540-8-90-502
USEPA CONTRACT LABORATORY PROGRAM
       STATEMENT OF WORK
             FOR
      INORGANICS ANALYSIS
          Multi-Media
      Multi-Concentration

    Document Number ILM01.0
      A _rf

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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
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                            GENERAL REQUIREMENTS
The Contractor shall employ procedures specified in this Statement of Work
(SOW) in the preparation and analysis of aqueous (water) 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.

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.

The samples to be analyzed by the Contractor are from known or suspected
hazardous waste 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 may also be used in litigation against Potentially Responsible
Parties in the enforcement of Superfund legislation.

Prior to accepting any samples from the Agency, the Contractor shall have,
in house, the appropriate standards for all target analytes listed in
Exhibit C.
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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 lower 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 paragraphs 2., 3. and 4.,
          following.  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;
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     and cyanide analysis.   The identification and quantitation of
     analytes other than cyanide shall be accomplished using the TCP or
     AA methods specified in Exhibit D, whichever method will achieve
     the Contract Required Detection Limit (CRDL) 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.,  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 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) 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  receipt
          through identification and quantitation produce reliable  data.
          The  Contractor must analyze the  LCS concurrently with  the analysis
          of the samples in the SDG.

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  SOW and  within the
     time specified in  the Contract  Performance/Delivery Schedule.

     1.    Use  of formats other than  those  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
          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 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  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
     perform  these  functions. The EPA reserves  the  right to review
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     personnel qualifications and experience.   See  Section III,  Detailed
     Technical & Management Requirements.
     1.    Laboratory  Supervisor
     2.    Quality Assurance Officer
     3.    Systems Manager
     4.    Programmer  Analyst
     5.    1CP 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 in a timely manner (within 7 days of the
     originator's request)  to requests from data  recipients for additional
     information or  explanations  that result from the Government's
     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 stored 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
     proc'ess 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 laboratory conditions that affect the timeliness of
     analyses and data  reporting.  In particular,  the Contractor shall
     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
     area over a finite time period,  and will include one or more field
     samples with associated blanks.   Samples may be shipped to the

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     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 Group(s).  A Sample Delivery Group  (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 (said period beginning with the receipt of
             the first sample in the Sample Delivery Group).

     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 a Sample Delivery Group  must be submitted
     together (in one package) in the order specified in Exhibit B.   The
     Sample Delivery Group 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  Sample Delivery
     Group  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 EPA
     sample number,  and accompanied by a Traffic  Report  form bearing the
     sample number and descriptive information regarding the sample.   EPA
     field sample 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 must also  follow  the instructions
     given on the Traffic Report  in choosing the  QC samples 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 3  calendar days
     following receipt of the  last sample in the  Sample  Delivery Group.
     Traffic Reports shall be  submitted in Sample Delivery  Group sets (i.e.,
     all  Traffic Reports for a Sample Delivery Group  shall  be  clipped
     together)  with an SDG Cover  Sheet containing information  regarding the
     Sample Delivery Group,  as specified in Exhibit B.

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.
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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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                           PERSONNEL REQUIREMENTS


I.    TECHNICAL CAPABILITY

     A.   Technical  Supervisory  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 discipline.

                   (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.

               b.   Qualifications:

                   (1)  Education:

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

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

              (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.    ICP  Spectroscopist Qualifications

          a.   Education:

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

              Specialized training in ICP Spectroscopy.
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     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.

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

          Minimum  of  six months experience  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

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              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.

     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.  Samples and
         standards  must be stored separately.
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D.
3.    Sample  Preparation Area
     Adequate,  contamination-free, well-ventilated  work space
     provided with:
     a.    Benches with  chemical resistant tops.
     b.    Exhaust hoods.  Note:  Standards 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.
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.    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 tropho tome ter
Atomic Absorption
Spec tropho 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
There are no Secondary Instrument Requirements 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 truraent ( s )
1
3
2
12 distillation
units + 1
photometer
Type of
Instrument
ICP Emission
Spec tropho tome ter
Atomic Absorption
Spec tropho 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
Secondary Instrument Requirements for 300 Samples/Month Capacity

     The Contractor shall have the following instruments in place
     and operational at any one 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  IBM  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.

                    Modem  capable of  at  least 2,400 baud  transmission speed
                    which  is  compatible  with  the  EPA  Telecommunications
                    Network.

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

                    Editing and updating databases.

                   QC of automated deliverables.

                    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.
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Project Manager

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

Sample Custodian

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

Quality Assurance Officer

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

Data Reporting and Delivery Officer

Responsible for all aspects of data deliverables:   organization,
packaging, copying, and delivery.
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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-15

SECTION IV:   Data Reporting Forms  	   B-42
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                                        SECTION I

                        CONTRACT REPORTS/DELIVERABLES  DISTRIBUTION

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.
                             No.
Delivery
Distribution
Item
A. Updated SOPs

B. Sample Traffic
Reports
**C. Sample Data
Package
D. Data in Computer
Readable Format
****£. Complete SDG File
*F. Quarterly/ Annual
Verification
of Instrument
Parameters
*****G . Qual ity
Assurance
Plan

Copies
2

1
2
1
1
2
copy

Schedule
45 days after
contract receipt
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
Submit copy
within 7 days
of written
request by APO
(D


X
X
X

X
A£

(2)
X




X

3 direct

(3)
X


X


X
:ed

Distribution:
(1)  Sample Management Office (SMO)
(2)  Region-Client
(3)  Environmental Monitoring Systems Laboratory (EMSL)
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      *     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 and not exceeding 20
            samples.  Data for all samples in the SDG are due concurrently.
            (See SOW Exhibit A, paragraph I., 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 N. Lee Street
     Alexandria,  VA  22313

(2)  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
     thr9ughout the period of the contract and identify other client
     recipients on a case-by-case basis.

(3)  USEPA Environmental Monitoring  Systems Laboratory  (EMSL)
     944 E. Harmon Avenue
     Las Vegas, NV  89109
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                                  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

     o   Legible,

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

     o   Arranged in the order specified in this Section,

     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 APO/TPO action, the
data must be clearly  marked as ADDITIONAL DATA and must be sent to all three
contractual data recipients (SMO,  EMSL,  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 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.

      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.
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A.   Updated SOPs

     The Contractor shall submit updated copies of all required Standard
     Operating Procedures (SOPs) that were submitted with the prebid
     Performance Evaluation sample results.   The updated SOPs must address
     any and all issues of laboratory performance and operation identified
     through the review of the Performance Evaluation sample data and the
     evaluation of Bidder-Supplied Documentation.

     The Contractor must supply SOPs for the following:

          1.    Sample  receipt  and logging.

          2.    Sample  storage.

          3.    Preventing sample contamination.

          4.    Security for  laboratory and samples.

          5.    Standards purity/preparation.

          6.    Maintaining instrument records and logbooks.

          7.    Sample  analysis and data  control  systems.

          8.    Glassware cleaning.

          9.    Technical and managerial  review  of laboratory  operation and
               data package  preparation.

          10.   Internal review of contractually-required  quality  assurance and
               quality control data for  each individual data  package.

          11.   Sample  analysis,  data handling and reporting.

          12.   Chain-of-custody procedures and  document control including  SDG
               file preparation

          13.   Sample  data validation/Self-inspection  system

               a.    Data flow  and chain-of-command for data 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
                    requirements  in Exhibits B and H

               e.    Procedures  to  assure that hardcopy deliverables are in
                    agreement  with  their comparable diskette deliverables
                                   B-5                                 ILM01.0

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         f.   Demonstration of internal QA inspection procedure
              (demonstrated by supervisory sign-off on personal
              notebooks, etc.)

         g.   Frequency and type of internal audits (e.g., random,
              quarterly, spot checks, perceived trouble areas)

         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.

     14.  Data Management and Handling

         a.   Procedures for controlling and estimating data entry
              errors.

         b.   Procedures for reviewing changes to data and deliverables
              and enduring 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.   Individual(s) responsible for system operation,
              maintenance, data integrity and security.

         g.   Specifications for staff training procedures.

Sample Traffic Reports

 Original Sample Traffic Report page marked "Lab Copy for Return to SMO"
 with lab receipt information and signed in 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
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      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 lowest sample number
      (considering both alpha and numeric designations);  the "last" sample
      received would be 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.

      EPA 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 alpha 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 with each SDG cover sheet.

C.    Sample Data Package

      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.

      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.
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     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 resolution.

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 must 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  micrograms 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 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 Form I 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 Linear Range Analysis  for ICP
               [FORM II (PART  2) - IN]


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     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]

     Quarterly Verification of Instrument Parameters

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

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

     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 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.
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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.

6)   Spikes (indicating standard solutions used, final spike
     concentrations,  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.

9)   Time and date of each analysis.  Instrument run logs can
     be submitted if they contain this information.  If the
     instrument does not automatically provide times of
     analysis, these must be manually entered  on all raw data
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                   for initial and continuing calibration verification and
                   blanks, as well as interference check samples and 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 to 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.

     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
          must also be submitted.

D.   Data in Computer  Readable  Form

      The Contractor  shall provide a computer-readable copy of the  data on
      data 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 Exhibit H,  Data Dictionary and Format for Data
      Deliverables in  Computer-Readable  Format.

      When submitted,  diskettes shall be packaged and shipped in such a
      manner that the  diskette(s)  cannot be bent or folded,  and will 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 diskette
      mailer.
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                                   Table 1

                           Codes  for  Labelling Data
      Sample                                                   XXXXXX
      Sample not part of the SDG                               ZZZZZZ
      Duplicate                                               XXXXXXD
      Matrix Spike                                            XXXXXXS
      Serial Dilution                                         XXXXXXL
      Analytical Spike                                        XXXXXXA
      Post Digestion/Distillation Spike                       XXXXXXA
      MSA:
        Zero Addition                                         XXXXXXO
        First Addition                                        XXXXXX1
        Second Addition                                       XXXXXX2
        Third Addition                                        XXXXXX3
      Instrument Calibration Standards:
        ICP                                S or SO for blank standard
        Atomic Absorption and Cyanide                 SO, S10,. . .etc.
        Initial Calibration Verification                          ICV
        Initial Calibration Blank                                 ICB
      Continuing Calibration Verification                         CCV
      Continuing Calibration Blank                                CCB
      Interference Check Samples:
        Solution A                                               ICSA
        Solution AB                                              ICSAB
      CRDL Standard for AA                                        CRA
      CRDL Standard for ICP                                       CRI
      Laboratory Control Samples:
        Aqueous  (Water)                                          LCSW
        Solid  (Soil/Sediment)                                    LCSS
      Preparation Blank (Water)                                    PBU
      Preparation Blank (Soil)                                    PBS
      Linear Range Analysis Standard                              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.
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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.
E.   Results  of Intercomparison/Performance  Evaluation  (PE)  Sample  Analyses

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

F.   Complete SPG File  (CSF)

     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 EMSL/LV.   The contents of the  CSF will be numbered  according
     to  the specifications described in Section  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 logbook maintained by the laboratory.  The CSF  will contain
     all original documents  specified in Section III  and IV,  and Form  DC-2 of
     Exhibit  B of the SOW.

     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.   Form DC-1

          b.   Other  receiving  forms or copies of receiving logbooks.
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          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.

     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 well as copies
          that are altered in any fashion, are also deliverables 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 Instrument  Parameters

     The Contractor  shall perform and report quarterly verification of
     instrument  detection limits  and  linear range  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 Forms  X, XIA, XIB,
     and XII.   Submission of  Quarterly/Annual Verification of  Instrument
     Parameters  shall include the raw data used to determine  those values
     reported.
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                                 SECTION III


                            FORM INSTRUCTION GUIDE


This section contains specific instructions for the completion of all
required Inorganic Data Reporting Forms.  This section is organized 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 -  IN]

     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 1)  -  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-15                                ILM01.0

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A.   General Information and Header Information

     The data reporting forms presented of 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 the Data
     Dictionary (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 filled out completely for all analytes before proceeding to the next
     form of the same type.  Multiple forms cannot be submitted 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
     ALL 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 more detailed
     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 must 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.

                                   B-16                                ILM01.0

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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.

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 samples.  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 Exhibit
B and Exhibit 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

                              B-17                                ILM01.0

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for that result, then zeros must be used for dec
specified number of reporting decimals for that
form. The following examples are provided:
Raw Data Result Specified Format
95.99653 5.4 (to four decimal places)
95.99653 5.3 (to three decimal places)
95.99653 5.2 (to two decimal places)
95.996 5.4 (to four decimal places)
95.9 5.4 (to four decimal places)
imal places to the
result for a specific
Correct Entry on Form
95.9965
95.997
96.00
95.9960
95.9000
     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 equals 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 "3/90" 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,  MA1111D, etc.
                                   B-18                                ILM01.0

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     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.

     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  SDG 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 Part 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 the 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).

     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.
                                   B-19                               ILM01.0

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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.

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  must 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).
    W   -    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 spectrophotometric.
         "AS" for  Semi-Automated Spectrophotometric
         "C"  for Manual Spectrophotometric
         "T"  for Titrimetric
         "  "  where no  data has  been entered.
         "Nil" if the analyte is not required to  be  analyzed.

A brief physical description of the sample, both before and after
digestion, must 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.
                              B-20                                ILM01.0

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     The  following descriptive terms are recommended:

           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)

     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


                                   B-21                               ILM01.0

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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.

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)	 xlOQ              (22)
                   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

                              B-22                                ILM01.0

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     all analytes  must be reported on the  first  Form IIA.   In a run where
     three CCVs  were analyzed,  the first CCV must  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 same form.   The third CCV must be reported in the
     left CCV column of the second Form IIA.   On the second Form IIA,  Che 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.

E.   CRDL Standard for AA and ICP [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      -.QQ    /o -^\
                       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      -^QQ       ,^ ^\
                     CRDL Standard for ICP True

                                   B-23                                ILM01.0

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Under "CRDL Standard for ICP  Final Found",  enter the value (in ug/L, to
two decimal places) of the concentration of each 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 100    ,2 5)
                      CRDL Standard for ICP  True

All %R values reported in equations 2.3,  2.4, and 2.5 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 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 IIB's 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 prodeeding to the next
wavelength.

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 the absolute
value of the analyte concentration is less than the CRDL but greater

                              B-24                                ILM01.0

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     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  detected  in 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 CCB's 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.

     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 must  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
     III'.s as explained in Part 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).

                                   B-25                                ILM01.0

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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 (to one decimal place) of the'
percent recovery computed for true solution AB greater than zero
according to the following equation:

    %R     =         Initial Found Solution AB     -,QQ          ,~ g-j
                         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       -,QQ          ,~ -,^
                         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

                              B-26                                ILM01.0

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and continuing to the following Form IVs as appropriate.  When multiple
wavelengths are used for one analyte, all the results of one wavelength
must be reported before prodeeding to the next wavelength,

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

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 Parts 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.

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 must 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  '  SR)	  x 100                (2.8)
                              SA

                              B-27                                ILM01.0

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%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 must be submitted for each
sample as appropriate.

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.

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 two
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.
                              B-28                                ILM01.0

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     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,  preceding.

     %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 IDL.

     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.

J-   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.

     For "% Solids for Sample," enter to 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 less than the CRDL or 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.

                                   B-29                                ILM01.0

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     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  =         * S  ' D *      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 must 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 must 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 "M",  enter method used as explained  in Part C.

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, complete 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, to  one decimal place) of
     the concentration of each  analyte  in the Aqueous LCS  Standard Source.
                                   B-30                                ILM01.0

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     Under "Aqueous Found",  enter Che 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 WQ                   (2 1Q)
                    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 ^                   (2 R)
                      Solid LCS True

     The  values for true and found aqueous and solid LCS's 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.

L.   Standard 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 VIII-IN.   Samples must be
                                   B-31                                ILM01.0

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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.

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.
                              B-32                                ILM01.0

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     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  y  x.v.   —  y x.  y v.
                            "  L   i"i      L xi  L Ji
              r	_	_	±_	—     (2.13)
     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  Dilution [FORM IX-IN]

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

     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 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.

     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)" 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:

                                   B-33                                ILM01.0

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       % Difference   =         ' T ' S '    x 10°                 (2.14)


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

     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).

     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.

     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".
                                   B-34                                ILM01.0

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     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.   Except for
     Mercury,  the  instrument detection limit must be rounded  to  a whole
     number.

     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 the 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 must 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.

     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
                                   B-35                                ILM01.0

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     zero.   If correction factors  are applied for more  than one additional
     analyte,  use  FORM XI(PART 2)-IN.

P.   ICP 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.

     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.
                                   B-36                                ILM01.0

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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, LCS's, PB's 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 Part 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.

     Note that the date never changes on 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.

     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.
                                   B-37                                ILM01.0

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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 standards,  ICVs,  CCVs, ICBs, CCBs, CRAs,  CRIs,  ICSs,  LRSs,
     LCSs,  PBs,  duplicates,  serial dilutions, pre-digestion spikes,  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 XIV must be organized  by  method, by run.   Later runs
     within a method must follow earlier  ones.   Each  analytical run  must
     start on a separate Form XIV. Therefore,  instrument calibration must  be
     the first entry on the form for  each new run.  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 Part  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.

     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

                                   B-38                                ILM01.0

-------
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 digestate 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 "Time", enter the time, (in military format - HHMM), 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.

Under "Analytes", enter "X" in the column of the designated analyte to
indicate that the analyte value was used from the reported analysis to
                              B-39                                ILM01.0

-------
     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 [Form 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., 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 the SMO and
      document the contact as  well as resolution  of the problem on a CLP

                                   B-40                                 ILM01.0

-------
      Communication Log.   Following resolution,  sign and date the forms as
      specified in the preceding paragraph and note, where appropriate, the
      resolution of the problem.

      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 and date the
      sample transfer block.

