United States
Environmental Protection
Oflice of Water
Washington. DC 20460
October 1998
Procuring Analytical Services:
Guidance for Industrial Pretreatment
Md RMpOHM for Analytic of EMwvnt »nd Marin* Wotef S*mp»*«
    lor Trac* Ntotel* by l«OO-S*c*»t Mtthodt
           IqjteX ««-•»«• wl t»
                11 "I in

This document was prepared under the direction of William A. Telliard of the Engineering and
Analysis Division within EPA's Office of Water. This document was prepared under EPA
Contract No. 68-C-98-139 by DynCorp Information & Engineering Technology.
Questions concerning the guidance in this document should be addressed to:

      William A. Telliard
      Engineering and Analysis Division (4303)
      U.S. Environmental Protection Agency
      401 M Street. SW
      Washington. DC 20460
      Fax:  (202)260-7185
Requests for additional copies of this document should be directed to:

      Water Resource Center
      Mail Code RC-4100
      401 M Street. SW
      Washington. DC 20460
      (202) 260-7786 or (202) 260-2814

       When Should You Outsource Analytical Services''

       Developing an Analytical Contract  	
                        ._._	5
       Client Information 	5
       Number, Frequency, and Matrix of Samples	5
       Project Background 	6
Defining the Project Parameters
       Project Schedule and Data Turnaround Times  	7
       Methodology  	7
Selecting Appropriate Methods	8
3.2.1   Methods Approved for Nationwide Use  	8
3.2.2   Methods Approved for Specific Industrial Categories	9
3.2.3   Other Methods	9
Determining Appropriate Quality Control Requirements  	10
3.3.1   Established Laboratory Quality System	\\
3.3.2   Purity and Traceability of Reference Standards	11
3.3.3   Calibration Range 	11
3.3.4   Linearity of Calibration 	12
3.3.5   Calibration Verification	13
3.3.6   Method Detection Limit, Minimum Level, or Quantitation Limit	13
3.3.7   Initial Precision and Recovery	13
3.3.8   Ongoing Precision and Recovery   	14
3.3.9   Analysis of Blanks	14
3.3.10  Matrix Spikes and Labeled Compound Spikes  	15
3.3.11  Statements of Data Quality for Recovery of Spiked Analytes
       or Labeled Compounds in Samples	15
Writing the Contract  	16
3.4.1   Deliverables	16
3.4.2   Data Turnaround Times	17
3.4.3   Liquidated Damages and Penalties 	18
3.4.4   Reanalysis Costs  	18
3.4.5   Dilutions	18
Developing a Bid Sheet 	19
Estimating Costs  	20

4      Soliciting and Awarding the Contract 	21
       4.1     Identifying Capable Laboratories and Transmitting the Requirements	22
       4.2     Evaluating Bids  	22
       4.3     Conducting Responsibility Determinations	23
              4.3.1   Method Performance Data	24
              4.3.2   Performance Evaluation Sample Results	24
              4.3.3   Certifications  	25
              4.3.4   References 	25
              4.3.5   Prequalification Analyses  	26
       4.4     Awarding the Contract	28

5      Transporting Samples and Communicating with the Laboratory  	29
       5.1     Transporting and Tracking Samples  	29
       5.2     Communicating with the Laboratory	31

6      Reviewing Analytical Data 	33
       6.1     Purity and Traceability of Reference Standards	33
       6.2     Calibration Range  	33
       6.3     Linearity of Calibration  	34
       6.4     Calibration Verification	34
       6.5     Method Detection Limit.  Minimum Level, or Quantitation Limit 	34
       6.6     Initial Precision and Recovery	35
       6.7     Ongoing Precision and Recovery	35
       6.8     Analysis of Blanks	36
       6.9     Matrix Spikes and  Labeled Compound Spikes  	37
       6.10   Statements of Data Quality for Recovery of Spiked Analytes
              or Labeled Compounds in Samples	38
       6.1 1    Field  Duplicates	38

7      References  	41
Appendix A:  Analytical Services Request Form Example

Appendix B:  Bid Sheet Example

Appendix C:  Technical Proposal Request Example and Scoring Sheet

Appendix D:  General Laboratory Audit Checklist Example

Appendix E:  Data Inspection Checklist Example

This document is intended to provide pretreatment authorities and industrial users (Il's) with
guidance for procuring analytical services necessary to support Clean Water Act programs. It was
developed in response to a 1996 EPA survey of 14 industrial pretreatment programs in
California. Indiana, and Virginia. That survey, which included site visits and interviews with
personnel responsible for implementing each program, was conducted as pan of EPA's Common
Sense Initiative for the Metal Finishing Industry. The primary objective of the survey was to
identify initiatives that could improve pretreatment program performance and environmental

One of the initiatives identified was development of guidance for pretreatment authorities and
IlJs on contracting for analytical services. Specific issues raised during the pretreatment program
visits included the need for guidance on when to use a contract laboratory rather than perform in-
house analyses, how to structure requests for analytical services, and how to evaluate laboratory
performance. This document provides guidance on these issues, and covers the entire laboratory
contracting process, from development of the analytical requirements and solicitation of the
contract, to evaluation of laboratories and data review. Although the primary objective in
developing this guidance was to respond to needs identified under the Common Sense Initiative
for the Metal Finishing Industry-, this guidance also is applicable to other direct and indirect
dischargers with little experience in laboratory contracting.

Pretreatment authorities and  IDs require analysis of source w ater. in-process waste streams, and
treated effluent for a variety of reasons. The most common is evaluating the lU's final discharge
for compliance with its permit limits. Other reasons for conducting analyses include: meeting
permit requirements that are  not expressed as permit limits, gathering information necessary for a
permit application or permit  renewal, determining causes of excursions, and evaluating the
efficiency of existing or proposed treatment systems.

The pollutants and pollutant  concentrations targeted for analyses by the pretreatment authority or
IU are likely to vary, depending on  the character of the waste stream and the type of pretreatment
processes. Guidance for determining appropriate target pollutants and pollutant concentrations
are beyond the scope of this document. This manual is intended to provide pretreatment
authorities and lUs with guidance for procuring laboratory services for analysis of pollutants that
already have been targeted.

A fundamental decision when planning for laboratory analyses is whether the analyses should be
performed by an in-house laboratory or whether the project should be contracted out to a
commercial laboratory. Two factors impact whether the in-house laboratory can accept an
analytical project: capacity and capability. An in-house laboratory must have: (1) the capacity to
analyze the quantity of samples requested within the required time period, and (2) the
instrumentation expertise to perform the required analyses.

If the laboratory operated by pretreatment authority or ILJ does not have the capacity or the
capability to handle the analytical requirements, the pretreatment authority must decide whether
it is appropriate to outsource the  analyses or to increase the capacity or capability of the in-house
laboratory. This decision is a  function of time and cost.

The time required to increase the laboratory's capacity or capability will include the time
required to identify and obtain the necessary equipment and instrumentation, the time necessary
to bring instrumentation on-line,  the time necessary to train staff in new procedures, and the time
required to perform any necessary start-up tests and demonstrations of analyst capability. Each of
these must be completed prior to project deadlines.

Determining the cost-effectiveness of increasing capacity or developing additional capability is a
complex issue, however, the equation below provides a framework for this decision:
                                                      R * U)O

  I  = cost of required instrumentation
  5  = years before instrument depreciation reaches 1009r

  F, = square footage required for instrument and work area

  F, = square-foot cost of total floor space per year

  A = number of analysts required to perform the analysis

  S  = annual salary of analysts

  P  = percentage of each analyst's time dedicated to the  new capability (for example. 0.80)

  C = number of hours of calibration and maintenance required per year

  T  = hourly cost of technician for maintenance, if not the primary analyst

  R  = annual cost of required reagents and other supplies, such as pressuri/ed gas or liquid

  U = increase in annual utility cost to power the instrument and provide air conditioning

       i; Anal\tu til .SVrvict'A  (.'ntuiaiu c t<» ImliiMruil Preirt'iiuneni Pr
  O  = overhead factor for management (generally 1.2 - 2.0)

  N  = number of analyses per year anticipated over five years

If x •  the average per-sample analysis cost at a commercial laboratory for the same analysis, the
preireatment authority or IU should consider expanding the POTW or industrial facility
laboratory accordingly, and began analyzing such samples in-house. However, if x  • the average
per-sample analysis cost at a commercial laboratory for the same analysis, the pretreatment
authority or II  should consider contracting the analyses out to a commercial laboratory. This
guidance manual addresses the subsequent steps that should be taken to ensure delivery of quality
data after the decision to contract out has been made.

Although most organi/.ations have established procedures and policies governing the purchase of
services and supplies, these procedures seldom lend themselves to the purchase of analytical
services, primarily due to the difficulty in defining the required services. This chapter provides a
basic framework for defining the technical and contractual requirements associated with
purchasing analytical services.

3.1    Defining the Project Parameters

Many laboratories have recognized the importance of customer service and employ staff who are
trained to assist clients in defining the requirements. Other laboratories, large and small, rely
solely on the client to define the specific requirements. Still another group of laboratories, albeit
a small group, perform analyses with little regard to the client's actual needs. One of the problems
that arises  when the client's requirements are poorly defined is the use of inappropriate  methods.
As detailed in Section 3.2. approved methods must be used for compliance monitoring  purposes.
It is not the laboratory's place to decide that an alternate method, even if it is an alternate EPA
method, is "close enough."  The permittee is responsible for defining and ensuring that  contract
laboratories adhere to requirements that are consistent with the terms of their permit. The first
step in developing an analytical services contract is identifying the who. what. why. when, and
how of the project. The remainder of this subsection provides pretreatment authorities and It's
with guidance for defining these project parameters.

3.1.1   Client Information
Who is the name of the client, whether this is a single POTW. the pretreatment authority that
oversees several POTWs. or the ILT. Client information should include specific contact  points for
use by the  laboratory, including the following:
•      The name of the person responsible for communicating with the laboratory regarding
       shipping delays and broken samples (a sample control contact)
•      A technical contact for resolution of analytical questions  or problems (a technical contact)

•      An administrative contact for invoicing and payment (a billing contact)

Include with contact name their address, telephone and fax numbers, and email, as these contacts
often are in different locations.

3.1.2  Number, Frequency, and Matrix of Samples
What describes the samples to be analyzed, including:

•      Number of samples

•      Frequency with which samples will be sent to the laboratory (for example, five  samples
       per week for eight weeks); this is particularly important for long-term projects,  as it
       allows laboratories to accurately evaluate whether they have the capacity to analy/e  the

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samples are being analyzed by various methods to characterize a waste stream, will help the
laboratory provide the data you want. To determine that the analytical laboratory used the correct
methods and did not perform any unapproved method modifications, the laboratory should be
audited frequently.

3.1.4  Project Schedule and Data Turnaround Times
When specifies the following dates:

•      The date by which bids should be received from laboratories interested in the project (this
       is discussed in greater detail in Section 3.5)

•      The approximate date that the samples will be shipped to the laboratory, including the
       means of shipment  (such as overnight delivery, hand-delivery, or laboratory pick-up)

•      The date the analytical results are required by the client (data turnaround time)

The data turnaround time specifies the number of calendar days after the laboratory receives the
sample that the results are to be received by the client. Common data turnaround times arc 30 to
45 days after the laboratory receives the last sample. The data turnaround time can be specified
on a method-specific basis, and often is a function of a reporting deadline under a permit.
Pretreatment authorities and IDs can reduce analytical costs by providing the laboratory w ith as
much time as possible to provide the data.  If liquidated damages or penalties apply to the
analytical contract, specific information concerning what penalties will be applied  if the
analytical laboratory fails to meet the required data turnaround times should be included.

3.1.5  Methodology
How is perhaps the most important question to be addressed in the analytical services contract.
and specifies the required methodology, the quality assurance/quality control (QA/QC). and the
reporting format. The analytical requirements must be very specific, and include the following:

•      Method source and number. The majority of methods applicable to wastewater analysis
       are listed in Tables  IA through ID at 40 CFR Part 136. Common method sources for
       wastewater analyses include EPA methods. Standard Methods. American Society for
       Testing and Materials (ASTM) methods, and U.S. Geological Survey (IJSGS) methods.
       Other relevant method sources include Solid Waste methods (SW-846) and Association
       of Official Analytical Chemists (AOAC) methods. Be sure to include the method revision
       date, if applicable, as analytical and QC procedures change as methods are  revised. If the
       samples  are to be analyzed for compliance monitoring purposes, the method must be
       approved for use under the terms of the discharge permit. Selection of appropriate
       methods is discussed in detail in Section 3.2.

