United States
                  Environmental Protection
                  Agency
Office of
Solid Waste and
Emergency Response
OSWER Document 9200.5-170-FS
EPA Publication 540-FS-07-004
January 2007
                   Multi-Media, Multi-Concentration,
                   Inorganic Analytical Service  for
                   Superfund  (ILM05.4)
     Office of Superfund Remediation & Technology Innovation
     Analytical Services Branch (5203P)
                                Quick Reference Fact Sheet
Under the legislative authority  granted to the U.S. Environmental Protection Agency  (EPA) under the Comprehensive
Environmental Response, Compensation, and Liability Act of 1980 (CERCLA) and  the Superfund Amendments and
Reauthorization Act of 1986 (SARA),  EPA  develops standardized analytical methods for the measurement of various
pollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are of
concern to EPA at such sites is a series of inorganic analytes and cyanide that are analyzed using Inductively Coupled
Plasma-Atomic Emission Spectroscopy (ICP-AES), Inductively Coupled Plasma-Mass  Spectrometry (ICP-MS), Cold
Vapor Atomic Absorption (CVAA), and colorimetric techniques. The Analytical Services Branch (ASB) of the Office of
Superfund Remediation  and Technology Innovation (OSRTI) offers an analytical  service that provides data from the
analysis of water/aqueous and soil/sediment samples for inorganic analytes for use  in the Superfund and other decision
making processes. Through a series of standardized procedures and a strict chain-of-custody,  the inorganic analytical
service produces  data of known and documented quality.  This  service is available  through the Superfund  Contract
Laboratory Program (CLP).
DESCRIPTION OF SERVICES

The inorganic analytical service provides a technical and
contractual   framework   for  laboratories  to  utilize
EPA/CLP analytical methods. These methods are used in
the isolation, detection and quantitative measurement of
23 target analyte metals (including mercury) and cyanide
in both water and soil/sediment environmental samples.
The  CLP provides the  methods to  be used and  the
specific   technical,   reporting,    and   contractual
requirements, including Quality Assurance (QA), Quality
Control  (QC), and  Standard  Operating  Procedures
(SOPs), by which EPA evaluates the data.

Three data  delivery  turnaround times are  available  to
CLP customers: 7,  14,  and  21-day turnaround after
receipt of  the last sample  in  the set.  A 72-hour
preliminary  data submission option also is available for
all turnaround  times. The data associated with these
Preliminary  Results is due within 72  hours after  receipt
of each sample at the laboratory. In addition, data users
may  include, but are not limited to, additional analytes
and modified quantitation limits.

The ILM05.4 analytical service is based on the previous
ILM05.3  analytical  service.  The  update  to  ILM05.4
includes a change to the  Contract Required Quantitation
Limits  (CRQL) for  the  Inductively  Coupled Plasma-
Mass Spectrometry  (ICP-MS) analysis for vanadium in
water matrices from 1 y.g/L to 5 jig/L.
           DATA USES

           This analytical service provides data that EPA uses for a
           variety of purposes.  Examples include determining the
           nature and extent of contamination at a hazardous waste
           site, assessing priorities for response based on risks  to
           human  health  and  the   environment,  determining
           appropriate  cleanup actions,  and  determining when
           remedial actions are complete. The data may be used  in
           all stages in the investigation of a hazardous waste site
           including:  site  inspections,  Hazard  Ranking  System
           scoring,   remedial   investigations/feasibility   studies,
           remedial design, treatability studies, and removal actions.
           In addition, this service provides data that are available
           for use in Superfund enforcement/litigation activities.

           TARGET ANALYTES

           The inorganic analytes and quantitation limits for which
           this service is  applicable are listed in Table 1.  Specific
           detection limits are method and matrix dependent.

           The list of target analytes for this service was originally
           derived from the EPA Priority  Pollutant  List of 129
           compounds. In the years since the inception of the CLP,
           analytes have been added to and deleted from the Target
           Analyte  List (TAL), based on advances in analytical
           methods, evaluation of method performance  data, and the
           needs of the Superfund program.