U.   Document 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 Section 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 "NA"  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-41                               ILM01.0

-------
     SECTION IV




DATA REPORTING FORMS
     B-42                                ILM01.0

-------
Lab Name:

Lab Code:

SOW 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 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.
Signature:

Date:
                             Name:

                            Title:
                                COVER PAGE - IN
                                                     3/90

-------
                               U.S. EPA - CLP
                                                            EPA  SAMPLE  NO.
Lab Name:



Lab Code:
                         INORGANIC ANALYSIS DATA SHEET
               Contract:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):



Level (low/med):




% Solids:
                           Lab Sample ID:




                           Date Received:
            Concentration Units (ug/L or mg/kg dry weight):
Color Before:



Color After:



Comments:
CAS No.
7429-90-5
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-70-2
7440-47-3
7440-48-4
7440-50-8
7439-89-6
7439-92-1
.7439-95-4
7439-96-5
7439-97-6
7440-02-0
7440-09-7
7782-49-2
7440-22-4
7440-23-5
7440-28-0
7440-62-2
7440-66-6


1
| Analyte
1
| Aluminum
[Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
(Iron
|Lead
[Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
(Zinc
| Cyanide
1
Concentration

























                                                            M
       Clarity Before:



       Clarity After:
                 Texture:



                 Artifacts:
                                  FOPJyi I  -  IN
                                              3/90

-------
                               U.S. EPA - CLP
                                     2A
               INITIAL AND CONTINUING CALIBRATION VERIFICATION
Lab Name:

Lab Code:
Case No.:
Initial Calibration Source:

Continuing Calibration Source:
Contract:

SAS No.:
SDG No.:
                          Concentration Units:  ug/L
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
|Lead
| Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
(Silver
| Sodium
[Thallium
| Vanadium
Zinc
Cyanide

Initial Calibration
True Found %R(1)











































































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










































































































	

















                                                                          M
(1)   Control Limits:  Mercury 80-120; Other Metals 90-110; Cyanide 85-115
                             FORM II (PART 1)  - IN
                                             3/90

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

Lab Code:
Case No.:
Contract:

SAS No.:
SDG No.:
AA CRDL Standard Source:

ICP CRDL Standard Source:
                          Concentration Units: ug/L
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
[Lead
[Magnesium
(Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
| Zinc
1
CRDL S
True
























tandard fo
Found
























r AA
%R
























                                             CRDL Standard for ICP
                                            Initial              Final
                                     True     Found    %R     Found    %R
                             FORM II (PART 2)  - IN
                                              3/90

-------
                               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):
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide

Initial
Calib.
Blank
(ug/L) C


















































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



























—







































































































—









~






Prepa-
ration
Blank C


















































M























—
                                 FORM III - IN
                                              3/90

-------
                               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
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
I Iron
|Lead
| Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
| Zinc
1
Ti
Sol.
A
























rue
Sol.
AB
























                                  Initial  Found
                              Sol.     Sol.
                                A        AB      %R
                                   Final Found
                               Sol.     Sol.
                                 A       AB
                             %R
                                  FORM  IV  -  IN
                                              3/90

-------
                               U.S. EPA - CLP
Lab Name:

Lab Code:
                                      5A
                             SPIKE SAMPLE RECOVERY
               Contract:
                                     EPA SAMPLE NO.
                                                            r
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
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
llron
[Lead
| Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
| Zinc
| Cyanide
1
Control
Limit
%R

























Spiked Sample
Result (SSR)

























c

























Sample
Result (SR)

























C

























Spike
Added (SA)

























%R

























Q

























M

























Comments:
                              FORM V (PART 1)  - IN
                                              3/90

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

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

























Spiked Sample
Result (SSR)

























                                        Sample
                                      Result (SR)  C
                                Spike
                              Added (SA)
                         %R
              M
Comments:
                              FORM V (PART 2)  - IN
                                              3/90

-------
Lab Name:




Lab Code:
                               U.S. EPA - CLP
                                  DUPLICATES
                                      Contract:
                                                             EPA  SAMPLE  NO.
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):
I
j Analyte
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
(Lead
(Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
| Zinc
| Cyanide
1
Control
Limit



















































Sample (S)

























C



















































Duplicate (D)

























Q



















































RPD


-
















































Q

























M

























                                  FORM VI - IN
                                              3/90

-------
Lab Name:

Lab Code:
                                U.S. EPA - CLP
                           LABORATORY CONTROL SAMPLE
Contract:

SAS No.:
Case No.:
SDG No.
Solid LCS Source:

Aqueous LCS Source:
Analyte
Aluminum_
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide
Aqueous (ug/L)
True Found %R































































1










Sol
True Found


















































                                                Solid  (mg/kg)
                                                     C        Limits
                                %R
                                   FORM VII - IN
                            3/90

-------
      U.S.  EPA - CLP
            8
STANDARD ADDITION  RESULTS
Lab Name
Lab Code
*
•
: Case No. :
Contract
SAS No . :
•
•
SDG
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.

-































r

































Q



—


—





















—


       FORM VIII - IN
3/90

-------
Lab Name:

Lab Code:
Case No.:
  U.S. EPA - CLP

          9
 ICP SERIAL DILUTIONS

	   Contract: 	

             SAS No.
                                                             EPA SAMPLE NO.
SDG No.:
Matrix (soil/water):
                              Level  (low/med):
                          Concentration Units:  ug/L
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
[Iron
ILead
1 Magnesium
[Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
(Vanadium
| Zinc
1

























Initial Sample
Result (I)
























C

















































Serial
Dilution
Result (S)
























C

















































%
Differ-
ence




1












































Q
























M
























                                  FORM IX - IN
                                              3/90

-------
                               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:
                                      SDG No.
Comments:
1
1
1
| Analyte
1
I Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
[Lead
| Magnesium
(Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
[Thallium
| Vanadium
| Zinc
Wave-
length
(ran)























Back-
ground























CRDL
(ug/L)
200
60
10
200
5
5
500O
10
50
25
100
3
5000
15
0.2
40
5000
5
10
5000
10
50
20
IDL
(ug/L)























                                                          M
                                  FORM X - IN
                                              3/90

-------
                                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
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
|Lead
| Magnesium
| Manganese
| Mercury
(Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
| Zinc
1
Wave-
length
(nm)

















































Ii
Al
























iterelement
Ca
























Correction
Fe
























Factors fo]
Mg

















































Comments:
                              FORM XI  (PART 1)  - IN
                                              3/90

-------
                               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.
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc

Wave-
length
(nm)

















































Ii
























iterelement
























Correction
























Factors fo:

-






















r:
























Comments:
                              FORM  XI  (PART 2)  - IN
                                              3/90

-------
                               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
| Analyte
1
| Aluminum
(Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
|Lead
| Magnesium
| Manganese
| Mercury
(Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
| Vanadium
| Zinc
1
Integ.
Time
(Sec.)
























Concentration
(ug/L)
























                                                       M
Comments:
                                  FORM  XII  -  IN
                                              3/90

-------
                                 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
                                                       3/90

-------
                               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

































Time

































% R

































Analytes
A
L

s
B

1






























































A
s

































B
A

































B
E

































1C
D

































c
A

































c
R

































c
o

































c
u

































F
E

































P
3

































M
/""*

































M
N

































H
G

































N
J.

































K

.































S
£

































A
G

































N
A

































T
L

































v

































z
N

































C
N









^






















                            FORM XIV - IN
                                              3/90

-------
                               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

































Time

































% R

































Analytes
A
L

































S
IB

































A
S

































IB
A

































B
E

































1C
D

































c
A

































c
R

































c
o

































c
|U

































F
E

































P
B

































|M
G

































M
N

































|H
G

































N
I

































K

.































S
E

































A
G

































IN
A

































T
|L

































IV
I

































|Z
N

































C
N
































1
                            FORM XIV - IN
                                              3/90

-------
SAMPLE LOG-IN SHEET
«
Lab Name: Pace of

Received By (Print Name): I^g-inDite:
Received By (Signature):

Case Number:
Sample Delivery
Group No.:
SAS Number:

REMARKS:
1. Custody Scal(s) Present/Absent*
Intact/Broken
2 Custody Seal Not:

3 . Ch»ini-of-Oistody Present/Absent*
Records
4. Traffic Reports or Present/ Absent"
Picking List
j 5. Aubill Aiibill/Stickcr
1 Present/Absent*
i 6. Aiibffl No.:

; 7. Sample Tags Present/Absent*
J S*mple Tag Listed/Not Listed
i Numbers oa Ch«in-of-
? Custody
T 8. Simple Condition: InUct/Brofccn*/
Leaking
9. Docs information oa
ccpocti, and simple

; 10- D»lc Received at L«b:

11. Time Received:

Sample Transfer


Arc* fr

T>u-
isy.
Oo:

EPA
SAMPLE
»


—






















CORRESPONDING
SAMPLE
TAG
*

























ASSIGNED
LAB
#


























REMARKS:
CONDITION
OF SAMPLE
SHIPMENT, ETC.





-



















* Contact SMO aftd attach record of rcsojotioa
Reviewed By:  ^_	
Dale:   	
Logbook  No.:   	
Logbook  Page  No:
                                                      PORMDC-1
                                                                                                          3/90

-------
                               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 VIII-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                               3/90

-------
                                                  Page  Nos .
23.
24.
25.
26.
27.
28.
29.
30.
31.
                                                 From
                                                    To
(Please Check:)
  Lab   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):
                                 (Print Name & Title)
     (Date)
          (Signature)
                                  (Print Name & Title)
     (Date)
                            Form DC-2 (continued)
                                                                    3/90

-------
          EXHIBIT C
INORGANIC TARGET ANALYTE LIST
                                                ILM01.0

-------
                       INORGANIC TARGET ANALYTE LIST (TAL)
          Analyte
Contract Required
  Detection Limit
      (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)   Subject  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 SOW Exhibit  D may be utilized  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
                           ILM01.0

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

(2)   The  CRDL 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
ILM01.0

-------
                                 EXHIBIT D
                             ANALYTICAL METHODS
                                                                  Page 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-6
     Part C - Microwave Digestion Method	    D-9
     Part D - Mercury and Cyanide Preparation	     D-16
SECTION IV  - SAMPLE ANALYSIS 	    D-17
     Part A - Inductively Coupled Plasma-Atomic
              Emission Spectrometric Method 	    D-18
     Part B - Atomic Absorption Methods,  Furnace Technique  ...    D-32
     Part C - Atomic Absorption Methods,  Flame Technique  ....    D-45
     Part D - Cold Vapor Methods for Mercury Analysis	    D-50
     Part E - Methods for Total Cyanide Analysis	    D-69
     Part F - Percent Solids Determination Procedure  	    D-98
     Part G - Alternate Methods (Catastrophic ICP Failure)  .  .  .    D-99
                                                                       ILM01.0

-------
                                  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  repo'rt the
 highest valid value for each analyte as  measured  from the undiluted  and
 diluted analyses.  Unless the  Contractor can submit proof that  dilution  was
 required to obtain valid results,  both diluted  and undiluted  sample
 measurements must be contained in the  raw data.   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                                ILM01.0

-------
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
take any pH adjustment action if the sample has not been properly
preserved.

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 run and for all Furnace AA measurements.  For 1CP
background correction requirements,  see  Exhibit D Section IV,  Part A,
paragraph 2.1.

Replicate Injections/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                                 ILM01.0

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                                  Figure  1
                       INORGANICS METHODS FLOW CHART
                         |   Field Sample   |
                         I	I
                                 I
                                .1.
                        Traffic Report or SMO
                         Specifies Parameters
                      Water
                      Matrix
|   Cyanide
|   Analysis
|   in Water
|Acid Digestion|
|  for Metals    j
|   Analysis    |
|   in Water    |
                 (Metal Anal.|
                 |  ICP/AAS   |
                  Soil/Sediment
                      Matrix
|Acid Digestion]
|   for Metals   |
|Analysis  in   |
|Soil/Sediment |
                   |Metals  Anal.
                   |  ICP/AAS
|%  Solids
|Determin-
I   ation
|Cyanide |
|Analysis|
|in Soil/I
I Sediment I
                         Data Reports
                                   D-3
                                                        ILM01.0

-------
                                 SECTION II

                    SAMPLE PRESERVATION AND HOLDING TIMES
     Sample Preservation
          Water  Sample  Preservation
         Measurement
           Parameter

         Metals(3)

         Cyanide,  total
            and  amenable
            to chlorination
          FOOTNOTES:
Container^ '

   P,G

   P,G
             (21
 Preservativev '

HN03 to pH <2

0.6g ascorbic acid(4)
NaOH to pH >12
Cool, maintain at 4°C(+2°C)
 until analysis
          (1)  Polyethylene  (P) or glass (G).
          (2)  Sample preservation is performed by the sampler immediately
              upon sample collection.
          (3)  Samples are filtered immediately on-site by the sampler
              before adding preservative for dissolved metals.
          (4)  Only used  in  the presence of  residual chlorine.

          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.
            Analyte


          Mercury
          Metals  (other than mercury)
          Cyanide
             No. of Days Following
                 Sample Receipt
                 by Contractor

                      26  days
                     180  days
                      12 days
                                    D-4
                                            ILM01.0

-------
                                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% H202  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) HCl 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".
                                   D-5                                 ILM01.0

-------
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:
                 Aluminum
                 Antimony
                 Arsenic
                 Barium
                 Beryllium
                 Cadmium
                 Calcium
              Summary of Method
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
              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).

              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 paper or equivalent
              Reagents

              (1)  ASTM Type II water (ASTM D1193) :
                   monitored.
                    Water  must  be
               (2)  Concentrated nitric acid (sp. gr.  1.41)

               (3)  Concentrated Hydrochloric Acid (sp. gr. 1.19)

                                   D-6
                                      ILM01.0

-------
     (4)  Hydrogen Peroxide  (30%)

e.   Sample Preservation and Handling

     Soil/sediment  (nonaqueous)  samples  must  be  refrigerated at
     4°C  (±2°)  from  receipt  until  analysis.

f.   Procedure

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

     (2)  Add 10 mL  of 1:1 nitric  acid (HN03), 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 HNOo,  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  (^C^) .  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% ^C^ 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% HoOo.)

     (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,  Mn,  Ni, K,  Ag,
         Na, Tl, V,  and  Zn, add 5 mL of 1:1  HC1 and 10 mL of Type
         II 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 II 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.
                          D-7                                 ILM01.0

-------
     (5b)  If the sample  is being prepared  for  the  furnace  analysis
          of As,  Be, Cd, Cr, Co, Cu, Fe, Pb, Mn, Ni, Se, Ag,  Tl,
          V,  and Zn, continue heating the  acid-peroxide  digestate
          until  the volume has been reduced to approximately  2 mL,
          add 10 raL 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 mixing) may  be
          centrifuged or allowed to settle by gravity overnight  to
          remove insoluble material.  The  diluted digestate
          solution contains approximately  2% (v/v) HNOo .   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
                                                 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

h.   Bibliography

     Modification (by committee) of Method 3050,  SW-846, 2nd  ed. ,
     Test  Methods for Evaluating Solid Waste.  EPA  Office of  Solid
     Waste and  Emergency Response, July 1982.
                          D-8                                ILM01.0

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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

2.     SUMMARY OF METHOD

      a.       Water Sample Preparation

              A representative 45 mL water sample is digested in 5 mL of
              concentrated Nitric acid in a Teflon  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 Sample Preparation

              A representative 0.5 g (wet weight) sample is digested in 10
              mL of concentrated Nitric acid in a Teflon  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.

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.
                                            D
      c.       The system must use PFA Teflon  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-9                                 ILM01.0

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      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).

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
              unit 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.

                                   D-10                               ILM01.0

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        The power available for heating is evaluated  so  that  the
        absolute power setting (watts) may be compared from one
        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 initial
        temperature of the water must 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 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:

                           (Co) (m) (DT)
Where:

P = 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),

C  = 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
                             D-ll                                ILM01.0

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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.

(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 HNO-j 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 sample 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 Sample Digestion Procedure
                                                            p
(1)   A 45 mL aliquot of the sample are measured into Teflon  digestion
      vessels using volumetric glassware.

(2)   5 mL of high purity concentrated HN02 is  added to the digestion
      vessels.

(3)   The weight of each vessel is recorded to  0.02 g.

(4)   The caps with the pressure release valves are placed on the vessels
      hand tight and then tightened, using constant torque, to 12 ft./lbs.
      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

                                   D-12                                ILM01.0

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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
        conditions.  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  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".
                             D-13                                ILM01.0

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b.        Soil Sample Digestion Procedure

(1)      Add a representative 0.5 +0.050 grams of sample to the              ^B
         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 vessel using
         TeflonR PFA tubing.

(5)      Weigh the vessel assembly to the nearest O.Olg.

(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 mL 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.
                             D-14                                ILM01.0

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(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 the 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 into the 50 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-15                               ILM01.0

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D.    MERCURY AND CYANIDE PREPARATION

      Refer to each specific method in this Exhibit for mercury and cyanide       ^B
      preparations.
                                   D-16                                ILM01.0

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                        SECTION IV


                      SAMPLE ANALYSIS



                                                          .Page No.

PART A - INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION
         SPECTROMETRIC METHOD                                D-18

PART B - ATOMIC ABSORPTION METHODS, FURNACE TECHNIQUE        D-32

PART C - ATOMIC ABSORPTION METHODS, FLAME TECHNIQUE          D-45

PART D - COLD VAPOR METHODS FOR MERCURY ANALYSIS             D-50

PART E - METHODS FOR CYANIDE ANALYSIS                        D-69

PART F - PERCENT SOLIDS DETERMINATION PROCEDURE              D-98

PART G - ALTERNATE METHODS (CATASTROPHIC ICP FAILURE)     "   D-99
                         D-I7                                ILM01.0

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  PART A  -  INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROMETRIC METHOD4"


                             Method 200.7 CLP-M*
       INDUCTIVELY  COUPLED PLASMA-ATOMIC EMISSION SPECTROMETRIC METHOD
                FOR TRACE ELEMENT ANALYSIS  OF WATER AND WASTES
1.     Scope and Application

1.1   Dissolved elements are determined in filtered and 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 are 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

2.1   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 (ICP).   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
 A bibliography citing method references appears in paragraph 11 of the
 method.

~k
 CLP-M modified for the Contract Laboratory Program.

                                   D-18                                ILM01.0

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      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
      correction is not required in cases of line broadening where a
      background correction measurement would actually degrade the 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.     Definitions

3.1   Dissolved -- Those elements which will pass through a 0.45 um membrane
      filter.

3.2   Suspended -- Those elements which are retained by a 0.45 um membrane
      filter.

3.3   Total -- The concentration determined on an unfiltered sample following
      vigorous digestion.

3.4   Instrumental detection limits -- See Exhibit E.

3.5   Sensitivity -- The slope of the analytical  curve, i.e.  functional
      relationship between emission intensity and concentration.

3.6   Instrument check standard -- A multi-element standard of known
      concentrations prepared by the analyst to monitor and verify instrument
      performance on a daily basis.  (See 7.6.1.)

3.7   Interference check sample -- A solution containing both interfering and
      analyte elements of known concentration that can be used to verify
      background and interelement correction factors.  (See 7.6.2.)

3.8   Quality control sample -- A solution obtained from an outside source
      having known concentration values to be used to verify the calibration
      standards.  (See 7.6.3.)

3.9   Calibration standards -- A series of known  standard solutions used by
      the analyst for calibration of the instrument  (i.e., preparation of the
      analytical curve).  (See 7.4.)

3.10  Linear dynamic range -- The concentration range over which the
      analytical curve remains linear as determined  in Exhibit E.

3.11  Reagent blank -- A volume of deionized, distilled water containing the
      same acid matrix as the calibration standards  carried through the entire
      analytical scheme.  (See 7.5.2.)

3.12  Calibration blank -- A volume of deionized,  distilled water acidified
      with HN03 and HC1.  (See 7.5.1.)
                                   D-19                               ILM01.0

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3.13  Method of standard addition -- The standard addition technique involves
      the use of the unknown and the unknown-plus-a-known amount of standard
      by adding known amounts of standard to one or more aliquots of the
      processed sample solution.

4.    Safety

4.1   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 5s 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.

5.    Interferences

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

      5.1.1    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.

               Listed 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
                        «U^U
               Laboratory   ,  is  expressed as analyte  concentration equivalents
               (i.e., false analyte  concentrations) arising from  100 mg/L  of
               the interferent element.
  .
  Ames Laboratory, USDOE, Iowa State University, Ames, Iowa 50011.

                                   D-20                                ILM01.0

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        The suggested use of this information is as follows:  Assume
        that arsenic (at 193.696 nm) 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.  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 forr each individual
        system.  Only those interferents listed were investigated and
        the blank spaces in Table 2 indicate 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 to 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 nm wavelength
        interferes with the listed potassium line at 766.491 nm.

5.1.2   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.

5.1.3   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.
                             D-21                                ILM01.0

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5.2  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 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.

6.    Apparatus

6.1   Inductively Coupled Plasma-Atomic  Emission Spectrometer.

      6.1.1    Computer controlled atomic emission  spectrometer with
               background correction.

      6.1.2    Radio  frequency  generator.

      6.1.3    Argon  gas supply, welding grade or better.

6.2   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 instrument 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.

7.    Reagents and Standards

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

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

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

      7.1.3    Hydrochloric  acid,  (1+1):  Add 500 mL cone.   HC1  (sp gr  1.19)
               to  400 mL deionized, distilled water and dilute to  1 liter.
                                   D-22                                ILM01.0

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

      7.1.5   Nitric acid, (1+1):  Add 500 mL cone.  HN03 (sp gr 1.41) to 400
              mL deionized, distilled water and dilute to 1 liter.

7.2   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 Specif icatr.on D 1193.

7.3   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.

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

      7.3.1   Aluminum solution, stock, 1 mL = 100 ug Al:  Dissolved  0.100 g
              of aluminum metal  in an acid mixture of 4 mL of (1+1)' HCl and 1
              mL of cone.  HNO-j  in a beaker.  Warm gently to effect solution.
              When solution is complete, transfer quantitatively to a liter
              flask, add an additional 10 mL of (1+1) HCl and dilute  to 1000
              mL with deionized, distilled water.