•      Holding time. The  holding time of a sample is the maximum amount of time that can
       elapse between sample collection and  analysis for an analysis to be considered valid. The
       sample holding time for each method is different, and always  should be specified. Table
       II at 40 CFR Part 136 specifies the  "Required Containers.  Preservation Techniques, and
       Holding  Times" for routine parameters. Samples should be analyzed as soon as possible
       after collection. Samples for many  analyses are not stable for long after collection, and
       daily shipment of samples to the laboratory should be considered. Delays in sampling and

Pun tinny AntilMiciil Sen-ices: (iiiulaiHf tor Industrial Preirftilnu-nt f'Hiy
       sample shipment may necessitate specifying a "contract" holding time in the contract.
       based on the analytical holding time minus any time required for sample shipment.

       Quality assurance/quality control. To ensure that data from wastewater analyses are
       valid and not a result of contamination or improperly calibrated instruments, laboratories
       must take rigorous QA/QC steps when performing the analyses. While EPA 6(K)- and
       1600-series methods specify the level of QA/QC to be performed, other methods are not
       as explicit regarding the QA/QC requirements. Specific guidance for defining QA/QC
       requirements is provided in Section 3.3. To ensure that the proper QA/QC steps are being
       routinely followed, all data must be reviewed and validated, and the laboratory should be
       audited at a frequency commensurate with the length, scope, and importance of the

•      Deliverable* and reporting format. The laboratory also needs to know how the data are
       to be reported, what information to provide in addition to the results, and how many
       copies of the data package are  required. Deliverables are discussed in greater detail in
       Section 3.4.1.

3.2   Selecting Appropriate Methods

The methods approved by EPA for nationwide use and for specific industrial categories under the
Clean Water Act (CWA) will satisfy the analytical needs of most pretreatment authorities and
Il's. However, some industrial wastewaters may cause matrix-specific analytical problems, while
others may contain analytes of interest for which there are no EPA-approved methods. Sections
3.2. 1 - 3.2.3  present information on methods generally applicable to analysis of industrial
wastewaters.  Exceptions to the information presented below may arise in specific permit
situations: therefore, all permittees must be familiar with the terms and requirements of their
individual permits.

3.2.1   Methods Approved for Nationwide Use
I'nder the authority of CWA Section 304(h). EPA promulgates test procedures for  measuring
regulated pollutants in wastewater, and publishes them for nationwide use at 40 CFR Part 1 36.
NPDES permittees are required to use the methods approved at 40 CFR Part 1 36. or industry-
specific methods (see Section 3.2.2) to demonstrate compliance with NPDES permit limitations.
The methods listed at 40 CFR Pan 1 36 apply to the following method categories:

•      Biological test procedures

•      Inorganic test procedures

•      Test procedures for non-pesticide organic compounds

•      Test procedures for pesticides

•      Radiological test procedures

The methods approved for use at 40 CFR Part 1 36 include EPA methods. Standard Methods.
ASTM methods, and USGS methods.  Pretreatment authorities and lUs should be aware that the
results of any final effluent analyses that arc conducted with test procedures approved at 40 CFR
Part 1 36 must be reported with the data submitted in the permit-required monitoring report, even
if those analyses were not required in the permit. Results of analyses conducted with non-

approved methods or conducted on unregulated waste streams are not required to be reported (40
CFR Part 122.41).

The 40 CFR Part 136 methods are applicable to a wide range of industrial effluents and were
used to generate the data necessary for developing each of the effluent guidelines promulgated by
EPA. Despite this wide applicability, EPA recognizes that these analytical methods may fail to
yield useful results  when used on certain sample matrices. EPA is prepared to consider claims
that the effluent is compliant in those instances in which the effects of the sample matrix make
measurements difficult or impossible. All such claims must be supported by specific analytical
data that demonstrates  reasonable, but unsuccessful,  attempts have been made to overcome
matrix interferences.

3.2.2  Methods Approved for Specific Industrial Categories
In addition to methods approved at 40 CFR Part  136 for all wastewaters. EPA promulgates
methods to measure pollutants specific to an industrial category. These methods are also
promulgated under  the authority of CWA Section 304(h). but are proposed and  promulgated only
for use by specific industries at 40 CFR Parts 405 - 471. along with that industry's categorical
effluent limitations and guidelines.

For the purpose of this document, all methods approved for nationwide use at 40 CFR Part 136
or for industry-specific use  at 40 CFR Parts 405-471 may be referred to as the "304(h) methods."

3.2.3  Other Methods
If no 304(h) approved methods are applicable to the analytes of interest or the matrix, selection
of non-approved  methods may be necessary (note, however, that non-304(h) methods, such as
Solid Waste (SW-846) methods, cannot be used  when a comparable 304(h) method is available
unless the discharge permit explicitly allows the  use of such alternate methods). In such
instances, appropriate QA/QC procedures must be performed and low  level detection limits must
be achievable as necessary to demonstrate compliance with applicable permit limits. As
mentioned above, the permitting authority must approve the use of these methods in advance.

3.2.4  Method Modifications
Many of the methods approved at 40 CFR Part 136 provide flexibility to modify the method to
improve method performance, reduce cost, or adapt the method to address more difficult
matrices. Example improvements include the use of additional cleanup techniques, alternative
gas chromatography or liquid chromatography columns, and more specific detectors. However.
the modifications to these methods cannot result in any  degradation of method performance and
the laboratory used  to analyze the samples with a modified method must first demonstrate that
the modifications result in performance equivalent to that of the base method. At present, the
only  methods approved at 40 CFR Part  136 that provide this flexibility are the 600- and 1600-
series methods. Modifications to any other methods must be approved by the permitting authority
prior to implementation.

In October 1995. EPA  proposed the use of several new and modified methods for monitoring
inorganic pollutants at  60 FR 53988. Most of the methods included in  that proposed rule provide

t'r<>( \inny. Analytical .SVrwcrv Cmuliiiu r (or Industrial Pretretitntcnt
laboratories with the flexibility described above. In March 1997. EPA proposed to expand and
extend this flexibility to nearly all methods approved for use at 40 CFR Part 136. Details of this
proposal, known as the streamlining initiative, are given at 62 FR 14976.

If methods approved at 40 CFR Part 136 fail to yield acceptable results in a specific matrix, the
pretreatment authority or IU should consider modifying an approved method to yield improved
and acceptable performance. Similarly, if methods approved at 40 CFR Part 136 are not
applicable to a specific pollutant that the pretreatment authority or IU wishes to  monitor.
approved methods applicable to similar pollutants may exist. In such cases, these entities may
w ish to consider modifying an approved method to target the pollutant of interest. In all cases.
the modifications must cither be allowed in the approved version of the method  through the
flexibility described above, or must be approved by the  permitting authority. Permittees seeking
approval of method modifications are encouraged to use the streamlining proposal at 62 FR
14976 as a basis for initiating discussions with their permitting authority.

3.3    Determining Appropriate Quality Control Requirements

Pretreatment authorities and IDs are strongly encouraged to use the guidelines provided in this
section, or similarly developed standard protocols, to establish strict data quality requirements for
the analyses performed by contract laboratories. These QA/QC requirements subsequently
provide end-users of the data with standard data inspection and acceptance procedures and
minimi/e differences that might otherwise result between data reviewers and laboratories.

A standardi/ed QA/QC approach should take the form of performance specifications for each
method and should contain the following elements.

•      Established laboratory quality system

•      Purity and traceability of reference standards

•      Calibration Range

•      Lineariu of calibration

•      Calibration verification

•      Method detection  limit  (MDL). minimum level (ML), or quantitation limit

•      Initial precision and recovery (IPR)

•      Ongoing precision and recovery  (OPR)

•      Analysis of blanks

•      Recovery of matrix spikes and labeled compound spikes

•      Statements of data quality for recovery of spiked analytes or labeled compounds in

•      Analysis of field duplicates

These elements are an integral part of many recent EPA methods. However, earlier methods may
not specify some or all of these elements. As such, you should ensure that any QA/QC elements


                                                              I)e\<'l<>l><»v nn .\nal\ncal ('untrm I
not specified in the method(s) required under the contract are specified in the contract itself. A
summary of each of the elements is provided below. Guidance on assessing data using these
QA/QC results is provided in Section 6. The analytical laboratory should be audited to ensure
that QA/QC procedures arc being implemented on a daily basis. The frequency of these audits
should be commensurate with the length, scope, and importance of the project. Audit information
on a laboratory may be obtained by contacting  the QA Officers or inspection staff in state and
EPA regional offices with jurisdiction.

3.3.1  Established Laboratory Quality System
Any laboratory that performs analyses to support permitting compliance and monitoring should
be required to  have an established quality system that is compliant with ISO/IEC Guide 25:
General Requirements for the Competence of Calibration and Testing Laboratories (Reference
3). This document sets forth general QA/QC guidelines for laboratories to follow, including
personnel, analysis environment, and equipment requirements, requirements for internal reviews
and audits, and the other requirements specified in Sections 3.3.2  - 3.3.11. It is essential for
laboratories  to employ comprehensive quality systems throughout the duration of the contract to
ensure data validity. The laboratory should implement the quality system, and should otherwise
use safe handling procedures and employ accepted Good Laboratory Practices in  all aspects of
laboratory performance.

3.3.2  Purity and  Traceability of Reference Standards
The accuracy of any non-absolute empirical measurement depends on the reference for that
measurement.  In determining pollutants in water or other sample matrices, laboratories must
calibrate analytical instruments and analytical processes with a known reference material. Most
of the methods approved at  40 CFR Part 136 require that the standards used for calibration and
other purposes be of known purity and be traceable to a reliable reference source. The ultimate
source for reference materials is typically EPA or the National Institute for Standards and
Technology  (NIST).

3.3.3  Calibration Range
Instrument calibration is required to establish the relationship of analyte concentration to
instrument response, and is  subsequently used  for the quantitative analysis of field samples. This
relationship  is  determined by analyzing a series of reference standards at different concentration
levels (calibration points) which encompass  the expected concentration range of field samples
and the expected linear range of the analytical instrument.

Most EPA methods  for organic pollutants specify a minimum of three calibration points. Newer
methods for  inorganic pollutants also  specify a minimum of three calibration points. The lowest
of these points is required to be at or near the MDL. The highest is required to be near the upper
linear range  of the analytical system, and the third point is approximately midway between the
two. The lowest calibration  point should never be greater than five times the MDL and should
ideally be within three times the MDL. The results for the lowest calibration standard are the
principal means by which to assure that measurements at levels near the MDL are reliable. The
EPA Office  of Water uses the lowest calibration standard as one means of defining the ML of

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The flexibility in selecting the levels of the calibration points in many EPA methods has led to a
wide variety of calibration ranges as each laboratory may determine its own calibration range.
Some laboratories establish a relatively narrow calibration range, such as a five-fold increase in
concentration, because it makes it simpler to meet the linearity specifications of the method.
Other laboratories choose wider calibration ranges in order to minimize the number of samples
that have to be diluted and reanalyzed because the concentration of one or more analytes exceeds
the calibration range.  Understanding these differences is particularly important if a narrow
concentration range results in increased costs of sample dilution or if the laboratory's
concentration range prevents the laboratories from achieving the required detection or
quantitation limits.

3.3.4  Linearity of Calibration
The relationship between the response of an analytical instrument to the concentration or amount
of an analyte introduced into the instrument is referred to as the "calibration curve."  An
analytical instrument can be said to be calibrated when this relationship has been established. The
ratio of the response of the instrument to the concentration of the analyte introduced into the
instrument is called the response factor (RF). relative response factor (RR). or calibration factor
•      Relative response (RR) for isotope dilution calibration
•      Response factor (RF) for internal standard calibration
•      Calibration factor (CF) for external standard calibration

A plot of instrument response and concentrations is generated, and the linearity of response is
measured by the shape of the calibration curve. While the shape of calibration curves can be
modeled by quadratic equations or higher order mathematical functions, most analytical methods
recommend establishing a linear calibration. The advantage of the linear calibration is that  the RF
or RR  represents the slope of calibration curve, simplifying calculations and data interpretation.
The  16(K) Series Analysis Methods contain specific criteria for determining the linearity of
calibration curves determined by either an internal or external standard technique. When  the
applicable criterion is met. the calibration curve is sufficiently  linear to permit the laboratory' to
use an average RF or  RR. and  it is assumed that the calibration curve is a straight line that passes
through the /.ero//ero calibration point. Linearity is determined by calculating the relative
standard deviation (RSD) of the RF or RR for each analyte and comparing this RSD to the
specified limit.