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           Table 1. Inorganic Target Analyte List and Contract Required Quantitation Limits (CRQLs)


1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
Analvte

Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide
ICP-AES CROL
for Water (ug/L)
200
60
10
200
5
5
5000
10
50
25
100
10
5000
15
0.2
40
5000
35
10
5000
25
50
60
10
ICP-AES CROL
for Soil (mg/kg)
20
6
1
20
0.5
0.5
500
1
5
2.5
10
1
500
1.5
0.1
4
500
3.5
1
500
2.5
5
6
2.5
ICP-MS CROL
for Water (ug/L)
—
2
1
10
1
1

2
1
2

1
--
1

1

5
1

1
5
2
--
METHODS AND INSTRUMENTATION

The  Contractor will demonstrate the ability to meet
certain program data quality objectives prior to analyzing
field samples. The laboratories must document methods
used to generate analytical results and determine Method
Detection  Limits   (MDLs).  ICP-Atomic  Emission
Spectroscopy (ICP-AES)  is  used  to  analyze  water,
sediment, sludge, and soil samples.  Water and  soil
samples are treated with acids and heated. The digestates
are then analyzed for trace metals by an atomic emission
optical   spectroscopic  technique.   The   samples  are
nebulized and the  aerosol  is transported to a plasma
torch. The atomic-line emission spectra are dispersed and
a photosensitive device monitors line intensities.

ICP-Mass Spectrometry (ICP-MS) is used to determine
the concentration of  dissolved  and total  recoverable
elements in water/aqueous samples. The sample material
is introduced, by  nebulization,  into  radio frequency
plasma where desolvation,  atomization,  and ionization
take  place.  The ions  are  extracted from  the plasma
through a differentially pumped  vacuum interface  and
separated based on their mass-to-charge ratio.

Cold  Vapor  Atomic Absorption (CVAA)  is used to
analyze water, sediment,  sludge, and  soil samples for
total mercury. Organo-mercury compounds may also be
present and will need to be broken down and converted
to mercuric ions to respond to the  CVAA techniques. For
water samples, organic compounds are oxidized and then
reacted with a strong reducing agent.  The volatile free
mercury  is  then driven from  the reaction  flask by
bubbling air through the solution. The  air stream carries
the mercury atoms to an absorption cell, which is then
placed in the light path of the AA spectrophotometer. For
soil/sediment,     the     samples     undergo    acid
digestion/oxidation   followed   by   reduction   and
measurement by conventional cold vapor technique.

Various water types, sediment, sludge, and soil samples
are also  analyzed for total cyanide. Hydrocyanic acid
(HCN)  is  released  through a  reflux-distillation  and
absorbed in a scrubber  containing sodium hydroxide
solution.  The cyanide  ion is determined colorimetrically
by converting it to cyanogen chloride (CNC1).

Table 2  summarizes the methods and  instruments used
in this analytical service.

DATA DELIVERABLES

Data  deliverables  for  this  service   include  both
hardcopy/electronic  data reporting forms  and supporting
raw data. The laboratory must submit data to EPA within
7-, 14- or 21-days, or preliminary data must be submitted
within 72 hours after laboratory receipt  of each sample in
the set, if requested.  EPA then processes the data through
an automated Data  Assessment Tool (DAT). DAT is a
complete   CLP   data   assessment   package.   DAT
incorporates Contract Compliance Screening (CCS) and
Computer-Aided Data Review and Evaluation (CADRE)

