1/4 inch floppy diskette;  and 2" to 2 1/4" long by  2
             1/8" to 2  3/8" wide for 3.5 inch IBM-compatible diskette.
9/91
H-7
ILM02.1

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     9.
Record Listing
           Following  is a  listing of every record type required to report data from a
           single SDG.
     MAXIMUM
     LENGTH

     2
     1
     2
     1
     2
     1
     2
     1
     2
     1
     2
     1
     5
     1
     8
     1
     3
     1
     6
     4
     11
     1
     10
     2
     25
     1
     2
     1
     5
     4
        FORMAT  OF THE  PRODUCTION RUN FIRST HEADER RECORD  (TYPE  10)


         CONTENTS                               FORMAT/CONTENTS
         RECORD TYPE
         Delimiter
         ANALYSIS START YEAR
         Delimiter
         ANALYSIS START MONTH
         Delimiter
         ANALYSIS START DAY
         Delimiter
         ANALYSIS START HOUR
         Delimiter
         ANALYSIS START MINUTE
         Delimiter
         METHOD TYPE
         Delimiter
         METHOD NUMBER
         Delimiter
         MANAGER'S INITIALS
         Delimiter
         LAB CODE
         Delimiter
         CONTRACT NUMBER
         Delimiter
         INSTRUMENT ID
         Delimiter
         LABORATORY NAME
         Delimiter
         RUN NUMBER
         Delimiter
         RECORD SEQUENCE NUMBER
         CHECKSUM
"10"
I
YY
I
MM
I
DD
I
HH
I
MM

CHARACTER1
I
"ILM02.1" (SOW)
I
CHARACTER
I
CHARACTER
MM
CHARACTER
I
CHARACTER
II
CHARACTER

NUMERIC2
I
NUMERIC
CHARACTER
        Method Types  are
       "P" for ICP
       "A" for Flame AA
       "F" for Furnace AA
       "PM" for ICP when Microwave Digestion is used
       "AM" for Flame AA when Microwave Digestion is used
       "FM" for Furnace AA when Microwave Digestion is used
       "CV" for Manual Cold Vapor AA
       "AV" for Automated Cold Vapor AA
       "CA" for Midi-Distillation Spectrophotometric
       "AS" for Semi-Automated Spectrophotometric
       "C" for Manual Spectrophotometric
       "T" for Titrimetric

        Run number values are 01 through 99.  Each production run will be  assigned  a
        unique Run Number.  Run Numbers are to be assigned sequentially  beginning with  01
        and will  equal the number of production runs.
/91
                                     H-8
                  ILM02.1

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                   FORMAT OF THE PRODUCTION  RUN SECOND HEADER  RECORD  (TYPE 16)
      MAXIMUM
      LENGTH

      2
      1
      2
      1
      2
      1
      2
      1
      2
      1
      2
      1
      1
      1
      1
      1
      1
      1
      1
      1
      5
      4
CONTENTS

RECORD TYPE
Delimiter
ANALYSIS END YEAR
Delimiter
ANALYSIS END MONTH
Delimiter
ANALYSIS END DAY
Delimiter
ANALYSIS END HOUR
Delimiter
ANALYSIS END MINUTE
Delimiter
AUTO-SAMPLER USED
Delimiter
INTERELEMENT CORRECTIONS APPLIED
Delimiter
BACKGROUND CORRECTIONS APPLIED
Delimiter
RAW DATA GENERATED
Delimiter
RECORD SEQUENCE NUMBER
CHECKSUM
FORMAT/CONTENTS

"16"
I
YY
I
MM
I
DD
I
HH
I
MM

"Y" or "N"l

"Y" or "N"^

"Y" or "N"2
1
11 Y" or "N" or "B"-
I
NUMERIC
CHARACTER
      1   Enter "Y" if an auto-sampler is used with equal analysis time and intervals
         between analysis.

      2   These are the answers to the first two questions on the Cover Page.   "Y"  equals
         "YES", and "N" equals "NO".