The number of calibration points  is dependent on the error of the measuring technique.
Measurement technique error is determined by ( 1 ) calibrating the instrument at the ML of
quantitation and a minimum of two additional points, and (2) determining the RSD of the RR.
RF, or CF. For most analyses,  such as the determination of semi-volatile organic compounds by
extraction, concentration, and gas chromatography. the measuring instrument is calibrated, and
sample preparation processes are excluded from  the calibration process; for others, such as the
determination  of purgeable organic compounds by purge-and-trap gas chromatography.
calibration encompasses the entire analytical process. Table 3-1 below gives  the number of
calibration points required depending  on the calibration linearity.

                                                                            Analytical (.'onrrai t
Table 3-1.     Minimum Number of Points Required for Calibration
Percent RSD'
2 - <10
Minimum Number of Calibration
'Percent RSD shall be determined from the calibration linearity test for replicate measurements at a fixed concentration
'Assumes linearity through the origin (0,0) For analytes for which there is no origin (such as pH), a two-point calibration shall be
performed In almost no cases should only one calibration point be used One calibration point most oflen leads to senous error

The maximum RSD specification is applicable to calibration with three or more calibration
points. Alternatively, a minimum correlation coefficient for the linear relationship may be
specified, below which the calibration linearity is not acceptable. If the calibration curve is non-
linear, a second order (y = ax: +  bx + c) calibration curve may be used. Calibration functions
higher than the second order are  not allowed.

3.3.5  Calibration Verification
Calibration verification involves the  analysis of a single standard, typically in the middle of the
calibration range, at the beginning (and in some cases, at the end) of each analytical shift. The
concentration of each analyte in  the reference standard is determined using  the initial calibration
curve, and the results are compared with method specifications. This test is used to periodically
verify that instrument performance has not changed significantly.  Specifications  for calibration
verification are developed to define the allowable deviation of the RR. RF,  or CF of the
calibration verification standard  from the mean RR, RF. or CF of the initial calibration; or in
cases where the initial calibration curve did not meet linearity specifications, deviation from a
prior calibration verification standard or a single point of the calibration curve.

3.3.6  Method Detection Limit,  Minimum Level,  or Quantitation Limit
The Minimum Level (ML) is defined as the lowest level at which the entire analytical system
gives a recognizable signal and,  in most instances, an acceptable calibration point. Procedures for
determining an MDL are provided at 40 CFR Part 136, Appendix B. Most of the 40 CFR Part
136. Appendix A. methods contain MDLs, although few of the methods explicitly require
laboratories to demonstrate their ability to achieve these MDLs. Laboratories that wish to
practice any method on a routine basis should be required  to demonstrate that they can measure
pollutants at the MDL or the detection limit specified in the  method. Performance of an MDL
study in accordance with the 40 CFR Part 136. Appendix B, procedure is one means of
demonstrating such proficiency.

3.3.7  Initial Precision and Recovery
The IPR test  is used as an initial demonstration of a laboratory's capability to produce results at
least as  precise and accurate as those of other laboratories. The IPR test is also used to
demonstrate that a method modification will produce results as precise and accurate as results
produced  by the approved (reference) method. The IPR test consists of four aliquots of reagent
water spiked with the analytes of interest and with either surrogate compounds, or for isotope
dilution analysis, with the labeled compounds. The spike concentration of the target analytes in


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the spike solution may van. between one and five times the lowest concentration used to
establish the calibration curve (such as one to five times the ML). The spiked aliquots are carried
through the entire analytical process. The mean concentration (x) and the standard deviation (si
are calculated for each analyte and compared to the specifications in the method. The IPR lest is
performed by the laboratory before it uses a method or a method modification for analysis of
actual field samples.

3.3.8  Ongoing Precision and Recovery
The OPR test, sometimes termed a "laboratory control sample," "quality control check sample."
or "laboratory -fortified blank." is used to ensure that the laboratory remains in control during the
period that samples are analyzed, and separates laboratory performance from  method
performance on the sample matrix. The test consists of a single aliquot of reagent water spiked
with the analyte(s) of interest, which is carried through the entire analytical process with each
batch of samples. Typically, the concentration  of the target analyte(s) in the OPR sample is
between one and five times the lowest concentration used in the calibration curve (such as one to
five times the ML). The results of the OPR are compared with method specifications.

3.3.9  Analysis of Blanks
Blanks are analyzed either periodically or with each sample batch, and are analyzed to
demonstrate that no contamination is present that would affect the analysis of standards and
samples for the analytes of interest. Different types of blanks are analyzed to more precisely
determine if and  when contamination was introduced. The follow ing are different types of blanks
that may be required by the methods selected for analysis:

•      Initial and continuing calibration blanks (ICB/CCB). These blanks are required for all
       calibrated instrumentation. Deionized distilled water that contains the same reagents as
       the prepared samples is analyzed after analysis of the calibration standard to demonstrate
       the absence of carryover from the standard into the sample.

•      Preparation blanks. Deionized distilled water is carried through preparation and
       analysis,  using the same sample preparation, reagents, and analysis methods used for field
       samples.  Preparation blanks are prepared and analyzed with each  sample set to
       demonstrate that contamination  is not introduced during any of the sample preparation or
       analysis steps.

•      Blanks. Blanks are required for titrimetric and gravimetric methods, and any other
       method which does not require instrument calibration or sample preparation. Deionized
       distilled water which is not prepared, but contains the same reagents as the prepared field
       samples,  is analyzed to determine if the method analyte or other interferences are present
       in the laboratory environment, reagents, or apparatus.

•      Trip blanks. Trip blanks  are generated by the sampler for volatile compounds and low
       level metals, such as mercury. These blanks consist of vials of water that accompany each
       sample shipment to determine whether contamination has occurred from permeation of
       volatile organic compounds or low-level metals during sample transportation.

•      Equipment blanks. These blanks are sampler generated to determine contamination
       from compositor sampling line or tubing.

                                                              Developing tin Anal\nml
The types of blanks required for analysis is dependent on the requirements of each method, and
the period or hatch size for which these blanks are required is also defined in each method. QC
acceptance criteria are given in most methods. Generally, the source of contamination in a blank
analysis must be identified and eliminated before the analysis of standards and samples may
begin. Samples analyzed with an associated contaminated blank must be reanalyzed and. for
contaminated preparation blanks, reprepared.

3.3.10 Matrix Spikes and Labeled Compound Spikes
The non-isotope dilution methods require that laboratories spike the analytes of interest into a
second aliquot of a field sample and analyze this spiked sample with the non-spiked field sample.
The purpose of spiking the sample (often termed a matrix spike) is to determine if the method is
applicable to the sample matrix in question. Most EPA methods were developed for the analysis
of wastewater effluent or treated drinking water samples, and may not be appropriate for in-
process samples. While many wastewater methods were tested using effluents from a w ide
variety of industries, samples from some sources may not  yield acceptable results. It is therefore
important to evaluate method performance in the sample matrix of interest.

If the recovery of the matrix spike is within the limits specified in the method, then the method is
judged to be applicable to that sample matrix. If. however, the recovery of the spike is not  within
the recovery range specified, either the method does not work on the sample, or the sample
preparation process is out of control. If the method is not appropriate for the sample matrix, then
changes to the method are required. Matrix spike results are necessary in evaluating the modified
method. If the  analytical process is out of control, the laboratory must take immediate corrective
action before any more samples are analyzed.

To separate indications of method performance from those of laboratory performance, the
laboratory should prepare and analyze a  QC check standard consisting of a spike of the analytes
in reagent water. If the results for the QC standard are not within the range specified, then  the
analytical system must be repaired and the sample and spiked sample analyses repeated. If the
recovery1  of this spike is within the range specified, then the analytical process is judged to be in

3.3.11 Statements of Data Quality for Recovery of Spiked Analytes or Labeled
       Compounds  in Samples
EPA methods specify that after the analyses of five spiked samples, a statement of data quality  is
constructed for each analyte. The statement of data quality for each analyte is computed as the
mean percent recovery plus and minus two times the standard deviation of percent recovery for
each analyte. The statements of data quality should then be updated by the laboratory after each
five to ten subsequent spiked sample analyses.

For non-isotope dilution results, the statement of data quality can be used to estimate the true
value of a reported result and to construct confidence bounds around the result. For example, if
the result reported for analysis of phenol is 25 ^g/L. and the statement of data quality for phenol
is 70*/r ± 15^ (i.e.. the mean recovery is 709J- and the standard deviation of the recovery is \5c/c).
the true value for phenol will be in the range of 28 - 43 Mg/L, with 959r confidence. This range is
derived as follows:


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       Lower limit = [(25 -=- 0.7) - (25 x 0.3)]  = [35.7-7.5] =  28 /ug/L
       Upper limit = [(25 -=-0.7) + (25 x 0.3)]  = [35.7 + 7.5] = 43 ^g/L

Statements of data quality for isotope dilution methods are based on the recoveries of the labeled
compounds. L'sing an isotope dilution method, the sample result has already been corrected for
the recovery of the labeled analog of the compound. Therefore, for a reported result for phenol of
25 ,ug/L where the standard deviation of the labeled phenol recovery is l5c/(. the true value for
phenol will be in the range of 21.25-28.75 ^g/L. with 957f confidence, derived as follows:

       Lower limit = [25 - (25 x 0.15)] =21.25^g/L
       Upper limit = [25 + (25 x 0.15)]  = 28.75
3.4   Writing the Contract

Before writing a contract for any analytical services, consult with the appropriate legal staff at the
pretreatment authority or IU. A well-written contract will include the who, what,  why, when, how
issues outlined in Section 3.1. above. It also will address your right to review the data as needed.
the timeliness of payment to the laboratory, and your ultimate right to determine that the work
does not meet the requirements established in the contract. A general format for an analytical
services contract is provided in Appendix A. Please note that the information requested in
Appendices A and B may not be  adequate for competitive, written solicitations to multiple
laboratories: depending on the project, more information may need to be requested in order to
ensure the laboratory will be able to meet the requirements of the analytical contract.

The best way to ensure that the pretreatment authority or IU  gets the required data within the
required time period is to specify these requirements in detail in the contract. Combined with a
careful analysis of the requirements discussed in Sections 3.1 to 3.3. a well-written contract can
minimi/e or eliminate many common problems in procuring analytical services. It should enable
the client to obtain technically sound, legally defensible, and timely analytical data to meet a
variety of compliance monitoring needs. Once generated, the basic form of the contract should be
viewed as a dynamic document that is routinely updated to clarify ambiguities that arise during
its implementation.  (Note: Active contracts typically require a formal contract modification that
is approved by both sides before  its terms can be changed: expired or closed contracts can be
modified before they are re-issued.)

General issues that should be specified in the contract are detailed in  Sections 3.4.1 - 3.4.5.

3.4.1  Deliverables
The pretreatment authority or IU must ensure that the laboratory provides data that can be easily
reviewed and that includes non-quantitative information related to the analyses,  such as
descriptions of any problems encountered. Laboratories should be required to have the following
data from samples analyzed available for review:

•      Summary  reports of all analytical results in hardcopy and electronic data format. The
       summary report must contain a summary of analytical results  for all QC and field
       samples.  For the IPR analysis, the spiking level, individual results of the four replicates.


                                                              Developing an .Am'M'( ul (. Oninu 1
       and the mean recovery and relative standard deviation of the tour replicates must he
       reported. For the OPR. standard reference material (SRM)/quality control sample (QCS).
       and calihration verification analyses, the true (or expected) concentration of the QC
       sample, the measured concentration, and  the percent recovers' must he reported. For
       MS/MSD analyses, the background concentration of the field sample, the spiking level.
       the individual results of the MS and MSD analyses, the percent recovery  for the MS and
       MSD, the average concentration found in the MS/MSD samples, and the RPD between
       the MS and MSD should be reported. The results for all  other QC. including calibration
       and blanks, also must be reported.
•       A list of the sample numbers analyzed and a run chronology.
•      Copies of all  raw data, including quantitation reports, strip charts, spectra, bench sheets
       and laboratory notebooks showing tare and sample weights, sample volumes, and other
       data that will allow the final results reported to be traced back to the analytical steps
       performed. Each data element shall be clearly identified  in the laboratory's data package.
•      A written report that details any problems associated with the analysis of the samples.
•      A detailed written description of any approved modifications to  the procedures specified
       in the referenced method that were used during the performance of this study.