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Table 2. Methods and Instruments
Analyte
Al, Sb, As, Ba, Be, Cd, Ca, Cr, Co, Cu, Fe,
Pb, Mg, Mn, Ni, K, Se, Ag, Na, Tl, V, Zn
Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn, Ni,
Se, Ag, Tl, V, Zn
Mercury (Hg)
Cyanide (CN)
Instrument
Inductively Coupled Plasma - Atomic
Emission Spectroscopy (ICP-AES)
ICP - Mass Spectrometry (ICP-MS)
Cold Vapor Atomic Absorption (C VAA)
Colorimeter or Spectrophotometer
Method
ICP analysis of atomic-line emission
spectra.
ICP analysis of ions separated on basis of
mass-to-charge ratio.
Acid digestion/oxidation followed by
reduction and CVAA analysis.
Distillation followed by colorimetric
analysis.
    Table 3. Quality Control
QC Operation
Instrument Calibration
Initial Calibration Verification
Initial Calibration Blank
Continuing Calibration Verification
Continuing Calibration Blank
CRQL Check Standard (CRI)
Interference Check Sample
Serial Dilution for ICP
Preparation Blank
Laboratory Control Sample
Spike Sample
Post Digestion/Distillation Spike
Duplicate Sample Analysis
ICP-MS Tune
Method Detection Limit Determination
Interelement Corrections
Linear Range Analysis
Frequency
Daily or each time instrument is set up.
Following each instrument calibration for each wavelength or mass used.
Following each instrument calibration, immediately after the Initial Calibration
Verification (ICV).
For each wavelength or mass used, at a frequency of 10% or every two hours of a run,
whichever is more frequent, and at the beginning and end of each run.
10% or every two hours of a run, whichever is more frequent, and at the beginning and
end of each run. Performed immediately after the last Continuing Calibration
Verification (CCV).
Every 20 analytical samples and at the beginning and end of each run, but not before
the ICV. Performed before the Interference Check Sample.
For ICP-AES, every 20 analytical samples and at the beginning and end of each run,
immediately after the CRI. For ICP-MS, at the beginning of the run.
For each matrix type or for each SDG, whichever is more frequent.
For each SDG or each sample preparation and analysis procedure per batch of
prepared samples.
For each SDG or each sample preparation and analysis procedure per batch of
prepared samples, except aqueous mercury and cyanide.
For each matrix type or for each SDG, whichever is more frequent.
Each time Spike Sample Recovery is outside QC limits.
For each matrix type or for each SDG, whichever is more frequent.
Prior to calibration.
Prior to contract, annually thereafter, and after major instrument maintenance.
Prior to contract, quarterly thereafter, and after major instrument adjustment.
Prior to contract, and quarterly thereafter.

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review to provide EPA Regions with electronic  reports
(PC-compatible  reports, spreadsheets,  and  electronic
files) within 24 to 48 hours from the receipt of the data
This automated tool facilitates the transfer of analytical
data into Regional databases. DAT  can also be used to
assist in the  data validation process at the  Region. In
addition to  the  Regional electronic reports,  the  CLP
laboratories are provided with a data assessment report
that  documents  the instances of noncompliance.  The
laboratory has four  business days to reconcile  defective
data and resubmit the data to EPA. EPA then reviews the
data for noncompliance and sends a final data assessment
report to the CLP laboratory and the Region.

QUALITY ASSURANCE

The  Quality  Assurance  (QA)  process  consists  of
management  review  and  oversight  at the  planning,
implementation,   and   completion  stages  of   the
environmental data  collection  activity and ensures that
the data provided are of the quality required. During the
data collection  effort,  QA activities  ensure  that  the
Quality Control  (QC) system  is functioning effectively
and that the deficiencies uncovered by the QC system are
corrected. After environmental data are collected,  QA
activities focus on assessing the quality of data obtained
to determine its suitability to  support  enforcement or
remedial  decisions.  Each  contract  laboratory  will
establish a  Quality Assurance  Plan (QAP)  with  the
objective  of providing  sound analytical   chemical
measurements.  The QAP  must specify  the  policies,
organization,   objectives,  functional  guidelines,   and
specific QA/QC activities designed  to  achieve the data
quality   requirements   for   this   analytical   service.
QUALITY CONTROL

The QC process includes those activities required during
analytical data collection to produce data of known and
documented quality.

The  analytical  data acquired from QC procedures are
used to estimate and evaluate the analytical results and to
determine the necessity for, or the effect  of,  corrective
action procedures. The QC procedures required for this
analytical service are shown in Table 3.

PERFORMANCE MONITORING ACTIVITIES

Laboratory   performance  monitoring  activities   are
provided primarily by  ASB and the Regions to ensure
that  contract laboratories  are  producing  data of the
appropriate quality. EPA performs  on-site  laboratory
audits, data  package  audits, and  evaluates  laboratory
performance with blind performance evaluation samples.

For more information, or for suggestions to improve this
analytical service, please contact:

    JohnD. Nebelsick
    Inorganic Program Manager
    USEPA/ASB
    Ariel Rios Building (5203P)
    1200 Pennsylvania Avenue, NW
    Washington, DC 20460
    Tel: 703-603-8845
    Fax: 703-603-9135

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