      7.3.2   Antimony solution  stock, 1 mL = 100 ug Sb:  Dissolve 0.2669 g
              K(SbO)C4H406 in deionized distilled water, add 10 mL  (1+1) HCl
              and dilute to 1000 mL with deionized, distilled water.

      7.3.3   Arsenic solution,  stock, 1 mL = 100 ug As:  Dissolve 0.1320 g
              of As20^ in 100 mL of deionized, distilled water containing 0.4
              g NaOH.  Acidify the solution with 2 mL cone.   HNO-i and dilute
              to 1,000 mL with deionized, distilled water.

      7.3.4   Barium solution, stock, 1 mL = 100 ug Ba:  Dissolve 0.1516 g
              BaCl2 (dried at 250°C for 2 hrs) in 10 mL deionized, distilled
              water with 1 mL (1+1) HCl.  Add 10.0 mL (1+1) HCl and dilute to
              1,000 mL with deionized, distilled water.

      7.3.5   Beryllium solution, stock, 1 mL =• 100 ug Be:   Do not dry.
              Dissolve 1.966 g BeSO^^^O, in deionized, distilled water, add
              10.0 mL cone. HNO-j and dilute to 1,000 mL with deionized,
              distilled water.

      7.3.6   Boron solution, stock, 1 mL = 100 ug B:  Do not dry.  Dissolve
              0.5716 g anhydrous ^BOo 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.
                                   D-23                                 ILM01.0

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

7.3.8   Calcium solution, stock, 1 mL = 100 ug Ca:  Suspend 0.2498 g
        CaCOo 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.

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

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

7.3.11  Copper solution, stock, 1 mL - 100 ug Cu:  Dissolve 0.1252 g
        CuO in a minimum amount of (1+1) HN03.   Add 10.0 mL cone.  HN03
        and dilute to 1,000 mL with deionized,  distilled water.

7.3.12  Iron solution, stock, 1 mL = 100 ug Fe:  Dissolve 0.1430 g
        Fe203 in a warm mixture of 20 mL (1+1)  HCl 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.

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

7.3.14  Magnesium solution, stock, 1 mL = 100 ug Mg:  Dissolve 0.1658 g
        MgO in a minimum amount of (1+1) HNCK.   Add 10.0 mL cone.  HNOn
        and dilute to 1,000 mL with deionized,  distilled water.

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

7.3.16  Molybdenum solution, stock, 1 mL = 100 ug Mo:  Dissolve 0.2043
        g  (NH^)2Mo04  in deionized, distilled water and dilute to 1,000
        mL.

7.3.17  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.
                             D-24                                ILM01.0

-------
      7.3.18  Potassium solution, stock, 1 mL = 100 ug K:  Dissolve 0.1907 g
              KC1, dried at 110°C, in deionized, distilled water.  Dilute to
              1,000 mL.

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

      7.3.20  Silica solution, stock, 1 mL - 100 ug Si02:  Do not dry.
              Dissolve 0.4730 g Na2Si03'9H20 in deionized, distilled water.
              Add 10.0 mL cone.  HNOo and dilute to 1,000 mL with deionized,
              distilled water.

      7.3.21  Silver solution, stock, 1 mL = 100 ug Ag:  Dissolve 0.1575 g
              AgNO-j in 100 mL of deionized, distilled water and  10 mL cone.
              HN03.  Dilute to 1,000 mL with deionized, distilled water.

      7.3.22  Sodium solution, stock, 1 mL = 100 ug Na:  Dissolve 0.2542 g
              NaCl in deionized, distilled water.  Add 10.0 mL cone.  HN03
              and dilute to 1,000 mL with deionized, distilled water.

      7.3.23  Thallium solution, stock, 1 mL = 100 ug Tl:  Dissolve 0.1303 g
              T1N03 in deionized, distilled water.  Add
              10.0 mL cone.  HNOj and dilute to 1,000 mL with deionized,
              distilled water.

      7.3.24  Vanadium solution, stock, 1 mL = 100 ug V:  Dissolve 0.2297
              NH/VOo in a minimum amount of cone.  HNO-j.  Heat to increase
              rate of dissolution.  Add 10.0 mL cone.  HNO-j and  dilute to
              1,000 mL with deionized,  distilled water.
      7.3.25  Zinc solution, stock, 1 mL = 100 ug Zn:  Dissolve 0.1245 g ZnO
              in a minimum amount of dilute HNOo.  Add 10.0 mL cone. HNOn an
              dilute to 1,000 mL with deionized, distilled water.
7.4   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 when preparing the mixed standards that the
      elements are compatible and stable.  Transfer the mixed standard
      solutions to a FEP fluorocarbon or unused polyethylene bottle for
      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.

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

                                   D-25                                ILM01.0

-------
      7.4.2   Mixed standard solution II -- Barium, copper, iron, vanadium,
              and cobalt.                                                         ^m

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

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

      7.4.5   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.

7.5   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.

      7.5.1   The calibration blank is prepared by diluting 2 mL of  (1+1)         ^|
              HN03 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.

      7.5.2   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.

7.6   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.

      7.6.1   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.)

      7.6.2   The interference check sample is prepared by the analyst, or
              obtained from EPA if available  (Exhibit E).
                                   D-26                                ILM01.0

-------
      7.6.3   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.)

8.     Procedure

8.1   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.

8.2   Initiate appropriate  operating configuration of computer.

8.3   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.)

8.4   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.

8.5   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.

9.     Calculation

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

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

9.3   Units must be clearly specified.

10.   Quality Control (Instrumental)

10.1  Quality control must  be performed as  specified in Exhibit E.

11-  Bibliography

     1.  Winge,  R.K., V.J. Peterson, and V.A. Fassel,  "Inductively  Coupled
         Plasma-Atomic Emission Spectroscopy  Prominent  Lines," EPA-600/4-79-
         017.
                                   D-27                               ILM01.0

-------
2.   Winefordner, J.D.,  "Trace Analysis:  Spectroscopic Methods for
     Elements,"  Chemical Analysis, Vol. 46, pp. 41-42.

3.   Handbook  for Analytical Quality Control in Water and Uastewater
     Laboratories,  EPA-600/4-79-019.

4.   Garbarino,  J.R.  and Taylor, U.S.,  "An Inductively-Coupled Plasma
     Atomic  Emission  Spectrometric Method for Routine Water Quality
     Testing," Applied  Spectroscopy 33, No. 3(1979).

5.   "Methods  for Chemical Analysis of  Water and Wastes," EPA-600/4-79-
     020.

6.   Annual  Book of ASTM Standards, Part 31.

7.   "Carcinogens - Working With Carcinogens," Department of Health,
     Education,  and Welfare, Public Health Service, Center for Disease
     Control,  National  Institute for Occupational Safety and Health,
     Publication No.  77-206, Aug. 1977.

8.   "OSHA Safety and Health Standards, General Industry," (29 CFR 1910),
     Occupational Safety and Health Administration, OSHA 2206, (Revised,
     January 1976).

9.   "Safety in  Academic Chemistry Laboratories, American Chemical
     Society Publications, Committee on Chemical Safety, 3rd Edition,
     1979.

10.   "Inductively Coupled Plasma-Atomic Emission Spectrometric Method of
     Trace Elements Analysis of Water and Waste", Method 200.7 modified
     by CLP  Inorganic Data/Protocol Review Committee; original method by
     Theodore  D. Martin, EMSL/Cincinnati.
                              D-28                                ILM01.0

-------
               TABLE 1  -  RECOMMENDED WAVELENGTHS(2)  AND ESTIMATED
                         INSTRUMENTAL DETECTION LIMITS
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
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  may
     vary  as  the sample matrix varies.

(3)   Highly dependent on operating conditions and plasma  position.
                                    D-29                               ILM01.0

-------







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-------
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
I
1
1
10
1
1
1
1
1
1
10
10
10
10
10
10
1
10
1
10
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Ca
Cr
Cu
Fe
Mg
Mn
Ni
Ti
V













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













                              D-31                                ILM01.0

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           PART B -  ATOMIC ABSORPTION METHODS.  FURNACE TECHNIQUE"*"
      Analyte/Method                                         Page No.

      Antimony - Method 204.2 CLP-M*                           D-33
      Arsenic - Method 206.2 CLP-M                             D-34
      Beryllium - Method 210.2 CLP-M                           D-36
      Cadmium - Method 213.2 CLP-M                             D-37
      Chromium - Method 218.2 CLP-M                            D-38
      Lead - Method 239.2 CLP-M                                D-39
      Selenium - Method 270.2 CLP-M                            D-41
      Silver - Method 272.2 CLP-M                              D-43
      Thallium - Method 279.2 CLP-M                            D-44
+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-32                               ILM01.0

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                                  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.

Instrument Parameters (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 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, 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
     sett-ings.

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-33                               ILM01.0

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                                  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,  As20o
     (analytical reagent grade)  in 100 mL of deionized distilled water
     containing 4 g NaOH.   Acidify the solution with 20 mL cone. HNO-, 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(NO-j)2' 6^0 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. HNO-i,  2
     mL of 30% 1^02 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.
Instrument Parameters (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
     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.

     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.
 CLP-M modified for the Contract Laboratory Program.
                                   D-34                                ILM01.0

-------
For every sample analyzed, verification is necessary to determine that
method of standard addition is not required (see Exhibit E).
If method of standard addition is required, follow the procedure given
in Exhibit E).
The use of the Electrodeless Discharge Lamps (EDL) for the light source
is recommended.
                              D-35                                ILM01.0

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                                 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,  BeSO/,  in
     deionized distilled water  containing 2 mL concentrated nitric acid and
     dilute to 1 Liter.  1 inL =  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  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 @ 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
     ins trument manufac tur e r.

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 Program.
                                   D-36                                ILM01.0

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                                   CADMIUM

         Method 213.2 CLP-M   (Atomic Absorption, Furnace Technique)
Optimum Concentration Ranp,e :   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 CdSO^'  8
     t^O (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,  (NH^)2HPO^ (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.

Instrument Parameters  (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-37                               ILM01.0

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                                  CHROMIUM

         Method 218.2 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 Part C methods,  AA Flame
     Technique.

2.   Calcium Nitrate  solution:   Dissolve 11.8  grams  of calcium nitrate,
     Ca(NOo)2'4^0 (analytical  reagent grade)  in deionized 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% H202 and 1 mL of the calcium nitrate  solution.

Instrument 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 @ 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  mg/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-38                               ILM01.0

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                                    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,  PbCNO-j^
     (analytical reagent grade), and dissolve in deionized distilled water.
     When solution is complete,  acidify with 10 mL redistilled  HNC^ and
     dilute to 1 Liter with deionized distilled water.  1 mL = 1 mg Pb
     (lOOOmg/L).
2.   Lanthanum Nitrate solution:  Dissolve 58.64 g of ACS reagent grade
     La2Cs in 100 mL cone.  HNOo  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
     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 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.

Instrument Parameters (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.
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.
 CLP-M modified for the Contract Laboratory Program.

                                   D-39                               ILM01.0

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3.    Greater sensitivity can be  acheived  using  the  217.0  run 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 ppm)  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-40                                ILM01.0

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                                  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% t^SeOn) 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
     Ni(NOo)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 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.

Instrument 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 nm
6.   Other operating parameters should be set as specified by the particular
     ins trument manufac tur er.
Notes
     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.

     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).   If conditions
 CLP-M modified for the Contract Laboratory Program.
                                                                      ILM01.0

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     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.    Selenium 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-42                                ILM01.0

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                                   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 1.575 g of AgNOo  (analytical reagent grade)
     in deionized distilled water.  Add 10 mL of concentrated HNOo  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 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 @ 400°C.
3.   Atomizing Time and Temp:  10 sec @ 2700°C.
4.   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 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.   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-43                                ILM01.0

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                                  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,  TINO^  (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.

Instrument Parameters (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  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.
 CLP-M modified for the Contract Laboratory Program.
                                   D-44                               ILM01.0

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            PART C - ATOMIC ABSORPTION METHODS. FLAME TECHNIQUE"1"
      Analyte/Method                                          Page No.

      Calcium - Method 215.1 CLP-M*                            D-46
      Magnesium - Method 242.1 CLP-M                           D-47
      Potassium - Method 238.1 CLP-M                           D-48
      Sodium - Method 273.1 CLP-M                              D-49
 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-45                               ILM01.0

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                                   CALCIUM
                            "ft
          Method 215.1 CLP-M  (Atomic Absorption,  Flame Technique)

Optimum Concentration Range:  0.2-7 mg/L using a wavelength of 422.7 run
Sensitivity:  0.08 mg/L
Detection Limit:  0.01 mg/L
Preparation of Standard Solution

1.   Stock Solution:   Suspend 1.250 g of CaCOo (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 La20o,  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  LaClo = 22
     mL.
Instrumental Parameters (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 inteferences.   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]).
               1
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-46                               ILM01.0

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                                 MAGNESIUM

          Method 242.1 CLP-M* (Atomic Absorption,  Flame Technique)

Optimum Concentration Range:  0.02-0.5 mg/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 HNO-j  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 l^^®^,  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 LaClo = 22
     mL.
Instrumental Parameters (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-47                               ILM01.0

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                                 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 rcg/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 time 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 either  directly  or  after
     processing.

Instrumental Parameters (General)
1.   Potassium hollow cathode lamp
2.   Wavelength:  766.5 nm
3.   Fuel:  Acetylene
4.   Oxidant:  Air
5.   Type of flame:  Slightly oxidizing
Notes
     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 10.  Any enhancement due to sodium can  be stabilized by
     adding excess sodium (1000 ug/mL) to both sample and standard
     solutions. If more stringent control of ionization is required,  the
     addition of cesium should be considered.   Reagent  blanks must be
     analyzed to correct for potassium impurities  in the buffer  zone.
     The 404.4 nm line may also be used.   This line has a relative
     sensitivity of 500.
     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-48                                ILM01.0

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                                   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 mg/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 time 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 either directly or after
     processing.
Instrumental Parameters (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-49                               ILM01.0

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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-50
Method 245.1 CLP-M*

Mercury Analysis in Water by Automated Cold Vapor Technique         D-58
Method 245.2 CLP-M

Mercury Analysis in Soil/Sediment by Manual Cold Vapor Technique    D-64
Method 245.5 CLP-M
 A bibliography citing method references follows each method.

JL.
 CLP-M modified for the Contract Laboratory Program.

                                   D-50                                ILM01.0

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          MERCURY ANALYSIS IN WATER BY MANUAL COLD 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.     Summary of Method

2.1   The flameless AA procedure is a physical method based on the
      absorption of radiation at 253.7 nm 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).
1CLP-M modified for the Contract Laboratory Program.

                                   D-51                                ILM01.0

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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.                                                ^B

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:  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 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.
                                   D-52                                ILM01.0

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5.8   Drying Tube:  6" X 3/4" diameter tube containing 20 g of magnesium
      perchlorate (see Noce 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 60U' bulb na" 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.

      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 i~eagent 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 hydroxylamine 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.
                                   D-53                                ILM01.0

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         Figure 1.  Apparatus for Flameless Mercury Determination
                      ABSORPTION
                         CELL
SAMPLE SOLUTION
IN BOD BOTTLE
SCRUBBER
CONTAINING
A MERCURY
ABSORBING
MEDIA
                             D-54
        ILM01.0

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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 KMnO/ (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 che bottle to the aeration apparatus forming a
      closed system.  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 (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 M KMnO^,  and 10% F^SO^  or
      b) 0.25% iodine in a 3% a KI solution.   A specially treated charcoal
      that will adsorb mercury vapor is available.
                                   D-55                               ILM01.0

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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  KMnO/ 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

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-56                                ILM01.0

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Bibliography

1.    Kopp,  J.F.,  Longbottoin,  M.C.  and Lobring,  L.B.  "Cold Vapor  Method for
     Determining Mercury",  AWWA, vol.  64,  p.  20,  Jan.  1972.

2.    Annual Book of ASTM Standards,  Part 31,  "Water",  Standard D3223-73,  p.
     343  (1976).

3.    Standard Methods  for the Examination of  Water and Wastewater  14th
     Edition,  p.  156 (1975).
                                  D-57                                ILM01.0

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        MERCURY  ANALYSIS  IN ..WATER  BY  AUTOMATED  COLD VAPOR TECHNIQUE

                                   MERCURY
            Method 245.2 CI.P-M* (Automated Cold Vapor Technique)


1.     Scope and Application

1.1   The working range is 0.2 to  20.0 ug Hg/L.

2.     Summary of Method

2.1   The flameless AA procedure is a physical method based on the
      absorption of radiation at 253.7 nm 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 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.     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.     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.
'CLP-M modified for the Contract Laboratory Program.

                                   D-58                                ILM01.0

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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.

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:  Westinghouse 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 acid, 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:  Dilute 5 mL of concentrated
              nitric acid  to 1  liter with distilled water.
                                   D-59                               ILM01.0

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6.3   Stannous Sulfate (Sec Note 3):   Add 50 g stannous 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.

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.

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
      persulfate 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 0.2 to 20.0 ug Hg/L in sampler
      and start sampling.  Complete  loading of sample tray with  unknown
      samples.
                                   D-60                               ILM01.0

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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 t^SO^ line in
      distilled water to wash out system.  After flushing,  wash out the
      H^SO,  line.   Also flush the coils in the high temperature heating
      bath by pumping stannous sulfate (6.3) through the sample lines
      followed by distilled water.  This will prevent build-up of oxides of
      manganese.

      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.

Bibliography

1.   Wallace R.A.,  Fulkerson, W. ,  Shults, W.D.,  and Lyon, W.S.,  "Mercury in
     the Environment-The Human Element", Oak Ridge National Laboratory,
     ORNL/NSF-EP-1 p. 31,  (January,  1971).

2.   Hatch,  W.R.  and Ott,  W.L., "Determination of Sub-Microgram Quantities
     of Mercury by Atomic Absorption Specrophotometry".   Anal.  Chem. 40,
     2085 (1968).

3.   Brandenberger,  H. and Bader,  H.,  "The Determination of Nanogram Levels
     of Mercury in Solution by a Flameless Atomic Absorption Technique",
     Atomic Absorption Newsletter 6, 101 (1967).

4.   Brandenberger,  H. and Bader,  H.,  "The Determination of Mercury by
     Flameless Atomic Absorption II, A Static Vapor Method", Atomic
    A&sorption Newsletter 7,53 (1968).

5.   Goulden, P.O.  and Afghan,  B.K.  "An Automated Method for Determining
     Mercury in Water",  Technicon, Adv.  in Auto.  Analy.  2,  p.  317 (1970).

6.   "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.

7.   Op.  cit.  (#1),  Methods 245.1  or 245.2.
                                   D-61                                ILM01.0

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AIR  AND
SOLUTION
                               7/25 T
O.7 Cm 10
                O.4 cm ID
                                              AIR
                                              OUT
                                                         Kcm
                                                 SOLUTION
                                                   OUT
             Figure 1.  Vapor liquid separator
                           D-62
                                                           ILM01.0

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Figure 2.  Mercury Manifold AA-1
              D-63
ILM01.0

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      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

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.     Summary of 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 ('.2)

3.     Sample Handling and Preservation

3.1   Because of the extreme sensitivity of the  analytical procedure and
      the onmipresence 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 mercury contamination

3.2   Refrigerate solid samples at 4°C (±2°) upon receipt until analysis
      (see Exhibit D, Section II).

3.3   The t=mple should be analyzed without drying.   A separate percent
      soli:s 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 thisoccurs,  the
      recovery of organic mercury will be low.   The problem can be
      eliminated by reducing the weight of the original sample or by
^CLP-M modified for the Contract Laboratory Program.

                                   D-64                                ILM01.0

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      increasing the amount of potassium persulfate (and consequently
      stannous chloride) used in the digestion.

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 system.)