      3   This is the answer to the  third question on  the Cover  Page.   "Y"  equals "YES",
         "B" equals BLANK and "N" equals "NO".
9/91
                             H-9
                                                                             ILM02.1

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                   FORMAT FOR THE MANDATORY  SAMPLE HEADER DATA RECORD  (TYPE 201
      MAXIMUM
      LENGTH

      2
      1
      2
      1
      12
      1
      5
      1
      3
      1
      3
      1
      5
      1
      6
      L
      2
      1
      2
      1
      2
      1
      2
      1
      2
      2
      2
      1
      5
      1
      3
      1
      5
      4
CONTENTS

RECORD TYPE
Delimiter
REGION
Delimiter
EPA SAMPLE NUMBER
Delimiter
MATRIX
Delimiter
QC CODE
Delimiter
SAMPLE QUALIFIER
Delimiter
CASE NUMBER
Delimiter
SDG NUMBER
Delimiter
ANALYSIS YEAR/YEAR COMPUTED
Delimiter
ANALYSIS MONTH/MONTH COMPUTED
Delimiter
ANALYSIS DAY/DAY COMPUTED
Delimiter
ANALYSIS HOUR
Delimiter
ANALYSIS MINUTE
Delimiter
SAMPLE WT/VOL UNITS
Delimiter
SAMPLE WT/VOL
Delimiter
ANALYTE COUNT
Delimiter
RECORD SEQUENCE NUMBER
CHECKSUM
FORMAT/CONTENTS

"20"
I
NUMERIC

CHARACTER1

CHARACTER2
I
CHARACTER

CHARACTER3
I
CHARACTER
I
CHARACTER
I
YY
I
MM
I
DD
I
HH
I
MM
il      ,
"G"/"ML"4

NUMERIC5
I
NUMERIC
I
NUMERIC
CHARACTER
      1  EPA Sample Number as appears on Form XIV except for the first three type 20
         records.  The first type  20 record must have an EPA Sample Number of "IDL"; the
         second, an EPA sample number of "LRV"; the third, an EPA sample number of  "ICF".

      2  For matrix,  "1" equals  "WATER", and "F" equals "SOIL".

      3  "REJ" sample qualifier  is  for  the unacceptable (one of the two) MSA results; this
         sample qualifier appears  on the type 20 record containing the zero (0) addition
         EPA Sample Number (XXXXXXO).

      ^  "G" equals grams, and "ML" equals milliliters.

      ^  This is the  size of the sample at the beginning of the digestion procedure.
9/91
                            H-10
                  ILM02.1

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                               SAMPLE QC CODES LISTING FOR TYPE 20
          QCC     Name

          LRB   LABORATORY (REAGENT)
                BLANK

          LCB   LABORATORY CALIBRATION
               . BLANK

          LIB   LABORATORY INITIAL BLANK
                                          Definition

                          The Preparation or Method Blank
                          (See Exhibit G).

                          The Continuing Calibration Blank (CCB)
                          (See Exhibit G).

                           The Initial Calibration Blank (ICB)
                           (See Exhibit G).
          LCM   LABORATORY CONTROL
                SOLUTION
                          The Laboratory Control Sample (LCS)
                          (See Exhibit G).
          LD1   LABORATORY DUPLICATE
                FIRST MEMBER
          LD2   LABORATORY DUPLICATE
                SECOND MEMBER
                           This is the same as the Sample Result "(S)"
                           that is reported on the Duplicate Form of
                           hardcopy (Form VI).

                           This is the second aliquot and is identified
                           as "D" on the Duplicate Form of hardcopy
                           (Form VI).
          LVM   LABORATORY CALIBRATION
                VERIFICATION SOLUTION
          LVC   LABORATORY CONTINUING
                CALIBRATION VERIFICATION
                           These values are identified as "Initial
                           Calibration Verification"  (ICV) on Form II
                           (Part 1).