With the possible exception of electronically formatted data. EPA recommends that pretreatment
authorities and lUs require all of the  above deliverablcs as part of the data submission by their
contract laboratory(ies).

3.4.2  Data Turnaround Times
The required data turnaround must be stated clearly in the contract. Unless the pretreatment
authority or IU can guarantee to the laboratory that the samples will arrive when the laboratory
opens in the morning, the data turnaround time calculations should consider the day that the
sample is received at the laboratory "day zero." and the following day as "day one." In addition to
stating the time that the laboratory has to generate and deliver the data, it may be useful to  assign
some specific consequences to the possibility of late delivery. One approach is to assess a penalty
of some percentage of the analytical price per day of lateness. In the past. EPA has used values of
\7i or 29r  per day after the due date that the data were delivered. Obviously, lateness penalties
should not be assessed if the delays were due to changes in the requirements made after the
samples were sent, or to the fact that the methods requested were not  applicable to the samples.
Many of the remedies to matrix problems cannot be expected to be carried out in the original
turnaround time assigned to the sample unless those remedies were explicitly detailed and
required in the contract (see Section 3.1.2). However, after you have established that your
samples can routinely be analyzed by the requested methods, lateness becomes an issue of
laboratory management practices, not sample matrix.

If it is anticipated that some samples will have to be analy/ed in a faster than normal turnaround
time during the performance of the analytical contract, a cost for these shorter turnaround time
samples should be negotiated prior to award of a contract. The bids should be broken out into
time periods that apply to the turnaround needs of the project (i.e. 2-day turnaround. 5-day
turnaround. 10-dav turnaround, etc.).

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3.4.3  Liquidated Damages and Penalties
In many cases, prctrcatment authorities and Il's  should consider including penalty or damage
clauses in their contracts as incentives to preclude laboratories from defaulting on the contract.
submitting data late, or performing analyses improperly. Due to the nature of the services
provided, it is often difficult to assess actual damages caused by improperly performed analyses.
Liquidated damages often are used in many contracts in lieu of actual damages. Liquidated
damages typically specify that, if the laboratory  fails to deliver the data specified in the
deliverables section of the contract, or fails to perform the services within the specified data
turnaround time, the laboratory  will pay a fixed, agreed, price to compensate the organi/ation to
whom the services should have  been delivered. For example, some EPA contracts specify that
the laboratory will pay. as fixed, agreed, and liquidated damages, 2^ of the analysis price per
calendar day  of delay, to a maximum reduction of 50^ of the analysis price.

Other types of damages  that should be considered and may be included in the contract include
costs for resampling, fines incurred as a result of improperly conducted analyses, and
administrative costs associated with the evaluation and processing of unacceptable data.

It is important to note that if the damages section of the contract is too stringent, the contract may
pose too great a risk for  commercial laboratories to accept. Therefore, the contract should specify
that the laboratory will not be charged with liquidated damages when the delay in delivery or
performance  arises out of causes beyond the control and without the fault or negligence of the
laboratory. It also may be necessary to limit damages to a certain dollar value or scope.

3.4.4  Reanalysis Costs
Every laboratory periodically produces data that are of little use for the intended purpose. While
well-run laboratories will contact the client as soon as they identify the problem and work with
the client to make the best of the situation, the pretreatment authority or IU still may find itself
with no useful data and a deadline approaching.  The contract should stipulate that the laboratory
will reanaly/e samples at no cost to the client  if the problems are due to laboratory error.  It also
should state that the client has the right to inspect the results, and if they do not meet the
requirements in the contract, the client has the right to reject the data, returning them to the
laboratory without payment. Rejection of data should be based  on sound  technical review of the
results. It also obligates  the client to make no use of those results without making some payment
to the laboratory.

3.4.5  Dilutions
The contract  should discuss the instances in which dilutions of samples and reanalyses would be
considered billable by the purchaser. Again, a laboratory should be prepared to do the job right
the first time and not bill for reanalyses required due to  their errors. In contrast, some samples
may need to be diluted and  reanaly/ed in order to bring  the results within the demonstrated
calibration range of the instrumentation. This typically occurs when the concentration of
pollutants in  the sample turns out to be higher than projected by the organization issuing  the
contract. Dilutions also may be  necessary when  several  pollutants are to be measured by a single
method, and  the concentrations  of some pollutants are within the calibration range of the
instrument but the concentrations of other pollutants are not.  When this occurs, the laboratory

ought to he paid for their efforts to dilute the sample as necessary to quantify all pollutants. Such
reanalyses can he figured into the original price, inflating the per-sample price for all samples to
account for the need to reanalyze some samples, or it can he hroken out as a separate cost. For
analyses involving an extraction or digestion as well as an analysis, it may he useful to specify
the price for the extraction step and the analysis separately, as it may he acceptahle to simply
dilute and reanalyze the sample extract instead of diluting, re-extracting, and reanalyzing the
entire sample.

3.5   Developing a Bid Sheet

After all project requirements have heen established, the pretreatment authority or IU can
develop a hid sheet to accompany the analytical requirements summary during the solicitation.
The hid sheet allows laboratories to submit bids in the same format, making hid evaluations
easier, and also clarifies the project. Bid sheets for analytical services typically are formatted as a
chart, with analytical requirements along one axis and number of samples and prices along the
other. An example of a hid sheet is attached as Appendix B.

The bid sheet should include the following information:

•      Project identifier

•      Space for laboratory identification information

•      Day, date, and time of the bid deadline

•      Estimated award date

•      Laboratory period of performance (period of time during  which the laboratory is obliged
       to resolve issues associated with analysis of the samples—generally six  months after
       shipment of last sample)

•      Required delivery date (data turnaround time and the basis of its calculation, such as from
       receipt of each sample or from receipt of last  sample)

•      Bid validity period (period of time during which hid prices are considered
       valid—generally 45 days after the bid deadline, if the project is awarded after this period.
       the pretreatment authority or IU must contact bidding laboratories to determine if bids
       need to be revised)

•      Parameters to he analyzed (typically the type  of analysis and/or method)

•      Number of field samples to be analyzed for each parameter

•      Number and type of billable QC samples (such as MS or SRM)

•      Total number of samples (field samples plus QC samples)

•      Columns for laboratories to submit per-analysis and total  costs

Please  note that, depending on the requirements of the project, additional information may need
to be requested with the hid sheet to ensure that the laboratory will  be able to meet the
requirements of the analytical contract.

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3.6   Estimating Costs

Before soliciting an analytical project, the anticipated cost of the work should he identified to
ensure that the solicitation and procurement procedures are appropriate. Analytical projects
typically are costed-out using per-sample analysis prices. The most common  methods for
estimating per-sample costs are: (1) reviewing current, published laboratory fee schedules for the
same or comparable analyses, and (2) reviewing historic per-sample costs for the same or
comparable analyses.  Laboratory fee schedules are available by request from most commercial
laboratories. Invoice and payment records at the pretreatment authority or IU can be used to
research historical costs. If the pretreatment authority or IU frequently outsources analytical
work, it may be helpful to copy the per-sample prices from these records into a separate file for
future use in estimating project  costs and establishing the  reasonableness of laboratory bid prices.


Procedures for soliciting and awarding contracts to perform analytical services can vary.
depending upon the scope of the project and purchasing requirements within the organi/.ation that
is issuing the contract. At one end of the spectrum are contracts that are awarded after placing a
single phone call and obtaining a quote from a single laboratory. The opposite end of the
spectrum are contracts awarded after a competitive solicitation and bidding process involving the
distribution of a detailed project description and a formal bid sheet via fax or mail. Determining
whether an analytical services request will be solicited on a casual basis, through a rigidly
documented formal solicitation, or somewhere in between, depends on the following factors:

•      The nature of the analyses. Projects for routine analyses for which laboratories have
       published fee schedules are less problematic to solicit than projects for experimental or
       esoteric analyses. Phone solicitations to local laboratories or laboratories nationwide
       typically can be used for routine analyses to confirm laboratory prices. If the purchasing
       organization's procurement policies allow,  an award can be made after per-sample prices
       are confirmed over the phone with a laboratory.

       The anticipated cost and the procurement system of the organization purchasing the
       analytical services. If the anticipated cost of the project  is minor and the pretreatment
       authority or IU purchasing the analytical services docs not have a highly structured
       procurement system, the most straightforward means of soliciting the project  is  to call
       one or more local laboratories, receive and  evaluate the quotes, and award the work.
       However, if the anticipated cost of the project is substantial and/or the procurement
       system requires a competitive solicitation, enough laboratories should be solicited to
       ensure that  at least three bids are received (a minimum of three bids is required  to qualify
       as a competitively awarded contract according to the Federal Acquisition Regulation
       (FAR)). The project then can be awarded to the lowest of the three responsive, responsible
       bidders (Section 4.4).

       The pretreatment authority's or lU's knowledge of capable laboratories. If the
       pretreatment authority or IU frequently outsources projects to  the same laboratory or
       laboratories, solicitations to these laboratories generally will not require the submission of
       prequalification data or references.  Projects that are solicited to laboratories that are
       unknown to the pretreatment authority or IU may warrant additional  steps, such as those
       described in Section 4.3. to ensure that the  laboratory is capable of performing the
       requested analyses.

Because of the relatively straightforward nature of phone solicitations of routine projects, the
remainder of this chapter provides general  guidelines for conducting competitive, written
solicitations to multiple laboratories nationwide. Before implementing these procedures.
permitting authorities and lUs should consult with their legal or procurement departments to
ensure that the procedures are consistent  with those required within their organi/.ation.

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4.1    Identifying Capable Laboratories and Transmitting the
Capable laboratories generally are defined as laboratories that have the instrumentation and
expertise to perform the analyses you require according to the methods you specify. Thus.
although a frequently used local laboratory may be perfectly capable of performing routine wet
chemistry or metals work for your pretreatment authority or IU, that laboratory may not be
considered capable w hen you require samples to be analyzed for dioxins. Several laboratory
indices are available as resources to enable pretreatment authorities and IL's to identify
laboratories to target in a solicitation, including the ASTM International Directory of Testing
Litbs. the American Council of Independent Laboratories' Directory, and the DynCorp Directory
of Environmental Testing Laboratories. Each of these directories is readily available (see
Reference 2 to 4).

After laboratories capable of performing the requested analyses are identified, a written bid
package needs to be transmitted to them. This bid package should include the analytical services
request and the bid sheet, at a minimum. The package also should include the required methods.
if non-routine analytical methods are required, and a cover letter if any additional or introductory
information needs to be provided 10  the laboratories. If possible, allow at least two weeks for the
laboratories to submit bids. This deadline is noted on the bid sheet.

Traditionally, the general rule for transmitting solicitation packages was to use fax for
solicitations of 10 pages or less, and use mail or overnight services if the package was more than
l() pages. However, most laboratories now have email addresses, and transmitting solicitations
via email is typically more efficient than faxing or mailing the package.

4.2    Evaluating  Bids

After the laboratories have received  the solicitation and submitted bids, the pretreatment
authority or IU  must evaluate the bids to identify the laboratory that will be awarded the
analytical services contract. Specific procedures for evaluating bids may vary, depending upon
the requirements of the organization that is soliciting the contract. Therefore, it is recommended
that the procedures that will be used to evaluate the bids be communicated to all laboratories
involved in a competitive solicitation before they submit their bids. One way to confirm the
requirements will be met is to require the laboratories to submit a technical proposal w ith their
bids.  An example technical proposal request and technical proposal scoring sheet is provided in
Appendix C.

Pretreatment authorities and lUs should consult their legal departments or purchasing
departments to identify any applicable requirements for evaluating competitive bids within their
organization. In the absence of explicitly defined bid evaluation procedures, pretreatment
authorities and lUs may wish to follow the procedures outlined below. These procedures, which
have  been adapted from those published in the FAR. begin with evaluation of all bids received to
identify  the lowest responsive,  responsible bid. A bid is considered responsive if the following
criteria are met:
•      The bid was submitted without contingencies or with acceptable contingencies

                                                             .SVilicitiny and Awtirtlnn; the
•      The hid was submitted before the bid deadline

•      The bid sheet (if required) contains no errors or omissions

The organi/.ation responsible for awarding the contract also should recalculate bid prices based
on each laboratory's per-sample price to ensure that the bidding laboratories did not make any
mathematical errors. If any incorrect calculations are identified, the laboratory should be
contacted to confirm the corrected total bid price. In addition, the pretreatment authority or II'
should ensure that there are no unacceptable contingencies associated with any of the bids (such
as the use of an unacceptable method). After all bids have been checked for errors and
contingencies, the  pretreatment authority or IU can identify the lowest, responsive bidding
laboratory for the project. If there is a question regarding a laboratory's ability to perform the
work, the pretreatment authority or IU should perform  a responsibility determination, as well (see
Section 4.3).