5.6   Flowmeter:  Capable of measuring an air flow of 1 liter per minute

5.7   Aeration Tubing:  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 60W 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-65                                ILM01.0

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6.     Reagents

6.1   Sulfuric acid,  cone.:   Reagent  grade  of  low mercury content

6.2   Nitric acid,  cone.:   Reagent grade  of low  mercury content

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.  t^SO/  (6.1) and 2.5 mL of
      cone.   HNO-j (6.2)  and heat 2 minutes  in  a  water  bath at 95°C.   Allow
      the sample to cool and add 50 mL distilled water,  15 mL of KMnO/
      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 ahsorbance,  as exhibited either on the
      spectrophotometer or  the recorder,  will  increase and reach maximum

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      within 30 seconds.   As soon as the recorder pen levels off,
      approximately 1 minuLe,  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 SOD
      bottle and continue the aeration.  Proceed with the standards and
      construct a standard curve by plotting peak height versus micrograms
      of mercury

      NOTE 4:     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 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.  ^SO/  and 2 mL of cone.  HNOo
      are added to the 0.2 g of sample.  5 mL of saturated KMnO^ 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
          ug  g/g - wt Of Che  aliquot in gms
                    (based upon dry wt of the sample)
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9.3   Report mercury concentrations  as  described for  aqueous mercury
      samples converted to units of  rag/kg.   The  sample  result or the
      detection limit for each sample must  be  corrected for sample weight
      and % solids before reporting.

Bibliography

1.    Bishop,  J.   N.,  "Mercury in Sediments", Ontario  Water  Resources Comm.,
     Toronto,  Ontario,  Canada,  1971

2.    Salma,  M.,  private communication,  EPA  Cal/Nev.   Basin  Office,  Almeda,
     California

3.    "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

4.    Op.   cit.   (#3), Methods 245.1 or  245.2
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                    PART E -  METHODS  FOR CYANIDE ANALYSIS
Method                                                             Page No.

Method for Total Cyanide Analysis in Water"1"
Method 335.2 CLP-M                                                 D-70

Method for Total Cyanide Analysis in Soil/Sediment+
Method 335.2 CLP-M                                                 D-79

Method for Total Cyanide Analysis by Midi Distillation
Method 335.2 CLP-M                                                 D-91
 A bibliography citing method references follows the method.

 CLP-M Modified for the Contract Laboratory Program.

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                 METHOD FOR TOTAL CYANIDE ANALYSIS  IN WATER

                         CYANIDE, TOTAL  (in Water)
Method 335.2 CLP-M* (Titrimetric; Manual Spectrophotometrie; Semi-Automated
                            Spectrophotometrie)

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 1
      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.     Summary 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
      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
      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 same 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

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.
 CLP-M Modified for the Contract Laboratory Program.
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4.    Sample Handling and Preservation

4.L   All bottles must be thoroughly cleansed and rinsed to remove soluble
      material from containers.

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 40C(+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-Milligan
      scrubber.

6.2   Microburet,  5.0 mL (for titration)
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6.3   Spectrophotometer suitable for measurements at 578 run or 620 run 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

      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 MgCl2'6H20 into
              a 1000 mL flask, dissolved 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
              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 AgNO^ crystals and drying to
              constant weight at 40°C.  Weight out 3.2647 g of dried AgN03,

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              dissolve in distilled water, and dilute to 1000 mL (1 mL - 1
              rag CN).

      7.2.5   Rhodanine indicator:  Dissolve 20 mg of p-dimethyl-
              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  Spectrophotoraetric Reagents

      7.3.1   Sodium dihydrogenphosphate,  1 M:  Dissolve 138 g of
              Nal^PO^'i^O in a liter of distilled water.  Refrigerate this
              solution.

      7.3.2   Chloramine-T solution:  Dissolve 1.0 g of white, water
              soluble chloraraine-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-l-phenyl-2-
                         pyrazolin-5-one to 50 mL of distilled water,  heat
                         to 60°C with stirring.   Cool to room temperature.

                         7.3.3.2.1     3-Methyl-lphenyl-2-pyrazolin-5-one
                                      reagent,  saturated  solution:  Add
                                      0.25  g of  3-methyl-l-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'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
                                      nonacid-washed  filter paper.  Collect
                                      the filtrate.  Through  the same
                                      filter paper pour solution
                                      (7.3.3.2.2)  collecting  the filtrate

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                                      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 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 NaH2PO^'H20 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 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 air
                  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) into the
              air inlet and wash down with a stream of water.

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      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 raL 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.

      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 (7.3.1)
              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
                         run 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.
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      8.3.2   Prepare a minimum of 3 standards and a blank by pipetting
              suitable volumes of standard solution into 250 mL 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 water.  Standards must bracket the
              concentration of the samples.  If dilution is required, use
              the blank solution.

              As an example, standard solutions could be prepared as
              follows:

                        mL of Standard Solution      Cone,  ug CN
                            (1.0  - 5  ug CN)           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
                         ensure that the distillation 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 Spectrophotometric 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:
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                          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 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 titrimetric procedure,  calculate concentration of CN as
      follows:

                        (A-B) 1.000 mL/L     	250 mL	
          CN, mg/L =     mL orig.  sample  x  mL of aliquot titrated

          WHERE:   A - volume of AgNO-,  for  titration of sample
                     (1 mL = 1 mg Ag)

                  B = volume of AgNC^  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 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.
      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.


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      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 colorimetric 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.

Bibliography

1.     Methods  for "Chemical Analysis of Water and Wastes",  March 1979, EPA
      publication #600/4-79-02.

2.     "Operation RN Manual for Technicon Auto Analyzer IIC System", 1980.
      Technical publication #TA9-0460-00.    Technicon Industrial Systems,
      Tarrytown,  NY, 10591.

3.     "Users Guide for the Continuous Flow Analyzer Automation System",
      EMSL U.S. EPA, Cincinnati, OH (1981).

4.     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.

5.     Op. cit.  (#4), Methods 335.2.
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             METHOD FOR TOTAL CYANIDE ANALYSIS IN SOIL/SEDIMENT
                        CYANIDE, TOTAL  (in Sediments)
                          "A1
                       ,P-M  (Titrimetric; Manual Spec
                     Semi-Automated Spectrophotometric)
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.    Summary 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 run 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 and 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.
 CLP-M  Modified for the Contract Laboratory Program.

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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.

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 the
      alkaline titration conditions, making the end point almost impossible
      to detect.  When this occurs, one of the spectrophotometrie methods
      should be used.

6.     Apparatus

6.1   Reflux distillation apparatus such as shown in Figure I 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 run or 620 nm 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

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      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
              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 (1 mL
              = 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 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 AgNO-j crystals and drying to
              constant weight at 40°C.  Weigh out 3.2647 g of dried AgNO-j,
              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
              Nal^PO^'^O 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 HCl  (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:


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                         7.3.3.2.1    3-Methyl-l-phenyl-2-pyrazolin-5-one
                                      reagent,  saturated solution:   Add
                                      0.25 g of 3-raethyl-l-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 'Dimethyl- 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 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 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^PO^'l^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) to the absorbing tube
              and dilute if necessary with distilled water to obtain an

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               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 mix 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.

      8.1.5    Heat the  solution to boiling, taking  care to  prevent'the
               solution  from backing up and  overflowing into 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.

      8.1.6    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 blank 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.

                                   D-83                                ILM01.0

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        8.3.1.1    Pyridlne-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 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.

    As an example,  standard solutions could be prepared as follows:

                  mL of Standard Solution      Cone,  ug CN
                      (1.0 - 5 ug CN)            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 distillation 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)

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8.4   Serai-Automated Spectrophotometric 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 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 	25° mL	 x 1000  g/kg
                                         mL aliquot titrated
                  CN,  mg/kg ••	
                                               %solids
                                           c  x    100
                                   D-85                                ILM01.0

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           WHERE:  A - mL of AgNC>3 for titration of sample
                        (1 mL - 1 mg Ag)
                   B - mL of AgNO-j 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  Spectrophotometric)

                                        50 mL
                      CN,  mg/kg  -  A x   B
                                    C x %
                                           100

            WHERE:   A  -  ug CN read from standard curve (per 250 mL)
                    B  -  mL of distillate taken for colorime'tric
                          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)

    9.2.3   (Semi -Automated Spectrophotometric)

            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,  mg/kg  =  c x % solids
                                           100
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                  WHERE:  A  -  ug/L determined from standard curve
                          C  -  wet weight of original 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.

Bibliography

1.    Modification of Method 335.2:  Cyanide, Total

2.    Methods for "Chemical Analysis of Water and Wastes",  March 1979.  EPA
      Publication #600/4-79-02.

3.    "Operation Manual for Technicon Auto Analyzer IIC System", 1980.
      Technical publication #TA9-0460-00.   Technicon Industrial Systems,
      Tarrytown, NY, 10591.

4.    "Users Guide for the Continuous Flow Analyzer Automation System",
      ESL, U.S. EPA, Cincinnati, Ohio (1981).

5.    "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.

6.    Op.  cit. (#5), Methods 335.2, modified (by committee).
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ALLIHN CONDENSER	

AIR INLET  TUBE\
ONE LITER	
BOILING  FLASK
— CONNECTING TUBING
                                              SUCTION
    Figure 1.  Cyanide  distillation apparatus
                     D-88
                       ILM01.0

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COOLING WATER
IHIET TUBE'
      HEATER-
                                       TO  IOW VACUUM
                                           SOURCE
                                   - ABSORBER
                              DlSTIltlHG FLASK
  Figure  2.   Cyanide distillation apparatus
                    D-89
ILM01.0

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                                            5G
                         tO O


                         «°.
                         -3 ~*
                                             I


                                            Z
        O

        o   cT

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        oc   o
        O   «-'
                                            o
                                         o
                                         oc —<
                                         O •«-'
                                                o  o
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                                                           a:
                                                           o
               Figure 3.
Cyanide Manifold

 D-90
                                                                    ILM01.0

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            METHOD FOR TOTAL CYANIDE ANALYSIS BY MIDI DISTILLATION

                       CYANIDE, TOTAL (water and soils)

            Method 335.2 CLP-M (Serai-automated Spectrophotometrie)

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 colorimetric analysis of the distillate.

1.3   The detection limit for the semi-automated colorimetric method is
      approximately 10 ug/L.

2.     Summary of Method

2.1   The cyanide as hydrocyanic acid (HCN) is released from cyanide
      complexes by means of a midi reflux-distillation operation and 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 at 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 N 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.
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4.     Interferences

4.1   Interferences are eliminated or reduced by using the distillation
      procedure.

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 antifoaming 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  580 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 I^SO^ to an equal portion of ASTM Type II water.

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      6.1.4   Sodium hydroxide solution, 1.25 N.  Dissolve 50 g of NaOH  in
              ASTM Type II water and dilute to one liter.

6.2   Standards

      6.2.1   Stock cyanide solution, 1000 mg/L CN.  Dissolve 2.51 g of  KCN
              and 2.0 g KOH in ASTM Type II water and dilute one liter.
              Standardize with 0.0192 N AgNO-j.

      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 water.  Prepare
              this solution at time of analysis.

      6.2.3   Rhodamine indicator.  Dissolve 20 rag of p-dimethylamino-benzal-
              rhodamine in 100 mL acetone.

      6.2.4   Silver nitrate solution, 0.0192 N.  Prepare by crushing
              approximately 5 g AgNCK crystals and drying to a constant
              weight at 104°C.  Weigh out 3.2647 g of dried AgN03 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^CRO^ 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 Spectrophotometrie  Reagents

      6.3.1   Phosphate buffer solution, 1 M.  Dissolve 138 g of NaH2PO4-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 mL.
              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 Erlenmeyer 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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7.     Procedure

7.1   Distillation

      7.1.1   The procedure described here utilizes a midi distillation
              apparatus and requires a sample aliquot of 50 mLs or less for
              aqueous samples and one gram for solid materials.  NOTE:  All
              samples must initally 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 the impingers in each
              reaction vessel.

      7.1.7   After five minutes of vacuum flow, inject 5 mL of 50% (v/v)
              H2S04 (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 into 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 a half hours of refluxing, turn off the heat and
              continue the vacuum for an additional 15 minutes.  The flasks
              should be cool at this time.

      7.1.11  After cooling, close off the vacuum at the gang valve and
              remove the absorber.  Seal the receiving solutions and store

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              them at 4°C until analyzed.  The solutions must be analyzed for
              cyanide within the 12 day holding time specified in Section II.

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         mL 10 mg/L CN       mL 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 manner 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  must  find
                         and correct the cause of  the error before
                         proceeding.
                                  D-95                                ILM01.0

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      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.

8.     Calculations

8.1   Calculations for Semi-automated Colorimetric 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  from 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) .
                                   D-96                                ILM01.0

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8.1.5.2    The concentration  of  cyanide  in the  sample  is
           determined as  follows:

                            A x D x F
             CN, mg/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  -  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-97                                ILM01.0

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              PART F - PERCENT SOLIDS DETERMINATION 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 the 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 1QO
                                    Sample Wet  Weight
*For the purpose of paragraph 3,  drying time 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 must be recorded for a
 minimum of two repetitive weigh/dry/dessicate/weigh cycles with a minimum
 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-98                                ILM01.0

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           PART G - ALTERNATE METHODS (CATASTROPHIC ICP FAILURE)+
      Analyte                                                 Page No,

      Aluminum - Method 202.2 CLP-M*, Furnace AA             D-101
      Barium - Method 208.2 CLP-M, Furnace AA                D-102
      Cobalt - Method 219.2 CLP-M, Furnace AA                D-103
      Copper - Method 220.2 CLP-M, Furnace AA                D-104
      Iron - Method 236.2 CLP-M, Furnace AA                  D-105
      Manganese - Method 243.2 CLP-M, Furnace AA             D-106
      Nickel - Method 249.2 CLP-M, Furnace AA                D-107 -
      Vanadium - Method 286.2 CLP-M, Furnace AA              D-108
      Zinc - Method 289.2 CLP-M, Furnace AA                  D-109
      Aluminum - Method 202.1 CLP-M, Flame AA                D-lll
      Antimony - Method 204.1 CLP-M, Flame AA                D-113
      Barium - Method 208.1 CLP-M, Flame AA                  D-114
      Beryllium - Method 210.1 CLP-M, Flame AA               D-115
      Cadmium - Method 213.1 CLP-M,  Flame AA                 D-116
      Chromium - Method 218.1 CLP-M, Flame AA                D-117
      Cobalt - Method 219.1 CLP-M, Flame AA                  D-118
      Copper - Method 220.1 CLP-M, Flame AA                  D-119
      Iron - Method 236.1 CLP-M, Flame AA                    D-120
      Lead - Method 239.1 CLP-M, Flame AA                    D-121
      Manganese - Method 243.1 CLP-M, Flame AA               D-122
      Nickel - Method 249.1 CLP-M, Flame AA                  D-123
      Silver - Method 272.1 CLP-M, Flame AA                  D-125
      Thallium - Method 279.1 CLP-M, Flame AA                D-126
      Vanadium - Method 286.1 CLP-M, Flame AA                D-127
      Zinc - Method 289.1 CLP-M, Flame AA                    D-128
 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-99                                 ILM01.0

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                  CONDITIONS FOR USE OF ALTERNATE METHODS


The methods contained in Part G may be used only if all 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.
                                                                                  i
                                  D-100                                ILM01.0

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                                  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.

Instrument Parameters (General)

      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 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.   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-101                                ILM01.0

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                                  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.

Instrument Parameters (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 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,
     continuous  flow purge gas and pyrolytic graphite and are to be used as
     guidelines  only.

2.   The use of halide  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 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-102                                ILM01.0

-------
                                   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 u.  .d
     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 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.

                                  D-103                                ILM01.0

-------
                                   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 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,
     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 may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

                                  D-104                                ILM01.0

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                                    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.

Instrument 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 @ 2700°C.
       4.  Purge Gas Atmosphere:   Argon
       5.  Wavelength:  248.3 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,
     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 under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

                                  D-105                                ILM01.0

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                                 MANGANESE*

        Method 243.2 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:   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.
Instrument Parameters (General)

      1.  Drying Time and Temp:
      2.  Ashing Time and Temp:   30  sec  @  1000°C.
1.   Drying  Time  and Temp:   30 sec @ 125°C.
      3.  Atomizing Time and Temp:   10  sec  @  2700°G.
      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 may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

                                  D-106                                ILM01.0

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                                   NICKEL*
         Method 249.2 CLP-M** (Atomic Absorption,  Furnace Technique)

Optimum  Concentration Range:  5-100  ug/L
Approximate Detection Limi t:  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 @ 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:  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 under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

                                  D-107                               ILM01.0

-------
                                 VANADIUM*
        Method  286.2  CLP-M**  (Atomic Absorption, Furnace Technique)

Optimum Concentration Ranker  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 t_he  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 @ 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.

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.   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-108                                ILM01.0

-------
                                    ZINC*
Method 289.2 CLP-M**  (Atomic Absorption, Furnace Technique)

Optimum Concentration Range:   0.2-4 ug/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 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 @ 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-109                               ILM01.0

-------
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.
                                  D-110                                ILM01.0

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                                  ALUMINUM*

          Method 202.1 CLP-M** (Atomic  Absorption,  Flame  Technique)


Optimum Concentration Range:  5-50 mg/L using a wavelength of 309.3 nm
Sensitivity:  1 rog/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.   HNCU 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.

Instrument Parameters  (General)

      1.  Aluminum hollow cathode lamp
      2.  Wavelength:   309.3 nm
      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-lll                               ILM01.0

-------
Notes

 1.  The following may also be used:
       308.2 nm Relative Sensitivity 1
       396.2 run 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.
                                  D-112                                ILM01.0

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                                  ANTIMONY*

          Method 204.1 CLP-'-I** (Atomic Absorption,  Flame Technique)


Optimum Concentration Ran<->- :  1-40 mg/L using a wavelength of 217.6 nm
Sensitivity:  0.5 mg/L
Approximate Detection Limit:  0.2 rag/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 rhe 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.

Instrumental Parameters (General)

      1.  Antimony hollow cathode lamp
      2.  Wavelength:   217.6 nm
      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-113                               ILM01.0

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                                  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 (BaClo^HoO,
     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 Parameters (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-114                                ILM01.0

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                                 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 rag/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 same 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-115                               ILM01.0

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                                  CADMIUM*

         Method  213.1  CLP-N**  (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
     (SCdSO/ ' 8^0,  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.

Instrumental Parameters (General)

      1.  Cadmium hollow cathode lamp
      2.  Wavelength:   228.8 nm
      3.  Fuel:   Acetylene
      4.  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-116                               ILM01.0

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                                  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 HNOo and dilute to 1 liter with deionized
     distilled water.  1 mL - 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.

Instrument Parameters (General)

          Chromium hollow cathode lamp
          Wavelength:  357.9 nra
          Fuel:   Acetylene
          Oxidant:   Nitrous oxide
          Type of flame:   Fuel rich


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-117                               ILM01.0

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                                  COBALT*

         Method  219.1** CLP-M  (Atomic Absorption, Flame Technique)
Optimum Concentration Rant;*1 :   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.

Instrument 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-118                                ILM01.0

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                                   COPPER*

          Method 220.1 CLP-M** (Atomic Absorption,  Flame Technique)


Optimum Concentration Rangf:  0.2-5 mg/L using a wavelength of 324.7 nm
Sensitivity:  0.1 rr.g/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 HNOo 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 Siimple to be analyzed after sample preparation.

Instrumental Parameters (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 a,re 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-119                                ILM01.0

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                                    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 HMO,,  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 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 Parameters (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) Ls recommended.
*This method may only be used under specified conditions.

**CLP-M Modified for the Contract Laboratory Program.

                                  D-120                               ILM01.0

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                                    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(NO-j)2
     (analytical reagent grade), and dissolve deionized distilled water.
     When solution is complete acidify with 10 mL redistilled HNOo 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 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.

Instrumental Parameters  (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.  Then, 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-121                                ILM01.0

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                                 MANGANESE*

         Method 243.1 CLP-M**  (Atomic Absorption, Flame Technique)


Optimum Concentration Ram;e :   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 HNOo.   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.

Instrumental Parameters (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.

                                  D-122                                ILM01.0

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                                   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(NO-j)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 time 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.