                           These values are identified as "Continuing
                           Calibration Verification" (CCV) on Form II
                           (Part 1).
          LSO   LABORATORY SPIKED SAMPLE
                BACKGROUND (ORIGINAL)
                VALUES

          LSF   LABORATORY SPIKED SAMPLE-
                FINAL VALUES
                           These values are identified as "Sample Result
                           (SR)" on the "Spike Sample Recovery" Form of
                           hardcopy (Form V (Part 1)).

                           These are the "Spiked Sample Result (SSR)"
                           values on the "Spike Sample Recovery" Form of
                           hardcopy (Form V (Part 1)) .
          LDO
          LDF
LABORATORY DILUTED SAMPLE  These values are the "Initial Sample Result
BACKGROUND                 (I)" values on the "Serial Dilution" Form of
(ORIGINAL) VALUES          hardcopy (Form IX).
LABORATORY DILUTED
SAMPLE - FINAL VALUES
These are the "Serial Dilution Result(S)"
values on the "Serial Dilution" Form of
hardcopy (Form IX).
9/91
                                 H-ll
                                  ILM02.1

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                               SAMPLE QC CODES LISTING FOR TYPE 20
          QCC
Name
Definition
          MSO   STANDARD ADDITION
                RESULTS ORIGINAL VALUE
                         This value is identified as "0 ADD"
                         on "Standard Addition Results",  Form VIII.
          MSI   STANDARD ADDITION
                RESULTS FIRST
                ADDITION

          MS2   STANDARD ADDITION
                RESULTS SECOND
                ADDITION

          MS3   STANDARD ADDITION
                RESULTS THIRD
                ADDITION
                         This value is  identified as  "1  ADD"
                         on "Standard Addition Results",  Form VIII.
                         This  value  is  identified  as  "2  ADD"
                         on "Standard Addition Results",  Form VIII.
                         This  value  is  identified  as  "3  ADD"
                         on "Standard Addition Results",  Form  VIII.
          PDO   POST DIGESTION SPIKE
                BACKGROUND (ORIGINAL)
                VALUES
          PDF   POST DIGESTION
                SPIKE BACKGROUND
                (FINAL) VALUES
                         This value  is  identified  as  "Sample  Result"
                         (SR) on  the "Post  Digest  Spike  Sample
                         Recovery",  Form V  (Part 2),  or  GFAA  original
                         sample analysis.

                         This value  is  identified  as  "Spiked  Sample
                         Result"  (SSR)  on the  "Post Digest  Spike  Sample
                         Recovery",  Form V  (Part 2),  or  GFAA  post
                         digestion spiked sample analysis.
          LPC   CRDL STANDARD
          LII   LABORATORY INTERFERENCE
                CHECK-SOLUTION (INITIAL)
          LIF   LABORATORY INTERFERENCE
                CHECK SOLUTION (FINAL)
                         Laboratory Performance Check Solution for
                         ICP  (CRI) and Graphite Furnace  (CRA).

                         The  results of this solution analysis  are
                         reported on the  "Interference Check  Sample"
                         (ICS), Form IV.

                         The  results of this solution analysis  are
                         reported on the  "Interference Check  Sample"
                         (ICS), Form IV.
9/91
                              H-12
                   ILM02.1

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                          FORMAT OF THE SAMPLE HEADER RECORD (TYPE 21)
      MAXIMUM
      LENGTH

      2
      2
      3
      3
      6
      1
      14
      1
      2
      1
      2
      1
      2
      2
      2
      1
      2
      1
      2
      1
      9
      1
      8
      1
      2
      1
      5
      4
CONTENTS

RECORD TYPE
Delimiter
LEVEL
Delimiter
SAS NUMBER
Delimiter
LAB SAMPLE ID
Delimiter
PREPARATION YEAR
Delimiter
PREPARATION MONTH
Delimiter
PREPARATION DAY
Delimiter
YEAR RECEIVED
Delimiter
MONTH RECEIVED
Delimiter
DAY RECEIVED
Delimiter
COMPOUND SOURCE
Delimiter
INJECTION/ALIQUOT VOLUME
Delimiter
PREPARATION START HOUR
Delimiter
RECORD SEQUENCE NUMBER
CHECKSUM
FORMAT/CONTENTS