If three or more responsive bids were received, then the low bid may be deemed reasonable based
on the closeness of the bid prices to each other and current market conditions. If fewer than three
bids were received, price reasonableness can be determined using bid prices submitted for
comparable projects, price quotes from current laboratory fee schedules, or  information requested
from the laboratory, including a breakdown of costs or invoices to other clients for comparable
work. The lower bid may be deemed  unreasonable if it is significantly lower than the other bids.
and may not be considered for award.

4.3   Conducting Responsibility Determinations

If the  low-bidding  laboratory is unknown to the pretreatment authority or IL:. or the importance
of the project merits special effort to ensure that the awarded laboratory is capable of reliably
performing the requested analyses, then a laboratory responsibility determination should be
performed. The best means of confirming that a laboratory is capable of reliably performing an
analytical requirement is to assess data recently produced by the laboratory using the same
method on similar  sample matrices. A less  expensive approach is to rely on other information
applicable to the analyses in question, such as performance evaluation (PE) sample results.
federal or state certifications, and corporate references. Sections 4.3.1 - 4.3.4 provide guidance
for using the laboratory's method performance data. PE sample results, certifications, or
references to evaluate their capability.

If laboratory performance cannot be assessed based on  existing data or references, another
alternative is to require laboratories that bid on the project to analyze samples specific to the
project and submit these results with their bids. Bids then are evaluated in terms of cost and
performance. Laboratories that do not submit acceptable data are not qualified to perform work
under the project, and can be eliminated  from consideration for award. Section 4.3.5 provides
additional guidance concerning the use of prequalification analyses as a means of evaluating
laboratory capability.

For long-term, critical, or very costly  projects, the utility or II' should consider auditing the
laboratory before an award is made. Section 4.3.6 provides guidance on conducting pre-award
audits. Audits  may be announced, or an alternate technique to determining that a laboratory is
capable of reliably performing the contract is to make an unannounced visit to the laboratory.

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4.3.1  Method Performance Data
Many laboratories routinely use 3()4(h (-approved methods for analysis of samples collected by
their clients. In such cases, the pretreatment authority or IL; can ask a laboratory to provide
historical data that demonstrates the laboratory is capable of reliably analyzing the required
sample matrices with the required methodology. Data requested should include results from all
QC parameters required by the  method, including results from calibration standards, blanks.
initial and ongoing precision and recovery samples, and spiked matrix samples. The pretreatment
authority or IU should request historical data generated within the past six months. Older data
still may be relevant, but the laboratory should indicate any personnel, instrument, or facility
changes that have occurred since the data were generated.

4.3.2  Performance Evaluation  Sample Results
Several  EPA and state laboratory programs send performance evaluation (PE) samples to
laboratories that are pan of their program on a periodic or regular basis to monitor laboratory
performance. PE samples typically consist of a synthetic matrix spiked with concentrations of
analytes known to the program  office but unknown to the laboratory (single-blind samples). The
program laboratories analyze the samples and report the results, and the program office compares
these results to the true values of the PE samples. The program office or laboratories that
participate in programs that issue PE samples should be able  to provide you with the assessment
of their latest PE sample results.

Several  PE studies programs are administered by EPA in support of the Clean Water Act.  the
Safe Drinking Water Act. and Superfund:

•      Water Pollution (WP). Laboratories in the WP program receive chemistry PE samples;
       the program  tests laboratories' abilities to analyze for common surface  water quality
       parameters and pollutants. The  WP program supports more than 25 state wastewater and
       other environmental laboratory certification programs.

•      Discharge Monitoring Report Quality Assurance (DMRQA). Laboratories in the
       DMRQA program receive chemistry and whole effluent toxicity PE samples. This
       national program is used by EPA and the  states to ensure the quality of monitoring data
       submitted by more than 7.000 major NPDES permittees each year.

•      Water Supply (WS). The Water Supply program includes chemistry, microbiology, and
       radiochemistry PE studies and supports the Safe Drinking Water Act.

•      Effluent Guidelines Program. Laboratories awarded contracts to analyze samples for
       EPA's Engineering Analysis  Division within the  Office of Water's Office of Science and
       Technology are sent periodic PE samples for organics. metals, and wet  chemistry analyses
       to monitor performance.

•      Contract Laboratory Program (CLP). Laboratories in EPA's Contract  Laboratory
       Program, which supports Superfund sample analyses, receive PE samples for organics
       and inorganics analyses on  a quarterly basis.

A  laboratory not participating in a PE sample program or equivalent should not be considered for
the contract. In addition, pretreatment authorities and IUs should note that PE sample results are
only useful if the analyses are applicable to the project for which the laboratory is considered. A


                                                             Solit'itltn; unit AiuinttHV thf
laboratory 's ability to perform well on organics PE samples is not an indication of how reliable
its metals laboratory is.

4.3.3  Certifications
Pretreatment authorities and ILJs also can ask laboratories to supply a list of their current
certifications, such as state drinking water certifications. In addition, information about
laboratory certifications can  be obtained through Internet searches or by telephone or email from
the NPDES/pretreatment staff or QA officer in the state or EPA regional office with jurisdiction
over the certified laboratory.

Certifications are particularly useful if they  apply directly to the analyses required by the
pretreatment authority or ILJ, but also provide an indication of the overall standing of the
laboratory. Most certification programs entail laboratory audits and PE sample analyses, and thus
provide some assurance that the laboratory is generally capable of providing reliable analytical
services. However, pretreatment authorities and IUs should note that a state drinking water
certification is no guarantee that a laboratory is capable  of performing industrial wastewater
analyses by methods not covered by that certification.

Currently, guidance and standards for a national laboratory accreditation program are being
developed through a state/EPA organized group known  as the National Environmental
Laboratory Accreditation Program (NELAP). Current information on NELAP and the National
Environmental Laboratory Accreditation Conference (NELAC) is available on the Internet.

4.3.4  References
This means of establishing a laboratory's reliability and capability is. perhaps, the easiest. If a
pretreatment authority or IU  has not worked with a particular laboratory before, the laboratory
can be asked to provide contacts and phone  numbers of corporate or government clients for
which the laboratory has performed  services comparable to the project at hand. Questions to ask
the references include:

•      Did the laboratory provide data by the required due date'.'

•      Were the data reviewed upon receipt to ensure that the laboratory performed the
       requested analyses according to the specified methods and with the required QA/QC '.' (If
       the answer to this question is no. the reference is not likely to be capable of providing
       sufficient information to adequately  assess the laboratory's capability.)

•      Does the laboratory have a documentation system  for  sample control that retains accurate
       records of chain-of-custody;  sample  holding, handling, preservation,  and analyses; raw
       data: QA/QC, and processed data0 Have you audited this system'.'

•      Were laboratory personnel easy to work with when problems arose during all phases of
       the project, including sample scheduling, sample analysis, and data review'' If problems
       were noted during data review, was the laboratory prompt and responsive in addressing
       your concerns'.'

•      Do you have anv reservations in recommending  this laboratory'.'

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4.3.5  Prequalification Analyses
As noted above, prequalification analyses may he required if laboratory performance cannot be
assessed based on existing data, certifications, or references. Two options are available regarding
payment of prequalification analyses. The first is to require  laboratories to provide
prequalification data at no cost with their bids. Laboratories can recoup this cost if they are
awarded the contract. This approach generally will not work if the project is small, and the
laboratory has little incentive to provide prequalification data at no cost. If. however, the project
entails analysis of a sufficient number of samples to justify  a loss leader from the laboratory, this
approach should be considered.

The second option entails payment for prequalification analyses. In such a situation, laboratories
would bid on the project in two parts: one portion of the bid would apply only to prequalification
analyses, while the balance of the bid would apply only to analysis of the real samples. The bids
would be evaluated based on overall cost, and the laboratories with the lowest cost would be
awarded contracts to perform only the prequalification analyses. After prequalification data have
been submitted and evaluated, the lowest bidding laboratory with acceptable prequalification data
would be awarded the contract to analyze the real samples during the balance of the project.

Prequalification  analyses can  take several forms, including:
•      Analysis of single blind samples. The best way of determining laboratory performance
       before award is requiring bidding laboratories to analyze samples that are spiked with the
       target unulyte(s) at concentrations unknown to the bidding laboratories. Such samples are
       essentially identical in concept to the PE samples described in 4.3.2. Pretreatment
       authorities and IL's can either prepare their own single blind samples or they can purchase
       these samples from commercial vendors.

       Vendors  typically carry several types of stock PE samples applicable to a variety of
       pollutants, matrices, and analytical methods. To ensure that laboratories are unable to
       "predict" the pollutants and associated concentrations in their PE samples, vendors offer
       PE  samples that contain a minimum number of pollutants from a selected list (such as at
       least 7 of 10 listed metals), each of which  will be present within a specified "range" (such
       as 1 - 50  ug/L). Vendors  routinely prepare and distribute new batches in order to  further
       protect the integrity of their PE sample program. Actual pollutants and pollutant
       concentrations in each batch are certified,  and these  "certified values" are provided to the
       organization that purchases and distributes the PE sample)s). Pretreatment authorities or
       IL's should purchase the PE sample that most closely matches their target pollutant list
       and concentration range.

•      Analysis of samples spiked at the laboratory. A simpler, and potentially more cost-
       effective approach to the single-blind sample analysis scenario is to require laboratories to
       spike samples m-house and provide the spiking  levels and recoveries for evaluation. If
       this approach  is chosen, it is recommended that  the laboratory be required to spike and
       analyze four replicate  samples so that both precision and accuracy can  be assessed. The
       matrix used can  include reagent water, wastewater provided by the pretreatment  authority
       or industry, or a representative matrix that can be selected by the laboratory. If the
       laboratory is permitted to select a matrix type for this analysis (such as municipal

                                                                    tint! An (injury the
       wastewater or ambient water), the data reported should include characterization data, such
       as turbidity, hardness, background concentrations of the unspiked sample, etc.

       Analysis of a standard reference matrix. A third, similar approach is analysis of a
       commercially available SRM. The SRMs should be chosen by the client, and can be
       purchased by the laboratory or purchased by the client and sent to the laboratory for

•      Analysis of method blanks and method detection limit studies. If the project entails
       detection of analytes at very low levels, the laboratory*ies) awarded  the project should be
       required to demonstrate  that laboratory contamination does not exceed acceptable levels
       and demonstrate that they are capable reaching the low end of the detection range. The
       latter is accomplished by performing a method detection limit study according to the
       procedure at 40 CFR Part 136 Appendix B (essentially,  analysis of seven replicate reagent
       water samples spiked with the analyte of interest at one  to five times the method's
       minimum level). A method blank analyzed with these MDL samples can be used to
       demonstrate freedom from contamination at low levels.

4.3.6  Laboratory Audits
The goal of a prequalification audit is to ensure that the laboratory has the capability and
commitment to meet the program goals of timely delivery and high-quality  analytical services.
Audits can focus on any or all of the following areas:

•      Laboratory personnel qualifications

•      Sample receiving and  storage areas

•      Sample preparation  and  analysis areas

•      Instrumentation

•      Laboratory quality assurance plan (QAP)

•      Laboratory standard operating procedures (SOPs)

Although laboratory  audits generally are specific to the project, general criteria are applicable to
each of the above areas. The best approach to evaluating a laboratory, based on these criteria, is
through the use of checklists.  Examples of laboratory  audit checklists are provided in Appendix
D C of this document. These checklists should be modified as necessary to  adapt them to the
specific project.

Contact the appropriate state or  EPA regional office via phone or email to obtain audit or
inspection information about the laboratory. The Internet can  be used to identify the appropriate
state or EPA regional contact.

If a laboratory fails an audit, two options are available to the pretreatment authority or II'. The
laboratory can be eliminated from consideration for the project  or the laboratory can be provided
the opportunity to correct the deficiencies identified in the audit and request a revaluation. If the
laboratory passes the audit,  the pretreatment authority or II' can proceed to contract award.