Instrumental 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.
                                  D-123                                ILM01.0

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                                   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 AgNOo,  (analytical reagent grade)
     in deionized distilled water,  add 10 mL cone.  HNO-j 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.  NH^OH, 6.5 grams KCN, and 5.0 mL of  1.0 N I2
     solution.  Mix and dilute to 100 mL with deionized distilled water.
     Fresh solution should be prepared every two weeks.(1)                        ^B

Instrumental Parameters  (General)

          Silver  hollow cathode lamp
          Wavelength:  328.1 nm
          Fuel:   Acetylene
         . Oxidant:   Air
          Type of flame:   Oxidizing
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-124                               ILM01.0

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3.   If absorption to container walls or the formation of AgCl  is  suspected,
     make the sample basic using cone.  NH/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.

References

1.   "The Use of Cyanogen Iodide (CNI)  as  a Stabilizing Agent for  Silver  in
     Photographic Processing Effluent Sample",  Owerbach,  Daniel,
     Photographic Technology Division,  Eastman Kodak Company, Rochester,
     N.Y.  14650.
                                  D-125                               ILM01.0

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                                 THALLIUM*

         Method  279.1  CLP-M**  (Atomic Absorption, Flame Technique)
Optimum Concentration Range;  1-20 mg/L using a wavelength of 276.8 nm
Sensitivity:  0.5 mg/L
Approximate Detection Limit:  0.1 mg/L

Preparation of Standard Solution

1.   Stock Solution:   Dissolve 1.303 g 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 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 nitric acid and at the same concentration as will result
     in the  sample to be analyzed after sample preparation.

Instrumental Parameters (General)

      1. Thallium hollow cathode lamp
      2. Wavelength:   276.8 nm
      3. Fuel:   Acetylene
      4. Oxidant:  Air
      5. Type of flame:   Oxidizing
      Notes
1.   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-126                                ILM01.0

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                                  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,  V^Oc;
     (analytical reagent grade)  in 10 mL of cone,  nitric acid and dilute to
     1 liter with deionized distilled water.  1 mL = 1 mg 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.

Instrumental Parameters (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-127                               ILM01.0

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                                   ZINC*

         Method 289.1 CLP-H**  (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 HNOo.   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 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.

Instrumental Parameters (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.

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                              EXHIBIT E







           QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS







                                                          Page No,




SECTION I   - GENERAL QA/QC PRACTICES                        E-l




SECTION II  - SPECIFIC QA/QC PROCEDURES                      E-2




SECTION III - QUALITY ASSURANCE PLAN                         E-5




SECTION IV  - DATA MANAGEMENT                                E-7




SECTION V   - REQUIRED QA/QC OPERATIONS                      E-9




SECTION VI  - LABORATORY EVALUATION PROCESS                 E-25
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                                 SECTION I

                          GENERAL QA/QC PRACTICES

                                                                                 i
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 Uastewater Laboratories EPA-600/4-79-019,  USEPA Environmental
Monitoring and Support Laboratory,  Cincinnati, Ohio, March 1979.
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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 D.   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 all 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 data.  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
Intercomparison 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 (QAP) (see Section III) which describes the
procedures that are implemented to achieve the following:

      Maintain data 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

     5.   Procedures for Preparation, Approval, Review,  Revision, and
          Distribution  of SOPs


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     6.    Process  for Revision  of Technical  or  Documentation  Procedures

D.   Analytical Methodology

     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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                                 SECTION IV

                              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 resubrait 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 resubmitted 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.

c   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 must 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  arid  quality
    control.

o   Data  and  system security, backup  and  archiving.
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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.    Instrument Calibration

     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.

     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 each time an analysis is
     to be made and  discarded after  use.  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 except
     for  mercury.  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
     within + 5% of  the true  value.  Each standards  concentration and  the

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     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 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 ICP calibration.
     One of  the standards  must  be a  blank.

2.    Initial Calibration Verification (ICV)  and Continuing  Calibration
     Verification (CCV)

     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
         particular  ICV.  The  values for the initial and subsequent
         continuing  calibration verifications  shall be  recorded on FORM II-
         IN for ICP, AA,  and cyanide analyses, as indicated.

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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.   NBS  SRM  1643a
          3.   A Contractor-prepared standard solution
          TABLE  1.   INITIAL AND CONTINUING CALIBRATION  VERIFICATION
                    CONTROL LIMITS FOR INORGANIC  ANALYSES
Analytical Method
ICP/AA
Cold Vapor AA
Other
Inorganic
Species
Metals
Mercury
Cyanide
% of True
Low Limit
90
80
85
Value CEPA Set)
High Limit
110
120
115
     The same continuing calibration standard must 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.

     If the deviation of the continuing calibration verification  is
     greater than the control limits specified in Table 1-Initial  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
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          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 A A (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.

     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),
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         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 III-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  (ICS) 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.

     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 mixed 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.
 A group of samples prepared at the same time.
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     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
1
0
0
0
0
1
1
0
1
.0
.5
.5
.0
.5
.5
.5
.5
.0
.0
.5
.0
Al 500
Ca 500
Fe 200
Mg 500








6.    Spike Sample  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

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     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  must be added in the amount given in Table 3-Spiking
     Levels  for  Spike Sample Analysis,  for each element analyzed.   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-
     digestion/post-distillation spike  must be performed for those elements
     that do not meet the  specified criteria (exception: Ag).   Spike  the
     unspiked 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:

                        %Recovery  = (SSR-SR) 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
2
 EPA may require additional- spike sample analysis,  upon Administrative
 Project Officer request, for which the Contractor will be paid.

                                   E-15                               ILM01.0

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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 (i.e., ug/L for aqueous
and mg/Kg dry weight basis for solid).
                                                                            I
                               E-16                               ILM01.0

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           TABLE 3.   SPIKING LEVELS FOR SPIKE SAMPLE ANALYSIS
                    For ICP/AA
For Furnace AA
Other
                                                                   (1)
Element

Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide
Water
(ug/L)
2,000
500
2,000
2,000
50
50
*
200
500
250
1,000
500
*
500
500
*
2,000
50
*
2,000
500
500
Soil(2) Water Soil(2)
(mgAg) (ug/L) (mg/kg)
•XT
100 100 20
400 40 8
400
10
10 5 1
*
40
100
50
*
100 20 4
*
100
1
100
*
400 10 2
10
*
400 50 10
100
100
ioo<3>
 No spike required.  NOTE:  Elements without spike levels and not
designated with an asterisk, must be spiked at appropriate levels.

 Spiking level reported is for both water and soil/sediment matrices.
o
 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
(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 gram 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
                              E-17
                         ILM01.0

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     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 50  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
     midi-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.,
     ICP,  GFAA),  duplicate samples  must be  run by each method  used.

     The relative percent differences  (RPD)  for  each  component are
     calculated as follows:

                       RPD  = IS - D|  x 100
                              (S+D)/2

      Where, RPD  =  Relative Percent Difference
               S  =  First Sample Value (original)
               D  =  Second Sample Value  (duplicate)

     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
     for sample values 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.
 EPA may require additional duplicate sample analyses,  upon Administrative
 Project Officer request, for which the Contractor will be paid.


                                   E-18                                ILM01.0

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     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 Sample (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 must 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.

9.    ICP Serial Dilution Analysis (L)

     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

                                   E-19                                ILM01.0

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     dilution analysis  for  one  or  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:

                             |I - SI
            % Difference =	   x 100
                                 I

     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" flags must be reported  on  FORM
     IX-IN.

10.   Instrument Detection 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.

     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 ICPs.
                                   E-20                                ILM01.0

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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)  QC 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
          (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 must be rerun once  (i.e.,  two  additional  burns).
          If the readings  are  still out,  flag  the  value  reported on FORM I-

                                  E-21                                ILM01.0

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         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.

         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 quantisation .  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
         that  sample.  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.

         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.
Analytical Spikes are post-digestion spikes to be prepared prior to
analysis by adding a known quantity of the analyte 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.

"Spike" is defined as [absorbance or concentration of spike sample]  minus
[absorbance or concentration of the sample].
                                  E-22                                ILM01.0

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     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 MSAs,  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
          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
          I-IN.
                              E-23                                ILM01.0

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                                        Figure 1.
                         FURNACE ATOMIC ABSORPTION ANALYSIS SCHEME
      PREPARE AND ANALYZE
     SAMPLE  AND  ONE SPIKE
          (2   X CRDL)
  (Pouole  Injections Required)
       ANALYSES WITHIN
      CALIBRATION RANGE
                YES
      RECOVERY OF SPIKE
        LESS  THAN 40%
               NO
    SAMPLE ABSORBANCE OR
  CONCENTRATION LESS_ THAN
  50%  OF SPIKE ASSORBANCE
       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
  QUANTITATE BY MSA WITH 3
  SPIKES  AT 50, 100 4 1SOX
    OF  SAMPLE ABSORBANCE
      OR  CONCENTRATION
{Only Single  Injections R«
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                                    SECTION VI

                          LABORATORY EVALUATION FROCESS

      This document outlines the procedures which will be used by the
Administrative Project Officer or his/her authorized representative to
conduct laboratory audits to determine the Contractor's ability to meet the
terms and conditions of thi-~ contract.   The evaluation process incorporates
two major steps:   1) evaluation of laboratory performance, and 2) on-site
inspection of the laboratory to verify continuity of personnel,
instrumentation and quality control requirements of the contract.

1.    Evaluation of Laboratory Performance

     a.    Performance  Evaluation Sample Analysis

          1)   The Performance Evaluation  (PE) sample set  will be  sent  to a
              participating  laboratory on a quarterly basis to verify  the
              laboratory's continuing ability to produce  acceptable
              analytical results.  These samples will be  provided either
              single blind  (recognizable as a PE material and of unknown
              composition),  or  double blind (not recognizable as PE
              material and of unknown composition).  If received as a
              single blind,  the  Contractor is required to submit PE sample
              data  in a  separate SDG package in accordance with Delivery
              Schedule requirements for PE Sample  data.   PE samples
              received as double blind would be treated as routine samples
              and data would be  submitted in the SDG deliverables package
              per normal procedure.

          2)   When  the PE data  are received by EPA, results will be scored
              routinely  for  identification and quantitation.  Results  of
              these scorings will be provided for  the Contractor via coded
              evaluation spreadsheets by analyte.  The Government may
              adjust  the scores  on any given PE sample to compensate for
              unanticipated  difficulties with a particular sample.

          3)   If the Contractor  laboratory performs unacceptably, the
              Contractor will be notified by the Administrative Project
              Officer.  A laboratory so notified may expect, but the
              Government is  not  limited to, the following actions:  a  site
              visit, a full  data audit, cessation  of sample shipments,
              and/or laboratory  analysis of a second PE sample.  Failure by
              the laboratory to  take corrective actions and/or failure of
              two successive PE  sample analyses is indicative of Contractor
              failure to maintain technical competence and will require
              that  the laboratory discontinue analysis of samples until
              such  time as the Administrative Project Officer has
              determined that the laboratory has corrected the problem and
              may resume analyses.
     b.    Inorganic  Data  Audit

          Inorganic  data  audits  are conducted by EMSL-LV on the Contractor's
          sample data packages.   The inorganic data audit  provides the
          Agency with  an  in-depth inspection and evaluation of the data
          packages with regard to achieving QA/QC acceptability.

                                   E-25                                 ILM01.0

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2 .    On-Site Laboratory Evaluation

      The on-site laboratory evaluation helps to ensure that technical
      competence is maintained and that all the necessary quality control
      is being applied by the Contractor in order to deliver a quality
      product.

     a.    Or.-site laboratory evaluations  allow  the  evaluators  to  determine
          that:

          1)   The  organization and personnel are qualified  to perform
              assigned tasks;

          2)   Adequate facilities and  equipment are available;

          3)   Complete documentation,  including chain-of-custody of  samples
              is being implemented;

          4)   Proper  analytical methodology  is being used;

          5)   Adequate analytical quality  control,  including  reference
              samples,  control charts, and documented  corrective action
              measures,  is  being provided; and

          6)   Acceptable data handling and documentation  techniques  are
              being used.

     b.    The on-site  visit  also  serves as  a  mechanism  for discussing
          weaknesses  identified  through Performance Evaluation sample
          analysis or  through Contract  Compliance  Screening or other  review
          of data deliverables.   Lastly,  the  on-site visit allows the
          evaluation  team to determine  if the laboratory has implemented  the
          recommended  and/or required corrective  actions,  with respect to
          quality assurance, that  were  made during  the  previous  on-site
          visit.
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             EXHIBIT F
CHAIN-OF-CUSTODY, DOCUMENT CONTROL,
 AND STANDARD OPERATING PROCEDURES
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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   Sample 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.
                t
      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
               I
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 the 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 snail 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,  pers-:.al anl instrument logs,  and other
      relevant deliverables to ensure zhat 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 Deliverable^

      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 STANDARD OPERATING 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.

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   Condition of the 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 SOPs 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.

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

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      all documents including logbook pages,  sample  tracking records,
      chromatographic 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.
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    EXHIBIT G
GLOSSARY OF TERMS
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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 sample preparation.

CALIBRATION BLANK - a volume of acidified deionized/distilled water.

CASE - a finite,  usually predetermined number of samples collected over a
given time period from a particular  site.  Case numbers are assigned by the
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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 um 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.

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.

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      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.

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.

LABORATORY RECEIPT DATE - the date on which a sample is received at the
Contractor's facility, as recorded on the shipper's 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).
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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 rr.ethod
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) - an analytical control
that contains distilled, deionized water and reagents, which is carried
through the entire analytical procedure (digested and analyzed).   An
aqueous method blank is treated with the same reagents as a sample with a
vater 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
sample receipt and handling, analytical methods, data reporting and
deliverables, and document control.  Used synonymously with Statement of
Work (SOW).

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 those 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.
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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   Each 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.

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.

SOIL - synonymous with soil/sediment or sediment as used herein.

STOCK SOLUTION - a standard solution which can be diluted to derive other
standards.

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.

WET 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.
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                                  EXHIBIT H

               DATA DICTIONARY AND FORMAT FOR DATA DELIVERABLES
                          IN COMPUTER-READABLE FORMAT
                                                                      Page No,
SECTION I:     Description of Deliverables 	  H-l
SECTION II:     Format A Specification 	  H-3
SECTION III:    Format B Specification 	  H-26
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                                  SECTION I

                         DESCRIPTION OF DELIVERABLES
1.   Introduction

1.1   Two file formats are specified for delivery of computer-readable data.
      Format A is oriented to the structure of the hardcopy reporting forms
      required by the contract.   Format B is oriented to the general data
      required by the contract.   Information sufficient to generate required
      hardcopy forms is contained in either format.  NOTE:  Beginning in
      March, 1991, all data submitted in electronic form shall be submitted
      using the USEPA Standard for Electronic Transmission of Laboratory
      Results, EPA Order 2180.2

1.2   The file or files for a Sample Delivery Group (SDG, see Exhibit A,
      Section I, B) must be submitted on a diskette or diskettes (see
      paragraph, 2.1).  Information on a diskette or diskettes for any single
      SDG must be in one, and only one, of the two formats.  The format used
      13 at the option of the laboratory.  The option used must be included
      in the File Name specification (paragraph 2.2).

1.3   Format A consists of variable length ASCII records, and Format B
      consists of fixed-length 80-byte ASCII records.

1.4   All information for one SDG must be in one file if format A is used.
      Use of Format B may require information for one SDG to be in a number
      of files.  Format B may require more than one 360 K diskette for a
      valid SDG.

2.     Deliverable

2.1   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 in either format should not be included on the
      diskettes.
                                      H-l                         ILM01.0

-------
2.2   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.INY

               where  XXXXXX  is the SDG identifier
Examples :

      Format A

      Format 3
                      I
                      N
                              indicates Inorganics analysis

                              is a continuation number used to identify
                              multiple files corresponding to the same SDG.
                              For Format A, "N" must be "I".  For Format B,
                              "N" must be "1" for the only, or first file of
                              the SDG, and must be incremented to "2", "3",
                              etc., for subsequent files of the SDG.  "N"
                              cannot be greater than 9 .  If "N" is greater
                              than 9 then replace Y with a digit to continue
                              incrementing.  The files must be incremented in
                              chronological order.

                              is "A" for Format A
                              is "B" for Format B, or a digit (0 to 9) if
                              more than 9 Format B files are used.
                        ABC123.I1A

                        ABC123.I1B
                        ABC123.I2B
                        ABC123.I3B
                        ABC123.I9B
                        ABC123.I10
                        ABC123.I11
                        ABC123.I99
      Dimensions of the label must be in the range 4-3/4" to 5" long by 1-1/4
      to 1-1/2" wide.
                                   H-2
                                                                       ILM01.0

-------
                                  SECTION II

                            FORMAT A SPECIFICATION
1.     Format Characteristics

1.1   Format A is based upon the structure of the hardcopy reporting forms
      required by the contract.  With two exceptions,  Form Suffix and Record
      Type,  all fields in the format correspond directly with entries or
      items  on the hardcopy forms.

1.2   Format A includes detailed specifications for the required format of
      each Inorganic Reporting Form's HEADER and DETAIL records.   The exact
      columns in which each field is to be contained are shown,  as well as
      the length of the field.  Each field's required contents are specified
      either as a literal (contained in single quotes) which must appear
      exactly as shown (without the quotes),  or as a variable for which a
      format is listed in the format column.   Each field's required format is
      specified either as an option of two or more choices (divided by
      slashes), as MM/DD/YY for a date, as a CHARACTER field, or as a NUMERIC
      field.

1.3   Format fields listed as CHARACTER may contain any standard ASCII
      characters, and must be left-justified and padded with blanks.  Formats
      listed as NUMERIC may contain numeric digits, a decimal point, and a
      leading plus or minus sign, and must be right-justified and padded with
      blanks.  The numbers following the word NUMERIC specify the maximum
      number of digits which are allowed on either side of the decimal.  The
      decimal point is not assumed and must be contained in the field in its
      correct position.  For example, the format "NUMERIC 3.2" allows 3
      digits preceding the decimal point and 2 following it (a total length
      of 6 characters).  The format "NUMERIC S3.2" allows a leading plus or
      minus  sign (a total length of 7).  If a field's format description does
      not; contain a decimal point,  then a decimal point is not allowed in the
      field.  If a field's format description does not contain an "S", then a
      sign is not allowed in the field.

      Explanation of NUMERIC fields in Format A.

      In the examples below the format NUMERIC 3.2 is described.

      (Quotation marks indicate limits of the field described and are not
      included in the format.)

      If the value of the field is  10.1:
      The columns in the format will appear as:   "10.10" (six columns).
                                   H-3                                ILM01.0

-------
      The table below demonstrates several examples:
Value
10.1
10.11
100.11
100
.29
-100.129
-10.1
The following table presents
Value
10.1
-10.11
-100.11
-1000.1
100
-.22
-.239
Appears on Format
"10.10"
"10.11"
"100.11"
"100.00"
"0.29"
Invalid
Invalid
examples of NUMERIC S3. 2:
Appears on Format
" 10.10" (seven columns)
" -10.11"
"-100.11"
Invalid
" 100.00"
" -0.22"
" -0.24"
2.    Record Types

2.1   Format A consists of variable length ASCII records.   The last two bytes
      of each record must contain "carriage return" and "line feed",
      respectively.   Unused bytes in partially filled fields must be  blank-
      filled.

2.2   Format A has three types of records:   Header Records,  Detail Records
      and Comment Records.

          Type              Tyoe ID            Contents

          Header               H               Nonrepeating fields which
                                               together are  unique to the
                                               associated  hardcopy form
          Detail               D               A group of  fields  that are
                                               repeated on a form, and are
                                               uniquely positioned by (e.g.,
                                               Analyte Chemical Symbol)

          Comment              C               Nonrepeating  fields containing
                                               text that comments on  informa-
                                               tion reported on the form

      The format for Comment Records is  the same for all forms,  and is
      described after all other formats.