"?1"
II
"LOW"/"MED"
111
CHARACTER
I
CHARACTER
I
YY
I
MM
I
DD
II
YY
I
MM
I
DD
1
CHARACTER

NUMERIC!-

HH2
I
NUMERIC
CHARACTER
        This  is  the  portion of  the  sample  that  is  injected into  the  instrument excitation
         system for the purpose of measuring the absorbance, emission or concentration of
         an analyte.
         This  is  the  hour at which the  preparation  is  started.
         between different batches on  the same day.
                                           It  is used to differentiate
9/91
                            H-13
                                                                             ILM02.1

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                 FORMAT OF THE ASSOCIATED INJECTION AND COUNTER RECORD  (TYPE  22)
      MAXIMUM
      LENGTH         CONTENTS                               FORMAT/CONTENTS

      2              RECORD TYPE                            "22"
      10             Delimiter                              I I I I I I I I I I
      8              EXTRACT VOLUME                         NUMERIC1
      1              Delimiter                              |
      8              DILUTION FACTOR                        NUMERIC
      3              Delimiter                              |||
      5              PERCENT SOLIDS                         NUMERIC
      1              Delimiter                              |
      5              RECORD SEQUENCE NUMBER                 NUMERIC
      4              CHECKSUM                               CHARACTER
      1  This is the final volume of the digestion procedure that is currently reported on
         Form XIII  of  the hardcopy.


9/91                                             H-14                         ILM02.1

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                           FORMAT OF THE RESULTS DATA RECORD  (TYPE  30)
      MAXIMUM
      LENGTH

      2
      1
      1
      1
      9
      2
      5
      1
      3
      1
      10
      1
      1
      1
      10
      1
      1
      1
      10
      1
      2
      1
      10
      1
      10
      1
      1
      1
      10
      1
      1
      1
      10
      1
      1
      1
      10
      1
      1
      1
      10
      1
      5
      4
CONTENTS

RECORD TYPE
Delimiter
ANALYTE IDENTIFIER
Delimiter
ANALYTE CAS NUMBER
Delimiter
CONCENTRATION UNITS
Delimiter
CONCENTRATION QUALIFIER
Delimiter
CONCENTRATION
Delimiter
VALUE DESCRIPTOR
Delimiter
AMOUNT ADDED OR TRUE VALUE
Delimiter
QC VALUE DESCRIPTOR
Delimiter
QC VALUE
Delimiter
QC LIMIT QUALIFIER
Delimiter
QC LOWER LIMIT
Delimiter
QC UPPER LIMIT
Delimiter
IDL LABEL
Delimiter
IDL
Delimiter
RAW DATA AVERAGE QUALIFIER
Delimiter
RAW DATA AVERAGE
Delimiter
RAW DATA %RSD QUALIFIER
Delimiter
RAW DATA %RSD
Delimiter
RAW DATA "MSA-TREE" QUALIFIER
Delimiter
RAW DATA ANALYTICAL SPIKE %R
Delimiter
RECORD SEQUENCE NO.
CHECKSUM
FORMAT/CONTENTS

"30"
I

I
CHARACTER
II
"UG/L"/"MG/KG"

CHARACTER2
I
NUMERIC

11T / " F "
i
NUMERIC
I
NUMERIC

"N"/" *"/"+"/" E"^
I
NUMERIC
I
NUMERIC
1
"U" for undetected

NUMERIC6
NUMERIC
"M"/BLANK
I
NUMERIC
I
"E"/"W" /BLANK
NUMERIC
I
NUMERIC
CHARACTER
9/91
                            H-15
                  ILM02.1

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                       FORMAT OF THE RESULTS DATA RECORD (TYPE 30) FOOTNOTES
          "C" (CAS Registry Number) is used for all analytes except cyanide.   "I"  is used
          for cyanide .