/'rociirint; Aniil\rn ill Sen-ices: (initlani•<• fi>r Industrial Pretrcanni'nt Programs	

4.4   Awarding the Contract

Contract awards typically should he made over the phone, then followed by a written contract for
laboratory signature. Awarding the contract over the phone enables the pretreatment authority or
II' to verify the scope of the analytical work and verify laboratory information. This information
should include the name of the person assigned to receive the samples and the street address to
which the samples will be shipped—overnight delivery services, such as Federal Express, will
not accept samples w ith post-office-box addresses. Laboratory information also should include
the name and address of the laboratory's administrative personnel that handle billing issues, as
these may differ from the address  to which samples are shipped.



After the analytical services contract is awarded, samples are collected and shipped to the
laboratory. Although it is the laboratory's responsibility to contact the client if problems occur
after sample receipt, the pretreatmeru authority or IU still should initiate communications with
the laboratory periodically to monitor progress.

5.1   Transporting and Tracking Samples

The pretreatment authority or IU must ensure sample integrity from collection to data reporting
to  use the data for anything other than internal purposes. This includes the ability to trace
possession and handling of the sample from the time of collection through analysis. The
following items and steps will ensure that samples are processed accurately and  that the data
produced are defensible: sample labels, sample seals, field log books, chain-of-custody records.
sample analysis request sheets, tracking of sample delivery to laboratory, receipt and logging of
samples  by  the laboratory, and documentation of sampling project from sample collection
through  sample analysis. This process of tracking samples is considered a "sample control
system." and should be established as a documentation system for the laboratory.

•     Sample labels. Sample labels always should be used to prevent sample misidentification.
      The sample number and required analysis should be stated clearly on the label. If space
      allows, the name of sampler, date and time of collection, and place of collection also
      should be included. Waterproof markers should be used to write on sample labels.

•     Sample seals. When chain-of-custody is critical, sample seals can be used to detect any
      unauthorized tampering with samples up to the time of analysis. The seal should be
      attached in such a way that it is necessary to break it to open the sample container.

•     Field log book. A field log book should be used to record all information pertinent to
      sample collection. The field log book should include the following: the purpose of
      sampling, the location of the sampling point, the name and address of the field contact.
      the producer of the material being sampled and address (if different from sampling
      location), the type of sample being collected (such as wastewaler. soil, or sludge), and. if
      the sample is a wastewater, the identification of the process producing the waste stream.
      In addition, the number of samples and volume of sample taken, the description of the
      sampling point and sampling method, the  date and time of collection, and the sampling
      label number should be included. Other items that are useful to keep with the field log
      book are references such as maps or photographs of the sampling site,  field observations
      and  measurements, and signatures of personnel responsible for observations. Sampling
      situations vary, so no general rule can be given as to the information to be entered in the
      log book, but as much information as possible should be provided.

•     Chain-of-custody record. The ability to trace possession and handling of a sample from
      the time of collection through analysis is referred to as chain-of-custody. A sample is
      considered to be in an individual's custody if any of the following criteria are met: (I) the
      sample is in your possession or it is in your view after being in your possession. (2) it was
      in your possession and then locked up or sealed to prevent tampering, or (3) it is in a

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       secured area. The chain-of-custody record is used as physical evidence of sample custody.
       The sampler completes a chain-of-custody record to accompany each sample or group of
       samples shipped from the field to the laboratory. The record includes the following:
       sample number, signature of sampler, date. time, and location of collection, sample type.
       signatures of persons involved in the chain of possession and inclusive dates of
       possession.  The original signature copy of the chain-of-custody record is enclosed  in
       plastic and secured to the inside of the container used for sample shipment. A copy of the
       custody record is retained for the sampler's file. The shipping containers are secured and
       custody seals arc placed across the cooler openings. The laboratory representative who
       accepts the  incoming sample shipment signs and dates the chain-of-custody record to
       acknowledge receipt of the samples.

•      Sample analysis request sheet. A sample analysis request sheet or traffic report should
       accompany  the samples to the laboratory. The sampler should complete the field portion
       of this sheet with most of the pertinent information noted in the log book. The laboratory
       representative should complete the laboratory portion of this form, which includes: the
       name of the person receiving the sample, laboratory sample number, date of sample
       receipt, condition of samples  upon receipt, and  analyses to be performed.

•      Sample delivery to laboratory. The samples should be delivered to the laboratory as
       soon as practicable. Commercial carriers often  are the best method of shipment if the
       samples cannot be delivered to the laboratory the same day as collection. To facilitate
       return of the shipping containers, shippers should clearly mark the name and address of
       the return destination on the containers. The laboratory must be contacted every day they
       are to receive samples to confirm receipt of samples. The pretreatment authority or II'. as
       well as the laboratory should  document this confirmation.

•      Receipt and log-in of samples. At the laboratory, the sample custodian receives the
       samples and should perform the following tasks with each sample: ( 1 ) inspect the
       condition of the sample. (2) inspect the condition of the  sample seal (if present). (3)
       reconcile sample label information and seal against the chain-of-custody record. (4)
       assign a laboratory sample number, and  (5) log the sample in the laboratory log book.

•      Documentation of sampling project from sample collection through sample analysis.
       Documentation of the entire sampling project from sample collection through sample
       analysis, including any problems and resolutions that occur during the event, should be

•      Sample holding times.  Sample analysis results may not be valid if the prescribed holding
       times and other requirements for each parameter arc not met. These requirements arc
       listed in Table II of 40 CFR Part 136. Required Containers. Preservation Techniques, and
       Holding Times.

Samples should be  packaged for shipment in compliance with the most current U.S. Department
of Transportation, state, local, and commercial carrier  regulations.  All required government and
commercial carrier shipping papers must be filled out and shipment classifications made
according to these regulations.

                                        Transnomny Suninlc.'i unit Coinninniciiiiny mil'
Waterproof, metal or hard plastic ice chests or coolers should he used for shipment. Inside the
cooler, sample containers should he enclosed in clear plastic hags so that sample tags and labels
are visible. Water and soil samples suspected to contain dioxin must be enclosed in a metal can
with a clipped or sealed lid (paint cans typically are used). The outer metal can must be labeled
with the number of the sample contained inside. Containers that do not fit into paint cans should
be double bagged.

Shipping containers should be packed with noncombustible. absorbent packing material, such as
vermiculitc. The material should surround the sample bottles or metals cans containing sample to
prevent breakage during transport. Earth or loose ice should never be used to pack samples; earth
is a contaminant, and ice melts, resulting in container breakage.

The sampling and shipping conditions for each sample will depend on the analysis required for
that sample, and will be specified in the method. When shipping with ice. the  ice should be in
sealed plastic bags to prevent melting ice from soaking packing material which, when soaked.
makes handling of samples difficult in the laboratory. The Sample Analysis Request Sheet.
chain-of-custody record and any other sample documentation accompanying the shipment must
be enclosed in a waterproof plastic bag and taped to the underside of the cooler lid. Coolers
should be sealed with custody seals in such a manner that the custody seal would be broken if the
cooler were open. Shipping coolers must have clearly visible return  address labels on the outside.

Samples should be shipped through a reliable commercial carrier, such as Federal Express.
Emery, and Airborne Express, or equivalent  if the samples cannot be delivered to the laboratory
by the sampler on the day or day after the sampling occurs. Consideration also should be given to
requesting the laboratory to pick up the samples. Laboratories typically will have more flexibility
in choosing a carrier or changing carriers if there are difficulties with a deliver)' service.

5.2   Communicating with  the Laboratory

The pretreatment authority or IU must maintain communications with the laboratory to confirm
sample shipment receipt, timely analysis, and quality data. In addition, it is important that the
laboratory is able to communicate immediately with the sampler or person responsible for the
sampling event in case of sample shipment problems or analysis issues that may affect data

Although phone communications currently are the norm, these communications ideally should be
conducted via email. Email communications not only should provide virtually immediate
responses, but also enables both the contracting party and the laboratory to maintain a written
record of sample receipt confirmations, problem notifications, and problem resolutions. In
addition, email communications reduce misunderstandings and miscommunications.


When reviewing data submitted by contract laboratories, you must ensure the test data include
the QA/QC elements listed in the analytical method and in your contract (see Section
3.3);otherwise. the data can be considered noncompliant. As a result.. These supporting QA/QC
results provide you with the simplest means of assessing the quality of your data.

In many of its early analytical programs. EPA relied upon laboratories to maintain records of the
QA/QC data. This practice was cumbersome for the laboratories, because many of the QA/QC
data were common to the analytical results for a variety of clients. Retrieving these data from the
laboratory to resolve questions of permit compliance was time-consuming for the permittee and
the permit writer. More importantly, this practice occasionally resulted in unscrupulous
laboratories  failing to perform the necessary QA/QC testing, or performing the  QA/QC testing
"after the fact" to satisfy an audit or data submission request.  In particular, many laboratories did
not perform  the IPR test prior to practice of the method and did not perform a spike of the
analytes into the sample matrix to prove that the method would work on a particular sample.
Therefore, while the data provided by those laboratories may have been valid, there w as no way
to prove their validity.

Sections 6.1  through 6.11, below, provide guidance on evaluating sample data based on QA/QC
data. A data  inspection checklist is provided in Appendix E, providing a standardi/ed format for
the data review process and the documentation of findings.

6.1    Purity and Traceability of Reference Standards

Laboratories submitting analytical data must be able to trace the reference standards  used in the
analysis to EPA or NIST. The proof of this traceability is a written certification from the supplier
of the standard. Documentation of the purity and traceability of the standards need not be
provided with every sample analysis. Rather, it should be maintained on file at the laboratory and
provided on  request. When analyses are conducted in a contract laboratory, such documentation
ought to be provided to the permittee the first time that a laboratory is employed for specific
analyses and then updated as needed.

6.2   Calibration  Range

The data reviewer must make certain that the calibration range encompasses the minimum level
and that all measurements are within the calibration range of the instrument. Samples with
analytes outside of the calibration range should be diluted and reanalyzed. The diluted sample
results need only apply to those analytes that exceeded the calibration range in the initial analysis.
In other words, it is acceptable to use data for different analytes from different levels of dilution
within the same sample.

If data from an analysis of the diluted  sample are not provided, limited use can be made of the
data that are  above the calibration range. The response of the  analytical  instrument to
concentrations of analytes will eventually level off at concentrations above the calibration range.
While it is not possible  to specify at what concentration this will occur from the calibration data
provided, it is generally safe to assume that the reported concentration above the calibrated range

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is a lower limit of the actual concentration. Therefore, if concentration above the calibration
range is also above a regulatory limit, it is highly likely that the actual concentration would also
be above that limit.

6.3   Linearity of Calibration

Linearity specifications vary from method to method, depending on the quantitation technique.
Typical limits on the RSD are as follows:

       Itt for GC and HPLC methods
•      35rr for analytes determined by the internal standard technique in GC/MS methods

•      20c/( for analytes determined by isotope dilution in GC/MS methods

If the calibration is not linear, as determined by the RSD of the response factor or calibration
factor, the calibration curve, as opposed to the average response factor, must be used for
quantitation This means that a regression line or other mathematical function must be employed
to relate the instrument response to the concentration. Properly maintained and operated lab
instrumentation should have no difficulty  in meeting linearity specifications for the EPA-
approved methods.

Whatever calibration range is used, the laboratory must provide the RSD results by which one
can judge linearity, even in instances where the laboratory is using a calibration curve. In
instances where the laboratory employs a curve rather than an average response factor, the data
reviewer should review each calibration point to assure that the response increases as the
concentration increases. If it does not. the instrument is not  operating  properly, or the calibration
curve is out of the range of that instrument, and data are not considered valid.. The analysis of
samples should not proceed until  linearity on that  instrumentation is demonstrated.

6.4   Calibration  Verification

Calibration verification results should be within method specifications. If any individual value
falls outside the range given, system performance is considered unacceptable, and the laboratory
may cither recalibrate the instrument or prepare a  new calibration standard and make a second
attempt to verify calibration.  If the laboratory was not able to verify calibration, the data should
be evaluated to determine if it is usable with a qualification of high or low bias, or if the bias
precludes use of the data.

6.5   Method Detection Limit,  Minimum Level, or Quantitation Limit

l:nless specific data gathering requirements require otherwise, the laboratory should report the
concentration of all  sample results that are at or above the ML. It  should be noted that this ML is
a sample-specific ML and. therefore, reflects any sample dilutions that were performed.  If sample
results are reported below the ML. the data reviewer should require the responsible party to
correct and resubmit the data, or if this course of action is not possible, the reviewer should
determine the sample-specific ML and consider results below that level to be non-detects for
regulatory purposes.

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       the true concentration, and data users should he cautioned when using the data tor
       enforcement purposes.