2.3   The first 5 bytes of each record contain the FORM ID,  identifying the
      Inorganic Analysis Reporting Form  for which the record contains data.
      The ID must be left-justified in the  field.
                                   H-4                                ILM01.0

-------
        FORM ID                      FORM NAME
         COVER      COVER PAGE  -  INORGANIC ANALYSES DATA PACKAGE
         I          INORGANIC ANALYSIS DATA SHEET
         11(1)      INITIAL AND CONTINUING CALIBRATION VERIFICATION
         11(2)      CRDL STANDARD FOR AA AND ICP
         III        BLANKS
         17         1C? INTERFERENCE CHECK SAMPLE
         V(l)       SPIKE SAMPLE  RECOVERY
         V(2)       POST DIGEST SPIKE SAMPLE RECOVERY
         VI         DUPLICATES
         VII        LABORATORY  CONTROL SAMPLE
         VIII       STANDARD ADDITION RESULTS
         IX         ICP SERIAL  DILUTIONS
         X          INSTRUMENT  DETECTION LIMITS  (QUARTERLY)
         XI         ICP INTERELEMENT CORRECTION FACTORS (ANNUALLY)
         XII        ICP LINEAR  RANGES (QUARTERLY)
         XIII       PREPARATION LOG
         XIV        ANALYSIS RUN  LOG

  Following the  FORM  ID is a two-byte, left-justified, FORM  SUFFIX, which
  must be unique for  each set of  records that correspond to  one hardcopy
  form.  For example,  records for the first occurrence of a  form must
  contain the suffix  AA.  Records for the second occurrence  must contain
  AB, and the twenty-seventh occurrence would contain BA.

  The 8th byte of each record contains the TYPE ID, which specifies what
  kind of data the record contains  (see paragraph  2.2).

  Records with the same FORM ID and FORM SUFFIX must be grouped together
  in the file.   Within each FORM  ID/FORM SUFFIX group, there may be only
  one HEADER record,  and it must  come first.  DETAIL records must follow
  the HEADER record.   The COMMENT records, which are optional, must come
  last in the group,  and be in  sequence corresponding to the form.

  The FORM ID/FORM SUFFIX group(s) for the COVER PAGE(S) must come first
  in the file.   After the COVER PAGE(S), the FORM  ID/FORM SUFFIX groups
  do not have to be in any specific order.  For example, a set of
  HEADER/DETAIL/COMMENT records for FORM V could come before records for
  FORM I, as long as  the records  within the group  are in the correct
  order.

  Record Length

Table 3.1 summarizes  the length (excluding carriage return/line feed)  and
(in parentheses)   the number of  records in Format A.  The maximum number
of detail and comment  records is  shown,  corresponding to a submission of
hardcopy forms on which information is written on all possible lines.
                                H-5                                 ILM01.0

-------
                           Table 3.1  Format  A Summary
      Form
      Cover
      I
      IKD
      11(2)
      III
      IV
      V(2)
      VI
      VII
      VIII
      IX
      X
      XI(2)
      XII
      XIII
      XIV
Record
Header
80a(l)b
90(1)
32(1)
32(1)
18(1)
32(1)
33(1)
23(1)
38(1)
32(1)
8(1)
23(1)
52(1)
28(1)
28(1)
28(1)
10(1)
38(1)
Detail
25(20)
31(24)
65(24)
66(23)
59(24)
64(23)
66(24)
62(24)
56(24)
68(24)
69(32)
44(23)
29(23)
77(23)
77(23)
29(23)
32(32)
59(32)
Comment
78(4)
73(4)




78(4)
78(4)




78(4)
78(4)
78(4)
78(4)


      a Length of record in bytes (excluding carriage return/line feed).
        Maximum number of records required for a form.


  Record Listing

The remainder of this section contains detailed specifications for every
record required for a full set of hardcopy forms.
                               H-6
ILM01.0

-------
                                  COVER PAGE


INORGANIC ANALYSES DATA PACKAGE COVER PAGE HEADER RECORD:

COLUMN(S)    LENGTH       CONTENTS                    FORMAT

   1-5          5         'COVER'
   6-7          2         FORM  SUFFIX
    8           1         'H'
   9-33        25         LAB NAME                    CHARACTER
  34-43        10         CONTRACT                    CHARACTER
  44-49         6         LAB CODE                    CHARACTER
  50-54         5         CASE  NUMBER                 CHARACTER
  55-60         6         SAS NUMBER                  CHARACTER
  61-66         6         SDG NUMBER                  CHARACTER
  67-71         5         SOW NUMBER                  CHARACTER
  72-74         3         ICP INT CORRECTIONS         'YES'/'NO'
  75-77         3         ICP BG CORRECTIONS          'YES'/'NO'
  78-80         3         RAW DATA BEFORE             'YES'/'NO'/BLANK
NOTE:   The LAB NAME, CONTRACT, LAB CODE, CASE NUMBER, SAS  NUMBER, AND SDG
        NUMBER, which are contained in the  COVER PAGE HEADER record, are not
        repeated in the  HEADER records of the other forms.  Each form's
        HEADER record contains only data which are unique to  the DETAIL
        records which follow it.
INOP,GANIC ANALYSES DATA PACKAGE COVER PAGE DETAIL RECORDS:

COLUMNSS)    LENGTH       CONTENTS                    FORMAT

   1-5   -       5         'COVER'
   6-7          2         FORM SUFFIX
    8           1         'D'
   9-15         7         EPA SAMPLE NO.              CHARACTER
  16-25        10         LAB SAMPLE ID NO.           CHARACTER
                                   H-7                                 ILM01.0

-------
                                    FORM I
INORGANIC ANALYSIS DATA SHEET HEADER RECORD:
COLUMN (S).
LENGTH
CONTENTS
FORMAT
1-5
6-7
8
9-15
16-20
21-30
31-33
34-41
42-46
47-51
52-60
61-69
70-75
76-81
82-87
88-90
5
2
1
7
5
10
3
8
5
5
9
9
6
6
6
3
                          'I
                          FORM SUFFIX
                          'H'
                          EPA SAMPLE NO.
                          MATRIX
                          LAB SAMPLE ID
                          LEVEL
                          DATE RECEIVED
                          PERCENT SOLIDS
                          CONCENTRATION UNITS
                          COLOR BEFORE
                          COLOR AFTER
                          CLARITY BEFORE
                          CLARITY AFTER
                          TEXTURE
                          ARTIFACTS
                                        CHARACTER
                                        'WATER'/'SOIL'
                                        CHARACTER
                                        'LOW/'MED'
                                        MM/DD/YY
                                        NUMERIC 3.1
                                        'UG/L '/ 'MG/KG'
                                        CHARACTER
                                        CHARACTER
                                        CHARACTER
                                        CHARACTER
                                        CHARACTER
                                        'YES'/BLANK
INORGANIC ANALYSIS DATA SHEET DETAIL RECORDS:
COLUMN(S)    LENGTH
   1-5
   6-7
    8
   9-10
  11-22
   23
  24-29
  30-31
   5
   2
   1
   2
  12
   1
   6
CONTENTS

'I
FORM SUFFIX
'D'
ANALYTE SYMBOL
CONCENTRATION
CONG FLAG (C)
QUALIFIER (Q)
            METHOD  (M)
                                        FORMAT
CHARACTER
NUMERIC 9.2
'B'/'U'/BLANK
UP TO 6 ONE-CHARACTER
FLAGS (OTHER THAN  'B'
OR 'U')
METHOD CODE/'NR'
                                   H-8
                                                          ILM01.0

-------
                               FORM II (PART 1)
INITIAL AND CONTINUING CALIBRATION VERIFICATION HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT
                          'IKD'
                         FORM SUFFIX
                          'H'
                         INIT CAL SOURCE             CHARACTER
                         CONT CAL SOURCE             CHARACTER
1-5
6-7
8
9-20
21-32
5
2
1
12
12
INITIAL AND CONTINUING CALIBRATION VERIFICATION DETAIL RECORDS:
COLUMN(S)
LENGTH
1-5
6-7
8
9-10
11-17
18-25
26-30
31-37
38-45
46-50
51-58
59-63
64-65
5
2
1
2
7
8
5
7
8
5
3
5
2
CONTENTS

'II(l)'
FORM SUFFIX
'D'
ANALYTE SYMBOL
INITIAL CAL TRUE
INITIAL CAL FOUND
INITIAL CAL %R
CONT CAL TRUE
CONT CAL FOUND 1
CONT CAL %R 1
CONT CAL FOUND 2
CONT CAL %R 2
METHOD (M)
70RMAT
                                                     CHARACTER
                                                     NUMERIC  5.1
                                                     NUMERIC  5.2
                                                     NUMERIC
                                                     NUMERIC
                                                     NUMERIC
                                                     NUMERIC
                                                     NUMERIC
                                                     NUMERIC
                                                3.1
                                                5.1
                                                5.2
                                                3.1
                                                5.2
                                                3.1
                                                     METHOD  CODE/'
                                   H-9
                                                          ILM01.0

-------
                               FORM II (PART 2)
CRDL STANDARD FOR AA AND ICP HEADER RECORD:

COLUMNfS)    LENGTH       CONTENTS
                         '11(2)'
                         FORM SUFFIX
                         'H'
                         AA STANDARD SOURCE
                         ICP STANDARD SOURCE
1-5
6-7
8
9-20
21-32
5
2
1
12
12
                            FORMAT
                            CHARACTER
                            CHARACTER
CRDL STANDARD FOR AA AND ICP DETAIL RECORDS:
COLUMN(SI    LENGTH
1-5
6-7
8
9-10
11-17
18-26
27-31
32-38
39-47
48-52
53-61
62-66
5
2
1
2
7
9
5
7
9
5
9
5
CONTENTS

'11(2)'
FORM SUFFIX
'D'
ANALYTE SYMBOL
AA TRUE
AA FOUND
AA %R
ICP INIT TRUE
ICP INIT FOUND
ICP INIT %R
ICP FINAL FOUND
1C? FINAL %R
FORMAT
                                                     CHARACTER
                                                     NUMERIC 5.1
                                                     NUMERIC 6.2
                                                     NUMERIC 3.1
                                                     NUMERIC 5.1
                                                     NUMERIC 6.2
                                                     NUMERIC 3.1
                                                     NUMERIC 6.2
                                                     NUMERIC 3.1
                                   H-10
                                              ILM01.0

-------
                                   FORM III
BLANKS HEADER RECORD:

COLUMN(S)    LENGTH
   1-5
   6-7
    8
   9-13
  14-18
   5
   2
   1
   5
   5
CONTENTS

'III  '
FORM SUFFIX
'H'
PREP BLANK MATRIX
PREP BLANK UNITS
                                        FORMAT
 'WATER'/'SOIL  '
 'UG/L  '/'MG/KG'
BLANKS DETAIL RECORDS:
COLUMN(S)

   1-5
   6-7
    8
   9-10
  11-18
   19
  20-27
   28
  29-36
   37
  38-45
   46
  47-55
   57
  58-59
LENGTH

   5
   2
   1
   2
   8
   1
   8
   1
   8
   1
   8
   1
  10
   1
   2
CONTENTS

'III  '
FORM SUFFIX
'D'
ANALYTE SYMBOL
INITIAL CAL BLANK
INITIAL CAL FLAG (C)
CONT CAL BLANK 1
CC BLANK 1 FLAG (C)
CONT CAL BLANK 2
CC BLANK 2 FLAG (C)
CONT CAL BLANK 3
CC BLANK 3 FLAG (C)
PREPARATION BLANK
PREP BLANK FLAG (C)
METHOD (M)
FORMAT
CHARACTER
NUMERIC S5.1
'B'/'U'/BLANK
NUMERIC S5.1
'B'/'U'/BLANK
NUMERIC S5.1
'B'/'U'/BLANK
NUMERIC S5.1
'B'/'U'/BLANK
NUMERIC S5.3
'B'/'U'/BLANK
METHOD CODE/'NR'
                                   H-ll
                                                          ILM01.0

-------
                                   FORM IV


ICP INTERFERENCE CHECK SAMPLE HEADER RECORD:

COLUMN(S)    LENGTH       CONTENTS                    FORMAT

   1-5          5         'IV
   6-7          2         FORM SUFFIX
    8           I         'H'
   9-20        12         ICP ID NUMBER               CHARACTER
  21-32        12         ICS SOURCE                  CHARACTER
ICP INTERFERENCE CHECK SAMPLE DETAIL RECORDS:

COLUMN CS")    LENGTH      CONTENTS                    FORMAT

   1-5          5         'IV
   6-7          2         FORM SUFFIX
    8           1         'D'
   9-10         2         ANALYTE SYMBOL              CHARACTER
  11-16         6         TRUE A                      NUMERIC 6
  17-22         6         TRUE AB                     NUMERIC 6
  23-29         7         INITIAL A                   NUMERIC S6
  30-38         9         INITIAL AB                  NUMERIC S6.1
  39-43         5         INITIAL %R                  NUMERIC 3.1
  44-50         7         FINAL A                     NUMERIC S6
  51-59         9         FINAL AB                    NUMERIC S6.1
  60-64         5         FINAL %R                    NUMERIC 3.1
                                   H-12                                ILM01.0

-------
                                FORM V  (PART  1)


SPIKE SAMPLE RECOVERY HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT

   1-5          5         'V(l)  '
   6-7          2         FORM SUFFIX
    8           1         'H'
   9-15         7         EPA SAMPLE NO.              CHARACTER
  16-20         5         MATRIX                      'WATER'/'SOIL '
  21-23         3         LEVEL                       'LOW'/'MED'
  24-28         5         CONCENTRATION UNITS         'UG/L '/ 'MG/KG'
  29-33         5         SAMPLE % SOLIDS             NUMERIC 3.1
SPIKE SAMPLE RECOVERY DETAIL RECORDS:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT

   1-5          5        'V(l)  '
   6-7          2        FORM SUFFIX
    8           1        'D'
   9-10         2        ANALYTE SYMBOL              CHARACTER
  11-16         6        CONTROL LIMIT %R            '75-125'/BLANK
  17-30        14        SPIKED SAMPLE RESULT NUMERIC 9.4
   31           1        SSR FLAG  (C)                'B'/'U'/BLANK
  32-44        13        SAMPLE RESULT                NUMERIC 8.4
   45           1        SR FLAG (C)                 'B'/'U'/BLANK
  46-56        11        SPIKE ADDED                 NUMERIC 8.2
  57-63         7        PERCENT RECOVERED           NUMERIC S4.1
   64           1        QUALIFIER (Q)               'N'/BLANK
  65-66  -       2        METHOD (M)                  METHOD CODE/'NR'
                                   H-13                               ILM01.0

-------
                                FORM V  (PART  2)
POST DIGEST SPIKE SAMPLE RECOVERY HEADER RECORD:

COLUMN(S)    LENGTH       CONTENTS
                          'V(2)  '
                          FORM SUFFIX
                          'H'
                          EPA SAMPLE NO.
                          MATRIX
                          LEVEL
1-5
6-7
8
9-15
16-20
21-23
5
2
1
7
5
3
                                        FORMAT
                                        CHARACTER
                                        'WATER'/'SOIL
                                        'LOW'/'MED'
POST DIGEST SPIKE SAMPLE RECOVERY DETAIL RECORDS:
COLUMN(S)
LENGTH
1-5
6-7
8
9-10
11-16
17-28
29
30-41
42
43-52
53-59
60
61-62
5
2
1
2
6
12
1
12
1
10
7
1
2
CONTENTS

'V(2) '
FORM SUFFIX
'D'
ANALYTE SYMBOL
CONTROL LIMIT %R
SPIKED SAMPLE RESULT
SSR FLAG (C)
SAMPLE RESULT
SR FLAG (C)
SPIKE ADDED
PERCENT RECOVERED
QUALIFIER (Q)
METHOD (M)
FORMAT
                                                     CHARACTER
                                                     BLANK
                                                     NUMERIC 9.2
                                                     'B'/'U'/BLANK
                                                     NUMERIC 9.2
                                                     NUMERIC 8.1
                                                     NUMERIC S4.1
                                                     BLANK
                                                     METHOD CODE/'NR'
                                   H-14
                                                          ILM01.0

-------
                                    FORM VI
DUPLICATES HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS
   1-5
   6-7
    8
   9-15
  16-20
  21-23
  24-28
  29-33
  34-38
5
2
1
7
5
3
5
5
5
'VI
FORM SUFFIX
'H'
EPA SAMPLE NO.
MATRIX
LEVEL
CONCENTRATION UNITS
SAMPLE % SOLIDS
DUPLICATE % SOLIDS
                                     FORMAT
CHARACTER
'WATER'/'SOIL '
'LOW/'MED'
'UG/L '/'MG/KG'
NUMERIC 3.1
NUMERIC 3.1
DUPLICATES DETAIL RECORDS:

COLUMN(S)    LENGTH      CONTENTS

   1-5          5          'VI    '
   6-7          2         FORM SUFFIX
    8           1          'D'
   9-10         2         ANALYTE SYMBOL
  11-17         7         CONTROL LIMIT
  18-31        14         SAMPLE
   32           1         SAMPLE FLAG  (C)
  33-46        14         DUPLICATE
   47           1         DUPLICATE FLAG  (C)
  48-53         6         RPD
   54           1         QUALIFIER (Q)
  55-56         2         METHOD (M)
                                     FORMAT
                                     CHARACTER
                                      NUMERIC 5.1
                                     NUMERIC 9.4
                                     'B'/'U'/BLANK
                                     NUMERIC 9.4
                                     'B'/'U'/BLANK
                                     NUMERIC 4.1
                                     '*'/BLANK
                                     METHOD CODE/'NR'
                                   H-15
                                                       ILM01.0

-------
                                   FORM VII
LABORATORY CONTROL SAMPLE HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS
   1-5
   6-7
    8
   9-20
  21-32
 5
 2
 I
12
12
'VII  '
FORM SUFFIX
'H'
SOLID LCS SOURCE
AQUEOUS LCS SOURCE
                                      FORMAT
CHARACTER
CHARACTER
LABORATORY CONTROL SAMPLE DETAIL RECORDS:

COLUMN(S)    LENGTH       CONTENTS

   1-5          5         'VII  '
   6-7          2         FORM SUFFIX
    8           I         'D'
   9-10         2         ANALYTE SYMBOL
  11-17         7         AQUEOUS TRUE
  18-25         8         AQUEOUS FOUND
  26-30         5         AQUEOUS % RECOVERED
  31-38         8         SOLID TRUE
  39-46         8         SOLID FOUND
   47           1         SOLID FOUND FLAG (C)
  48-55         8         SOLID LOWER LIMIT
  56-63         8         SOLID UPPER LIMIT
  64-68         5         SOLID % RECOVERED
                                      FORMAT
                                      CHARACTER
                                      NUMERIC 5.1
                                      NUMERIC 5.2
                                      NUMERIC 3.1
                                      NUMERIC 6.1
                                      NUMERIC 6.1
                                      'B'/'U'/BLANK
                                      NUMERIC 6.1
                                      NUMERIC 6.1
                                      NUMERIC 3.1
                                   H-16
                                                        ILM01.0

-------
                                  FORM VIII
STANDARD ADDITION RESULTS HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS
   1-5
   6-7
   5
   2
   I
                                        FORMAT
'VIII '
FORM SUFFIX
'H'
NOTE:   Although there are no fields which occur only once per FORM VIII, the
        HEADER record must be included as a place holder, indicating that
        DETAIL records follow.
STANDARD ADDITION RESULTS DETAIL RECORDS:
COLUMN(S)

   1-5
   6-7
    8
   9-15
  16-17
  18-22
  23-28
  29-33
  34-39
  40-44
  45-50
  51-55
  56-62
  63-68
   69
LENGTH

   5
   2
   1
   7
   2
   5
   6
   5
   6
   5
   6
   5
   7
   6
   1
'VIII '
FORM SUFFIX
'D'
EPA SAMPLE NO.
ANALYTE SYMBOL
0 ADD ABSORBANCE
1 ADD CONCENTRATION
1 ADD ABSORBANCE
2 ADD CONCENTRATION
2 ADD ABSORBANCE
3 ADD CONCENTRATION
3 ADD ABSORBANCE
FINAL CONCENTRATION
CORRELATION COEF (R)
QUALIFIER (Q)
CHARACTER
CHARACTER
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
1.3
3.2
1.3
3.2
1.3
3.2
1.3
5.1
1.4
'+'/BLANK
                                   H-17
                                                          ILM01.0