          "BDL" means below detection limit.
          "NSQ" means there is not sufficient quantity to  analyze  sample  according to the
          protocol .
          "NAI" not analyzed due to interference,  "NAR"  no analysis result  required.
          Note that there is no absolute equivalent to the final concentration on  Form VIII
          in Standard EPA Format.
          "LTC" means less than the CRDL but  greater than  or equal to  the IDL.
          "FQC" means failed quality control  criteria.

          "GTL" means greater than the linear range.
          "RIN" means that the analysis result were not  used to  report data in the SDG.
          The results are reported from a later reanalysis of the  same sample  aliquot.

          "REX" means that the analysis result were not  used to  report data in the SDG.
          The results are reported from a later reanalysis of a  repreparation  of same
          sample .
          Note that,  except for "NAR",  none of these codes the Contractor from reporting a
          valid result.   They only explain why or  if the result  is qualified.
          "T" stands  for a true value  of the  solution.   This includes  the concentration of
          all (ICP as well) instrument calibration standards.  "F" stands for  an added
          concentration to a sample such as a pre  or post  digestion spike,  or  MSA
          additions .

          "P" equals  percent,  "C"  equals correlation coefficient,  and  "L" equals control
          limit.

          "N" equals  spiked sample recovery not within control limits,  "*"  equals  duplicate
          analysis not  within control  limits,  "+"  equals correlation coefficient for the
          MSA less than 0.995,  "E" equals the estimated  reported value because of  the
          presence of interference.   "S" flag is not applicable  for Standard EPA Format.

          The IDL  must  be a whole  number for  all analytes  except for mercury.   Mercury must
          be reported to one decimal place.

          "U" means less than the  IDL,  "B"  means less than the CRDL and greater than or
          equal to the  IDL,  "L" means  greater than the linear range.
9/91                                             H-16                        ILM02.1

-------
                       FORMAT FOR THE INSTRUMENTAL DATA READOUT (TYPE 31)
      MAXIMUM
       SNGTlr

      2
      1
      1
      1
      1
      2
      8
      1
      10
      2
      10
      2
      10
      2
      10
      2
      10
      1
      5
      4
CONTENTS

RECORD TYPE
Delimiter
TYPE OF DATA
Delimiter
TYPE OF VALUE
Delimiter
ANALYTE WAVELENGTH
Delimiter
FIRST INSTRUMENT VALUE
Delimiter
SECOND INSTRUMENT VALUE
Delimiter
THIRD INSTRUMENT VALUE
Delimiter
FOURTH INSTRUMENT VALUE
Delimiter
FIFTH INSTRUMENT VALUE
Delimiter
RECORD SEQUENCE NUMBER
CHECKSUM
FORMAT/CONTENTS

"31"

"W"1

CHARACTER2
II
NUMERIC (TO 2 DECIMAL PLACES)

1
NUMERIC3,4

11     3
NUMERIC3
II     3
NUMERIC3

11     3
NUMERIC3

11     *
NUMERIC3
I
NUMERIC
CHARACTER
         "W equals wavelength.

         "C" equals concentration in ug/L, "T" equals concentration in ug/250 ml, "F"
         equals concentration in ug/50 ml, "B" equals absorbance,  "I" equals intensity,
         "A" equals peak area in cm square, and "H" equals peak height in cm.

         This is used to report data for method analyses that require replicate  injections
         or exposures.  If a single instrument measurement is used, then enter it in the
         first instrument value field, and leave the other four fields empty.  If two
         instrument measurements are used, then enter them in the first and second
         instrument value fields in the order of their analyses, and leave the other three
         fields empty; etc.