•      If the concentration of the OPR is below method specification hut that analyte is detected
       in an associated sample, then the sample result may represent the lower limit of the true
       concentration for that analyte.

•      If the concentration of the OPR is below method specification and that analyte is not
       detected in an associated sample, then the sample data are suspect and cannot he
       considered valid for regulatory compliance purposes.

If the OPR standard has not been run. there is no way to verify that the laboratory processes were
in control. In such cases, a data  reviewer may be able to utilize the field sample data by
examining the matrix spike recovery results (see item 9), the IPR results. OPR results from
previous and subsequent batches, and any available historical data from both the laboratory and
the sample site. If the matrix spike results associated w ith the sample batch do not meet the
performance criteria in the methods, then the results for that set of samples cannot he considered
valid. If the laboratory's IPR results and the matrix spike results associated w ith the sample batch
in question meet the all applicable performance criteria in the methods, then the data reviewer
may he reasonably confident that laboratory performance was in control during field sample
analysis. This level of confidence may he further increased  if there is a strong history of both
laboratory performance with the method and method performance with the sample matrix in
question, as  indicated by additional OPR and matrix spike data collected from the laboratory and
samples from the same site.

6.8    Analysis of Blanks

I'nless the samples are still within analytical holding time and reanalysis is possible, there is no
corrective action if unacceptable blank data are submitted with sample data. Therefore, the
reviewer has several options in making use of the sample data.  First, if a contaminant is present
in a blank, hut not present in a sample, then  there is little need for concern about the sample
result, though it may be  useful to occasionally review the raw data for samples without the
contaminant to ensure that the laboratory did not edit the results for this compound.

The second approach deals with instances where the blank contaminant is also reported in a
sample. Some general guidance  will help you determine the degree to which the contaminant  is
affecting sample results:

       If the sample contains the contaminant at levels of at least 10 times that in the blank, then
       the likely contribution to the sample  from the contaminant in the laboratory environment
       is at most  lO'/r. Since most of the methods in question are no more accurate than that
       level, the possible contamination is negligible.

•      If the sample contains the contaminant at levels of at least 5 times but less than 10 times
       the blank result, the compound is probably present in the sample, but  the numerical result
       should be considered an  upper limit of the true concentration.

•      If the sample contains the contaminant at levels below 5 times the level in the blank, there
       is no adequate means by which to judge  whether or not the sample result is attributable to
       laboratory' contamination. The results for that compound in that sample are then suspect.

There are two difficulties in evaluating sample results  relative to blank contamination. First, the
reviewer must be able to associate the samples with the correct blanks. The second difficulty
involves samples that  have been diluted. The dilution of the sample with reagent water or the
dilution of the extract  with solvent represents an additional potential source of contamination that
will not be reflected in the results for the blank unless  the blank was similarly diluted. Therefore.
in applying the 10-f.mes rule, the concentration  of the  sample is compared to the blank result
multiplied by the dilution factor of the sample or sample  extract. For instance, if 12 ppb of a
contaminant are found in the blank, and the associated sample extract was diluted by a factor of 6
relative to the extract from the blank prior to analysis,  then the sample result would have to be
greater than  12x6x10. or 720 ppb, to be acceptable. Between 360 ppb and 720 ppb. the sample
result would best be considered an upper limit of the actual concentration. Below 360 ppb. the
sample result is not acceptable for compliance monitoring.

In most cases, the practice of subtracting the concentration reported in the blank from the
concentration in the sample is not recommended as a tool to evaluate sample results associated
w ith blank data. One of the most common problems with this approach is that blank
concentrations are sometimes higher than one or more associated  sample  results, yielding
negative results.

6.9   Matrix Spikes and Labeled Compound Spikes

When evaluating matrix spike results, the data reviewer must verify the following:

•      An appropriate spike concentration was used

•      The unspiked sample has been analy/.ed

•      The spiked sample has been analyzed

•      The recovery of the spike is within the range specified

•      If the spike recovery is not within the range specified, a QC check standard has been

•      If a QC check standard has been analyzed, the results are within the  range specified

For isotope dilution analyses, the evaluation of the data is simpler because isotopically labeled
analogs of the pollutants are spiked into each sample allowing recovery to be evaluated for every
analyte in every sample, and because a QC check standard (termed the "ongoing precision and
recovery standard," or OPR) is analyzed with each sample set.

If the recovery of a labeled compound spiked into the sample is not within the range specified in
the method, and the results of analysis of the ongoing precision and recovery standard are within
the respective limits, the sample results are considered reportable. with qualification that the
results may be  biased.  When labeled compound  recoveries are outside of the method
specifications,  the problem may be related to the sample matrix. In these instances, the sample
may be diluted with  reagent water and reanalyzed. If the labeled compound  recoveries meet the


        Anuhticul .SVn ;  Guidance tor Induatnul Prcncatnu-nt
method specifications after dilution of the sample, then the results arc acceptable, although the
sensitivity of the analysis will he decreased by the dilution.

In instances where matrix spike or labeled compound recoveries are not within the specifications.
it may still be possible to use the sample results for compliance monitoring purposes. In
particular, if ( 1 ) the recovery of the spiked compound is above the method specifications and (2)
the compound is not detected in the sample analysis, it is unlikely that the compound is present in
the sample. This is because the factors that caused the analysis to over-estimate the concentration
in the spiked sample would not likely have resulted in an under-estimate in the unspiked  sample.
For samples in which the compound is detected but the matrix spike or labeled compound
recovery is above the method specifications, the concentration reported in the unspiked sample is
likely an upper limit of the true concentration.

Unfortunately, for some sample matrices, even dilution will not resolve  the problem, and for
other matrices, the loss of sensitivity will preclude the use of the results  for determining
compliance. In these instances, additional steps need to be taken to achieve acceptable results.

6.10  Statements of Data  Quality for Recovery of Spiked Analytes or
       Labeled Compounds in  Samples
Many laboratories do not provide the data quality statements with the sample results, in which
case the data reviewer  must determine if the data quality statements are being maintained for
each analyte and may need to obtain the data. If necessary, the reviewer  can construct the data
quality statement from the individual data points.

The lack of a statement of data quality does not invalidate results but makes some compliance
decisions more difficult. If statements of data quality are not being maintained by the laboratory.
there may be increased concern about both specific sample results and the laboratory's overall
quality assurance program.

6.11  Field Duplicates

The field duplicate provides an indication of the overall precision associated with entire data
gathering effort, including sample collection, preservation, transportation, storage, and analysis
procedures. The data reviewer should examine field duplicate results and use the following
equation to calculate the relative percent difference between the duplicate and its associated
               Dl = concentration of the analyte in the field sample
               D2 = concentration of the analyte in the duplicate field sample

                                                                      Ki'\ tf\\nn; AnalMu ill
If the analyte of interest was not detected in either replicate of the field sample, then the RPD
will he /.ero. If the analytc was detected in each field sample replicate, hut the results are highly
disparate (indicated by a large RSD). the reviewer should apply the following guidelines when
making use of the data:
•      If the analyte was detected in each replicate and at similarly variable concentrations in the
       blank samples, then the  field sample variability may be attributable to variable
       contamination, and the data  may not be valid for regulatory compliance purposes.

•      If the analyte was detected in each replicate at a concentration well above the regulatory
       compliance level, but was not detected in the associated blank samples, then it is likely
       that the sample results arc not adversely affected.

Ideally, the RPD between  field duplicates and MS/MSD samples will be close to zero. Any
difference between the two duplicates is attributable to variability associated with the field
sampling process.

1      International Organization for Standardi?.ation (ISO) and International Electrotcchnical
          Commission (IEC). 1990. Guide 25: General Requirements for the Competence of
          Calibration and Testing Laboratories.

2      American Society for Testing and Materials. 1998. ASTM International Director* of
          Testing Laboratories.

3      American Council of Independent Laboratories. Inc. 1992-1993. Director*: A Guide to
          Leading Independent Testing, Research, and Inspection Firms in America.

4      DynCorp. 1996. Directory of Environmental Testing Laboratories.

5      EPA Guidelines Establishing Test Procedures for the Analysis of Pollutants at Federal
          Regulations Title 40 CFR Pan 136. Tables I A-E and Table II.

6      U.S. EPA. September  1994. NPDES Compliance Inspection Manual. EPA 300-B-94-014.
          Chapter 4 (laboratory procedures) and Chapter 9 (pretreatment).

7      U.S. EPA. April 1994. Industrial User Inspection and Sampling Manual, EPA 83 l-B-94-
          001. Chapter 3.

               APPENDIX A


                          Analytical Services Request

Client Name:

Point of Contact (name, telephone and fax number, and email address):

Date of Request:

1.      General description of analytical services requested:

2.      Definition and number of samples involved (specify wastewater. groundwater. sludge.
       soil, etc.):

3.      Purpose of analysis (NPDES. SDWA. RCRA compliance monitoring, etc.):

4.      Estimated date(s) of sample collection:

5.      Estimated date(s) and method of shipment:

6.      Sampling/shipping contact (name and telephone number):

7.      Holding times associated with analysis (specify number of days, or state "per method"):

8.      Number of days after sample receipt that data arc required:

9.      Analytical method  required (specify method number, source, and date, and attach copy
       where practical):

10.     Special technical instructions (provide information on known problems, possible
       solutions, matrix effects, etc.):

11.     Data reporting requirements (specify format of data. QA/QC reports, number of copies.

12.     Sensitivity required (specify "per requested method." or list analyte names. CAS numbers.
       and quantitation limits required):

13.     Quality control requirements (summarize QC operations specified  in the referenced
       method, and any additional requirements):

14.     Action required if QC limits exceeded (specify reanalysis. contacting client immediately.

15.     Other (use additional sheets or attach supplementary information, as needed):



                Bid Response for Analysis of Effluent and Marine Water Samples
                            for Trace Metals by 1600-Series Methods
Laboratory Name
Laboratory Contact
Contact Phone Number

Bid Deadline (Day. Date. Time)
Fnday. 7/31/98. 8:00 pm EST
Estimated Award Date:
Data dehverables due within 30 calendar days from receipt
ol last sample at lab
Liquidated damages will be assessed at a rate of 2°o of the
per-sample cost for each day that data is late
Period of performance From the date your bid price is
accepted until 2/21/99
Bid prices listed below shall be valid for a period of 45
calendar days from the bid deadline date








POTW effluent
Marine Water

POTW effluent
Marine Water

POTW effluent

POTW effluent
Marine Water

POTW effluent

POTW effluent

POTW effluent
Marine Water





















(A) (B) (A x B)







Cost per

Total Project
Bid Price

Notes to bidding laboratories:
Bid sheets must be accompanied by the following performance information:
1   Method blank analysis results tor each method on which you submit a bid
2   Method detection limit study for each method and each matrix

            APPENDIX C


                         TECHNICAL PROPOSAL REQUEST

The following information shall he provided to the Contracting Office prior to award of this

Technical Approach

The contractor shall describe its overall understanding of the requirements of the Analytical
Requirements Summary (ARS). Its proposal shall discuss its ability to meet technical
requirements as stated in the following sub-factors:

a.      Completed copies of applicable wastewater. drinking water, and non-aqueous matrix
       analytical results.

b.      At least three examples of results of EPA performance evaluation samples.
       intralaboratory samples, or other analyses that demonstrate the laboratory's proficiency
       for analyzing unknown performance evaluation samples (i.e. EPA DMRQA-QA Study
       results, or similar studies).

c.      Resumes of key personnel.

d.      A copy of the laboratory's chain of custody form that will be used as a signature and time
       audit trail for each sample.

Schedule/Reporting Approach

The contractor shall describe its overall understanding of the requirements of the ARS. Its
proposal shall discuss its ability to meet scheduling and reporting requirements as stated in  the
following sub-factors:

a.      A copy of the laboratory's plan for routine and non-routine pick-ups that shows how the
       contractor plans to meet holding times based on travel time, laboratory hours, etc.

b.      A copy of the report format that will be used.

c.      A brief discussion of the procedure that will be established to handle phone reports.

Management Approach

The contractor shall describe its plan for providing direction over the management aspects of the
ARS as stated in the following sub-factors:

a.      A notarized copy of the laboratory's certifications specifying the categories of specific
       tests and parameters w ithin each category for which the laboratory is certified.

h.      A copy of the laboratory's current quality systems documentation which demonstrates
       compliance with ISO/IEC Guide 25: General Requirements for rh<' Competence of
       Calihrcition and Testing Laboratories.

c.      Information regarding the use of. and percentage of use of. subcontractor s) and proof that
       the contractor and any proposed subcontractor!s) have obtained all required
       appointments, licenses,  and permits and comply with all requirements under Quality
       Assurance and Quality Control in the ARS.

d.      Describe your plan for staying abreast of all rules/standards for performance (e.g..
       maintains copies of the  Federal Register}.