-------
                                   FORM IX


ICP SERIAL DILUTIONS HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT

   1-5          5         'IX
   6-7          2         FORM SUFFIX
    8           1         'H'
   9-15         7         EPA SAMPLE NO.              CHARACTER
  16-20         5         MATRIX                      'WATER'/'SOIL
  21-23         3         LEVEL                       'LOW'/'MED'
ICP SERIAL DILUTIONS DETAIL RECORDS:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT

   1-5          5         'IX
   6-7          2         FORM SUFFIX
    8           1         'D'
   9-10         2         ANALYTE SYMBOL              CHARACTER
  11-22        12         INIT SAMPLE (I)             NUMERIC 9.2
   23           1         INIT SAMPLE FLAG (C)        ' B' /'U' /BLANK
  24-35        12         SERIAL DILUTION (S)         NUMERIC 9.2
   36           1         DILUTION FLAG (C)           'B'/'U'/BLANK
  37-41         5         PERCENT DIFFERENCE          NUMERIC 3.1
   42           1         QUALIFIER  (Q)               'E'/BLANK
  43-44         2         METHOD (M)                  METHOD CODE/'NR'
                                   H-18                                ILM01.0

-------
                                    FORM X
INSTRUMENT DETECTION LIMITS (QUARTERLY) HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT
   1-5
   6-7
    8
   9-16
  17-28
  29-40
  41-52
 5
 2
 1
 8
12
12
12
 'X
FORM SUFFIX
 'H'
DATE
ICP ID NUMBER
FLAME AA ID NUMBER
FURNACE AA ID NUMBER
MM/DD/YY
CHARACTER
CHARACTER
CHARACTER
INSTRUMENT DETECTION LIMITS (QUARTERLY) DETAIL RECORDS:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT
   1-5
   6-7
    8
   9-10
  11-17
  18-19
  20-27
  28-29
 5
 2
 1
 2
 7
 2
 8
 2
'X
FORK SUFFIX
'D'
ANALYTE SYMBOL
WAVELENGTH
BACKGROUND
IDL
METHOD (M)
CHARACTER
NUMERIC 4.2
'BS'/'BD'/'BZ'/BLANK
NUMERIC 6.1
METHOD CODE/'NR'
                                   H-19
                                                        ILM01.0

-------
                               FORM XI (PART 1)
ICP TNTERELEMENT CORRECTION FACTORS (ANNUALLY) HEADER RECORD:

COLUMN(S)    LENGTH       CONTENTS                    FORMAT
   1-5
   6-7
    8
   9-20
  21-28
 5
 2
 1
12
 8
'XI(l)'
FORM SUFFIX
'H'
ICP ID NUMBER
DATE
CHARACTER
MM/DD/YY
ICP INTERELEMENT CORRECTION FACTORS (ANNUALLY)  DETAIL RECORDS:

COLUMN(S)    LENGTH       CONTENTS                    FORMAT
   1-5
   6-7
    8
   9-10
  11-17
  18-19
  20-29
  30-31
  32-41
  42-43
  44-53
  54-55
  56-65
  66-67
  68-77
 5
 2
 1
 2
 7
 2
10
 2
10
 2
10
 2
10
 2
10
'XI(l)'
FORM SUFFIX
'D'
ANALYTE SYMBOL
WAVELENGTH
ELEMENT
ELEMENT
ELEMENT
ELEMENT
ELEMENT
ELEMENT
ELEMENT
ELEMENT
ELEMENT
ELEMENT
1 SYMBOL
1 FACTOR
2 SYMBOL
2 FACTOR
3 SYMBOL
3 FACTOR
4 SYMBOL
4 FACTOR
5 SYMBOL
5 FACTOR
CHARACTER
NUMERIC 4,2
AL
NUMERIC SI.7
CA
NUMERIC SI. 7
FE
NUMERIC SI.7
MG
NUMERIC SI.7
CHARACTER
NUMERIC SI.7
NOTE:   ELEMENTS 1,2,3 and 4 SYMBOL can only be AL,  CA,  FE and MG
        respectively.  ELEMENT 5 Symbol can be any other analyte symbol.
                                   H-20
                                                        ILM01.0

-------
                               FORM XI (PART 2)
ICP INTERELEMENT CORRECTION FACTORS (ANNUALLY) HEADER RECORD:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT
1-5
6-7
8
9-20
21-28
5
2
1
12
8
FORM SUFFIX
'H'
ICP ID NUMBER
DATE
                                                     CHARACTER
                                                     MM/DD/YY
ICP INTERELEMENT CORRECTION FACTORS (ANNUALLY) DETAIL RECORDS:

COLUMN(S)    LENGTH      CONTENTS                    FORMAT
1-5
6-7
r
w
9-10
11-17
18-19
20-29
30-31
32-41
42-43
44-53
54-55
56-65
66-67
68-77
5
2
1
2
7
2
10
2
10
2
10
2
10
2
10
                         FORM SUFFIX
                         'D'
                         ANALYTE SYMBOL
                         WAVELENGTH
                         ELEMENT
                         ELEMENT
                         ELEMENT
                         ELEMENT
                         ELEMENT
                         ELEMENT
        1 SYMBOL
        1 FACTOR
        2 SYMBOL
        2 FACTOR
        3 SYMBOL
        3 FACTOR
                         ELEMENT 4 SYMBOL
                         ELEMENT 4 FACTOR
                         ELEMENT 5 SYMBOL
                         ELEMENT 5 FACTOR
CHARACTER
NUMERIC 4.2
CHARACTER
NUMERIC SI.7
CHARACTER
NUMERIC SI.7
CHARACTER
NUMERIC SI.7
CHARACTER
NUMERIC SI.7
CHARACTER
NUMERIC SI.7
                                   H-21
                                             ILM01.0

-------
                                   FORM XII
ICP LINEAR RANGES (QUARTERLY) HEADER RECORD:

COLUMN(S)    LENGTH       CONTENTS
   1-5
   6-7
    8
   9-20
  21-28
 5
 2
 1
12
 8
                                      FORMAT
'XII  '
FORM SUFFIX
'H'
ICP ID NUMBER
DATE
CHARACTER
MM/DD/YY
ICP LINEAR RANGES (QUARTERLY) DETAIL RECORDS:

COLUMN(S)    LENGTH       CONTENTS
                                      FORMAT
   1-5
   6-7
    8
   9-10
  11-16
  17-27
  28-29
 5
 2
 i
 2
 6
11
 2
'XII  '
FORM SUFFIX
'D'
ANALYZE SYMBOL
INTEGRATION TIME
CONCENTRATION
METHOD (M)
(ICP IS ASSUMED
IF BLANK)
CHARACTER
NUMERIC 3.2  (SECONDS)
NUMERIC 9.1
'NR'/BLANK
                                   H-22
                                                        ILM01.0

-------
                                   FORM XIII


PREPARATION LOG HEADER RECORD:

COLUMN(S)    LENGTH       CONTENTS                   FORMAT

  1-5           5         'XIII  '
  6-7           2         FORM SUFFIX
    8           1         'H'
 9-10           2         METHOD                     METHOD  CODE
PREPARATION LOG DETAIL RECORDS:

COLUMN(S>    LENGTH       CONTENTS                    FORMAT

   1-5          5         'XIII  '
   6-7          2         FORM SUFFIX
    8           1         ' D'
   9-15         7         SPA  SAIIPLE  17J:.3ER          CHARACTER
  16-23                   PREP DATS                   MM/DD/YY
  24-28         5         WEIGHT                     NUMERIC 2.
  29-32         4         VOLUME                     NUMERIC 4
                                   H-23                                ILM01.0

-------
                                   FORM XIV
ANALYSIS RUN LOG HEADER RECORD:
COLUMN(S)
LENGTH
CONTENTS
FORMAT
1-5
6-7
8
9-20
21-22
23-30
31-38
5
2
1
12
2
8
8
                          'XIV   '
                          FORM SUFFIX
                          'H'
                          INSTRUMENT ID NUMBER
                          METHOD
                          START DATE
                          END DATE
                                        CHARACTER
                                        METHOD CODE
                                        MM/DD/YY
                                        MM/DD/YY
ANALYSIS RUN LOG DETAIL RECORDS:
COLUMN(S)
LENGTH
CONTENTS
FORMAT
1-5
6-7
8
9-16
17-24
25-28
29-35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
5
2
1
8
8
4
7
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
                          ' XIV   '
                          FORM SUFFIX
                          'D'
                          EPA SAMPLE NUMBER
                          DILUTION FACTOR
                          TIME
                          PERCENT RECOVERED
                          ANALYTE (AL)
                          ANALYTE (SB)
                          ANALYTE (AS)
                          ANALYTE (BA)
                          ANALYTE (BE)
                          ANALYTE (CD)
                          ANALYTE (CA)
                          ANALYTE (CR)
                          ANALYTE (CO)
                          ANALYTE (CU)
                          ANALYTE (FE)
                          ANALYTE (PB)
                          ANALYTE (MG)
                          ANALYTE (MN)
                          ANALYTE (HG)
                          ANALYTE (NI)
                          ANALYTE (K)
                          ANALYTE (SE)
                          ANALYTE (AG)
                          ANALYTE (NA)
                          ANALYTE (TL)
                          ANALYTE (V)
                          ANALYTE (ZN)
                          ANALYTE (CN)
                                        CHARACTER
                                        NUMERIC 5.2
                                        HHMM
                                        NUMERIC S4.;
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                        "X"/BLANK
                                   H-24
                                                          ILM01.0

-------
                                COMMENT RECORDS
COMMENT records are optional for any FORM ID/FORM SUFFIX group. There may be
up to 4 COMMENT records per group.  They must come after the DETAIL records
and be formatted as follows:
COLUMN(S)    LENGTH      CONTENTS                    FORMAT '

   1-5          5         FORM ID
   6-7          2         FORM SUFFIX
    8           1         'C'
   9-78        70         COMMENTS                    FREE FORM TEXT
The text may be in paragraph form if desired, but must be contained in columns
9 through 78 only.  The key fields must be repeated in columns 1 through 8 of
each line.
                                   H-25                                ILM01.0

-------
                                  SECTION III
                             FORMAT B SPECIFICATION
1.    Introduction

1.1   This constitutes the implementation of the EPA standard for media and
      record formats to be used in transmission of analytical results for the
      CLP inorganics program.  The following points should be noted:

      1.1.1   The column border "|" is placed between fields to permit these
              records  to be  prepared by programs written for laboratory and
              quality  assurance automation systems, and the detection of
              possible field shift.  They also assist in visual clarity.

      1.1.2   Record formats contain sequence numbers and checksums  to be
              consistent with requirements for a future error-free
              telecommunications format.

2.    Record Types

2.L   There are four groups of record, types  in the reporting format, as shc';.-ii
      below.   Detailed record formats follow.

Type    Name                Contents

10      Run Header          Contains information pertinent to the
                            whole  production run.   See production
                            run definition below.

20      Sample Header       Contains sample-identifying information,
                            or corresponding information for calibra-
                            tions,  QC samples,  instrument performance
                            checks, etc.

30      Results Record      Contains any final result on a sample,
                            calibration or QC sample and identifying
                            information.

90      Comments Record     Contains free-form comments and/or other
                            miscellaneous information.

2.2   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 indentifier to
                                       H-26                        ILM01.0

-------
      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 initialicalibration 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.

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 arc not
      allowed.

      A type 16 record must immediately follow the type 10 record.  Further
      occurrences of the type 15 record in the file are not allowed.

      A type 20 record must immediately follow the type 16 record as a header
      for the calculated run-wide instrument parameters (the quarterly and
      annual instrument parameters).   This is the only occurrence of type 20
      record that does not correspond to an actual analysis in the run.
      Therefore, The only fields that are not blank in this occurrence of type
      20 record are the RECORD TYPE ("20"), EPA SAMPLE NUMBER ("SIDICF"), and
      WAVELENGTH COUNT.

      A r.inimum of one group of type  32, 34, and 35 records -".?•; ir:::r.3C.lately
      follow the type 16 record.  Each group consists of a type 32 record
      immediately followed by a type  34 record immediately followed by a type
      35 record.  The information in each group must pertain to one and only
      one analyte's wavelength.  The  number of groups must be equivalent to the
      WAVELENGTH COUNT value and the  number of wavelengths used for analysis in
      the run.  The last group must immediately be followed by the first type
      20 record which corresponds to  an actual analysis of an instrument
      calibration standard.   After the appearance of the second 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 sample is
      represented by a group composed of a type 20, 21, 22, 28 records, which
      holds sample level identifying information, followed, by a ninirnvm of one
      group composed of type 30, 31,  and 33 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 WAVELENGTH COUNTER must


                                        H-27                        ILM01.0

-------
      have a value equivalent to the number of type 30 groups associated with
      each type 20 record.

      Except for the first type 20 record,  all type 20 records should occur in
      the order of sample analysis.  Excluding the first type 20 record, the
      number of type 20 records in a file (run) must be equivalent to the
      number of entries reported on Form XIV for that run.

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.

5.     File/Record Integrity

      All record types must contain the following check fields to ens'ure file
      and record integrity:

Record       Field
Positior.     Length     Contents                      Remarks

 1-2          2         Record type or identifier     "10" or as appropriate

72-74         3         Record sequence number        000-999, repeated as
                        within file                   necessary
                                                                             ^t.
75-78         4         Record checksum               Four hexadecimal digits ;
                                                      Calculation algorithm to
                                                      be supplied

79-80         2         Contains CR and LF

6.     Dates and Times

      Wherever a date or time-of-day is required, the information consists of
      successive groups of two right justified decimal digits each, separated
      by "[".  Dates are given in the order YY MM DD, and times as HH MM.  All
      hours will be given as 0 to 23 using a 24 hour clock and will be local
      time.  Since some computers generating the date and time sequence may
      have difficulty producing leading zeros, these will not be required.

7.     Field format listed as CHARACTER may contain any standard ASCII character
      other than "j".  It must be left justified and padded to the right with
      blanks.  Field format listed as NUMERIC may contain numeric digits, a
      decimal point, and a leading plus or minus sign.  It must be right
      justified and padded to the left with blanks.  Except where specified
      otherwise, the numeric field must contain the minimum significance
      specified in the forms instruction of Exhibit B.  If more significance is
      used, it must be applied uniformly.  Exponent fields are numeric fields


                                        H-28                        ILM01.0

-------
      that can contain only digits and plus or minus sign.  No decimal is
      allowed.  For field formats that are specified as a choice of stings or
      characters, only those choices shown may be used.

8.     Multiple Volume Data

      There is no requirement under this format that all the data from an
      entire sample delivery group fit onto a single diskette.  However, each
      single production run must fit onto a single diskette if possible.
      However, 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.  If it is necessary to
      split the data from a single sample onto multiple diskettes, then the
      type 20 and following type records for that sample must be repeated.  In
      this situation, it is mandatory that columns 7-30, which collectively
      identify the sample, be identical in each diskette.

8.     Record Listing

      The remainder of this section contains detailed specifications for every
      record required for a full run.
   The checksum is defined to be the sum of the thirty-five (35) INTEGERS that
make up the data in columns 1 to 70 when the data is represented in the format
35A2 on processors which store the data bytes in left to right order.  The sura I:,
taken module 65536 (2  ) and represented as four (4) hexadecimal digits.  For
processors which use an A70 character representation of the data, the checksum is
the sum of all the even character position values plus 256 times the sum of all
odd character position values.
                                       H-29                        ILM01.0

-------
         FORMAT  OF THE PRODUCTION RUN FIRST  HEADER RECORD CTYPE
COLUMNS
LENGTH
1 -
3 -
4 -
6 -
7 -
9 -
10 -
12 -
13 -
15 -
16 -
18 -
19 -
2
3
5
6
8
9
11
12
14
15
17
18
20
2
1
2
1
2
1
2
1
2
1
2
1
2
        CONTENTS


RECORD  TYPE
ii | ii

ANALYSIS  START YEAR
it I it

ANALYSIS  START MONTH
n I ii

ANALYSIS  START DAY
n I it

ANALYSIS  START HOUR
it I n

ANALYSIS  START MINUTE
n I n

METHOD
21
22
? i
32
35
36
42
43
58
59
69
70
71
72
75
- 21
- 30
- 31
- 34
- 35
- 41
- 42
- 57
- 58
- 68
- 69
- 70
- 71
- 74
- 78
1
9
T_
^
1
6
1
15
1
10
1
1
1
3
4
ii I ii
BLANK
"!"
MANAGER'S ITIT"' T :'
n I n
LAB CODE
n I n
BLANK
n | n
INSTRUMENT ID
n 1 n
BLANK
n | n
RECORD SEQUENCE NUMBER
RECORD CHECKSUM
 FORMAT


"10"


YY


MM


DD


HH


MM


n pny it ptiyti^ii/uppity "Ftfl"

"AM"/"CV"/"AV"/"C"/
"CA"/"AS"/"T"
                                                         CbARACTER
                                                         CHARACTER
                                                         NUMERIC
                                                         NUMERIC
                                       H-30
                                                      ILM01.0

-------
        FORMAT OF THE PRODUCTION RUN SECOND HEADER RECORD  (TYPE  16)
COLUMNS
LENGTH
1
3
4
6
7
9
10
12
13
15
16
18
19
21
22
23
24
25
26
27
28
53
r4

72
75
- 2
- 3
- 5
- 6
- 8
- 9
- 11
- 12
- 14
- 15
- 17
- 18
- 20
- 21
- 22
- 23
- 24
- 25
- 26
- 27
- 52
- 53
- 70
- 71
- 74
- 78
2
1
2
1
2
1
2
1
2
1
2
1
2
1
1
1
1
1
-
1
23
1
17
1
3
4
       CONTENTS


RECORD TYPE
it I it

ANALYSIS END YEAR
ii I ti

ANALYSIS END MONTH
ti I ii

ANALYSIS END DAY
it | n

ANALYSIS END HOUR
« I n

ANALYSIS END MINUTE
n I it
         AUTO-SAMPLER USED
         n | n

         INTERELEMENT CORRECTIONS  APPLIED  "Y"
         n I n

         BACKGROUND CORRECTIONS  APPLIED    "Y"
         ..,..

         RAW DATA GENERATED
         n | it

         LABORATORY KJ'u-S
         n I n

         BLANK
         n | ii

         RECORD SEQUENCE NUMBER
         RECORD CHECKSUM
 FORMAT


"16"


YY


MM


DD


HH


MM


"Y"/ BLANK


      "
                                                            "
                                                      NUMERIC
                                                      NUMERIC
  Enter "Y" if an auto-sampler  is  used with equal analysis time and
  intervals between analysis.