         For MSA,  the  absorbances  for  the  zero,  first,  second and  third additions with EPA
         Sample Numbers XXXXXXO, XXXXXX1, XXXXXX2, XXXXXX3 are reported in this,  the first
         instrument value, field; and the final concentration obtained from the  MSA is
         entered in the "concentration" field on the type 30 record which corresponds  to
         the type 20 record that contains the EPA Sample Number XXXXXXO.
9/91
                            H-17
                                                                             ILM02.1

-------
                          FORKAT OF THE AUXILLIARY DATA RECORD (TYPE 32)
      MAXIMUM
      LENGTH         CONTENTS                               FORMAT/CONTENTS

      2              RECORD TYPE                            "32"
      10             Delimiter                              I  I I ! I I I ! 1 I
      2              INTEGRATION TIME CODE                  "IT"
      1              Delimiter                              |
      10             INTEGRATION TIME                       IN SECONDS
      4              Delimiter                              ||||
      5              RECORD SEQUENCE NUMBER                 NUMERIC
      4              CHECKSUM                               CHARACTER
9/91                                             H-18                        ILM02.1

-------
                             FORMAT OF THE PC LIMIT  RECORD  (TYPE  341
      MAXIMUM
      LENGTH          CONTENTS                               FORMAT/CONTENTS

      2               RECORD TYPE                            "34"
      4               Delimiter                              | | | |
      8               ANALYTE WAVELENGTH                     NUMERIC  (TO  2  DECIMAL PLACES)
      1               Delimiter                              |
      10              CRDL                                   NUMERIC
      1               Delimiter                              |
      10              LINEAR RANGE                           NUMERIC
      6               Delimiter                              I I I I I I
      5               RECORD SEQUENCE  NO.                     NUMERIC
      4               CHECKSUM                               CHARACTER
9/91                                             H-19                        ILM02.1

-------
                         FORMAT OF THE CORRECTION DATA RECORD (TYPE 35)
     MAXIMUM
     LENGTH
     1
     3
     1
     5
     4
     9
     1
     8
     1
     10
     1
     5
     4
CONTENTS

RECORD TYPE
Delimiter
TYPE OF CORRECTION
Delimiter
TYPE OF BACKGROUND
Delimiter
INTERFERING ANALYTE
Delimiter
ANALYTE WAVELENGTH
Delimiter
CORRECTION FACTOR
Delimiter
RECORD SEQUENCE NO.
CHECKSUM
FORMAT/CONTENTS
                                                           "35
"BS"/"BD"/"BZ"
Illl
CHARACTER
I
NUMERIC (TO 2 DECIMAL PLACES)
I
NUMERIC
I
NUMERIC
CHARACTER
     1   "ICP"  indicates interelement correction,  while
         correction.
                                    'BG"  indicates  a background
/91
                            H-20
                 ILM02.1

-------
                             FORMAT OF THE COMMENT RECORD (TYPE 90")
      MAXIMUM
      LENGTH         CONTENTS                               FORMAT/CONTENTS

      2               RECORD TYPE                            "90"
      1               Delimiter                              |
      67              ANY COMMENT                            CHARACTER
      1               Delimiter                              |
      5               RECORD SEQUENCE NUMBER                 NUMERIC
      4               CHECKSUM                               CHARACTER
9/91                                             H-21                         ILM02.1

-------
                      FORMAT OF THE SAMPLE ASSOCIATED DATA RECORD (TYPE 921
      MAXIMUM
      LENGTH         CONTENTS                               FORMAT/CONTENTS

      2              RECORD TYPE                            "92"
      1              Delimiter                              |
      9              COLOR BEFORE                           CHARACTER
      1              Delimiter                              |
      9              COLOR AFTER                            CHARACTER
      1              Delimiter                              |
      6              CLARITY BEFORE                         CHARACTER
      1              Delimiter                              |
      6              CLARITY AFTER                          CHARACTER
      1              Delimiter                              |
      6              TEXTURE                                CHARACTER
      1              Delimiter                              |
      3              ARTIFACTS                              "YES"/BLANK
      1              Delimiter                              |
      5              RECORD SEQUENCE NUMBER                 NUMERIC
      4              CHECKSUM                               CHARACTER
9/91                                             H-22                        ILM02.1

-------

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