OFFEROR                        EVALUATOR	
                                  B - SUSCEPTIBLE TO BE MADE ACCEPTABLE
                                      (if proposal is revised)
                                  C - SUSCEPTIBLE TO BE MADE ACCEPTABLE
                                      (if specification is revised)
                                  D - UNACCEPTABLE

a Applicable wustewater, drinking water, and non-aqueous matrices have been analy/ed and information on
analytical detection limits and holding times are in accordance with the ARS.
                                                                       A   B   C   D
                                                                       D   D   D   D
b. Results of EPA performance evaluation samples, intralaboratory samples, or other analyses have been provided
and demonstrate the laboratory's proficiency in analy/mg samples of the type required under this contract

                                                                       A  B   C   D
                                                                       D  D   D   D
c. Resumes of key personnel have been provided.
                                                                       A   B   C   D
                                                                       D  D   D   D

d A copy ol the laboratory's chum ol custody lonn thai will be used as a signature and time audit trail lor each
sample has been provided
                                                                                  A   B    C   I)
                                                                                 D   D   D   D
a. A cop> ol the laboratory's plan tor routine and non-routine pickups has been provideJ and adequately shows how
contractor plans to meet holding times based on travel time, laboratory hours, etc.
                                                                                  A   B    C   D
                                                                                 D   D   D   D
b A copy ol the report tormat has been provided and contains all required information
                                                                                  A   B    C   D
                                                                                 D   D   D   D
c The laboratorv has established an adequate procedure to handle phone reports
                                                                                  A   B    C   D
                                                                                 D   D   D   D

a The contractor has submitted a notan/ed copy ot the laboratory's certifications specifying the categories ot
specific tests and parameters within each category tor which the laboratory is certified. The laboratory is properly
certified tor the work under this contract.
                                                                                     A   BCD
                                                                                     D   D   D  D
h. A copy of the laboratory's current quality systems documentation has been received and demonstrates compliance
with ISO/lUC Guide 25: General Requirements for the Competence of Calihration and Testing Ui bo intone*

                                                                                    A  B    C    D
                                                                                    D   D   D   D
c. The laboratory has provided a statement regarding the use of. and percentage of use of. subcontractor!s) and
proof that the contractor and any proposed subcontractor!s) have obtained all required appointments, licenses, and
permits and comply with all requirements under Quality Assurance/Quality C'ontrol in the ARS

                                                                                    A    BCD
                                                                                    D   D   D  D
d. The laboratory has an adequate plan for staying abreast of all rules/standards for performance

                                                                                     A   B   C   D
                                                                                     n   n   n  n

                APPENDIX D


                        General Laboratory Audit Checklist
Audit dates:
Audit team:
Section 1:    Quality Assurance Management Systems

1.      Is there a quality assurance program plan (or equivalent) for the contract under which
       this work is being performed?
2.     Are the staff familiar with the plan?
Strengths and weaknesses:

Section 2:    Project Management Systems

1.      Does a QAPP (or equivalent) exist for the project or work assignment?

2.      Are the staff familiar with the plan?

3.      Are all the specific elements in the QAPP included in the laboratory's QA plan?

4.      Has the QAPP (or equivalent) been approved?

5.      Have the requirements set forth in the QA plan been met?

6.      Are deliverables on time?

7.      Is sufficient coordination occurring between the laboratory and client project managers?

8.      Are project files available?

9.      Are software packages used by the laboratory for data reduction adequately described
       in project files?

Strengths and weaknesses:

Section 3:    Laboratory Management Systems

1.      Has sufficient laboratory space been allocated?

2.      Have contamination-free areas been provided for trace-level work?

3.      Are reagent-grade or higher purity chemicals used to prepare standards?

4.      Is the following information documented for all reagents/standards used?

       a.     Manufacturer

       b.     Date of receipt

       c.     Date opened

       d.     Purity

       e.     Lot number

5.      Are notebooks being kept in accordance with good laboratory practice? Are laboratory
       notebooks controlled?

6.      Have standard operating procedures (SOPs) been written where appropriate?

7.      Do staff have copies of current SOPs? Are SOPs controlled documents?

8.      Are staff performing operations according  to SOPs?

9.      Does documentation exist for standards preparation  that uniquely identifies the
       reagents/solvents used and the method of preparation?

10.    Does documentation exist for identification of standard preparer and date of standard

11.    Are calibration standards validated prior to use?

12.    Are standards replaced at the proper intervals?

13.    Are samples subject to a chain-of-custody system?

       a.     Are they uniquely identified?

       b.     Is their storage documented and inventoried?

14.    Are manufacturers' maintenance  manuals  available?

15.    Are maintenance logs kept for lab equipment/instrumentation?

16.    Is service on equipment instrumentation readily available?

17.    Are replacement parts for equipment/instrumentation available?


18.    Is the analytical balance located in an area free of drafts and rapid temperature

19.    Do balances have calibration stickers showing date of last certified calibration and date
       of next scheduled calibration?

20.    Are records available for in-house calibration/checking balances?

21.    Do micropipettes have logs indicating calibration checks performed in-house?

22.    Do records exist for monitoring of laboratory water systems?

23.    Is everyone aware of disposal plan? Is it adhered to?

24.    Are glassware cleaning procedures adequate?

25.    Are temperature logs available for freezers?

26.    Are certified material  standards used for all parameters such as material is available

Strengths and weaknesses:

Section 4:    Data Management Systems

1.     Are entries to logbooks signed, dated and legible?

2.     Are changes to logbooks dated and initialed by the person who made them?

3.     Can data be tracked from the project files?

4.     Do the project files identify the specific pieces of instrumentation that were used?

5.     Have lab data management systems been validated prior to use?

6.     Are data manipulation procedures adequately described?

7.     Are data (electronic and hardcopy) archived in a retrievable fashion?

8.     Is there a projection/run tracking/filing system in place?

9.     Is it possible to back-track and validate a final piece of data from it's beginning?

10.    Are data periodically confirmed by independent (i.e. manual) reduction?

11.    Are there written instructions for data receipt, storage, retrieval?

12.    Are documents issued by the work assignment subject to a document control system?

13.    Are data entered into the computer "checked at least three times by at least two people?

14.    Are lab notebooks inspected by the group leader?

15.    Is the inspection documented?

Strengths and weaknesses:

Section 5:    Problem Resolution

1.      Has a person been designated to follow-up on previously identified problems?

2.      Has a time frame been stipulated for resolving problems?

3.      Does documentation of the resolution of problems exist?

Strengths and weaknesses:

           APPENDIX E


                                      Data Inspection Checklist
                                        Summary Information
1  Name of Reviewer:
                Required Samples
                                Sample Results Provided
   Sample Location or
       Sample ID
Sample Location or
    Sample ID
2.  Method Used:

3.  Total No. of analytical shifts per instrument (determined from analysis run log):
                  No. of Shifts
4.  Total No. of CCVs Required.
(one for each  10 samples after the
first 10 samples on each instrument)

5.  Total No of CCBs Required:
(one for each  CCV)

6.  Total No. of Field Blanks Required.
(one per site or per 10 samples, whichever
is more frequent)

7.  Total no. of Lab Blanks Required.
(one per batch' per method/instrument)

8.  Total no. of OPR analyses Required:
(one per batch per method/instrument)

9.  Total no. of MS/MSD samples Required:
(one per 10%  per matrix per site)

10. Total no. Field Duplicates Required:
(one per 10 samples per site)

11. Total no. of MDL results required:
(one per method and per analyte)
                  Total No. of CCVs Reported:

                  Total No. of CCBs Reported:

                  Total No. of Field Blanks Reported:

                  Total No. of Lab Blanks Reported:

                  Total No. of OPR Analyses Reported:

                  Total No. of MS/MSD samples Reported:

                  Total No. of Field Duplicates Reported:

                  Total No. of MDL Results Reported:

12                                           Initial Calibration

a       Was a multiple point initial calibration performed ?                            Zyes   —no

b       Were all sample concentrations reported within the calibration range?           "yes   —no

        If no. list method and analytes tor which initial calibration was not performed or which exceeded the
        calibration range.

c       Analvte          No ICAL (Y/ISQ   Exceeded ICAL Range (V/N)
d       Did the initial calibration meet linearity criteria?                               Ulyes   "no

e       If no. was a calculation curve used to calculate sample concentrations7         Dyes   Cino

 A three point (minimum) initial calibration should be performed 'or each analyte. it the RSD ol trie mean RRF is less than 15% or it the RSD ol
the mean RF is less than 25% then the averaged RRF or RF. respectively, may be used (or that anatyie
13                           MethoJ Detection Limit (MDL)/Minimum Level (ML)

a       Did the laboratory demonstrate their ability to achieve the required MDL9        Gyes   Cno

b       Did the initial calibration range encompass the ML9                           Hyes   Gno

c       Were all field samples detected below the ML reported as non-detects?         -yes   "no

d.       If the answer to item a. b. or c above was "no", describe problem:
14                    Initial Calibration Verification (ICV)/lnitial Calibration Blanks (ICB):

a       Was an ICV run prior to field samples''                                       Dyes   3no

b       Were ICV results within the specified windows?                               Dyes   Gno

c       Was the ICV followed by an ICB9                                            3yes   3no

d       Was the ICB free from contamination''                                       Dyes   3no

e       If any item in a - d above was answered "no", list problems below:

        Analvte         Failed ICV Recovery      Concentration Detected ir ICB     Affected Samples

15                                Initial Precision and Recovery (IPR)

a       Were IPR data reported for each analyte?                                  Dyes   Dno

b.       Did all IPR aliquots meet required recovery criteria (x)9                       Dyes   Dno

c.       Did the standard deviation (s) of each IPR series meet the required criterion''    Dyes   Dno

d.       If any item in a - c above was answered "no", document problem below.

        Analvte    Ave. Result Reported (X)       RSD Reported   Affected Samples
16                              Ongoing Precision and Recovery (OPR)

a.       Were OPR data reported for each analyte, instrument, and batch1'             Dyes   Dno

b       Did all OPR samples meet required recovery criteria (x)?                     Dyes   Dno

c.       If item a or b above was answered "no", document problem below.

        Analvte   OPR Recovery (X) Reported     Shifts Missing QPR       Affected Samples
17.              Continuing Calibration Verification (CCV)/Contmuing Calibration Blank (CCB)

a.      Were CCVs run prior to each batch of 10 samples on each instrument9        Dyes   Dno

b      Were all CCV results within the specified windows?                         Dyes   Dno

c      Was each CCV followed by a CCB7                                      Dyes   Dno

d.      Was each CCB free from contamination?                                  Dyes   Dno

e.      If any item in a - d above was answered "no", list problems below:

       Analvte   Affected Samples      Shift Missing CCV/CCB     Failed CCV/CCB ID

18                                   Laboratory (Method) Blanks

a       Was a method blank analyzed for each instrument & sample batch"?            Dyes   Dno

b       Was each method blank demonstrated to be tree from contamination?          Dyes   Dno

c       If the answer to item a or b was "no", document problems below.

        Analvte    Aflected Samples      Blank Concentration Reported   Shift Missing MB
19                                          Field Blanks

a       Was a field blank analyzed for each 10 samples per site?                     Dyes   Dno

b       Was each field blank demonstrated to be free from contamination?            Dyes   Dno

c       If the answer to item a or b was "no", document problems below.

        Analvte    Affected Samples      Blank Concentration Reported   Shif: Missing FB
20                                        MS/MSD Results

a       Were appropriate number of MS/MSD pairs analyzed9                       Dyes   Dno

b       Were all MS/MSD recoveries within specified windows9                      Dyes   Dno

c       Were all RPDs within the specified window7                                Dyes   Dno

d       Was appropriate corrective  action (e.g.. MSA for GFAA. serial dilution
        for ICP) employed on affected samples9                                   Dyes   Dno

e       If the answer was "no" to items a - d above, document affected samples:

        Analvte   MS % R      MSP % R       MS/MSD RPD    Affected Samples
21                                     Additional Information

a       Were Instrument Tune Data Provided9                                    Dyes   Dno

b       Were equipment blanks demonstrated to be free from contamination9          Dyes   Dno

c       Were statements of data quality provided9                                 Dyes   Dno

d.       Did field duplicate demonstrate acceptable precision9                        Dyes   Dno