  These are the answers to the  first two questions on the Cover Page.   "Y"
  equals "YES", and "N" equals  "NO".
  This is the answer to the third  question on the Cover Page.
  "YES", and "A" equals BLANK.
                                                      "B" equals
                                     H-31
                                                   ILM01.0

-------
              FORMAT OF THE SAMPLE HEADER DATA RECORD (TYPE 20)
 COLUMNS
        LENGTH
1
3
4
6
7
15
16
17
18
25
26
32
33
38
39
41
42
44
^ ^
^ 7
48
50
51
53
54
55
56
57
58
66
67
70
71
72
75
« O
- 3
- 5
- 6
- 14
- 15
- 16
- 17
- 24
- 25
- 31
- 32
- 37
- 38
- 40
- 41
- 43
- ^4
- -16
- 47
- 49
- 50
- 52
- 53
- 54
- 55
- 56
- 57
- 65
- 66
- 69
- 70
- 71
- 74
- 78
2
1
2
1
8
1
1
1
7
1
6
1
5
1
2
1
2
1

„
'
1
2
1
1
1
1
1
8
1
_2
1
1
3
4
       CONTENTS


RECORD TYPE
ti I ti

BLANK
n I ii

EPA SAMPLE NUMBER
n I n

MATRIX
n I n

BLANK
n I n

CASE NUMBER
n I n

BLANK
n I n

ANALYSIS YEAR
n I n

ANALYSIS MONTH
                    I! | It

                    ANALYSIS HOUR
                    n I n

                    ANALYSIS MINUTE
                    n | n

                    BLANK
                    n I n

                    SAMPLE UNIT CODE
                    n | n

                    SAMPLE SIZE

                    (WET WEIGHT OR INITIAL VOLUME)
                    n i n

                    ANALYTS WAVELENGTH  COUNT
                    n i n
                    n i n

                    RECORD SEQUENCE NUMBER
                    RECORD CHECKSUM
 FORMAT


"20"





CHARACTER
                                                    CHARACTER





                                                    YY


                                                    MM


                                                    DD


                                                    HH


                                                    MM





                                                    "G"/"M"


                                                    NUMERIC



                                                    NUKERIC
                                                    NUMERIC
                                                    NUMERIC
2

3
   EPA Sample Number as appears on Form XIV  except for the first type 20
   record.  The first type 20 record must have  an EPA Sample Number of
   "SIDICF"
"1" equals "WATER", and "F" equals  "SOIL"

"G" equals grains, and "M" equals mL.
                                      H-32
                                                           ILM01.0

-------
•
                FORMAT OF  THE  SAMPLE HEADER DATA RECORD CTYPE 21)
COLUMNS   LENGTH           CONTENTS                    FORMAT

 1-2     2      RECORD TYPE                        "21"
 3-3     1      " | "
 4-4     1      BLANK
 5 -  5     1      " | "
 6-6     1      CONCENTRATION LEVEL               "M"/"L" X
 7-7     1      " | "
 8-16     9      BLANK
17-17     1      "|"
18-23     6      SAS NUMBER                        CHARACTER
24-24     1      "|"
25-34    10      LAB SAMPLE ID                     CHARACTER
35-35     1      "|"
36-36     1      "| "
37-38     2      PREPARATION  YEAR                  YY
39-39     1      "|"
40-41     2      PREPARATION  MONTH                 MM
42-42     1      "|"
43-44     2      PREPARATION  DAY                   DD
- 5 - 45     I      r | "
-16-46     i      ELAN:;
-7 - 47     1      " | "
48-49     2      LAB RECEIPT  YEAR                  YY
 0-50     1      " | "
 1-52     2      LAB RECEIPT  MONTH                 MM
53-53     1      "| "
54-55     2      LAB RECEIPT  DAY                   DD
56-56     1      "|"
57 - 68    12      SOLUTION SOURCE                   CHARACTER
69-69     1      "| "
70-70     1      BLANK                  "            NUMERIC
71-71     1      "| "
72-74     2      RECORD SEQUENCE NUMBER            NUMERIC
75-78     4      RECORD CHECKSUM                   NUMERIC
      •M" equals "MEDIUM",  and "L"  equals "LOW"
                                        H-33                     ILM01.0

-------
              FORMAT OF THE SAMPLE  HEADER DATA RECORD  (TYPE 22)
COLUMN'S
LENGTH
       CONTENTS
 FORMAT
 1-2
 3-3
 4-40
41 - 41
42 - 46
47 - 47
48 - 55
56 - 56
57 - 64
65 - 65
66 - 70

71 - 71
72 - 74
75 - 78
  2
  1
 37
  1
  5
  1
  8
  1
  8
  1
  5

  1
  3
  4
RECORD TYPE
ii I it
BLANK
it I ii
FINAL VOLUME  IN ML
it I ii
DILUTION FACTOR
it I it
BLANK
ii I ii
PERCENT SOLIDS

ii I ii
RECORD SEQUENCE NUMBER
RECORD CHECKSUM
"22"



NUMERIC

NUMERIC
NUMERIC
(to one  decimal place)

NUMERIC
NUMERIC
                                      H-34
                                                    ILM01.0

-------
              FORMAT OF THE SAMPLE HEADER DATA RECORD (TYPE 28)
 COLUMNS    LENGTH          CONTENTS                    FORMAT

  1-2      2      RECORD TYPE                       "28"
  3-3      1      " | "
  4-13     10      CONTRACT NUMBER                   CHARACTER
 14-14      1      "|"
 15-19      5      SOW NUMBER                        CHARACTER
 20-20      1      "|"
 21-26      6      SDG NUMBER                        CHARACTER
 27  -  27      1      "|"
 28-29      2      PREPARATION START HOUR            HH ^
 30-30      1      "I"
 31  -  70     40      BLANK
 71-71      1      "|"
 72-74      3      RECORD SEQUENCE NUMBER            NUMERIC
 75-78      4      RECORD CHECKSUM                   NUMERIC


L This is  the hour at  which the preparation is started.  It is used to
  differentiate between different batches on the same dav.
                                     H-35                    ILM01.0

-------
              FORMAT OF THE SAMPLE HEADER DATA RECORD (TYPE 30)
 COLUMNS
  1
  3
  4
  5
  6
 15
 16
 25
 26
 31
 32
    2
    3
    4
    5
   14
   15
   24
   25
   30
   31
   34
LENGTH

  2
  1
  1
  1
  9
  1
  9
  1
  5
  1
  3
35
36
42
43
46
47
48
49
55
56
59
60
61
62
67
68
71
72
75
- 35
- 41
- 42
- 45
- 46
- 47
- 48
- 54
- 55
- 58
- 59
- 60
- 61
- 66
- 67
- 70
- 71
- 74
- 78
1
6
1
3
1
1
1
6
1
3
1
1
1
5
1
3
1
3
4
       CONTENTS

RECORD TYPE
it | it
ANALYTE IDENTIFIER TYPE
it I it
ANALYTE CAS NUMBER
it I ii
BLANK
ii I ii
UNITS
it | ii
CONCENTRATION QUALIFIER
                    n I ti
                    CONCENTRATION

                    EXPONENT
                    ii i n
                    VALUE DESCRIPTOR
                    (i | ir
                    AMOUNT ADDED OP, TRUE VALUZ,

                    EXPONENT
                    n i n
                    QC VALUE DESCRIPTOR
                    n i ii
                    QC VALUE

                    EXPONENT
                    n i n
                    RECORD SEQUENCE NUMBER
                    RECORD CHECKSUM
 FORMAT

"30"

11 C "/"I" ^"

CN FOR CYANIDE



"UG/L"/"MG/KG"

"BDL"/"LTC"/"FQC"/
"GTL"/"NAR"/"RIN"/
11 REX "/BLANK 2

NUMERIC
"E"/ BLANK
NUMERIC

II mil / II 7711 3

NUMERIC
11 E"/ BLANK
NUMERIC
                                                    NUMERIC
                                                    "E"/ BLANK
                                                    NUMERIC

                                                    NUMERIC
                                                    NUliSRIC
1
2
"C" is used for all analytes except  cyanide.
"BDL" means below detection limit
                                       "I"  is used for cyanide.
   "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.  This is only used  for the first,  second,  and third addition  of
   MSA.  The zero addition must  contain the final sample result in ug/L or
   mg/Kg, as appropriate, whether the final result is reported on Form I or
   not.
   Note that there is no absolute equivalent to the final concentration on
   Form VIII in Format B.
                                      H-36
                                                           ILM01.0

-------
   "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 repreparatior
   of same sample

Note that, except for "NAR", none of these codes relief the contractor form
reporting a valid result.  They only explain why or if the result is
qualified.

3  nrpii 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.

4  "P" equals percent, "C" equals correlation coefficient, and "L" equals
   control limit
                                     H-37                    ILM01.0

-------
             FORMAT OF THE SAMPLE HEADER DATA RECORD  (TYPE
COLUMNS
 1 -
 3 -
 4 -
 5 -
 6 -
2
3
4
5
6
 7-7
 8-15
15
16
18
19
29
30
38
39
49
50
58
59
69
70
71
72
75
- 15
- 17
- 18
- 28
- 29
- 37
- 38
- 48
- 49
- 57
- 53
- CC.
- 69
- 70
- 71
- 74
- 78
LENGTH

  2
  1
  1
  1
  1

  1
  8

  1
  2
  1
 10
  1
  8
  1
 10
  1
  8
  1
 10
  1
  1
  1
  3
  4
                    CONTENTS
RECORD TYPE
n I ii
TYPE OF DATA
n I n
TYPE OF VALUE
             n I n
             ANALYTE WAVELENGTH

             n I n
             BLANK
             n I n
             FIRST INSTRUMENT VALUE
             n I n
             BLANK
             it f n
             SECOND INSTRUMENT VALUE
             ii I ii
             BLANK
             t< I n
             THIRD INSTT.U1L'-NT VALUE
             n I n
             BLANK
             n I n
             RECORD SEQUENCE NUMBER
             RECORD CHECKSUM
 FORMAT

"31"

"W"


"I»/"A"/"H" 1

NUMERIC
(to two decimal places



NUMERIC 2



NUMERIC 2



NUI-IEKTC 2
                                                     NUMERIC
                                                     NUMERIC
  "C" equals concentration in ug/L, "T" equals concentration  in  ug/250mL/
  "F" equals concentration in ug/50 mL, "B" equals absorbance, "I"  equals
  intensity, end "A" equals peak area in cm2.
  This is used to report replicate injection or exposures.  If a single
  instrument measurement is used, then enter it in the first  instrument
  value field, and leave the second and third empty.  If duplicate
  instrument measurements are used, then enter them in the  first and second
  instrument value fields in the order of their analysis, and leave the
  third field empty.  If triplicate instrument measurements were taken,  the
  enter the values in the order of their analysis.
                                     H-38
                                                       ILM01.0

-------
             FORMAT OF THE  SAMPLE HEADER DATA RECORD (TYPE 32)
COLUMNS   LENGTH           CONTENTS                    FORMAT

 1-2     2      RECORD TYPE                       "32"
 3-3     1      "|"
 4-7     4      BLANK
 8-8     1      " | "
 9-10     2      INTEGRATION TIME CODE             "IT"
11-11     1      "|"
12-17     6      INTEGRATION TIME IN SECONDS       NUMERIC
18-18     1                                         "E"/BLANK
19-21     3      EXPONENT                          NUMERIC
22-22     1      "|"
23 - 70    48      BLANK
71-71     1      "|"
72-74     3      RECORD SEQUENCE NUMBER            NUMERIC
75-78     4      RECORD CHECKSUM                   NUMERIC
                                     H-39                     ILM01.0

-------
             FORMAT  OF  THE SAMPLE HEADER DATA RECORD  (TYPE 33)
COLUMNS
LENGTH
1
3
4
13
14
15
16
26
27
28
29
35
36
39
40
41
42
48
49
52
53
59
60
63
64
71
72
75
- 2
- 3
- 12
- 13
- 14
- 15
- 25
- 26
- 27
- 28
- 34
- 35
- 38
- 39
- 40
- 41
- 47
- 48
- 51
- 52
- 58
- 59
- 62
- 63
- 70
- 71
- 74
- 78
2
1
9
1
1
1
10
1
1
1
6
1
3
1
1
1
6
1
3
1_
6
1
3
1
7
1
3
4
       CONTENTS


RECORD TYPE
it I ii

ANALYTE NAME
ti I it

RAW DATA AVERAGE QUALIFIER
it I it

RAW DATA AVERAGE
it I ii

RAW DATA %RSD QUALIFIER
ii I it

RAW DATA %RSD


EXPONENT
ii I it

QC LIMIT QUALIFIER
ii I ii

QC LOWER LIMIT
                    EXPONENT

                    "I"
                    QC UPPER LIMIT
                    EXPONENT
                    ii I ii

                    CRDL IN UG/L
                    ii I ii

                    RECORD SEQUENCE NUMBER
                    RECORD CHECKSUM
 FORMAT


"33"


CHARACTER
                                                      NUMERIC


                                                      "M"/BLANK


                                                      NUMERIC
                                                      "E"/BLANK
                                                      NUMERIC
                                            NUMERIC
                                            "E"/BLANK
                                            NUMERIC


                                            NUMERIC
                                            "E"/BLANK
                                            NUMERIC


                                            NUMERIC


                                            NUMERIC
                                            NUMERIC
                                                                         711 2
  "U" means less than  the IDL,  "B" means less the CRDL and greater than or
  equal to the IDL,  "L"  means greater than the linger  r^nge.

  "S" flag is not applicable for Format B.
                                     H-40
                                                    ILM01.0

-------
             FORMAT OF  THE  SAMPLE HEADER DATA RECORD  (TYPE  34)
COLUMNS
 1
 3
 4
14
15
 2
 3
13
14
22
LENGTH


  2
  1
 10
  1
  8
23
24
30
31
34
35
41
42
45
46
60
61
r- •?
64
66
67
I69

71
72
75
- 23
- 29
- 30
- 33
- 34
- 40
- 41
- 44
- 45
- 59
- 60
- 62
- 63
- 65
- 66
- 68
- 69
- 70
- 71
- 74
- 7B
I
6
1
3
1
6
1
3
1
14
1
2
~
2
1
2
1
1
1
3
4
       CONTENTS


RECORD TYPE
it I it

BLANK
it i it

ANALYTE WAVELENGTH


ii i it

IDL
n i ii

BLANK
n i n

LINEAR RANGE


EXPONENT
n i n

BLANK
n i n

YEAR COMPUTED
:- | IT

KONTH COMPUTED
it i n

DAY COMPUTED
n i n

BLANK
n i n

RECORD SEQUENCE NUMBER
RECORD CHECKSUM
 FORMAT


"34"
                                                      NUMERIC
                                                      (to two decimal  places


                                                      NUMERIC 1
                                                      NUMERIC
                                                      "E"/BLANK
                                                      NUMERIC
                                                      YY


                                                      KL-:

                                                      DD
                                                      NUMERIC
                                                      NUMERIC
  The IDL must be a whole number  for all analytes except for mercury.
  Mercury must be reported to  one decimal place.
                                     H-41
                                          ILM01.0

-------
              FORMAT OF THE SAMPLE HEADER DATA RECORD  fTYPE  35)
COLUMNS
     LENGTH
1
3
4
7
8
10
11
13
14
16
17
19
20
22
23
32
33
- 2
- 3
- 6
- 7
- 9
- 10
- 12
- 13
- 15
- 16
- 18
- 19
- 21
- 22
- 31
- 32
- 40
2
1
3
1
2
1
2
1
2
1
2
1
2
1
9
1
8
               CONTENTS

        RECORD TYPE
        it I it
        TYPE OF  CORRECTION
        it I ii
        TYPE OF  BACKGROUND
        it I it
        BLANK
        it I it
        YEAR COMPUTED
        it I ii
        MONTH COMPUTED
        ii I ii
        DAY COMPUTED
        ii I ii
        CAS # OF INTERFERING ANALYTE
        ii I M
        ANALYTE  WAVELENGTH
                                     FORMAT

                                    113511

                                    "ICP'V'BG" I

                                    "ES"/"BD"/"BZ"



                                    YY

                                    MM

                                    DD

                                    CHARACTER

                                    NUMERIC
                                    fto rvo decir.r.;
42
48
49
52
53
71
72
75
47
43
51
52
70
71
74
78
 6
 1
 3
 1
18
 1
 3
 4
CORRECTION  FACTOR

EXPONENT
it 1 ti
BLANK
ti I it
RECORD SEQUENCE  NUMBER
RECORD CHECKSUM
NUMERIC
"E"/BLANK
NUMERIC
NUMERIC
NUMERIC
  "ICP" indicates interelement correction,  while "BG" indicates a backgroun
  correction.
                                      H-42
                                                          ILM01.0

-------
             FORMAT OF  THE  SAMPLE HEADER DATA RECORD (TYPE 90)
COLUMNS   LENGTH           CONTENTS                    FORMAT

 1-2     2      RECORD TYPE                       "90"
 3-3     1      " | "
 4-70    67      ANY COMMENT                       CHARACTER
71-71     1      " | "
72-74     3      RECORD SEQUENCE NUMBER            NUMERIC
75-78     4      RECORD CHECKSUM                   NUMERIC
                                     H-43                    ILM01.0

-------
             FORMAT  OF  THE SAMPLE HEADER DATA RECORD  (TYPE  92)
COLUMNS   LENGTH           CONTENTS                    FORMAT

 1-2     2       RECORD TYPE                       "92"
 3-3     1       "I"
 4-12     9       COLOR BEFORE                      CHARACTER
13-13     1       "| "
14-22     9       COLOR AFTER                       CHARACTER
23-23     1       "|"
24-29     6       CLARITY BEFORE                    CHARACTER
30-30     1       "|"
31-36     6       CLARITY AFTER                     CHARACTER
37-37     1       "| "
38-43     6       TEXTURE                           CHARACTER
44-44     1       "|"
45-45     1       ARTIFACTS                          "YES"/BLANK
46-46     1       "|"
47 - 70    24       BLANK
71 - 71     1       "|"
72-74     3       RECORD SEQUENCE NUMBER            NUMERIC
75-78     4       RECORD CHECKSUM                   NUMERIC
                                     H-44                     ILM01.0

-------
9.    Example of the Sequence of Record Types in a Production Run

10  Contains run header  information.   Occurs once per  run.
15  Contains additional  run header  information.   Occurs  once per run.

20  Acts  as  a header for the following instrument parameters information.   Occurs
    once  per run.   EPA SAMPLE NUMBER  equals  "SIDICF".  WAVELENGTH COUNTER  equals
    the number  of the type  32,  34,  and 35  groups  that  follow.

      32   Contains integration time information for  the  wavelength on the  type  34
          and 35 records that follow.   Occurs once for each wavelength used in  the
          run.
      34   Contains the IDL  and Linear range  information  for the  first wavelength
          used  in the run.
      35   Contains the background and interelement correction information  for the
          first wavelength  used in  the run.
      32   Contains integration time information for  the  wavelength on the  type  34
          and 35 records that follow.   Occurs once for each wavelength used in  the
          run.
      34   Contains the IDL  and Linear range  information  for second wavelength used
          in the run.
      35   Contains the Background ana luizerelement correction information  for
          second wavele.  gth used in the run.

      32
      33

      35

          Continues as many times as  the value of the  WAVELENGTH COUNTER on the
          previous type  20  record.

20  Contains header information for sample and QC data.   Occurs  as many times as
    there are entries on Form XIV for the  run.

21  Contains additional  information for analytical and instrument QC samples.
    I.'ili  always follow type 20 record.
22  Contains additional  information for analytical samples.   Will usually  follow
    type  21  record.   It  is  not required for  instrument QC samples such as
    Instrument  Calibration  Standards  (S),  ICV,  ICB,  CCV,  CCB,  ICSA,  ICSAB,  CRI,
    and CRA.

28  Contains additional  information for analytical samples.   Will usually  follow
    type  22  record.   It  is  not required for  instrument QC samples such as
    Instrument  Calibration  Standards  (S),  ICV,  ICB,  CCV,  CCB,  ICSA,  ICSAB,  CRI,
    and CRA.

      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  follow type  30 record.   Occurs
          once  per type  30  record.
                                         H-45                        ILM01.0

-------
      33  Reports the average  of instrumental data,  instrument  related qualifier,
          and the QC limits  and qualifier  for the QC VALUE  reported on previous
          type 30 record.  Will always  follow type  31  record.   Occurs .. :>nce per
          type 30 record.
      30  Values  for the next  analyte wavelength being measured.
      31  Values  for the next  analyte wavelength being measured.
      33  Values  for the next  analyte wavelength being measured.
      30
      31
      33
          Continues  as many  times as the value of the  WAVELENGTH  COUNTER on the
          previous type 20 record.
20  Next Sample Header record  - The following applies  to  the next sample data.
21
22
28
      30
      31
      33
      30
      31
      33    etc.
20
21
22
2£
      30
      31
      32
                  etc.
I
                                         H-46                         ILM01.0

-------